AA-6800-6650 IM VerFocr

206-94425F
Shimadzu Atomic Absorption Spectrophotometer AA-6800F (P/N 206-50500-37, -92, -93) AA-6800G (P/N 206-50700-37, -92, -93) AA-6650F (P/N 206-51200-37, -92, -93) AA-6650G (P/N 206-51300-37, -92, -93) INSTRUCTION MANUAL
Read this instruction manual throughly before you use the product. Keep this instruction manual handy so that you can refer to it when necessary.
COPYRIGHT:
Copyright (C) Shimadzu Corporation 2000. All rights reserved. This publication may not be reproduced in whole or in part without written permission from Shimadzu Corporation. Since Shimadzu products are frequently upgraded and improved, information in this publication is subject to change without notice. The contents of this manual have been thoroughly inspected. Even if errors and omissions are found, however, we might not correct them immediately. MS-DOS, Windows, Windows95, Windows98, and Windows NT are trademarks and trade names of Microsoft. Other product names described in this manual are each manufacturer's trademarks or registered trademarks.
Precautions for Safe Operation
The atomic absorption spectrophotometer is used as an analytical equipment for quantitative analysis. To operate this equipment safely, strictly observe the following precautions. If not observed, the safety may be compromised. Do not use the equipment for any purpose other than the above-mentioned types of analysis. Follow the procedures described in the instruction manual. Observe all warnings and cautions. Do not disassemble or modify the equipment without the express approval of an authorized Shimadzu Representative. For internal repair of the equipment, contact your Shimadzu Representative. The meshed descriptions about installation in this instruction manual are intended for Shimadzu service personnel. Don t use them and install the parts by yourself because it is dangerous.
In this manual, the meaning of caution signs are provided as follows. WARNING indicates a potentially hazardous situation which, if not avoided, could result in death, serious injury or moderate injury. CAUTION indicates a potentially hazardous situation which, if not avoided, could result in minor injury, or may result in machine damage. NOTE is used to increase the work efficiency or to help comprehension of the description.
Precautions on the Installation Site and Handling
In the case of atomic absorption spectrophotometer, high pressure gas is generally used. Therefore, it is necessary to take the utmost care for the installation site and handling. Please observe strictly to each precaution described in this manual as well as the precautions listed below.
Ventilation
The inflammable gases used for the atomic absorption spectrophotometer are liable to cause a ignition. Be sure to ventilate the room.
Using fire
When measuring flammable samples, special care must be taken to handling fire. A fire extinguisher should be placed in case of accident.
Exhaust duct
Be sure to prepare a ventilation duct above the atomic absorption spectrophotometer so as to exhaust the combustion gas from the burner.
Condensation
Avoid using the equipment in the condition where condensation may occur. The equipment may not work properly.
Power requirements
The allowable voltage range and consumption power of the atomic absorption spectrophotometer and each attachment are shown as below. Be sure to connect them to the power sources which are suitable to these. AA-6800/6650 main unit Voltage Power capacity Connections fuse used GFA-6500 Voltage Power capacity Connections fuse used : AC200, 220, 230, 240V : 6kVA : Grounded M6 terminal block : 2A TYPE M (CONTROL), 1A TYPE M (PHASE) Allowable voltage range : 10% Source frequency : 50/60Hz : AC100, 120, 220, 230, 240V : 600VA : Grounded outlet : 6A TYPE M (100-120V), 3A TYPE T (220-240V) : 0.63A TYPE T (D2), 0.25A TYPE T (HCL) Allowable voltage range : 10% Source frequency : 50/60Hz
High temperature burner

When using a nitrous oxide-acetylene flame, be sure to use the high temperature burner.
Standard analytical conditions

The standard analytical conditions may be changed with the surrounding temperature and humidity, replacement of the atomizer chamber and graphite tube, and sample solution characteristics. Before starting the measurement, search the optimum analytical conditions for each element while varying the gas flow rate in the case of flame method and the temperature program in the case of furnace method.
Internal repair and maintenance

Since the ordinary maintenance can be performed without removing the main unit cover, do not remove the unit cover. Also, don t exchange the fuses. If the repair which requires to remove the cover is necessary, ask it for Shimadzu Representative.
Gas supply hoses

Whenever using the equipment, check the gas supply rubber hoses for a crack or deterioration caused by adhesive chemicals. If a crack or deterioration is found, replace it with a new hose.
10Drain tube
The drain tube connected to the chamber is not durable with petroleums (kerosene, naphtha, gasoline, etc). When measuring these samples, ask Shimadzu for information. Every time when using the instrument, check the drain tube and drain tank and confirm there is no liquid leak from the drain tube.
11. When a lightning surge from the power source line is given
When a momentary large voltage change is given to the instrument from the power source during using the instrument, the communication with PC is disconnected because some function is stopped to protect the instrument. In this case, once turn off the power of the main unit then turn on the power again and connect it to the PC again. Then the preparation for restarting the measurement is ready. If the instrument doesn't work properly when powered on, contact your Shimadzu representative.
Precautions on Handling High Pressure Gas
High pressure gas must be handled carefully observing the legal regulation. Not only to the following precautions, refer to regulations and laws regarding to handle the high pressure gas. Cautionary items in this manual should be read carefully.
Installation of gas cylinder

(1) Install the gas cylinders in the airy outdoors where they are not exposed to direct sunlight. (2) Take care that gas cylinders become no hotter than 40, and do not allow any flame within 2 meters of the gas cylinders. (3) Secure gas cylinders so that they cannot drop or fall over. Always keep liquefied gas cylinders (acetylene, nitrous oxide, etc.) in a vertical position and do not allow them to fall to a horizontal position.
Acetylene gas
(1) When using acetylene gas, please use a pressure reduction valve especially made for use with acetylene gas. Do not allow acetylene to flow through pipes, and do not use equipment made from copper, silver, mercury, or their alloys in order to prevent the formation of metal-acetylides. Decomposition of such compounds could result in adecomposition explosionresulting from a shock. (2) The acetylene gas cylinder contains solvents such as acetone. If the primary pressure reduced below 0.5MPa, it should be replaced with a new cylinder in order to prevent the outflow of solvents.
Oxygen gas
Do not use oxygen gas.
Air
Supply the dry air. If air containing much moisture is used, the moisture may adhere to the inside of the gas controller and prevent normal operation. Dehumidity with a drain separator provided on the way of piping from the air supply source.
After use of gas

After the gas was used, be sure to close the main valve as well as the stop valve.
Pressure gauge
Periodically inspect the pressure gauge to maintain its normal function.
Pressure regulator
(1) Use approved pressure regulators and connectors. For details, contact your Shimadzu Representative. (2) When installing the pressure regulator to the cylinder, be sure to wipe the dust at the outlet of the cylinder. (3) Damaged or cracked screws for installing the pressure regulator may cause gas leakage. Do not install the pressure regulator forcibly, but replace with a new gas cylinder.
Cylinder opening/closing
(1) Before opening the cylinder, be sure to check that the stop valve is closed. Turn the secondary pressure adjusting valve fully to the left, and open the cylinder using a special handle. Even if the main valve is too tight to open, do not hit the handle or main valve with the hammer or spanner. (2) After the main valve is opened, apply soapy water to the connection of the pressure regulator to check if no gas leak is generated. Also check the connection at the main valve. (3) Completely open the main valve of the cylinder for nitrous oxide gas, argon gas and hydrogen gas. If it is not completely opened, flow rate of the gas may fluctuate. (4) When opening the main valve of the cylinder for acetylene gas, rotate it by 1 rotation or 1.5 rotations from the state of complete closing. To prevent outflow of acetone from the inside of the cylinder, do not open the valve exceeding 1.5 rotations from the state of complete closing. On the contrary, if the main valve is not sufficiently opened in case of nitrous oxide-acetylene flame (high temperature flame), flashback may be caused due to insufficient acetylene when the flame is switched from an air-acetylene flame to nitrous oxide-acetylene flame.
Precautions on Handling Hollow Cathode Lamp
Electrodes of some hollow cathode lamps contain harmful metal elements (As, Be, Hg, Se, etc.). Some electrode metals may ignite when touched with air or water (K, Li and Na). Read the precautions attached to the hollow cathode lamp thoroughly and handle the lamp very carefully for safety.
When disposing of the lamp If the hollow cathode lamp should be broken or its life is finished, dispose of the lamp separately from general garbage. When disposing of the hollow cathode lamp supplied from Shimadzu Co., select a method which will not influence the environmental pollution or human body, or ask a special disposal dealer. The material of hollow cathode lamp are as follows. Metals(including electrode element) Quartz glass Plastic
Some electrode contains harmful metal(Hg, As, etc.).
Specifications change The specifications of the hollow cathode lamp are subject to change for improvement without notice. In this case, set the lighting current referring to the precautions attached to the hollow cathode lamp.
Precautions on Handling Deuterium(D2) Lamp
When disposing of the lamp If the deuterium(D2) lamp should be broken or its life is finished, dispose of the lamp separately from general garbage. When disposing of the deuterium(D2) lamp supplied from Shimadzu Co., select a method which will not influence the environmental pollution or human body, or ask a special disposal dealer. The material of deuterium(D2) lamp are as follows. Metals(Tungsten) Quartz glass Ceramic Plastic
Supply Period of Replacement Parts
Replacement parts are supplied by the Shimadzu Parts Center. The supply period of these parts is determined as below. As a general rule, ten (10) years after the discontinuation of the product. Note, however, that the availability of units or parts not manufactured by Shimadzu shall be determined by the relevant manufacturers. If Shimadzu should receive a notice of the discontinuation of the units or parts, the necessary quantity for the above period is immediately calculated and secured. However, such parts may cease to be available within ten years after the discontinuation of the product, depending on the situation of the relevant manufacturers or change of the necessary quantity.
Warning Marking on the Equipment
WARNING RISK OF BURN Do not touch the burner head and atomizer compartment till it has been cooled sufficiently.
Label, WARNING
Figure 1
WARNING HAZARDOUS VOLTAGE Do not touch the electrodes when the power is ON.
Label, WARNING
Figure 2
WARNING HOT SURFACE Risk of burn. Before replacing the lamp, set the power switch off and cool down the lamp.
Label, WARNING
Figure 3
WARNING FLAMMABLE GAS Before ignition, be sure to read the instruction manual.
Label, WARNING
Figure 4
WARNING RISK OF EXPLOSION Do not use oxygen gas.
Label, WARNING
Figure 5
Emergency Action
Take the following measures in case of emergency or when an abnormal condition is found in the atomic absorption spectrophotometer. Inspect the equipment before using it again and contact a service engineer if necessary. Emergency Action 1 . Turn OFF the power switch of the atomic absorption spectrophotometer. 2 . Turn OFF all the power switches of accessories. 3 . Close the main valves of the gas supply pipings for acetylene, air, nitrous oxide, hydrogen and argon. 4 . Close the main valve of the cooling water supply piping. 5 . Shut OFF the power supply. Turn OFF the switchboard when the power cable is fixed to the switchboard with screws. Disconnect the power cable when the power cable is connected with the plug.
Power switch Power cable
Figure 6
Power Switch and Power Cable of Atomic Absorption Spectrophotometer
Power cable
Power switch
Figure 7 Power Switch and Power Cable of GFA-6500
Inspection Procedure in Case of Flashback
Since the AA-6650/6800 is equipped with the several safety systems that prevent a flashback, there is little possibility a flashback occurs. In case a flashback should occur, however, a service engineer from Shimadzu will perform the following inspection procedure. Never ignite the flame before the safety is confirmed as the result of the inspection.
Chamber cover Cover mounting screw
Burner head Gas tube
Quick-connect joint
Burner head fixing port O-rings
O-ring
Ceramic ball Retaining plate Fixing screw
Safety valve
Chamber fixing screw
Mixer O-ring Drain tube
Nebulizer
Figure 8 Burner Unit

(1) Remove the burner head . Note that the burner head is still hot just after the flame is extinguished. (2) Loosen the chamber fixing screws (4 positions) and remove the chamber cover . (3) If the safety valve is released, check that the O-ring of the safety valve is not cracked or deteriorated then push the safety valve into the rear of the chamber unit. Even if the safety valve is not released, push the safety valve and check that it is properly mounted to the chamber. (4) Remove the chamber fixing screw .
Lift up the chamber upward and check that the drain tube is not damaged. Then put the chamber back to the original position and tighten the fixing screw. (5) Loosen the fixing screw on the nebulizer retaining plate and remove the nebulizer . If the ceramic ball has fallen in the chamber, take it out and mount it to the end of the nebulizer. (6) Check that the mixer in the chamber is not damaged. (7) Check that the O-ring in the nebulizer is not cracked or deteriorated then mount the nebulizer back to the chamber. At this time, be careful not to hit the ceramic ball to the chamber inner wall. Also, check that the nebulizer O-ring is not pressed out from the socket. (8) Fix the nebulizer firmly with the retaining plate. (9) Check that the gas tube connected with the chamber is not damaged. (10) Insert the gas tube connected with the quick-connect joint and check that it is not disconnected by pulling it. (11) Mount the chamber cover and fix it firmly with the screws. (12) Check that burner head slot is not clogged. If clogged, clean the burner head. (13) Check that the O-rings of the burner head fixing port are not cracked or deteriorated. Then mount the burner head to the port. (14) When checking the drain sensor, start up the AA unit and WizAArd software beforehand. Remove the drain tank lid and take out the liquid level sensor from the drain tank . Check that an error message appears on the PC screen. Finally put the liquid level sensor back into the drain tank and close the lid.
Drain tank lid
Liquid level sensor Drain tank
Figure 9 Drain Tank
General Precautions
In order to use the atomic absorption spectrophotometer safely, be sure to observe the following cautions. If not observed, the safety of this equipment may be compromised.
WARNING (1) When pressing the ignition button (at igniting), never put your face or hands in the burner compartment (combustion chamber). Do not look into from above the combustion chamber and do not hold your hands over the combustion chamber. When N2O-C2H2 flame is ignited, the flame goes up to the level of approx.40cm from the top of the equipment. Care should be taken. Before igniting a flame, be sure to close the flame shield (combustion chamber door). (2) Do not ignite a flame unless the burner is mounted to the chamber. (3) Do not ignite a flame unless the nebulizer is mounted to the chamber. (4) Do not ignite a flame unless the drain tank is filled with water. (5) Do not ignite a flame when the drain tube is removed from the chamber. (6) Do not remove the nebulizer from the chamber during combustion. (7) Do not remove the drain tube from the chamber during combustion. (8) Do not remove the burner during combustion. (9) Do not touch the burner while it is hot. (10) Do not touch the deuterium lamp while it is hot. (11) Do not touch the end of cleaning wire for nebulizer capillary directly by hand. Wire may stick your finger. (12) Do not touch the flame shield during combustion. It is very hot by the heat of flame and dangerous (13) Do not touch the flame shield and burner directly by your hand for 20 minutes after extinguishment of the flame. It is very hot by the heat of the flame.
CAUTIONS (1) Do not use the flame for other purpose than analysis. (2) Do not hold any substance over the flame. (3) Do not remove the thermal shield plate when using the atomic absorption spectrophotometer in flame method. If the thermal shield plate is removed, heat of flame is introduced to the instrument inside and measurement may be unreliable. (4) Check the setting of gas flow rate before igniting a flame. (5) Do not use the standard burner (10 cm slot burner) when the recognizing key is still left in the hole of the burner select sensor (BURNER SELECT). (6) Do not put any foreign objects in the hole of the burner select sensor. (7) Do not put any foreign objects in the lamp socket.
(8) Do not connect the power cable to the outlet that is not provided with grounding terminals. (9) Do not put your fingers or hands in the hold of lamp turret, igniter and flame monitor.
CONTENTS
Chapter 1 Overview 1.1 1.2 1.3 Overview of AA-6800/6650 1-1 Overview of GFA-65001-2 Specifications 1-3
Chapter 2 Installation 2.1 Parts Inspection 2-1 AA-6800/6650 Standard Parts 2-1 GFA-6500 Standard Parts 2-5 2.1.1 2.1.2 2.2 2.3
Instrument Placement and Site Requirements 2-7 Equipment Requirements 2-9 Power Requirements 2-9 Water Supply Requirements 2-9 Gas Requirements 2-9 Ventilation System 2-11 Use of an Air Compressor 2-12 General Precautions for Handling Gas Cylinders 2-13 Installing Pressure Regulators (Optional) and Checking for Leaks 2-14 Software Operation Minimum Requirements (provided by user) 2-16 Connecting the Drain Tube 2-18 Assembling the Burner2-19 Cable Connections 2-20 Hose Connections2-21 Replacing the AA-6650 Atomizer 2-22 Installation of PC software 2-24 Mounting the Graphite Furnace 2-26 Cable Connections 2-26 Tubing 2-28 Loading the Graphite Tube 2-29 Using a High Density Graphite Tube 2-29 Using a Pyrolytic Coating Graphite Tube 2-30
2.3.1 2.3.2 2.3.3 2.3.4 2.3.5 2.3.6 2.3.7 2.3.8 2.4 2.4.1 2.4.2 2.4.3 2.4.4 2.4.5 2.4.6 2.5 2.5.1 2.5.2 2.5.3 2.5.4
Assembling the AA-6800/6650 2-18
Assembling GFA-6500 2-26
2.5.4.1 2.5.4.2 2.6 2.7
Mounting a Hollow Cathode Lamp2-32 Installing the ACF-6800 2-33
Chapter 3 Instrument Constructions 3.1 AA-6800/6650 Configurations 3-1 Operation Switches3-1 Hollow Cathode Lamp Turret 3-2 3.1.1 3.1.2
3.1.3 3.1.4
Deuterium Lamp3-3 Burner Module 3-4 AA-6800 3-4 AA-6650 3-5
3.1.4.1 3.1.4.2 3.1.5 3.1.6 3.1.7 3.1.8 3.2.1 3.2.2 3.2.3
Burner3-6 Gas Control Panel 3-7 Optical System 3-9 Photometric System 3-10 Graphite Furnace 3-12 Main Unit (Power Supply) 3-14 Operation Principles 3-15
3.2 GFA-6500 Configuration 3-12
Chapter 4 Basic Operation 4.1 Switching On the Power and Starting Up the Software 4-1 4.1.1 4.1.2 4.2.1 Switching ON the Power to Hardware 4-1 Starting Up the Software 4-2 Software Basic Operation (Flame Method) 4-3 Operation Flowchart (Flame Method) 4-3 Wizard Selection 4-4 Element Selection4-4 Preparation Parameters4-6 Sample ID4-9 Sample Selection 4-11 Connect to Instrument/Send Parameters 4-12 Optics Parameters 4-13 Atomizer/Gas Flow Rate Setup (AA-6800) 4-16 Atomizer/Gas Flow Rate Setup (AA-6650) 4-18 Operation flowchart (Furnace method) 4-20 Wizard Selection 4-21 Element Selection 4-21 Preparation Parameters 4-24 Sample ID 4-30 Sample Selection 4-31 Connect to Instrument/Send Parameters 4-32 Optics Parameters 4-33 Furnace Program 4-36
4.2 Software Basic Operation 4-3 4.2.1.1 4.2.1.2 4.2.1.3 4.2.1.4 4.2.1.5 4.2.1.6 4.2.1.7 4.2.1.8 4.2.1.9 4.2.1.10 4.2.2 4.2.2.1 4.2.2.2 4.2.2.3 4.2.2.4 4.2.2.5 4.2.2.6 4.2.2.7 4.2.2.8 4.2.2.9 4.2.3
Software Basic Operation (Furnace Method) 4-20
Saving the Template4-38
4.3 Measurement Procedures 4-39
4.3.1 4.3.2 4.4 4.4.1 4.4.2 4.4.3 4.5 4.6
Measurement Operation (for Flame Method) 4-39 Measurement Operation (for Furnace Method) 4-41 Saving the Data 4-43 Printing the Data 4-43 Deleting the Data 4-43
Saving/Printing/Deleting the Data 4-43
Completing the Measurement 4-44 Explanation of Main Window 4-45 Menu bar 4-46 Standard tool bar 4-46 Measurement element tool bar 4-47 Absorbance digital display 4-47 Real time graph (and furnace program graph) 4-47 Peak Profile (Latest four measurements and overlay display) 4-49 Calibration Curve Display 4-51 MRT work sheet 4-53 Function buttons 4-54 Status bar 4-55 Fields of MRT work sheet 4-56 Right Mouse Button Menu 4-61 Right Mouse Button on Summary Table 4-64 Inserting and Deleting the Measurement Row 4-64 Active Cell Movement by Shortcut Key and Cell Selection 4-64 Moving an Active Cell 4-64 Selecting Cells 4-65 Copy 4-65 Paste 4-65
4.6.1 4.6.2 4.6.3 4.6.4 4.6.5 4.6.6 4.6.7 4.6.8 4.6.9 4.6.10 4.7 4.7.1 4.7.2 4.7.3 4.7.4 4.7.5
Operating the MRT work sheet 4-56
4.7.5.1 4.7.5.2 4.7.6 4.7.6.1 4.7.6.2 4.7.7 4.8 4.8.1 4.8.2 4.8.3 4.8.4 4.8.5 4.9 4.9.1 4.9.2 4.10
Copy and Paste 4-65
Changing Column Width and Column Header Height of MRT Worksheet 4-66 Operation Locations 4-67 Safety Precautions Prior to Ignition 4-67 Igniting and Extinguishing Air-C2H2, Air(Ar)-H2 flames4-68 Igniting and Extinguishing N2O-C2H2 flame 4-70 Flame Conditions When Analizing Organic Solvent Samples 4-73 Setting theEdit Preparation ParametrsDialog Box 4-75 Measurement Procedures on MRT work sheet 4-77
Igniting and Extinguishing the Flame 4-67
Standard Addition Method and Simple Standard Addition Method 4-74
Conditions and Operation for Flame Emission Analysis 4-79
4.10.1 Optics ParametersPage 4-79
4.10.2 Atomizer/Gas Flow Rate SetupPage 4-81 4.10.2.1 AA-6800 4-81 4.10.2.2 AA-6650 4-83 4.10.3 4.11 4.11.1 4.11.2 Line Search and Beam Balance 4-85 Setting the Optimum Condition of Burner Height 4-86 Setting the Optimum Condition of Fuel Gas Flow Rate 4-87 Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height (AA-6800) 4-86
Chapter 5 Functions of Operation Menu 5.1 Wizard Selection dialog box 5-1 5.1.1 Wizardpage 5-1 5.1.2 Recent Filespage 5-2 5.1.3 Recent Templatespage 5-2 5.2 [File] 5-3 [New] 5-3 [Open]5-4 [Save] 5-4 [Save As...] 5-4 [Additional Load] 5-5 [File Export...] 5-6 [Export Items]5-6 [Auto Save]5-7 [Print Data/Parameters...] 5-9 [Print Table Data...] 5-10 [Print Style] 5-11 "Print Style Setup" page 5-11 "Table Show/Hide" page 5-11 "Font" page 5-12 5.2.1 5.2.2 5.2.3 5.2.4 5.2.5 5.2.6 5.2.7 5.2.8 5.2.9 5.2.10 5.2.11
5.2.11.1 5.2.11.2 5.2.11.3 5.2.12 5.2.13 5.2.14 5.3.1 5.3.2 5.3.3 5.3.4 5.3.5 5.3.6 5.3.7 5.3.8
[Print Setup] 5-13 Recent Files 5-13 [Exit] 5-13 [Insert Row] 5-14 [Delete Rows] 5-14 [Import Other Schedule] 5-14 [Collective Edit] 5-14 [Remeasure Selected Range] 5-14 [Clear Measurement Result]5-14 [Copy] 5-15 [Paste] 5-15
5.3 [Edit] 5-14
5.4 5.5
[Refer to Parameters] 5-16 [Parameters]5-17 5.5.1.1 Cookbookpage 5-20 5.5.1.2 Templatepage 5-21
5.5.1 Element SelectionPage 5-18
5.5.2 Preparation ParametersPage 5-22 5.5.2.1 5.5.2.2 5.5.2.3 5.5.2.4 5.5.2.5 5.5.2.6 5.5.2.7 Weight Correction Factors 5-24 Preparataion Parameters for Standard 5-24 Preparation Parameters for Unknown 5-25 Preparation Parameters for Periodic Blank 5-25 Mixing Setup and Reagent Setup 5-26 Coating/Boost Cycle (only for furnace method) 5-27 Repeat Measurement Conditions 5-28
5.5.3 Sample IDPage 5-29 5.5.4 Sample SelectionPage 5-31 5.5.5 Connect to Instrument/Send ParametersPage5-31 5.5.6 Optics ParametersPage 5-32 5.5.6.1 5.5.6.3 5.5.7.1 5.5.7.2 5.5.7.3 5.5.7.4 5.5.8.1 5.5.8.2 5.5.9.1 5.5.9.2 5.5.9.3 5.5.9.4 5.5.9.5 5.6 <Lamp Pos. Setup> button 5-35 <Line Search> Button 5-37 Atomizer Position 5-38 <Burner Position Auto> Button 5-40 Fuel Gas Flow Rate 5-41 <Gas Flow Auto> Button 5-42 Atomizer Position 5-43 Fuel Gas Flow Rate 5-44 <Coating/Boost Cycle> Button 5-48 <Test Meas.> Button 5-49 <Cleaning> Button 5-50 <Change Graphite Tube> Button 5-50 <Temp. Search> Button 5-52 5.5.6.2 <Warmup Lamp> Button 5-36 5.5.7 Atomizer/Gas Flow Rate SetupPage (for flame method by AA-6800) 5-38
5.5.8 Atomizer/Gas Flow Rate SetupPage (for flame method by AA-6650) 5-43
5.5.9 Furnace ProgramPage (for furnace method) 5-46
[Edit Parameters] 5-54
5.6.1 Measurement Parameterspage 5-54 5.6.2 Repeat Measurement Conditionspage 5-57 5.6.3 Weight Correction Factorspage 5-59 5.6.4 Y-axis Print Rangepage 5-60 5.6.5 Analystpage 5-60
5.6.6 Commentpage5-60 5.6.7 Sequencepage 5-61 5.6.8 ASC Parameterspage 5-62 5.6.9 QA/QC Setuppage 5-63 5.6.10 Calibration Curve Parameterspage 5-66 5.6.11 Optics Parameterspage 5-67 5.6.12 Atomizer/Gas Flow Rate Setuppage (Flame method) 5-67 5.6.13 Furnace Programpage (Furnace method) 5-67 5.7 [Default Parameters] 5-68 5.7.1 5.7.2 5.7.3 5.7.4 5.8.1 5.8.2 5.8.3 5.8.4 5.8.5 5.8.6 [Flame] 5-68 [Furnace] 5-68 [Graph] 5-68 [Analyst] 5-68 [Connect] 5-70 [Option Connect] 5-72 [Configuration]5-72 [Lamp Position Setup] 5-76 [Lamp History] 5-77 [Maintenance] 5-79 [D2 Lamp Position] 5-79 [Wavelength Adjustment] 5-79 [Burner Origin Position Adjustment] (AA-6800) 5-80 [Furnace Origin Position Adjustment] (AA-6800) 5-81 [Furnace Origin Position Adjustment](AA-6650) 5-82 [ASC Maintenance] 5-83 [Set Syringe Volume] 5-83 [Change Syringe] 5-85
5.8 [Instrument] 5-69
5.8.6.1 5.8.6.2 5.8.6.3 5.8.6.4 5.8.6.6 5.8.6.7
5.8.6.5 [Burner Origin Position Adjustment](AA-6650) 5-82
5.8.6.7.1 5.8.6.7.2 5.8.6.8 5.8.7 5.8.8 5.8.9 5.8.10 5.8.11 5.8.12 5.8.13 5.8.14 5.8.15 5.8.16
[Maintenance only for service engineer] 5-85
[Lamp Status] 5-86 [Change Graphite Tube] 5-88 [Gas Controller Status]5-88 [Gas Leak Check] 5-89 [Remaining Gas Combustion] 5-89 [Execute Line Search] 5-91 [Cleaning] 5-91 [Rinse Nozzle] 5-91 [Flame Nozzle Position]5-91 [Furnace Nozzle Position] 5-92
5.9
[Help] 5-94 [Search for Help on...] 5-94 [About WizAArd...] 5-94
5.9.1 5.9.2
Chapter 6 Maintenance 6.1 Atomizer Positioning Adjustment 6-1 Burner Positioning Adjustment 6-1 AA-6800 6-1 AA-6650 6-2 AA-6800 6-3 AA-6650 6-3 6.1.1.1 6.1.1.2 6.1.2 6.1.2.1 6.1.2.2 6.2 6.2.1 6.2.2 6.1.1
Furnace Position Adjustment 6-3
Burner Maintenance 6-4 Cleaning the Burner Head 6-4 Nebulizer Maintenance 6-5 Cleaning the Nebulizer6-5 Replacing the Polyethylene Tube6-6
6.2.2.1 6.2.2.2 6.2.3 6.3 6.4
Cleaning the Chamber 6-7
Checking for Gas Leaks in Tubing 6-8 Replacing the Deuterium Lamp 6-9 Specifications of Deuterium Lamp6-9 Replacing Procedures of Deuterium Lamp 6-9 High Density Graphite Tube 6-11 Pyrolytic Coating Graphite Tube 6-11 Replacing Procedure Using the ASC 6-11
6.4.1 6.4.2 6.5 6.5.1 6.5.2 6.5.3 6.6 6.7 6.8 6.9 6.10 6.11
Replacing Graphite Tube (GFA-6500) 6-11
Cleaning Graphite Cap, Holder, Window Plate Sockets and Window Plates (GFA-6500) 6-13 Cleaning the Temperature Sensor (GFA-6500) 6-16 Cleaning the Slide Mechanism (GFA-6500) 6-17 Cleaning the Seal (GFA-6500) 6-18 GFA Performance Check (GFA-6500) 6-19 Maintenance Parts 6-21 AA-6800/6650 Maintenance Parts 6-21 GFA-6500 Maintenance Parts 6-22 For Flame Analysis 6-23 For Furnace Analysis (for GFA-6500) 6-23 For Furnace Analysis (for GFA-EX7) 6-23 Autosampler 6-23 Hollow Cathod Lamps (Single Element Lamps) 6-24
6.11.1 6.11.2 6.12 6.12.1 6.12.2 6.12.3 6.12.4 6.12.5
Special Accessories 6-23
6.12.6 6.12.7 6.12.8
Hollow Cathode Lamps (Single Element Lamps, Usable for SR method) 6-26 Hollow Cathod Lamp (Multi-element Lamps) 6-27 Other Accessories 6-27
Chapter 7 Appendix 7.1 Measurement Conditions Table for Flame Atomic Absorption Analysis7-1 7.2 Analysis Line Wavelength Table for Flame Emission Analysis 7-4 7.3 Graphite Tube Type Selection in Furnace Method 7-5 7.3.1 7.3.2 7.3.3 7.4 When Using a High Density Graphite Tube 7-5 When Using a Pyrolitic Coating Graphite Tube 7-6 When Using the Platform Type Tube7-6
Error Messages 7-9
1.3 Specifications
1
Overview
1-4
AA-6650F6650G Common Specifications

Measurement Wavelength Range Mounitng Bandwidth Number of Lamp Sockets Photometric Method Lamp Mode Software Environment Parameter Setting Measurement Mode Concentration Conversion Mode Repeat Measurement Data Processing Burner Unit Gas Controller 190900nm Aberration-corrected Czerny-Turner mount 0.1, 0.2, 0.5, 1.0, 2.0, 5.0 nm (6-step automatic switching) 8 lamp sockets, 2 lamps simultanously lit (1 for warming up) High-speed self reversal method (BGC-SR) High-speed 2-frequency simultanous measurement(BGC-D2) EMISSION, NON-BGC, BGC-SR, BGC-D2, D2 WindowsTM95, WindowsTM98, WindowsTMNT4.0 Wizard Method Flame continuous method, Furnace method Calibration Curve (selectable among 1st, 2nd, 3rd order function) Standard addition method/Simple standard addition method (1st order function) Max. 20 repetitions Indication of Average, Standard deviation (SD) and Relative Standard Deviation (RSD) Exclusion of deviant value based on SD value and RSD value Automatic baseline drift correction using electrical double beam signal processing (Furnace) Automatic calibration curve correction system by sensitivity observation Actual concentration calculation using Weight factor, Dilution factor, Volume factor and Correction factor. Word processor software or the like can be used while executing measurement. Template function MRT Work Sheet (MRT: Measurement Result Table) Summary Report Correlation factor, LCS, SPK, Sample upper limt, %RSD AC100, 120, 220, 230, 240V switching incorporated, 600VA, 50/60Hz Additional power for personal computer is necessary. W1080 D550 H460mm, 100kg (including gas controller, not including PC) 1035 45%80% (less than 70% if temperature is over 30) Spectro photometer Lamp
Baseline Correction Sensitivity Correction Table Data Processing Functions
Multitask Loading Parameters Procedure/Result Display Result Print QA/QC Power Requirements Dimensions, Weight Ambient Temperature Range Ambient Humidity Range
AA-6650F Specifications
Type Burner Head Nebulizer Chamber Positioning Flow Rate/Pressure Control Safety Measures Air-cooled pre-mix type Pure Titanium Pt-Ir capillary with Teflon orifice, Impact bead is inseparable. Fluoric acid is usable. Polypropylene Manual positioning by adjusting knob Automatic flow rate setting Automatic gas leak check Air-C2H2 flame priority ignition Air/N2O auto switching with C2H2 flow rate monitor (optical sensor) Prevents raw gas discharge Prevents usage of wrong burner head Pressure monitor to prevent flashback at abnormal pressure Safety extinction by automatic detection of momentary power failure Drain tank water level monitor to prevent flashback
AA-6650G Specifications
Heating Temperature Range Heating Control Method Heating Parameter settings Ambient3000 Drying: Current control method Ashing/Atomizing: Optical temperature control method Max. 20 stages Heating mode: RAMP/STEP Inner gas type: 2-line switching High sensitivity setting Furnace concentration boost cycle: Max 20 times Inner gas flow rate: 01.5 L/min Optimum furnace program search function
AA-6800/6650
1.3
Specifications
AA-6800F6800G Common Specifications

Measurement Wavelength Range Mounitng Bandwidth Number of Lamp Sockets Photometric Method Lamp Mode Software Environment Parameter Setting Measurement Mode Concentration Conversion Mode Repeat Measurement Data Processing Burner Unit Gas Controller 190900nm Aberration-corrected Czerny-Turner mount 0.1, 0.2, 0.5, 1.0, 2.0, 5.0 nm (6-step automatic switching) 8 lamp sockets, 2 lamps simultanously lit (1 for warming up) High-speed self reversal method (BGC-SR) High-speed 2-frequency simultanous measurement(BGC-D2) EMISSION, NON-BGC, BGC-SR, BGC-D2, D2 WindowsTM95, WindowsTM98, WindowsTMNT4.0 Wizard Method Flame continuous method, Furnace method Calibration Curve (selectable among 1st, 2nd, 3rd order function) Standard addition method/Simple standard addition method (1st order function) Max. 20 repetitions Indication of Average, Standard deviation (SD) and Relative Standard Deviation (RSD) Exclusion of deviant value based on SD value and RSD value Automatic baseline drift correction using electrical double beam signal processing (Furnace) Automatic calibration curve correction system by sensitivity observation Actual concentration calculation using Weight factor, Dilution factor, Volume factor and Correction factor. Word processor software or the like can be used while executing measurement. Template function MRT Work Sheet (MRT: Measurement Result Table) Summary Report Correlation factor, LCS, SPK, Sample upper limt, %RSD AC100, 120, 220, 230, 240V switching incorporated, 600VA, 50/60Hz Additional power for personal computer is necessary. W1080 D550 H460mm, 100kg (including gas controller, not including PC) 1035 45%80% (less than 70% if temperature is over 30) Spectro photometer Lamp
1
Overview
Baseline Correction Sensitivity Correction Table Data Processing Functions
Multitask Loading Parameters Procedure/Result Display Result Print QA/QC Power Requirements Dimensions, Weight Ambient Temperature Range Ambient Humidity Range
AA-6800F Specifications
Type Burner Head Nebulizer Chamber Positioning Flow Rate/Pressure Control Safety Measures Air-cooled pre-mix type Pure Titanium Pt-Ir capillary with Teflon orifice, Impact bead is inseparable. Fluoric acid is usable. Polypropylene Burner/Furnace automatic switching by motor drive Automatic searching for optimum burner height Automatic flow rate setting Automatic searching for optimum gas flow rate Automatic gas leak check Air-C2H2 flame priority ignition Air/N2O auto switching with C2H2 flow rate monitor (optical sensor) Prevents raw gas discharge Prevents usage of wrong burner head Pressure monitor to prevent flashback at abnormal pressure Safety extinction by automatic detection of momentary power failure Drain tank water level monitor to prevent flashback
AA-6800G Specifications
Heating Temperature Range Heating Control Method Heating Parameter settings Ambient3000 Drying: Current control method Ashing/Atomizing: Optical temperature control method Max. 20 stages Heating mode: RAMP/STEP Inner gas type: 2-line switching High sensitivity setting Furnace concentration boost cycle: Max 20 times Inner gas flow rate: 01.5 L/min Optimum furnace program search function
1-3 AA-6800/6650
1.2
Overview of GFA-6500
1
Overview
1-2
The GFA-6500 is the graphite furnace atomizer adapted for use with the Atomic Absorption Spectrophotometer. With the graphite furnace connected to the instrument, quantitative analysis of elements may be conducted using the furnace method. Following is a description of GFA-6500 features. (1) With the incorporated high sensitivity optical-thermal sensor and the automatic temperature correction function employing current control regions, simple temperature correction and accurate temperature repeatability are achieved. (2) Temperature control via the optical-thermal sensor is conducted from 400, thus making possible accurate temperature control from ashing to atomization. (3) At sample atomization, use of the high sensitivity mode allows trace analysis of even greater sensitivity and higher precision than previously possible with line of instruments. (4) Precise inner gas current control is possible at each heating stage and automatic switching of the gas type allows composition of flexible temperature programs. These features make the GFA-6500 extremely effective in analyzing a wide variety of sample types. NOTE The GFA-6500 cannot be connected with the AA-6650.
AA-6800/6650
1.1
Overview of AA-6800/6650
The Atomic Absorption Spectrophotometer AA-6800/6650 incorporates two background correction functions, the D2 method (Deuterium Lamp method) and the SR method (Self-Reversal method), enabling selection of the appropriate method for the measurement sample. The AA-6800 allows you to change the measurement mode while automatically switching the atomizer, thus enabling quick and easy switching back and forth between flame measurement and furnace measurement. In addition, wide ranging measurement operations are available, from manual operation to automatic continuous measurement of multi-elements with the use of an autosampler (ASC-6100). This enables selection of the appropriate combination to match the number of elements and samples to be analyzed as well as the skill of the operator. The PC software controlling the AA-6800/6650 operates on the MS-WindowsTM, and using the Wizard for parameter setting enables an operator, even an beginner of atomic absorption spectrophotometer, to make measurement conditions easily.
1
Overview
1-1
AA-6800/6650
1
Overview
Chapter 1
Overview
Contents
1.1 1.2 1.3
Overview of AA-6800/6650 1-1 Overview of GFA-6500 1-2 Specifications 1-3
AA-6800/6650
2
Installation
Chapter 2
Installation
Contents 2.1 Parts Inspection 2-1 AA-6800/6650 Standard Parts 2-1 GFA-6500 Standard Parts 2-5
2.1.1 2.1.2 2.2 2.3
Instrument Placement and Site Requirements 2-7 Equipment Requirements 2-9 Power Requirements 2-9 Water Supply Requirements 2-9 Gas Requirements 2-9 Ventilation System 2-11 Use of an Air Compressor 2-12 General Precautions for Handling Gas Cylinders 2-13 Installing Pressure Regulators (Optional) and Checking for Leaks 2-14 Software Operation Minimum Requirements (provided by user) 2-16 Connecting the Drain Tube 2-18 Assembling the Burner 2-19 Cable Connections 2-20 Hose Connections 2-21 Replacing the AA-6650 Atomizer 2-22 Installation of PC software 2-24 Mounting the Graphite Furnace 2-26
2.3.1 2.3.2 2.3.3 2.3.4 2.3.5 2.3.6 2.3.7 2.3.8 2.4 2.4.1 2.4.2 2.4.3 2.4.4 2.4.5 2.4.6 2.5 2.5.1
Assembling the AA-6800/6650 2-18
Assembling GFA-6500 2-26
AA-6800/6650
2.5.2 2.5.3 2.5.4
Cable Connections 2-26 Tubing 2-28 Loading the Graphite Tube 2-29
2
Installation
2.5.4.1 Using a High Density Graphite Tube 2-29 2.5.4.2 Using a Pyrolytic Coating Graphite Tube 2-30 2.6 Mounting a Hollow Cathode Lamp 2-32 2.7 Installing the ACF-6800 2-33
AA-6800/6650
2.1
Parts Inspection
CAUTION
Since this instrument is installed and adjusted by Shimadzu service engineer, stay and check it together. Read and strictly observe the sections 2.2 and 2.3 to maintain the instrument stability, to obtain the high reliability of analysis result and to use this instrument for a long time.
2
Installation
After unpacking, verify that the following parts are included in your shipment. The standard AA-6800/6650 system configurations are as designated below. System AA-6800F AA-6800G AA-6650F AA-6650G (206-50500) (206-50700) (206-51200) (206-51300) Standard Accessories Standard Accessories for Flame
Check the standard accessories referring to the above table. If any parts are missing or damaged, please contact your Shimadzu Representative.
2.1.1
AA-6800/6650 Standard Parts

Table 2.1 Item No. 1 2 -1 -2 -3 -4 Standard Accessories (AA-6800/6650) Parts Name Spectrophotometer Main Unit Standard Accessories Vinyl Cover Fuse, 313.250 (for HCL) Fuse, 189100 (for D2) AC Cable (for 100V, 120V) or Cord Set (for 220-240V) -5 Fuse, ULCS-61ML-6 (for 100V, 120V) or Fuse 313.003 (for 220-240V) -6 -7 -8 -9 -10 Disk Set, AA-6800E Element Label Sheet, HCL Instruction Manual Drive Unit Cover Cable RS-232C, 9.25 1 1 1 1 1 1 1 1 0 1 072-01664-30 206-50734-91 200-63653 206-94425 206-82031 200-79144-01 2 2 071-60814-05 072-01661-24 Qty 6800 6650 1 1 1 1 2 2 1 1 1 2 2 1 206-64902 072-01664-11 072-01667-12 206-13774 Part No
2-1 AA-6800/6650
2.1 Parts Inspection
NOTE
The hollow cathode lamps, high temperature burner head, pressure regulator and compressor are not included among the standard accessories.
2
Installation
Figure 2.1
Standard Accessories (AA)
NOTE
The instruction manual is not shown in the above figure. In the case of AA-6650 series, the Drive Cover Unit, -9 in the above figure, is not provided.
2-2 AA-6800/6650
Table 2.2 Item No. 1 -1 -2 -3 -4 -5 -6 -7 -8 -9 -10 -11 -12 -13 -14 -15 -16 -17 -18 -19
Standard Accessories (for Flame) Parts Name Standard Accessories for flame Hose Assy (for gas supply; AIR) Hose Assy (for gas supply; C2H2) Cleaning Wire (for cleaning capillary) Tube (Teflon tube for sample suction) Burner Position Adjustment Tool Seal Joint Assy (for gas leak check) Driver, #2 (Phillips+) Sample Stage Grease in cup Wire Band, 16mm (hose band) Polyethylene Tube, No.3 Gas Tube Assy (3 bundled nylon tube) Silicone Rubber Tube, 912 (drain tube) Vinyl Tube, R3603 3/81/16 (drain tube) Drain Assy Screw, SUS P3 BK M36 Wiring Band RF100 Sampling Tube ASSY HEX wrench 3.0 Qty 1 1(5m) 1(5m) 1 5 1 1 1 1 1 2 1(0.3m) 1 1(2.4m) 1(2.4m) 1 2 2 1 1 Part No. 206-64844-91 206-50389-91 206-50389-92 201-79229-01 204-05899-01 202-38757-02 204-27572-02 086-11002 206-63686 206-50442-91 037-61019 200-31328-01 206-65112 016-31350-22 016-31409 206-80771-91 020-46534 072-60315-01 206-50772-91 086-03804
2
Installation
2-3
AA-6800/6650
2
Installation
Figure 2.2 Standard Accessories (for flame) 2-4 AA-6800/6650
2.1.2 GFA-6500 Standard Parts

Table 2.3 Item No. 1 2 3 -1 -2 -3 -4 -5 -6 -7 -8 -9 -10 -11 -12 -13 -14 -15 -16 -17 Standard Accessories (GFA-6500) Parts Name Power Supply Assy Graphite Furnace Assy Standard Accessories, GFA Power Cable Assy Ground Wire (1.5m) Fuse, FGBO 250V 1A Fuse, FGBO 250V 2A Cooling Water Tube Assy (for cooling water inlet) Extension tube Assy (for cooling water outlet) Wrench 13 Wrench 12 Screw M38 (fixing screw) Wire Band, 14mm (hose band) Wire Band, 16mm (hose band) Protective plate Sleeve, SN-6 HEX wrench 1.5 Hose Assy (for AIR(O2)) Hose Assy (for SUPPORT(Ar)) Cable, GFA I/F, in package 1 1 2 2 1 1 2 1 2 2 2 1 2 1 1(5m) 1(5m) 1 Qty 1 1 Part No. 206-80203 206-80207
2
Installation
206-64751 206-16588 202-32982-02 072-01214-07 072-01214-08 206-17281 206-64752 086-03110 086-03108 020-46535 037-61018 037-61019 206-65236 035-68907 086-03818 204-05845-01 204-05845-02 206-50756-91
NOTE
Graphite tubes, micropipet, and argon gas pressure reduction valve are not included in the standard accessories.
2-5 AA-6800/6650
2
Installation
Figure 2.3 Standard Accessories (GFA-6500)
NOTE The Power Supply Assy (#1) and Graphite Furnace Assy (#2) are not shown in the above figure
2-6 AA-6800/6650
2.2
Instrument Placement and Site Requirements
The instrument components are positioned as shown in Figure 2.4. In addition to this, the installation site for personal computer and printer is necessary. (1) The installation site should be : (a) Sufficiently distant from devices that generate strong magnetic and electrical fields and high frequency (b) Sufficiently ventilated (c) Free from vibration (d) Free from excessive dust and moisture and should not be exposed to corrosive gases (e) The luminous intensity of installation site for this instrument should be below 1300Lx in the case of fluorescent lamp, below 800Lx in the case of indirect outdoor daylight, and below 400Lx in the case of heat light source like incandescent lamp. CAUTION The AA-6800/6650 series are equipped with the safety system using an optical sensor. When installing the instrument near a window, make sure that it is not exposed to strong outdoor daylight. Exposure to strong outdoor daylight may interfer with normal operation of the extinguished flame safety system for monitoring flame combustion (Flame Monitor). When using incandescent lamp or other heat light sources near the main unit, select the installation site where the luminous intensity by the light source only is below 400Lx. If not available, don t allow the direct light from the light source to come into the combustion chamber. (f) Ambient temperature range: 10 to 35 Humidity: 45 to 80% (but less than 70% if temperature is over 30) (g) Ground is available. NOTE Absorbance varies 0.005Abs as the temperature changes 1. When measuring many samples which requires long time and may result in temperature change influence, execute AUTO ZERO during the measurement if necessary. In the case of manual flame measurement (not using ASC), you can execute AUTO ZERO at any time by clicking on <AUTO ZERO> button on the left lower of the main window. In the case of automatic flame measurement (using ASC), setAUTO ZEROin [Action] field on the MRT work sheet. AUTO ZERO is executed during the nozzle rinsing. In the case of furnace measurement, setting is not necessary because the instrument automatically execute AUTO ZERO just before measurement. (2) The installation platform (table or counter top) must be capable of supporting the combined weights of AA-6800/6650 GFA-6500 ASC-6100 100kg 44kg 15kg
2
Installation
2-7
AA-6800/6650
2.2 Instrument Placement and Site Requirements
the components listed below and a personal computer system. (3) Since gas and water pipes cables are connected at the back of the AA main unit, there must be a space of about 15 to 20cm from the back of the AA main unit to a wall. (4) There must be a space of about 15 to 20cm between the personal computer and the AA main unit so that the pressure and flow rate adjusting knobs on the left side of the AA main unit can be operated.
2
Installation
2-8
Front view
Duct
About 700
Plane view
(Unit : mm)
Figure 2.4 Instrument Placement
AA-6800/6650
2.3
Equipment Requirements
2.3.1 Power Requirements

The following table gives the power requirements for each of the components (The power requirement for a personal computer system is not shown in the table). Table 2.4 Power Requirements AA-6800/6650 Voltage Allowable voltage range Power capacity Source frequency Connections Grounded outlet 100,120,220,230,240V 600VA 50/60Hz Grounded M6 terminal block GFA-6500 200,220,230,240V 6kVA
2
Installation
Within 10% (Free from sudden voltage change)
When the power voltage of AA-6800/6650 changes 5%, absorbance changes approx.0.005Abs.
2.3.2 Water Supply Requirements

Use of the GFA-6500 requires piped water for cooling the graphite furnace. The following requirements must be satisfied: (1) A water outlet and return water drain must be located within 7m of the instrument. (2) Water pressure of 0.07MPa is necessary. If the water pressure decreases below 0.05MPa, a safety device will activate to stop the operation. The upper limit of water pressure is about 0.1MPa. If the water pressure in your arrangement is too high, prepare the pressure reducing valve (Special Accessory, Regulator ASSY P/N 206-86147-91) additionally. (3) Water consumption under these conditions is approximately 1L/min.
2.3.3 Gas Requirements

(1) Gas Specifications Be sure that gases are supplied for flame analysis according to the specifications given in Table 2.5. Table 2.5 Air Nitrous oxide Argon Acetylene Hydrogen Gas Specifications Supply pressure 0.35MPa 0.35 0.35 0.09 0.09 Max.consumption 24 L/min 15 24 4.9 (Air-C2H2 flame) 9.9 (N2O-C2H2 flame) 30 Purity 99% Purity Free from oil,moisture and dust Purity 98%, moisture 1% Purity 99% Purity 98%
WARNING
Use only gases in Table 2.5 for flame analyses. Do not use oxygen gas.
2-9 AA-6800/6650
2.3 Equipment Requirement
CAUTION
If the gas supply pressure changes during the analysis, resultant changes in flame combustion will adversely affect measurement reproducibility. Ensure that gas pressure does not fluctuate.
2
Installation
2-10 AA-6800/6650
When the GFA-6500 is used, provide gases with the specifications shown in Table 2.6. Table 2.6 GFA-6500 Gas Specifications Supply pressure Max.consumption Argon Oxygen/Air 0.35MPa 0.35MPa 3.0L/min 1.5L/min Purity 99.9% Free from oil, moisture and dust
Oxygen or air is effective in accelerating the ashing of organic samples. Prepare piping if necessary. (2) Placement of gas cylinders For safety, it is recommended that the cylinders be placed outdoors. Select a location for the cylinders which satisfies the following conditions: (a) Not exposed to heat sources such as direct sunlight, furnaces, and heaters: Always keep the cylinders at a temperature below 40 (b) Away from spark sources such as switchboards, ground wires, and high voltage power sources (c) Away from flammable materials such as oil, gasoline, and organic solvents (d) Sufficiently ventilated (e) If outdoors, not exposed to wind and rain (3) Gas piping If the cylinders are placed outdoors, piping must be performed separately within 5m of the instrument. In this case, be sure follow the precautionary measures listed below. (a) Use stainless steel pipes for the piping. Do not use of pipes that contain over 62% copper for acetylene piping. (b) Ensure that the pipe diameters are not too small to supply gas at the pressures indicated in Table 2.5. A pipe diameter of at least 7mm will be sufficient. (c) Place a drain separator in the air piping system at the location indicated in Figure 2.5. If a sufficiently dry air supply source is used, a drain separator is unnecessary. (d) Figure 2.5 displays examples of recommended piping configurations. (e) Provide a hose nipple with an outside diameter of 8.4 to 8.9mm so that the provided gas supply hose (inside diameter 7.9mm) can be connected to the end of the gas piping.
Full Scale 0.2MPa 0.09MPa Full Scale 0.2MPa 0.09MPa
Stop cock Stainless steel Piping(inside Stop dia. 7mm) cock
2
Acetylene gas Hydrogen gas
Installation
Full Scale 0.5MPa 0.35MPa Full Scale 0.5MPa 0.35MPa Full Scale 0.5MPa 0.35MPa Analysis room Out doors Drain separator Air compressor Nitrous oxide gas
Argon gas
Figure 2.5 Recommended Piping Setups for AA-6800/6650 2.3.4 Ventilation System
Place a ventilation duct with a hood above the atomizer. (1) The hood, duct and ventilation fans used should be all be made of metal. Those made of plastic are inappropriate as they are softened by heat. (2) A cooling-fan air capacity of about 600 to 1200 m3/h is appropriate. Too much suction force will cause the flame to flicker as well as create excessive noise. Placement of a damper in the duct system is ideal for setting the optimum air flow.
Damper Fan
About 700
(Unit : mm)
Figure 2.6 Typical Ventilation System 2-11 AA-6800/6650
2.3.5 Use of an Air Compressor

The air compressor described in this section may not be available in all countries. Use of another brand of air compressor is acceptable providing that it supplies air which is free of oil, water and dust at the pressures indicated below. In addition, the air compressor should be equipped with the necessary safety devices and meet the standards required by the local regulations. The following procedure is used for confirming the operation status of the air compressor shown in Figure 2.7. (1) Confirm that the oil level is between the red lines on the oil gauge . (2) Shut the stop cock and drain cocks , , turn the secondary pressure control handle sufficiently counterclockwise, and then connect the compressor to the power source. (3) When the primary pressure reaches 0.5MPa, the motor will stop. Take out the safety valve by hand and confirm that it is working properly. (There will be a loud hissing sound at this time, but there is no danger.) (4) When the primary pressure reaches 0.4MPa, the motor will start. (5) After the primary pressure reaches 0.5MPa again, turn the secondary pressure control handle clockwise and set the secondary pressure to 0.35MPa. The compressor is normally used in this state. (6) Apply soapy water or another leak detector to the connecting parts of the pressure gauges, air transformer, etc. to check for leaks.
2
Installation
2-12
AA-6800/6650
Secondary pressure control handle Primary pressure gauge Safety valve (not visible in photo) Lubrication hole Oil gauge Drain cock
Drain cock Air transformer Air output port Stop cock Secondary pressure gauge
2
Installation
Figure 2.7 Air Compressor (Optional Accessory)

CAUTIONS 1. If the compressor does not work using the above procedure, refer to the instruction manual provided with the compressor. 2. In order to set the secondary pressure correctly, the secondary pressure must always be lowered to nearly 0Pa before turning the control handle . 3. During use, make sure that the oil level always stays between the red lines on the oil gauge. 4. After use, always open the drain cocks and discharge the water and oil inside the tank and the transformer. 5. If a hand compressor or compressed air pipe is to be used to supply air, verify the following: (a) That air is supplied at a pressure of 0.35 to 0.4MPa (b) That the pressure does not fluctuate (c) That the air supplied does not contain water, oil, or dust
2.3.6 General Precautions for Handling Gas Cylinders

Handle the cylinders carefully, observing the following precautions. (1) Before installing a pressure regulator on a cylinder, it is always necessary to blow away any dust in the cylinder outlet. (2) When opening the cylinder main valve, turn the secondary pressure control handle sufficiently counterclockwise, and after checking that there is no one standing on the outlet side, gently open the valve with a cylinder handle.
2-13 AA-6800/6650
(3) In the case of nitrous oxide, hydrogen, argon, oxygen, etc., open the cylinder main valve sufficiently. With acetylene, do not turn the cylinder main valve more than 1.5 turns in order to prevent the acetone or DMF (dimethylformamide) inside from flowing out. (4) When using a nitrous oxide-acetylene flame, always open the valve of the acetylene cylinder 1 to 1.5 turns. If the valve is opened less than this, the acetylene flow rate may be insufficient and cause flashback when switching from an air-acetylene flame to a nitrous oxide-acetylene flame. (5) In the case of nitrous oxide, the flow rate may become unstable if the main valve is not opened enough. Make sure that main valve is opened enough. (6) Place all the cylinders upright. (7) Always leave the cylinder handle attached to the main valve even during use. (8) After use, not only close the stopcock but also always shut the cylinder main valve. (9) When the source pressure of the acetylene cylinder decreases to 0.5MPa, replace the cylinder. In the case of acetylene gas, a porous mass inside the high-pressure container is soaked with acetone or DMF (demethylformamide), and the acetylene gas is dissolved in that by compression. If the internal pressure of the cylinder decreases to less than 0.5MPa, vapor of acetone or DMF will become mixed in the acetylene gas, and the gas flow rate will become unstable. If the internal pressure decreases to less than 0.3MPa, the acetone or DMF will flow out, and control of the gas flow rate will be impossible.
2
Installation
2-14
2.3.7 Installing Pressure Regulators (Optional) and Checking for Leaks

WARNING 1. If a mistake is made in the piping, it may cause flashback on ignition, so exercise sufficient caution. 2. Always set the gas supply pressures at the specified values. 3. Never use a broken regulator. This may result in an accident. (1) Wipe any dust adhering to the outlet of the cylinder. (2) Refer to Figures 2.8 to 2.10 to install these pressure regulators on the cylinders. If the screw for mounting the regulator on the cylinder appears ready to break, replace the cylinder without attempting to mount the regulator. (3) Open the cylinder main valve gently after closing the stopcock and turning the secondary pressure control handle sufficiently counterclockwise. (4) Turn the secondary pressure control handle clockwise and set the secondary pressure to the following values: Acetylene Hydrogen: Nitrous oxide Argon 0.09MPa 0.09MPa 0.35MPa 0.35MPa
(5) Apply soapy water to each of the connecting joints to check for leaks. Due care should be taken to detect and eliminate any leaking at the cylinder cock.
AA-6800/6650
Primary Secondary pressure gauge pressure gauge
Cylinder main valve
Open by turning counter-clockwise; close by turning clockwise. Use turned counter-clockwise 1.5 turns.
2
Installation
Secondary pressure control handle
( (
When turned clockwise, the secondary pressure rises; when turned counter-clockwise, it decreases. The secondary pressure is normally set to 0.09MPa.
Figure 2.8 Pressure Regulator for Acetylene

Secondary pressure control handle When turned clockwise, the secondary pressure rises; when turned counter-clockwise, it decreases. The secondary pressure is normally set to 0.35MPa.
Secondary pressure gauge
Cylinder main valve Open by turning counter-clockwise; close by turning clockwise. Use almost wide open.
) )
Stop cock
Connecting nut
Figure 2.9 Pressure Regulator for Nitrous oxide

Primary pressure gauge Cylinder main valve
Secondary pressure gauge
Open by turning counter-clockwise; close by turning clockwise. Use almost wide open.
Stop cock Connecting nut Flashback prevention valve
Secondary pressure control handle
When turned clockwise, the secondary pressure rises; when turned counter-clockwise, it decreases. The secondary pressure is normally set to 0.09 MPa.
)
2-15
Figure 2.10 Pressure Regulator for Hydrogen Gas
AA-6800/6650
2.3.8 Software Operation Minimum Requirements (provided by user)

In order to run the AA-6800/6650 software and control the instrument, the following software and hardware must be provided. 1) Personal computer (PC) and peripheral accessories 2) Operating system 3) Connection cable Table 2.7 PC Specifications Specifications Pentium 75 or faster(Pentium 200 or faster CPU recommended) 32MB or larger (64MB or larger RAM recommended) SVGA (800600 or higher) (1024768 or higher resolution recommended) Recording device I/O port Peripherals 1 floppy disk drive (for installing the program) (3.5inch size) (with at least 10MB free disk space for AA software) 1 serial port for AA Monitor Keyboard Mouse or other pointing device Printer Connection Cable In order to connect the PC and AA-6800/6650, the RS-232C reverse cable (cross cable) is provided as standard accessory. This cable has a male DSUB 25-pin connector for connecting to the RS-232C connector (PC) at the rear of the AA main unit, and a female 9-pin DSUB connector for connecting to the serial port connector on the typical IBM PC/AT and compatible computers. Figure 2.11 shows the wiring diagram of the standard accessory cable. If serial connector on your PC is not male 9-pin DSUB, appropriate cable for your PC must be provided by user. In such case, use Figure 2.11 and Figure 2.12 to obtain an appropriate cable (Figure 2.12 shows the wiring diagram of the cable which is appropriate for the PC with female 25-pin RS-232C port).
2
Installation
2-16
CPU RAM Screen resolution
AA-6800/6650
AA side D sub 25-pin male connector
PC side D side 9-pin female connector
2
Installation
Figure 2.11 RS-232C 9,25 Cable Pin Assignments (P/N200-79144-01)

D sub 25-pin male connector D sub 25-pin male connector
Figure 2.12 RS-232C Cable Pin Assignments (P/N208-94963-91)

Operating System The computer must contain the WindowsTM95 WindowsTM98 or WindowsTMNT4.0 software in order to run the AA-6800/6650 software (WindowsTM95, WindowsTM98, and WindowsTMNT4.0 are registered trademarks of Microsoft Co.).
2-17 AA-6800/6650
2.4
Assembling the AA-6800/6650
2.4.1 Connecting the Drain Tube

To prevent gas from leaking through the drain tube, the liquid in the drain tank placed in the drain line must be maintained at a constant level so that the water pressure may provide proper sealing. (1) Fasten the drain assy to the lower right on the front of the main unit using the two M36 screws. (2) Connect the drain liquid level sensor cable to the connector for drain monitor on the gas control panel (refer to 3.1.6). (3) Connect the tube from the chamber to the coupling at the drain tank bottom and fix it firmly with a band. (4) Connect the provided drain tube to the drain outlet. When analyzing water soluble samples, use vinyl tube R3603, and for organic solvents, use the silicone rubber tube. (5) Provide an appropriate container to receive the drained liquid. (6) Fill water via the breather at the top of the drain tank until the water overflows from the drain tank inside the gas flow control compartment. If the water level is not high enough, the liquid level sensor will be activated to prevent ignition. (7) To ensure that drainage is performed smoothly: (a) The drain tube should hang downward so that there is no crimping of the tube. (b) Leave the end of the drain tube free in the air. If drainage is not performed smoothly, excessive noise will be produced and reproducibility may be adversely affected.
2
Installation
2-18
CAUTION
1. Neither vinyl tube (R3603) nor silicone rubber tube can be used for petroleum solvents. 2. Especially for organic solvent waste, prepare a suitably sized drain container of appropriately resistant material. 3. Dispose frequently the drain generating hazardous gases.
Spray chamber
Liquid level sensor
Drain tank Drain tube
Drain container
Figure 2.13 AA-6800/6650
Connecting the Drain Tube
2.4 Assembling the AA-6800/6650
2.4.2 Assembling the Burner
CAUTION
O-rings are placed at the mounting surfaces of the burner head and the nebulizer to prevent gas leakage. When assembling, always verify that the Orings are in place.
2
Installation
Refer to Figure 2.14 in assembling the burner. (1) Pull out the burner head upward. If it is not pulled out easily, turn the burner head while pulling it out. (2) After confirming that O-ring is properly fitted inside, fit the burner head onto the chamber steadily to the end. (3) Loosen the screw at the front of the spray chamber, remove the nebulizer retaining plate and shift the nebulizer to the front. Confirm that the O-ring is properly fitted to the nebulizer. (4) Exercising maximum care so as not to damage the capillary, insert the capillary of the nebulizer into the provided sample aspiration Teflon tube (cut off cleanly at a right angle). (5) Insert the nebulizer to the chamber certainly, set the nebulizer retaining plate with the screw. (6) Mount the sample stage in the front of the burner compartment. (7) In the case of AA-6800 series, place the Drive Unit Cover onto the lower part of the burner compartment. At this time, set it so that the strut of the Drive Unit may fit in the notch of the Drive Unit Cover and so that the hole on the burner compartment floor may be covered. This is to prevent foreign substances from entering through the hole. NOTES 1. If it is difficult to fit the Teflon tube onto the capillary, warm up the end of the tube to enlarge the opening. Since the capillary is very thin and fragile, be careful that it does not break. 2. A polyethylene tube covers the capillary to ensure a snug fit between the Teflon tube and the capillary (refer to Figure 6.4 in the Section 6.2.2). 3. Insert the nebulizer steadily. If unsteadily, sensitivity gets down. 4. As the ceramic ball (impact bead) is easily taken off, be carefull not to hit it. If the ceramic ball is taken off, mount it to the right position. 5. When driving the atomizer unit, remove the Drive Unit Cover.
2-19 AA-6800/6650
Burner head
2
O-ring Spray chamber Nebulizer retaining plate O-ring
Installation
Ceramic ball
Nebulizer
Figure 2.14 2.4.3 Cable Connections
Assembling the Burner
Referring to Figure 2.15, connect the AC cable of standard accessory, and connect the RS-232C reverse cable to the PC. (For details on connecting PC to monitor, keyboard, mouse and printer, refer to the appropriate documentation.) Connect the RS-232C reverse cable to the connector labeled "PC" on the rear of the AA, and to the serial port on the PC. The PC serial port may be called "COM port" or "RS-232C port", depending on the PC model. Refer to the documentation provided with the PC. Be sure to check that the AA power switch is OFF before connecting the AC cable.
AA rear side
RS-232C cable
SERIAL1 SERIAL2 COM1 COM2 RS-232C etc. (called by various name.)
AC cable
Figure 2.15
CAUTION
Cable Connections
Before connecting or disconnecting the ground wire, be sure to remove the AC cable connector from the power socket.
2-20 AA-6800/6650
CAUTION
In the case of 2-wire socket, be sure to ground the earth terminal of AC cable .
2
2.4.4 Hose Connections
Refer to Figure 2.16 in connecting the hose.
Right rear of main unit To acetylene or hydrogen gas cylinder To compressor, air or argon gas cylinder To nitrous oxide gas cylinder Green Black Red Quick-connect hose joints
Installation
Black
Tube connectors Red
White
Figure 2.16
WARNING DO NOT USE OXYGEN GAS.
Hose Connections
(1) Hose connections between the compressor/gas cylinders and the connectors at right rear of main unit The hose joints are connected to the rubber hoses as follows: Black rubber hose AIR (large) for Air Black rubber hose SUPPORT (large) for Argon Green rubber hose N2O (small) for Nitrous oxide Red rubber hose C2H2 (small) for Acetylene Red rubber hose FUEL (small) for Hydrogen gas Connect one end of the rubber hoses to the compressor or gas cylinders and secure firmly with the hose bands. Connect the other end (with hose joint) of the rubber hose to the specified gas inlet at the rear of main unit. The gas inlet port is provided with cap nut and sleeve. First, pass the cap nut and sleeve through the hose joint. Next, insert the hose joint into the gas inlet port deeply to the bottom, and tighten the cap nut by hand. Finally, tighten the screw firmly using spanners.
2-21 AA-6800/6650
(2) Connections between burner unit and connectors at right rear of main unit Connect one end of the provided gas tubes (bundle of 3 nylon tubes) to the tube connectors on the rear of the main unit as follows: White tube SPRAY Black tube AUX Red tube FUEL
2
Installation
2-22
Push each tube onto the above tube connector to the end and tighten the cap nut firmly by hand. Connect the other end of the tubes to the provided seal joint, then check for gas leaks according to 6.3. After checking for gas leaks, detach the tubes from the seal joint. Then reconnect them to the specified gas inlet. NOTE Attach and detach the tubes to the quick-connect joints as follows: <To Attach> Grip the tube securely, and push it slowly and completely onto the joint. When inserted all the way, pull the tube lightly to confirm that it will not come off the joint. <To Detach> Push on the release bushing evenly while securing the tube in place with the other hand. When the release bushing is in its fully retracted position, pull on the tube to disconnect it from the joint. When reattaching the tube, confirm that there are no indentations in the tube. If indentations are noticeable, cut off that section of tube with a cutter knife, and reattach the tube.
2.4.5 Replacing the AA-6650 Atomizer

The AA-6650F and AA-6650G are the instruments designed for flame and furnace analyses, respectively. However, if the graphite furnace atomizer GFA and the base for furnace are prepared, the AA-6650F can be used also for furnace analysis. Part Name Graphite furnace atomizer GFA Base for furnace P/N 206-51000-93 (220V), -34 (230V), -35 (240V) 206-51141
Also, if the flame conversion unit ACF-6800 and the cover for flame are prepared, the AA-6650G can be used for the flame analysis. Part Name Flame conversion unit ACF-6800 Cover for flame P/N 206-64843-92 206-50554
AA-6800/6650
Replacing the burner with the graphite furnace The procedure for mounting the graphite furnace instead of the burner is described here. (1) Remove the flame shield. (2) Lift up the burner head and remove it from the chamber. (3) Remove the four screws fixing the cover for flame and remove the cover for flame (refer to Fig.2.17, upper). (4) Using the four screws removed at the step (3), mount the base for furnace instead of the cover for flame (refer to Fig.2.17, lower). (5) When mounting the graphite furnace, it is necessary to adjust the furnace position so that the optical axis and graphite furnace may have the optimum positional relation. Refer to the section 6.1.2.2 for mounting the graphite furnace and adjusting the furnace position. (6) After mounting the graphite furnace, check that the plumbing tubes are not bent and that no excessive force is given to the furnace heating cable. Replacing the graphite furnace with the burner The procedure for mounting the burner instead of the graphite furnace is described here. Refer to the section 6.1.1.2 for adjusting the burner position. (1) Remove the four screws fixing the base for furnace, and remove the base for furnace while keeping the graphite furnace mounted on it. (2) Using the four screws removed in the step (1), mount the cover for flame instead of the base for furnace. (3) Fit the burner head in the chamber firmly. (4) Mount the flame shield. (5) Check the gas plumbing before use.
Graphite furnace
2
Installation
Two screws M38 (inner)
Base for furnace Four screws
When using the Graphite Furnace

Burner head Cover for flame Four screws
When using the Burner
Fig.2.17 Replacing the Atomizer Unit AA-6800/6650
2-23
2.4.6 Installation of PC software

This procedure assumes that MS-WindowsTM is already installed on the PC. For its installation, refer to the appropriate documentation. 1) Start up MS-WindowsTM. 2) Insert the AA software setup disk #1 in the floppy disk drive of the PC. 3) Select [Run...] from <START> in the task bar. 4) Input "A:\setup" to the [Open] in the [Run] dialog box and click on <OK> (A: refers to the floppy disk drive name. Enter this or "B", "C", "D", etc., according to the PC configuration). 5) First, a note for installation is displayed. Read it and click on <Next> to go ahead. 6) Select the AA main unit type. If you have selected wrong AA main unit type and finished the installation, reinstall this AA software and select proper type here. Click on <Next> to go ahead. 7) Select GFA instrument type. Click on <Next> to go ahead. GFA instrument type can be selected after installation(refer to the section 5.8.3). 8) Check the installation destination folder. You may change the folder here, if desired. Click on <Next> to go ahead. 9) Select the program folder. Click on <Next> to start setup. 10) When the message appears to prompt inserting the next disk, insert the disk #2 into the floppy disk drive and click on <OK>. 11) Finally, when the message shows that the setup is completed, click on <Finish>. When the [Yes, I want to read README.TXT] check box is check-marked, the README.TXT is displayed by the Notepad. Be sure to read this, since the important information about AA software operation is described in the README.TXT. Exit the Notepad, then installation procedure is finished. NOTE Set all the electric power-saving functions to OFF both in the BIOS setup of PC and in the control panel of Windows. Otherwise, the electric power-saving function may cause a trouble in communication between the AA main unit and the PC. How to display the BIOS setup screen is different depending on the PC model. Refer to the instruction manual provided with the PC. When upgrading the WizAArd ver.1.xx to ver.2.xx Don't delete "wizaa.ini" file in the Windows directory when uninstalling the WizAArd ver.1.xx. Upgrading to ver.2.xx is performed more smoothly when the "wizaa.ini" file of WizAArd ver.1.xx remains. Also, It is highly recommended for you to back up "wizaa.ini" file before uninstalling the older version WizAArd. When upgrading the WizAArd ver.2.1x to ver.2.20 Don't uninstall the WizAArd ver.2.1x when it is already installed. If the WizAArd ver.2.1x is uninstalled, "wizaa.ini." file and lamp history data (lamphist.ref file) are deleted and, as the result, various parameters and its lamp use time are reset. For upgrading, execute the setup disk of ver.2.20 and install it to overwrite "ver.2.1x" on the folder in which the old version software
2
Installation
2-24
AA-6800/6650
has been installed. To keep ver2.1x, install ver.2.20 in another folder. At this time, to transfer the lamp history data from ver.2.1x, copy the "lamphist.ref" file of ver.2.1x to the folder in which ver.2.20 has been installed. When installing WizAArd to Windows NT4.0 When installing WizAArd to the Windows NT4.0, log in with the authorization of Administrator. When using the atomic muffle and performing the version-up of WizAArd If your instrument type is not available for flame measurement (AA6650G/6800G) and equipped with the atomic muffle SARF-16C, performing the PC software version-up to WizAArd ver.2.11 or later may make the operation complicated. Because an unnecessary checklist screen for starting a flame measurement appears at every time of initialization. To avoid this problem, remove the short plug inside the instrument. For details on the short plug, refer to the instruction manual for adapter set for mounting the atomic muffle.
2
Installation
2-25
AA-6800/6650
2.5
Assembling GFA-6500
WARNING
RISK OF ELECTRIC SHOCK Before attaching or detaching the graphite furnace or heating cables, make sure that the power is off.
2
Installation
2-26 AA-6800/6650
2.5.1 Mounting the Graphite Furnace

After removing the burner head of AA-6800, place the graphite furnace before the burner unit (this side) and fix it with the two retainig screws (M38). Remount the burner head as before, taking care not to catch in the cooling water tube of the graphite furnace.
Burner head
Retaining screw(M38)
Figure 2.18 Graphite Furnace Placement Diagram 2.5.2 Cable Connections

[Power cable and ground wire connections] (1) Connect the AA-6800 and GFA-6500 ground wires referring to Figure 2.19. (2) Confirm that the HEAT and CONTROL switches on the right side of the unit are OFF. And then connect the provided power cable to the connector at the rear of the GFA power supply unit. Of the 3 wires making up the other end of this power cable, the green one is the ground wire. Connect the three wires to suitable connector for the 200V power line. When a 3-phase 200V line is used as the power source, any 2 of 3 terminals may be used. (The "200V" is different according the region. It may be 200V, 220V, 230V or 240V.) CAUTIONS 1. When connecting or disconnecting a ground wire, always unplug the power cable. 2. Always verify proper grounding. 3. The input voltage is 200V and the power consumption is 6kVA. If the iput voltage decreases or power capacity is insufficient, heating to a maximum furnace temperature of 3000 may not be attainable. A difference of 5% is possible between the setting temperature and the heating temperature of the tube with an input voltage fluctuation of 200V10%.
2.5 Assembling GFA-6500
Power cable
Temperature sensor cable Thermistor cable Heating cable
2
Installation
Green wire
Cable, GFA I/F
Ground wire(GFA-6500) 2-pin connector 4-pin connector
Figure 2.19
[Connecting the AA-6800 with the GFA-6500]
Cable Connections
This must be performed by service engineer. For details, refer to the service manual. (1) Loosen the screws and demount the concealed cover on the left rear side of AA-6800. (2) Take out the 2-pin connector cable mounted on the rear side of the cover. (3) Connect the 2-pin cable coming from GFA-6500 with the cable taken out in (2). (4) Connect the 4-pin cable coming from GFA-6500 to the GFA connector on the rear side of AA6800 viaCable, GFA I/Fprovided with GFA. [Connecting the graphite furnace cables] (1) Connect each cable from the graphite furnace to the rear of the GFA-6500 as follows: TEMP SENS cable Thermistor cable TEMP SENS COOL CHK
Heating cables (two) Plate electrodes (right and left) (2) Place the terminal of each of the heating cables on the respective plate electrode and tighten the bolt and nut firmly using two wrenches.
Heating cable Nut GFA-6500 Spring washer Flat washer
Plate electrode
Bolt
Figure 2.20
Connecting the Heating Cable 2-27 AA-6800/6650
2.5.3 Tubing
Perform the tubing connections referring to Figure 2.21.
2
Installation

Fluororubber tube
Side of instrument Temperature sensor
Black rubber tubes To argon gas cylinder
Nylon tubes To O2 gas cylinder or compressor Connect to water faucet Tube for cooling water
Rear of instrument Cooling water INLET
Discharge Cooling water OUTLET Extension tube
Figure 2.21
Tubing Connections
(1) Connect one end of the black rubber tubes to the gas cylinder and secure it tightly with a hose band. Use either of the two hose band types to match the diameter of the connectors at the cylinder. Connect the other end of the rubber tube to the specified gas inlet at the rear of the GFA unit. Connect the hose to the ALT connector only when oxygen or air is required. (2) Pass the black nylon tube for cooling water through the sleeve and cap nut and then insert it up to the end. Hand-tighten the cap nut and then turn the nut 1.52 turns with the provided wrench. (3) Push the INLET and OUTLET tubes from the graphite furnace all the way onto the tube connectors and tighten the cap nut firmly by hand. (4) When the tubing is completed, check for leaks as follows. Run water to check for leaks in the cooling water line. Normally, the cooling water flows at a rate of about 1L/min. Supply gas to the unit by opening the cylinder main valve and adjusting the secondary pressure to 0.35MPa. Also, with the pressure-reducing valve and stopcock open, close only the cylinder cock to check the drop in secondary pressure during a set time. When the drop in pressure in 30 minutes is 0.03MPa or more, there is probably a gas leak in the line. Firmly tighten the connections again where the water and gas leaks are occurring. (5) Connect the fluororubber tube coming from the graphite furnace to the INNER connector at the side of the GFA unit. Also, push the black nylon tube coming from the sensor of the graphite furnace all the way onto the TEMP SENS connector. Push the remaining black nylon tube all the way onto the OUTER connector.
2-28 AA-6800/6650
2.5.4 Loading the Graphite Tube

Referring to Figure 2.22, load a graphite tube in the furnace following the procedures below.
2
Graphite cap Seal Graphite holder Socket adapter Window socket Window
Installation
Lock knob Release Lock
Figure 2.22
2.5.4.1 Using a High Density Graphite Tube
Graphite Furnace
(1) Press the knurled lock knob and turn it counterclockwise to release the lock, and then slide the righthand cooling block to the right. (2) Insert the graphite tube into the graphite cap, rotating the graphite tube so that the hole in the graphite cap upper and the hole in the graphite tube (sample injector port) are aligned. (3) Return the right-hand cooling block to its original position and lock it by pressing and turning the lock knob clockwise. At this time, confirm once more that the hole in the cap upper and the sample injector port of the graphite tube are still aligned. (4) After loading the graphite tube, select [Parameters]-[Element Selection Wizard] from the menu and set the analytical conditions for "Cu" or the element about to be measured. At this time, set the lamp mode to the BGC-D2 or BGC-SR background correction mode. Table 2.8
STAGE# 1 2 3 4 5 6 7
Furnace Program Example (Cu)

Temp () 150 250 800 800 800 2300 2500 Time (sec) 20 10 10 10 3 2 2 Heat Mode Sensitivity RAMP RAMP RAMP STEP STEP STEP STEP GAS Type #1 #1 #1 #1 #1 #1 #1 Flow Rate (L/min) 0.1 0.1 1.0 1.0 0.0 0.0 1.0
Sampling Stage No. : 6
2-29 AA-6800/6650
(5) After creating/preparing the furnace program, execute the <Test Meas.> on the "Furnace Program" page. At this time, don t inject the sample into the graphite tube. (6) When the test measurement is completed, execute the <Cleaning> for the graphite tube. (7) Once more execute the <Test Meas.>. (8) If the test measurement results indicate background due to the existence of smoke or other substance during atomization, repeat steps (6) and (7) until there are no longer any contaminants to produce background. (9) If, after performing the steps outlined above, background contaminants are not eliminated, there may be contamination at a location other than the graphite tube. In this case, perform cleaning of the graphite cap, etc. For details, refer to the section 6.6.
2
Installation
2-30
2.5.4.2 Using a Pyrolytic Coating Graphite Tube (1) Load the graphite tube in the furnace using the same procedure as for the high density graphite tube. (2) After loading the graphite tube, select [Parameters]-[Element Selection Wizard] from the menu and press the <Change Graphite Tube> button in the "Furnace Program" page to open the <Change Graphite Tube> dialog box. In the case of new pyrolytic coating graphite tube, actual tube temperature tends to be controlled a little higher than the programmed temperature. It may cause low sensitivity of measurement or poor reproducibility at starting time. To avoid this, it is necessary to perform conditioning. (3) Press the <Graphite Tube Conditioning> button to execute the conditioning. At this time, don t inject the sample into the graphite tube. (4) After completing the conditioning, repeat the <Test Meas.> and [Instrument]-[cleaning] in the same procedures as those for high density graphite tube (refer to (4) to (9) in the Section 2.5.4.1).
AA-6800/6650
NOTES 1. The positional relationship between the graphite cap and the left-hand cooling block is extremely important. You must match up the indicators on the front of the graphite cap with those on the right side of the left-hand cooling block. 2. Some elements such as Ca, Si or Fe, etc. are contained in the tube material. Therefore, blank peaks will appear when these elements are measured. Since the blank value will become constant after you perform the cleaning operation by the above procedure, start measurement after this point. 3. Inner gas (1.5L/min) and outer gas (1.5L/min) will automatically flow during the cleaning operation and for 60 seconds after the cleaning operation is completed. 4. When the high density graphite tube is loaded to the furnace and used at temperautre set to 2700 or higher, carbon coming from the tube may deposit the emission detecting hole for temperature sensor made on the graphite cap. For this reason, the amount of light reaching the temperature sensor may decrease and as the result the actual temperature may be higher than the programmed temperature. So when using the high density graphite tube in the above setting, clean the emission detecting hole of the graphite cap periodically. 5. Although the amount of carbon coming from the high density graphite tube is remarkably less compared with that coming from the high density graphite tube, periodical cleaning of the emission detecting hole of the graphite cap is recommended for the same reason of above 4. 6. When analyzing a sample containing nitric acid of 0.5% or higher with the high density graphite tube, reducing the inner gas flow rate (0.2L/min or less) is recommended. It will lessen the tube consumption.
2
Installation
2-31
AA-6800/6650
2.6
Mounting a Hollow Cathode Lamp
(1) Open the cover on the left side of the main unit. (2) Remove the lamp socket from the turret peg (socket holder). (3) Insert the hollow cathode lamp in the turret. (4) Plug the lamp socket into the lamp. (5) Put the provided HCL name sticker (sticker with element name) at an easy-to read location of the lamp.
2
Installation
2-32
AA-6800/6650
2.7
Installing the ACF-6800
Since various operations, such as removing the cover, connecting cables and plumbing gas tubes, etc., are required when adding the ACF-6800 flame unit to the furnace-dedicated AA-6800G/6650G, be sure to have a service representative from the nearest branch agent or office perform the installation.
2
Installation
2-33 AA-6800/6650
Chapter 3 Instrument Constructions
Instrument Constructions
Contents 3.1 AA-6800/6650 Configurations 3-1 Operation Switches 3-1 Hollow Cathode Lamp Turret 3-2 Deuterium Lamp 3-3 Burner Module 3-4 AA-6800 3-4 AA-6650 3-5
3.1.1 3.1.2 3.1.3 3.1.4
3.1.4.1 3.1.4.2 3.1.5 3.1.6 3.1.7 3.1.8 3.2 3.2.1 3.2.2 3.2.3
Burner 3-6 Gas Control Panel 3-7 Optical System 3-9 Photometric System 3-10 Graphite Furnace 3-12 Main Unit (Power Supply) 3-14 Operation Principles 3-15
GFA-6500 Configuration 3-12
AA-6800/6650
3.1
AA-6800/6650 Configurations
3.1.1 Operation Switches
3
Figure 3.1 AA-6800/6650 Main Unit

No. (in Fig 3.1) Name POWER switch BURNER SELECT switch Function Turns ON the instrument. This key switch is for preventing mistaken use of burner heads. When the high temperature burner head (optional) is to be used with the nitrous oxide-acetylene flame, a key attached to the burner head is used to change to the N2OC2H2 position. If not in this position, the nitrous oxide flame cannot be ignited. The Air-C2H2 position would normally be used for an air-acetylene flame or an argon (air)-hydrogen flame, but the N2O-C2H2 position can also be used. EXTINGUISH button IGNITE buttons Pressing this button extinguish the flame. When these two buttons are pressed at the same time, gas is fed to the burner and is ignited by the pilot flame.
3-1 AA-6800/6650
3.1 AA-6800/6650 Configurations
3.1.2 Hollow Cathode Lamp Turret

Eight lamps may be installed, two of which may be on at one time. For routine analysis in which the analysis elements are known, it is convenient if all the lamps to be used in measurement (up to eight) are installed in the turret and the lamp current values, lamp numbers (socket numbers) along with the other measurement parameters are stored beforehand in the instrument memory. This then allows the required lamp to be automatically set in the optical path by just loading the stored parameters. CAUTIONS 1. When installing a lamp, after inserting the lamp in the hole in the turret, insert the socket having the same number as the turret hole onto the lamp pins. Make sure that the socket is fully seated; if it is not, there is a danger from exposed pins carrying high voltage loads. Also, when removing the socket, make sure that this operation is performed only after the lamp current reads 0mA or OFF. 2. Mount unused sockets on the turret pegs near the turret holes.
3
3-2
Socket
Boss
Figure 3.2
Hollow Cathode Lamp Turret
AA-6800/6650
3.1.3 Deuterium Lamp

The deuterium lamp is of the hot cathode type and is used at the wavelength range of 190nm - 430nm in background correction and measurement. The lamp is socketed in the instrument to allow easy replacement. The adjusting screw is used to position the new lamp upon replacement.
Deuterium lamp
3
Adjusting screw
Figure 3.3 Deuterium Lamp
3-3 AA-6800/6650
3.1.4 Burner Module 3.1.4.1 AA-6800

The burner drive is performed by PC operation. Therefore, there are no positioning knobs for driving the burner module.
3
3-4 AA-6800/6650
Figure 3.4 Burner Module (AA-6800)

No. (in Fig 3.4) Name Burner head Function The types of flames which can be used with the standard burner head are 3 types, which are air-acetylene flame and air(argon)-hydrogen flames. Be sure to use the high temperature burner head (optional) when using a nitrous oxide-acetylene flame. Burner head angle adjustment lever These allow the angle of burner slot to be adjusted relative to the light path. Normally, the position at 0 on the scale (slot is parallel with light path) is used, but when measuring high-concentration samples, measurements of better linearity between concentration and absorbance can be obtained by angling the slot to decrease sensitivity. Flame Monitor An optical sensor is built in the instrument for monitoring the intensity of the light emitted by the flame. If the flame goes out and the light emission is lost, the solenoid valve in the gas control unit is closed by a signal from the sensor and the flow of raw gas is stopped. In addition, when switching between an air-acetylene flame and nitrous oxide-acetylen flame, an increase in the acetylene flow rate will be detected by an increase in the light emission intensity, and the air and nitrous oxide will be switched. Pilot flame Pressing the IGNITE buttons on the gas controller ignites the pilot flame.
3.1.4.2 AA-6650 On the front side of AA-6650 burner module, the knobs for adjusting the horizontal and vertical positions of the burner (or graphite furnace) are prepared. The atomizer is driven with these knobs.
3
Vertical mark line
Front-back indicating position
Height indicating position
Expanded figure of the part marked with
Figure 3.5 Burner Module (AA-6650)

No. (in Fig 3.5) Name Burner position indicator scale Function The scale shows the height of the burner, indicating the height from the light path to the top of the burner head. In addition, when the front-back indicating position of the burner is at the vertical mark line, the slot of the burner head is positioned right beneath the light path. For precise adjustment, refer to 6.1.1.2. Knob for adjusting burner vertical position Turning this knob adjusts the front-back position of the burner. When the knob is turned clockwise, the burner moves forward. Knob for adjusting burner horizontal position Turning this knob adjusts the burner height. When the knob is turned clockwise, the burner moves down.
3-5 AA-6800/6650
3.1.5 Burner
The AA-6800/6650 has a burner head with a 10cm length slot (standard accessory) mounted in the premixing atomizer chamber. This burner head can be used with air-acetylene flames and air(argon)hydrogen flames. Please specially install a high-temperature head (optional accessory) when using a nitrous oxide-acetylene flame.
3
Figure 3.6 Burner
No.(in Fig 3.6) Name Burner head fixing port Nebulizer Function Insert the burner head into this port. The burner head is fixed with the internal O-rings. This uses air negative pressure to suction the sample solution and spray it from the tip of the capillary as a mist of fine particles. Disperser This makes the fine particles of sprayed sample solution into even finer particles, and larger particles are separated out. Nebulizer retaining plate and fixing screw Spray chamber Mixer Safety valve Fixes the nebulizer to prevent from coming off. The particles of sprayed sample solution are mixed with the combustion gas in this chamber. Mixing of the particles and combustion gas is promoted. In case of flashback, this valve is open to prevent the burner unit from being damaged. A flashback means a combustion or explosion which occurs in the burner when the flame combustion rate is fast and the mixed gas flow rate is slow. In case a flashback should occur and the safety valve operates, set the safety valve back in the place. Drain discharge port Large particles are discharged from this port.
3-6 AA-6800/6650
NOTE
When measuring samples containing high-concentration coexistant like salts or when measuring samples with a nitrous-oxide flame, the mixer reduces the signal noises. Therefore, the mixer is usually mounted in the chamber. When measuring samples with low-concentration coexistant with air-acetylene flame, however, removing the mixer may improve the sensitivity. If a high sensitivity is required for such samples, you can remove the mixer if necessary. Remove the mixer referring to the section 6.2.3.
3
3.1.6 Gas Control Panel
Figure 3.7 Gas Control Panel
3-7 AA-6800/6650
No.(in Fig 3.7) Name Support gas pressure gauge Support gas flow adjusting knob
Function Displays the setting pressure for the support gas. Flow increases when turned to the left, and decreases when turned to the right. Usually, use the air or argon at 8L/min, and nitrous oxide at 6.5L/min.
3
3-8
Support gas flowmeter Support gas pressure adjusting knob
Displays the flow rate for the support gas. Read the flow at the center of the float (ball). Turning this clockwise increases the pressure, and turning this counterclockwise decreases it. This is set at 0.25MPa before shipping.
Fuel gas pressure gauge Fuel gas pressure adjusting knob BUZZER OFF button PURGE button Pilot flame adjusting knob (located on rear of unit)
Displays the setting pressure for the fuel gas. Adjust the pressure exactly to 0.05MPa. A buzzer sounds when a gas leak is detected. The buzzer may be turned off by pressing this button. Pressing this button with the gas cylinder or compressor closed off, the gas remaining inside the tubing is purged. This knob adjusts the flow of gas to the pilot flame. Only a service engineer is allowed to operate this. Don't touch it. The amount of acetylene increases when switching from an air-acetylene to nitrous oxide-acetylene flame, and this knob is used to adjust the amount of increase. At shipment, this is set for an increase of 5L/min. Only a service engineer is allowed to operate this. Don't touch it.
BYPASS flow adjusting knob
Drain tank (located on front of unit)
This prevents raw gas from leaking through the drain tube. With the drain tank placed midway along the tube, the liquid in the tube is maintained at a constant level to form a water pressure seal.
Drain monitor (Only the connector is shown in the figure.)
This monitors the level of the water inside the drain tank. If the water level decreases too far, the flame is automatically extinguished. The burner head must be removed and water added via the breather at the top of the tank to bring up the level before ignition is possible.
CAUTION
Pressing the PURGE button discharges the mixture of fuel gas and support gas. Since the gas is inflammable, don't ignite a flame immediately after the PURGE button is pressed.
AA-6800/6650
3.1.7 Optical System

The light from the hollow cathode lamp and the deuterium lamp is combined with a beam combiner, and while passing through the atomizer, the atoms and concomitant substances absorb light as signal and background absorption. The light then passes through the spectrophotometer into the photomultiplier tube. The spectrophotometer is a high resolution Czerny-Turner type. The wavelength is selected by rotating a diffraction grating to separate the absorption spectrum of the element being analyzed from the other spectra. The direct drive mechanism used for wavelength selection is automated with the use of a motor. All of the optical elements are shielded from the outside air with the quartz window plates and are protected from dust and corrosive gases. HCL D2 BS W1-W4 M1-M6 S1, S2 G PMT : Hollow cathode lamp : Deuterium lamp : Beam splitter : Windows : Mirrors : Slits : Diffraction grating : Photomultiplier tube
3
Figure 3.8 Diagram of Optical System
3-9 AA-6800/6650
3.1.8 Photometric System

Figure 3.9 shows the photometric system.
3
Hollow cathode Lamp
Lamp power supply
Deuterium Lamp Burner
Monochrometer Detector Analog signal processor
D2 mode
Half mirror
CPU
Gas Control Unit
PC
Figure 3.9 Photometric System

The following five measurement modes can be selected in the AA-6800/6650. EMISSION mode NON-BGC mode BGC-D2 mode BGC-SR mode Used for flame emission analysis. Used for atomic absorption analysis that doesn t require background correction. Used for atomic absorption analysis that requires background correction. Used for atomic absorption analysis that requires background correction and whose results are easily affected by nearby spectral lines. Used for background measurement and molecular absorption measurements. (1) EMISSION mode: The spectrum produced by atomization of the analysis element in the flame is selected by the monochromator, and its intensity is measured via photometric circuitry. (2) NON-BGC mode: The deuterium lamp is extinguished, and only the light from the hollow cathode lamp, pulsed at 400Hz, is passed through the atomizer. Then only the spectral line (analysis line) to be used for anaylysis by the monochromator is selected. By measuring the light absorption at this time, it is possible to determine the concentrations of the elements being analyzed. The detector outputs a signal which is the sum of a 400Hz pulsed signal proportional to the analysis line intensity and a direct current signal from the light emitted from the atomizer (flame or graphite tube).
3-10 AA-6800/6650
(3) BGC-D2 mode: Pulsed light at 400Hz from the hollow cathode lamp and light from a 800Hz pulsed deuterium lamp are passed through the atomizer simultaneously. The light from the HCL lamp is absorbed both by the atoms of the element being analyzed and the concomitant elements as background absorption, while light from the deuterium lamp is absorbed only as background. In the photometric circuit, after each signal is converted to logarithms, their difference in absorption is measured. This allows correction for the background concomitant substances and an accurate measurement of the absorption by the element being analyzed. Characteristically, this mode offers higher photometric sensitivity than the BGC-SR mode. (4) BGC-SR mode: Light from a hollow cathode lamp generated by alternating low current and high current pulses is passed through the atomizer. The low-current-generated light is absorbed both by the element being analyzed and the concomitant substances as background absorption, while the high-current-generated light is absorbed only as background. After both signals are converted to logarithms in the photometric circuit, the difference between them is calculated in order to correct for the background absorbance due to the concomitant substances and accurately determine the absorption by the analysis element. This mode is characterized by the elimination of the effects of nearby lines. (5) D2 mode: Light from the hollow cathode lamp is removed from the optical path and only the 800Hz pulsed light from the deuterium lamp is passed through the atomizer. This light is absorbed by molecules produced in the atomizer, and the photometric circuit determines the degree of absorption. Detector sensitivity adjustment When the measurement mode is selected in the AA-6800/6650, the detector sensitivity is automatically adjusted to the optimum condition. In the EMISSION mode, the emission signal is set to a fixed value; in the NON-BGC mode, the selected hollow cathode lamp signal is set; and in the BGC-D2 mode and the D2 mode, the deuterium lamp signal is set, while in the BGC-SR mode, the high current hollow cathode lamp signal is set so that optimum detector sensitivity is obtained for each mode.
3
3-11
AA-6800/6650
3.2
GFA-6500 Configuration
3.2.1 Graphite Furnace

As may be seen in Figure 3.10, the heating element is a graphite tube which is encased in a graphite cap and graphite holder on its left and right side, respectively. On the outside of these on the left and right, there is a metal cylinder block (coolant block) for supplying electrical current, which is connected by cable to the power source. Coolant water is circulated through this block to prevent damage due to high temperatures. The left and right graphite cap and holder exert a strong holding force on the graphite tube, as they are locked in position by cylindrical socket adapters from the ends.These socket adapters provide for installation of the window plate sockets on the outside of the cooling blocks. The cylindrical quartz window plates are held in place at each end of the window plate sockets. Inert gas flow is used to prevent oxidation of the graphite tube at high temperature. The inert gas flows inside the graphite tube (inner gas) as well as between the tube and the graphite cap (outer gas), and each is supplied separately. The inner gas flows into the tube from the space on the left and right, and is vented upward from the sample injection hole in the tube. The outer gas flows through two holes, in the graphite cap and holder surface to flow in the space between the tube and the cap. As shown in Figure 3.10, the graphite tube is firmly hold between the graphite cap and graphite holder by the spring force to maintain the electrical contact. There is a 2mm diameter hole in the graphite cap corresponding to the hole at the center of the graphite tube rear side. Through this hole, the temperature sensor monitors the amount of light emitted by the graphite tube. The heating element graphite tube is a 30mm long cylinder with a sample 2.0mm-diameter injection hole in which a micro-syringe or the like is inserted to inject the samples. The graphite cap has another hole for sample injection at a position of 90 angle from the hole for light detection as mentioned above. A sample is injected into the sample injection hole of the graphite tube through this hole.
3
3-12
AA-6800/6650
3.2 GFA-6500 Configuration
Graphite cap
Graphite holder Socket adapter Window plate socket Window plate
3
Spring Cooling water inlet Side view
Inner gas inlet
Cooling water outlet
Inner gas inlet
Outer gas inlet
Rear view Outer gas inlet
Figure 3.10
No (in Fig 3.10) Name Temperature Sensor Nozzle
Graphite Furnace
Function This sensor is used to control the graphite tube temperature. The opening for reading light emission of the graphite tube. Ar gas is also blown through the hole to prevent dust contamination from adhering to the sensor window.
Stainless steel tube Cooling water flow path Thermistor Protective plate Coiling spring Seal
Ar gas input to the nozzle Cooling water flows from the left holder toward the right holder. Used to detect whether or not the cooling block is being cooled normally. Operates at approx. 50. This should be used whenever Flame measurement is performed. This keep off the slackness of the socket adapter. This covers the gap between the graphite cap and the graphite holder, and also prevents oxidation of the graphite tube.
3-13 AA-6800/6650
3.2.2 Main Unit (Power Supply)

Two types of power are supplied to the GFA-6500. There is an AC 100V control system power supply which is used for communication with the AA-6800, for executing the GFA software and in general for controlling the GFA-6500. This AC 100V power is supplied by the AA-6800 via the 2-pin connector cable ( in Fig.3.11). The other power supply is an AC 200V heating system power supply, which supplies power to the graphite furnace for heating. The AC 200V is supplied via the provided power cable. (The200Vis different according to the region. It may be 200V, 220V, 230V, or 240V.)
3
Figure 3.11 External View of GFA Power Supply

No.(in Fig 3.11) Name HEAT switch CONTROL switch Function Circuit protector for AC 200V. When ON, current is supplied according to the temperature program. AC 100V switch. Switching this ON allows communication with the AA-6800 and execution of the GFA software. Indicator lamp 4-pin connector cable Displays green light when AC 100V current is flowing. Cable for RS-232C communications with the AA-6800. Connected to the AA-6800 via theCable, GFA I/F provided with the GFA. 2-pin connector cable Fuse holder (Control) Fuse holder (Phase) Cable to supply AC 100V from the AA-6800. This should be connected only by a service engineer. 2A capacity, Type M (normal) 1A capacity, Type M (normal)
3-14 AA-6800/6650
3.2.3 Operation Principles

Figure 3.12 shows a block diagram of the GFA heating control system.
Sensor amplifier Graphite tube Heating mode switch Photocell
3
Switch Sensor amplifier
Current sensor
Furnace program Differential Amplifier
Heating power supply
Figure 3.12 Block diagram of Heating Control System

When the temperature setting is within the range in which heating control is performed via the Current Control Method, the switch automatically connects to constant point "2". When the temperature setting is within the range in which heating control is performed via the Temperature Control Method, the switch automatically connects to contact point "1". In a standard graphite tube, the relation between the current sensor output and the tube temperature and that between the light sensor (photocell) output and the tube temperature are pre-determined and are recorded in the memory. (1) Heating by the Current Control Method In the Current Control Method, when heating is initiated, the standard signal Vr corresponding to the set temperature and the output signal Vc from the current sensor are compared via a comparator amplifier. The current flowing to the tube is automatically adjusted until the two becomes equivalent. In this method, as shown in Figure 3.13, even when the current is supplied in steps, there is same delay in the elevation of the tube temperature. Normally, the tube will reach 97% or more of the set temperature within 15 to 20 seconds after heating has commenced. Furthermore, since in this method a constant current is supplied which corresponds to the setting temperature, there are cases where the actual temperature could vary due to changes in tube resistance due to its consumption, or variations in resistance values in different tubes.
3-15 AA-6800/6650
Temperature control method Temperature ( )
Current control method
Current
Heating start
Heating start
Time
Figure 3.13
Temperature and Current Changes in Current/Temperature Control Methods
(2) Heating by the Temperature Control Method Light radiating from the tube passes through the light detection hole in the graphite cap into the temperature sensor and strikes the photocell. A constant relationship exists between the temperature inside the tube and the output signal from the photocell, and this relationship is recorded in the memory. When heating commences, a comparator amplifier compares the standard signal Vr corresponding to the setting temperature and the output signal Vt from the photocell, and current is automatically adjusted until these two signals are equal. In this method, initially there is a very rapid rise in temperature as an excessive current is passed to the tube. Also, since the temperature in the tube is detected directly without being affected by changes in resistance values, etc., the tube is heated so that it is accurately maintained at the set temperature. (3) Temperature Correction for the Current Control Method As described above, resistance variation in the tube may give rise to temperature differences when using the current control method. The GFA-6500 incorporates a temperature calibration function to correct for this phenomenon. Each time the heating program is executed, the resistance value of the tube is automatically measured, and the correction result is reflected in the next heating cycle. Since this correction is performed for each heating operation, complete correction of any gradual changes in the tube s resistance is conducted each time it is heated.
3-16 AA-6800/6650
Current (A)
3
Temperature
Chapter 4 Basic Operation
4
Basic Operation
Contents 4.1 Switching On the Power and Starting Up the Software 4-1 Switching ON the Power to Hardware 4-1 Starting Up the Software 4-2 Software Basic Operation (Flame Method) 4-3 Operation Flowchart (Flame Method) 4-3 Wizard Selection4-4 Element Selection 4-4 Preparation Parameters 4-6 Sample ID 4-9 Sample Selection 4-11 Connect to Instrument/Send Parameters 4-12 Optics Parameters 4-13 Atomizer/Gas Flow Rate Setup (AA-6800) 4-16 Atomizer/Gas Flow Rate Setup (AA-6650) 4-18 Operation flowchart (Furnace method) 4-20 Wizard Selection 4-21 Element Selection 4-21 Preparation Parameters 4-24 Sample ID 4-30 Sample Selection 4-31
4.1.1 4.1.2 4.2 4.2.1
Software Basic Operation 4-3 4.2.1.1 4.2.1.2 4.2.1.3 4.2.1.4 4.2.1.5 4.2.1.6 4.2.1.7 4.2.1.8 4.2.1.9 4.2.1.10
4.2.2
Software Basic Operation (Furnace Method) 4-20
4.2.2.1 4.2.2.2 4.2.2.3 4.2.2.4 4.2.2.5 4.2.2.6
AA-6800/6650
4.2.2.7 4.2.2.8 4.2.2.9 4.2.3 4.3.1 4.3.2
Connect to Instrument/Send Parameters 4-32 Optics Parameters 4-33 Furnace Program 4-36
Saving the Template 4-38 Measurement Operation (for Flame Method)4-39 Measurement Operation (for Furnace Method) 4-41 Saving the Data 4-43 Printing the Data 4-43 Deleting the Data 4-43
4.3 Measurement Procedures 4-39
4.4 Saving/Printing/Deleting the Data 4-43
4
Basic Operation
4.4.1 4.4.2 4.4.3
4.5 Completing the Measurement 4-44 4.6 Explanation of Main Window 4-45 4.6.1 4.6.2 4.6.3 4.6.4 4.6.5 4.6.6 4.6.7 4.6.8 4.6.9 4.6.10 4.7.1 4.7.2 4.7.3 4.7.4 4.7.5 Menu bar 4-46 Standard tool bar4-46 Measurement element tool bar 4-47 Absorbance digital display 4-47 Real time graph (and furnace program graph) 4-47 Peak Profile (Latest four measurements and overlay display) 4-49 Calibration Curve Display 4-51 MRT work sheet 4-53 Function buttons 4-54 Status bar 4-55 Fields of MRT work sheet 4-56 Right Mouse Button Menu 4-61 Right Mouse Button on Summary Table 4-64 Inserting and Deleting the Measurement Row 4-64 Active Cell Movement by Shortcut Key and Cell Selection 4-64 Moving an Active Cell 4-64 Selecting Cells 4-65 Copy 4-65 Paste 4-65
4.7 Operating the MRT work sheet 4-56
4.7.5.1 4.7.5.2 4.7.6 4.7.6.1 4.7.6.2 4.7.7 4.8.1 4.8.2 4.8.3 4.8.4
Copy and Paste 4-65
Changing Column Width and Column Header Height of MRT Worksheet 4-66 Operation Locations 4-67 Safety Precautions Prior to Ignition 4-67 Igniting and Extinguishing Air-C2H2, Air(Ar)-H2 flames 4-68 Igniting and Extinguishing N2O-C2H2 flame 4-70
4.8 Igniting and Extinguishing the Flame 4-67
AA-6800/6650
4.8.5 4.9 4.9.1 4.9.2 4.10
Flame Conditions When Analizing Organic Solvent Samples 4-73 Setting the "Edit Preparation Parametrs" Dialog Box 4-75 Measurement Procedures on MRT work sheet 4-77
Standard Addition Method and Simple Standard Addition Method 4-74
Conditions and Operation for Flame Emission Analysis 4-79
4.10.1 "Optics Parameters" Page 4-79 4.10.2 "Atomizer/Gas Flow Rate Setup" Page 4-81 4.10.2.1 AA-6800 4-81 4.10.2.2 AA-6650 4-83 4.10.3 4.11 4.11.1 4.11.2 Line Search and Beam Balance 4-85 Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height (AA-6800) 4-86
4
Basic Operation
Setting the Optimum Condition of Burner Height 4-86 Setting the Optimum Condition of Fuel Gas Flow Rate 4-87
AA-6800/6650
4.1
Switching On the Power and Starting Up the Software
4.1.1
Switching ON the Power to Hardware
(1) Verify that installation has been correctly completed. (2) When using the ASC-6100 or GFA-6500, set the ASC-6100 power switch (Figure 4.1) or the GFA6500 100V power switch (Figure 4.2-) to the ON position ( "" position). (3) Set the power switch of AA-6800/6650 main unit (Fig 4.3) to the ON position ( "" position). If the fuel gas is not supplied, a buzzer sounds. Press the "BUZZER OFF" button on the gas controller panel or supply the fuel gas to stop the buzzer. In addition, after 2 minutes, a buzzer sounds 3 times to indicate that the initialization of the CPU in AA main unit has been completed. (4) The GFA 100V power (CONTROL) is accessed via the AA main unit power supply, so unless the furnace measurement is not to be used for a long period, this switch can be left in the ON position ("" position). On the other hand, the GFA 200V power switch lever (HEAT) should normally be left in the
4
Basic Operation
down (OFF) position, and set it to the ON position when starting the furnace measurement (The "200V" is different according to the region. It may be 200V, 220V, 230V or 240V).
Power switch Figure 4.1 Power Switch of ASC-6100
4-1 AA-6800/6650
4.1 Switching On the Power and Starting Up the Software
4
Basic Operation
4-2 AA-6800/6650
100V Power swicth (CONTROL) 200V Power switch (HEAT) Figure 4.2 Power Switch of GFA-6500
Power switch Figure 4.3 Power Switch of AA-6800/6650
4.1.2 Starting Up the Software

Switch ON the personal computer to start up the MS-Windows. Doubleclick on the icon of AA Software. The "Wizard Selection" dialog box (Fig 4.4) will appear at the center of the screen.
4.2
Software Basic Operation
With the AA software, after starting up the software, you can set the necessary settings for the measurement just by following the instructions sequentially displayed on the screen (Wizard function). In this section, the easy operation using this Wizard function is described for each of flame and furnace methods in regular sequence. Refer to Chapter 5 for details of each items.
4.2.1 Software Basic Operation (Flame Method)

4.2.1.1 Operation Flowchart (Flame Method) This Wizard has a sequence for setting as shown below. You can proceed to the next step or return to the preceding step by using the <Next> or <Back> button, respectively. (Starting up the AA Software) Wizard Selection Element Selection Preparation Parameters Sample ID Sample Selection Connect to Instrument/Send Parameters Optics Parameters Atomizer/Gas Flow Rate Setup (Finish) (Start Measurement) NOTE When measuring plural elements, you cannot set parameters for the elements other than the current measurement one on the "Optics Parameters" and "Atomizer/Gas Flow Rate Setup" pages. If you use the ASC to measure plural elements automatically and you need to modify the parameters for other elements than the current measurement one, you can change these parameters by using the <Edit Parameters> button in the "Element Selection" page.
4
Basic Operation
4-3
AA-6800/6650
4.2 Software Basic Operation
4.2.1.2 Wizard Selection
4
Basic Operation
appear. 4.2.1.3 Element Selection
Figure 4.4 "Wizard Selection" Dialog Box

When the "Wizard Selection" dialog box appears, if you make a new parameter set, select the Element Selection icon on the Wizard sheet and click on the <OK>. Then the "Element Selection" page will
Figure 4.5 Element SelectionPage 4-4 AA-6800/6650
(1) First, click on the <Select Elements>. Then the "Load Parameters" will appear.
4
Basic Operation
Figure 4.6 "Cookbook" Page in "Load Parameters"

(2) In this page, select the element first. You can use one of the methods below to select the element. (a) Enter the element symbol directly in the element field from the keyboard. (b) Click on the button at the right of the element field, and select the element from the element symbol list shown in alphabetical order. (c) Click on <Periodic Table> button and select the element from the periodic table. (3) Next, select [Flame] for the measurement method by the radio button. (4) Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when the SR method is used as the background correction method). (5) When using the autosampler, click on [Uisng ASC] check box. (6) After completing the settings, click on <OK>. At this time, a message about lamp setup is displayed. Press <No> button here. The lamp setup is also possible later. Then the "Element Selection" page is displayed again and the selected element is shown in the table. (7) When plural elements are to be analyzed, return to this "Element Selection" page once and then click on <Select Elements> button again to select the next element. Repeat the procedure below as required. Click on <Select Elements> button Select an element Click on <OK> button (8) When returning to the Element Selection page after selecting an element, the selected element is added to the list one by one. If you need to delete any of them, click on the row to highlight it and then click on <Delete>. The [Meas. Element] at the right lower of the page indicates the element to be analyzed first. (9) For details on <Edit Parameters> button, refer to the section 5.6 in Chapter 5. Here, you can go ahead without using it.
4-5 AA-6800/6650
(10) Click on <Next> button. Although another message appears, go ahead by clicking on <Cancel> button. Then "Preparation Parameters" page will appear. NOTES When analyzing plural elements sequentially, the order on the "Element Selection" page becomes the measurement order. If you need to change the order, click on the element to highlight it and then click on <Up> or <Down> to move the row. If the [Meas. element] at the right lower of the page is different from the first row element, the measurement is started from the [Meas.
4
Basic Operation
4-6 AA-6800/6650
Element] and the elements upper than it are not to be measured. When analyzing plural elements sequentially, it is necessary to set the socket numbers in alternating odd/even. To set or change the socket number, select the [Instrument]-[Lamp Position Setup] from the Menu. For details, refer to the section 5.8.4. Also, the "Lamp Position Setup" can be opened if you press the <Lamp Pos. Setup> in the "Optics Parameters" page opened by clicking <Yes> in the warning message shown at the time of element selection.
4.2.1.4 Preparation Parameters
Figure 4.7
"Preparation Parameters" Page
First, select the row of the element to be set by clicking on its row to highlight it, then click on <Edit> button. The "Preparation Parameters" page will appear. Set the parameters as below.
4
Basic Operation
Figure 4.8
"Edit Preparation Parameters" Page
(1) Select "Calibration Curve" for [Measurement Type]. If you need to select "SMSA"(Simple Standard Addition Method) or use Standard Addition Method, refer to the section 4.9. (2) Select "1st" for [Order] of equation if the calibration curve is straight. You may also select "2nd" or "3rd" if it is curved. Anyway, you can change the order after measurement. So, select "1st" here. Loading and saving of preparation parameter files are not available. (3) Pressing <Repeat Conditions> button displays the "Repeat Measurement Conditions" page. The number of measurements for the same one sample is set here. The default value of the number of measurement repetitions is "1" in the case of flame measurement. (4) Select [Conc. Unit] of the prepared standard samples. Click on button to select it from the list. (5) Input the [Weight Correction Factors]. These factors are necessary for calculating the actual concentration. The [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] are used in the following equation.
4-7 AA-6800/6650
Actual concentration =(Conc.)[Volume Factor][Dilution Factor][Correction Factor]/[Weight Factor] The actual concentration is calculated with the above equation. Note that the unit is not converted automatically. Convert the unit using [Correction Factor] if necessary (Refer to the example below). If the above calculation for actual concentration is not necessary, leave all the factors as "1" . Each factor is expressed in MRT work sheet and data print as follows. [Volume Factor] [Dilution Factor] [VF] [DF] [CF] [WF]
4
Basic Operation
4-8
[Correction Factor] [Weight Factor] (Example)
2g of sample was weighted, filled with water to 50ml, diluted to 5 times and measured. In this case, the actual concentration is calculated with the following equation using the factors; [Weight Factor]: 2(g), [Volume Factor]: 50(mL), [Dilution Factor]: 5(times) and [Correction Factor]: 1. Actual conc. = (Conc.) (50mL) (5 times) 1 (2g) Also, if calculating the actual conc.(%) from the conc.(ppm) by converting the unit, use 0.0001 for [Correction Factor] since 1ppm is 0.0001%. Actual conc.(%) = (Conc.(ppm)) (50mL) (5 times) 0.0001 (2g) (Note) Generally, "ppm" is the concentration unit of 10-6. In the atomic absorption analysis, "ppm" indicates both "g/g" for solid samples and "g/mL (mg/L)" for liquid samples. (6) Enter the [Number of STD]. Then a table composed of as many rows as the sample number is created in the [STD samples] preparation parameters. (7) Input the actual concentrations of the prepared standards into the table, although the default values from the cookbook are indicated on the table. When using the ASC, also input the turntable positions (1 to 60, R1 to R8). (8) [Blank Samples] Set up the periodic blank measurement here. Periodic Blank Measurement is a function to create a measurement procedure on the MRT to remove the influence of baseline drift by inserting a blank measurement in a fixed interval. Use it when the sample number is large or the baseline drift occurs. When the [Periodic Blank] is not used Leave the [Periodic Blank] field "Off" . When the [Periodic Blank] is used Click on the [Periodic Blank] field and click on the button at the right of "Off" . Then the list
AA-6800/6650
for "On" / "Off" is displayed. Select "On" . Click on the [Meas. Interval] field and enter the numerical value to insert the blank measurement in every some samples. [Pos.] indicates the blank position on the ASC turn table. When using the ASC, click on the button at the right of [Pos.] and select the position from the list. NOTE In the case of flame analysis, the fields for mixing parameters (sample volume, diluent, 1st reagent, etc.) are not displayed on the dialog box. Loading and saving of preparation parameter files are not available. (9) After setting the parameters, click on <OK> to return to the "Preparation Parameters" page. In the
4
Basic Operation
case of multi-element analysis, click on the next row to highlight it, then click on <Edit> and set the parameters in the same way. (10) When completing all the settings, click on <Next>. Then the "Sample ID" page will appear. 4.2.1.5 Sample ID
Figure 4.9 "Sample ID" Page

(1) In this "Sample ID" page, enter the number of samples first. Then enter the sample ID (sample name) into the cell of [Sample ID] from the keyboard one by one. (2) When using the same name with successive No. for all the samples, click on <Collective Setup>. Then the "Sample ID Collective Setup" dialog box will appear.
4-9 AA-6800/6650
4
Basic Operation
not required. (5) After completing the settings, click on <Next>. Then the "Sample Selection" page will appear.
Figure 4.10 "Sample ID Collective Setup" Dialog Box

Put a check mark in the "Create Sample ID" check box, and enter a common sample name to [Name]. Then names with successive number are automatically created and shown in the table (e.g. Sample001, Sample002,...). Entering the first sample position in [ASC Start Pos.] sets the sample positions of the second and after in the table automatically. Click on <OK> to return to the "Sample ID" page. (3) You can input and change the name individually after the collective setup. (4) The [Pos.] in the table shows the sample position on ASC turntable. When not using the ASC, this is
4-10 AA-6800/6650
4.2.1.6 Sample Selection
4
Basic Operation
Figure 4.11 "Sample Selection" Page

In this Sample Selection page, the samples to be measured for each element are selected. When all the samples are to be measured for all elements Confirm that each field has a check mark and click on <Next> to proceed to the "Connect to Instrument/Send Parameters" page. When some of the samples are not to be measured for all elements (1) Click the check box of the sample not to be measured to clear it. To clear some check boxes together, drag the mouse cursor to select the range, and press the DEL key on the keyboard or select "Not Measure" by clicking the right mouse button. (2) After completing the settings, click on <Next> to proceed to the "Connect to Instrument/Send Parameters" page.
4-11 AA-6800/6650
4.2.1.7
Connect to Instrument/Send Parameters
4
Basic Operation
4-12 AA-6800/6650
Figure 4.12 "Connect to Instrument/Send Parameters" Page

Check that the power of the AA is already ON and click on <Connect/Send Parameters>. The "Initialize" dialog box is opened and AA main unit is initialized. At the step of [Start Leak Check], the following message appears. "Gas leak check will be started. Press the EXTINGUISH button on the instrument." According to this instruction, press the EXTINGUISH button on the right side of the combustion chamber and click on <OK> to close the message. The instrument automatically starts the gas leak check for 10 minutes. During this time, a flame cannot be ignited. If the fuel gas is not supplied, the following message appears. "Gas pressure was too low to execute gas leak check. Please check that the fuel gas supply pressure and perform the gas leak check." Supply the fuel gas and press the EXTINGUISH button then click on <Retry>. On the other hand, when you ignore the message and click on <Cancel>, the message box is closed and the initialization is finished without executing the gas leak check. If the gas leak check is not executed at the time of initialization, the instrument starts the 10-minute gas leak check automatically when the fuel gas is supplied. And after the 10 minutes, if a gas leak was not detected, you can ignite a flame.
NOTE
If the EXTINGUISH button is not pressed according to the message, the gas leak check may not be executed correctly. It may judge that a gas leak is detected even if the instrument is working properly. When supplying the fuel gas after the initialization, this does not occur.
After completing the initialization, click on <OK> to close the "Initialize" dialog box. Then, click on <Next> in the "Connect to Instrument/Send Parameters" page to proceed to the "Optics Parameters" page. 4.2.1.8 Optics Parameters
4
Basic Operation
Figure 4.13 "Optics Parameters" Page

The wavelength, slit width, socket number, lamp current and lamp mode for the element to be firstly analyzed are set here. Note that these settings are only for the element to be firstly analyzed (the element that was specified in [Measurement Element] at the right lower on the "Element Selection" page or "Connect to Instrument/Send Parameters" page). (1) For the [Wavelength] and [Slit Width], you usually need not to change the value since the appropriate set values in the cookbook for each element are indicated. If you want to change them specially, enter the numeric value for wavelength and select a slit width from 6 levels on the list that is displayed by clicking on the button.
4-13 AA-6800/6650
(2) Click on <Lamp Pos. Setup> button. Then "Lamp Position Setup" diaolg box will appear. Enter the "Element" and "Lamp Type" of the lamp actually mounted for each socket number. Select the element from the drop-down list. Select "Normal" or "SR" for "Lamp Type" from the drop-down list. Then select lamp ID in [Lamp ID] field. You can turn lamp turret manually and change lamp while the "Lamp Position Setup" dialog box is displayed. Click on <OK> to return to the "Optics Parameters" page.
4
Basic Operation
Figure 4.14 "Lamp Position Setup" Dialog Box
(3) In the [Socket #] field, set the socket number where the lamp of the selected element is set. If the same element lamps are set in two or more positions of the lamp turret, click on the button and select the socket # from the drop-down list. (4) In the [Lamp Mode], the appropriate mode according to the selected element and lamp is indicated, so you need not to change it for most cases. If you want to change it specially, click on the button and select the mode from the drop-down list. (5) In the [Lamp ID], the currently used lamp ID (set at the time of lamp history data registration) is displayed. (6) In the [Lamp Status], a necessary message, for example, "Line Search is necessary" is indicated. (7) Putting a check mark in the check box of [Lamp ON] lights on the lamp. (8) In the [Lamp Current], the lamp current according to the selected element and lamp type is indicated, so you need not to change it for most cases. In the case of normal lamp, the numeric value is shown in the [Low] and "0" is in the [High]. The lamp current changed here is actually set on the unit at the following timings. when the extinguished lamp is lit on. when Line Search/Beam Balance is executed in the case of main lighting lamp. when <Warmup Lamp> in the "Optics Parameters" page of the main lighting element is clicked then <Apply> is clicked in the "Select Warmup Lamp" dialog box in the case of warmup lamp.
4-14 AA-6800/6650
(9) <Warmup Lamp> button This is used to warm up the lamp of the next element to be analyzed after the current element. For details, refer to the section 5.5.6.2. (10) <Line Search> button If the <Line Search> is clicked on, the "Line Search/Beam Balance" dialog box appears. When the Line Search/Beam Balance is necessary, it is automatically executed. If the Line Search/Beam Balance has already finished, the result is displayed.
4
Basic Operation
Figure 4.15 "Line Search/Beam Balance" Dialog Box

When it is automatically executed, the line search (wavelength adjustment) is executed first, then the beam balance (gain adjustment for detector) is performed. If only the beam balance is necessary, only the beam balance is executed. After completed, click on <Close> to return to the "Optics Parameters" page. (11) After all the settings are completed, click on <Next> to proceed to the "Atomizer/Gas Flow Rate Setup" page. NOTE When measuring plural elements, you cannot set parameters for the elements other than the current measurement one on the "Optics Parameters" and "Atomizer/Gas Flow Rate Setup" pages. If you use the ASC to measure plural elements automatically and you need to modify the parameters for other elements than the current measurement one, you can change these parameters by using the <Edit Parameters> button in the "Element Selection" page.
4-15 AA-6800/6650
4.2.1.9 Atomizer/Gas Flow Rate Setup (AA-6800)
4
Basic Operation
Figure 4.16 "Atomizer/Gas Flow Rate Setup" Page (AA-6800)
In the "Atomizer/Gas Flow Rate Setup" page, the burner position and fuel gas flow rate are set. Select the operation object [Atomizer Position] or [Fuel Gas Flow Rate] by clicking on the radio button to switch the page display. You can set either of them first.
4-16 AA-6800/6650
When the [Fuel Gas Flow Rate] is selected (1) You can set the flame type and the fuel gas flow rate here. (2) In the [Flame Type] field, an suitable flame type is indicated according to the element. If you need to change it, click on the button and select the flame type from the list. Note that you must not use N2O-C2H2 flame with the provided standard burner head. The high temperature burner head of special accessory is required. (3) In the [Fuel Gas Flow Rate], an appropriate value is indicated according to the element. If you need to change it specially, enter the numeric value then click on <Flame Setup> button. (4) You can also increase or decrease the fuel gas flow rate by using the flame set buttons <Increase> or <Decrease> at the lower of the page. In this case, the set value in the [Fuel Gas Flow Rate] also changes accordingly.
4
Basic Operation
(5) The <Gas Flow Auto> is used to set the optimum fuel gas flow rate by measuring sample actually. For the procedure of <Gas Flow Auto>, refer to the section 4.11.2. When the [Atomizer Position] is selected (1) Leave the [Burner Angle] as "0" for an usual use. Change it only when you want to decrease the sensitivity by changing the angle for high concentration samples. (2) For the [Burner Height], an appropriate value is indicated according to the element, so you need not to change it for usual use. However, the optimum condition may differ depending on the gas flow rate or sample type. In that case, change it by entering the numeric value then clicking on <Set Position>. (3) You can also move the burner position upward or downward by clicking on the position setup buttons <Up> or <Down> at the lower of the page. In this case, the set value in the [Burner height] also changes accordingly. (4) The <Burner Position Auto> is used to set the optimum burner height condition by measuring sample actually. For the procedure of <Burner Position Auto>, refer to the section 4.11.1. After all the settings are completed, click on <Finish> button. The Wizard ends and the main window appears. If you want to save the set conditions as a template file, proceed to the section 4.2.3. If you want to start the measurement, proceed to the section 4.3.1.
4-17 AA-6800/6650
4.2.1.10 Atomizer/Gas Flow Rate Setup (AA-6650)
4
Basic Operation
Figure 4.17 "Atomizer/Gas Flow Rate Setup" Page (AA-6650)
In the "Atomizer/Gas Flow Rate Setup" page, the burner position and fuel gas flow rate are set. Select the operation object [Atomizer Position] or [Fuel Gas Flow Rate] by clicking on the radio button to switch the page display. You can set either of them first.
4-18 AA-6800/6650
When the [Fuel Gas Flow Rate] is selected (1) You can set the flame type and the fuel gas flow rate here. (2) In the [Flame Type] field, an suitable flame type is indicated according to the element. If you need to change it, click on the button and select the flame type from the list. Note that you must not use N2O-C2H2 flame with the provided standard burner head. The high temperature burner head of special accessory is required. (3) In the [Fuel Gas Flow Rate], an appropriate value is indicated according to the element. If you need to change it specially, enter the numeric value then click on <Flame Setup> button. (4) You can also increase or decrease the fuel gas flow rate by using the flame set buttons <Increase> or <Decrease> at the lower of the page. In this case, the set value in the [Fuel Gas Flow Rate] also changes accordingly.
4
Basic Operation
When the [Atomizer Position] is selected (1) The [Burner Height] indicates an appropriate value according to the element. Set the burner height using the knob for adjusting burner vertical position. The [Burner Height] indicates the distance from the optical axis down to the burner head using a positive value. The knob for adjusting burner vertical position is protruded on the lower part of the atomizer and labeled with "VERTICAL". The burner height can be read with a scale on the atomizer base unit (Fig.3.5 in the Section 3.1.4.2). The optimum condition of the burner height may be different from the standard parameter depending on the gas flow rate and sample type. In such cases, change the burner height while spraying the sample, and obtain the burner height with which the real time data profile shows a high and stable sensitivity. The knob labeled with "HORIZONTAL" on the upper surface of the atomizer lower unit is used to adjust the forward-back position of the burner. Usually, it is not necessary to change the horizontal position after adjusting it at the time of changing the atomizer (from graphite furnace to burner). Do not touch this knob if not necessary. (2) Leave the [Burner Angle] as "0" for a usual use. Change it only when you want to decrease the sensitivity by changing the angle for high concentration samples. After all the settings are completed, click on <Finish> button. The Wizard ends and the main window appears. If you want to save the set conditions as a template file, proceed to the section 4.2.3. If you want to start the measurement, proceed to the section 4.3.1.
4-19 AA-6800/6650
4.2.2 Software Basic Operation (Furnace Method)

4.2.2.1 Operation flowchart (Furnace method)
This Wizard has a sequence for setting as shown below. You can proceed to the next step or return to the preceding step by using the <Next> or <Back> button. (Starting up the AA Software) Wizard Selection Element Selection Preparation Parameters Sample ID Sample Selection Connect to Instrument/Send Parameters Optics Parameters Furnace Program (Finish) (Start Measurement)
4
Basic Operation
4-20
NOTE
When measuring plural elements, you cannot set parameters for the elements other than the current measurement one on the Optics Parameters and Furnace Program page. If you use the ASC to measure plural elements automatically and you need to change the parameters for other elements than the current measurement one, you can change these parameters by using the <Edit Parameters> button in theElement Selectionpage.
AA-6800/6650
4.2.2.2 Wizard Selection
4
Basic Operation
Figure 4.18 "Wizard Selection" Dialog Box

When the "Wizard Selection" dialog box appears, if you make a new parameter set, select the Element Selection icon on the Wizard sheet and click on <OK> button. Then the "Element Selection" page will appear. 4.2.2.3 Element Selection
Figure 4.19 "Element Selection" Page 4-21 AA-6800/6650
(1) First, click on <Select Elements> button. Then the "Load Parameters" sheet will appear.
4
Basic Operation
Figure 4.20 "Cookbook" Page in "Load Parameters" Sheet
(2) In this page, select the element first. You can use one of the methods below to select the element. (a) Enter the element symbol directly in the element field from the keyboard. (b) Click on the button at the right of the element field, and select the element from the element symbol list shown in alphabetical order. (c) Click on <Periodic Table> and select the element from the periodic table. (3) Next, select [Furnace] for the measurement method by clicking on the radio button. (4) Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when the SR method is used as the background correction method). (5) When using the autosampler, click on the [Using ASC] check box. (6) After completing the settings, click on <OK> to return to the "Element Selection" page (Figure 4.19). At this time, a message about lamp setup is displayed. Press <No> button here. The lamp setup is also possible later. The selected element is shown in the table on the page. (7) When plural elements are to be analyzed, return to this Element Selection page once and then click on <Select Elements> again to select the next element. Repeat the procedure below as required. Click on <Select Elements> Select the element Click on <OK> button (8) When returning to the "Element Selection" page after selecting an element, the selected elements are listed one by one. In the automatic measurement using the ASC, the measurement is executed in this order. To change the order of automatic measurement, click on and highlight the row whose order is to be changed first, then click on the button <Up> or <Down> at the right on the screen to move the row. To delete any of the elements, click on and highlight the row then click on the <Delete> button.
4-22 AA-6800/6650
(9) The [Meas. Element] at the right lower of the page indicates the element to be analyzed first. In the case of ASC automatic measurement, the measurement is started from the [Meas. Element] and the elements upper than it in the table are not to be measured. (10) When analyzing plural elements sequentially with the ASC, it is necessary to set the socket numbers in alternating odd/even. Follow the procedure below to set or change the socket number. Click on <Edit Parameters>. Click on "Optics Parameters" tab. Click on <Lamp Pos. Setup> to display the "Lamp Position Setup" dialog box. Enter [Element], [Lamp Type] and [Lamp ID] for each socket # and click on <OK> to close the "Lamp Position Setup" dialog box. These settings are saved, and also used when the software is
4
Basic Operation
started next time. When changing the lamp position in the lamp turret, set the parameters again in "Lamp Position Setup" dialog box. Click on the button in [Socket #] on the "Optics Parameters" page and select an appropriate number from the list. Click on <OK> to return to the Element Selection page. You may also set the socket number by using the [Instrument]-[Lamp Position Setup] in the Menu bar beforehand. Then the socket numbers are automatically indicated in the table in the "Element Selection" page. You can adjust the odd/even order by moving the row on the table or change lamp position again by using the <Lamp Pos. Setup> if necessary. (11) When measuring plural elements continuously by using the ASC, the default values according to each element are used as the parameters of "Optics Parameters" and "Furnace Program" for the elements other than the [Meas. Element] at the right lower of the Element Selection page. If you need to change them, follow the procedure below. Click on <Edit Parameters>. Click on "Optics Parameters" tab or "Furnace Program" tab. Set necessary items. For details on setup contents, refer to the section 5.5.6 or 5.5.9. Click on <OK> to return to the Element Selection page. (12) After completing all the settings, click on <Next>. The Preparation Parameters page will appear.
4-23 AA-6800/6650
4.2.2.4 Preparation Parameters
4
Basic Operation
Figure 4.21 "Preparation Parameters" Page
First, click on the element row to highlight it, then click on <Edit>. The "Preparation Parameters" page will appear. Set the parameters as below.
4-24 AA-6800/6650
4
Basic Operation
Figure 4.22 "Edit Preparation Parameters" Dialog Box

(1) Mixing Setup, Repeat Measurement Conditions, Reagent Setup, Coating and Boost Cycle If you want to mix the sample and reagents, put a check mark in the [Mixing ON] check box. Then click on <Mixing> to open the "Mixing Setup" dialog box.
Figure 4.23 "Mixing Setup" Dialog Box

In this step, set the [Volume] in [Injection Parameters]. The default value is 20(L). Leave other items in the "Mixing Setup" dialog box as the default values. Also, leave all the items in the "Reagent Setup" dialog box opened by clicking on <Reagent>, in the "Coating and Boost Cycles" opened by clicking on <Coating>, and in the "Repeat Measurement Conditions" opened by clicking on <Repeat Conditions>.
4-25 AA-6800/6650
4.2
Software Basic Operation
(2) Calibration Curve Parameters Select "Calibration Curve" for [Measurement Type]. If you need to select "SMSA"(Simple Standard Addition Method) or use Standard Addition Method, refer to the section 4.9. Select "1st" for [Order] of equation if the calibration curve is straight. You may also select "2nd" or "3rd" if it is curved. Anyway, you can change the order after measurement. So, select "1st" here. [Zero Intercept] is used to make a calibration curve equation that forcibly intercepts the origin. This setting can also be changed later. Select [Conc. Unit] of the prepared standard samples. Click on the button to select it from the
4
Basic Operation
4-26
list. (3) [STD Samples] Preparation Parameters Input the [Number of STD]. Then a table composed of as many rows as the sample number is created in the [STD Samples] preparation parameters table. Keyin the actual concentrations of the prepared standards in the table, although the default values from the cookbook are indicated on the table. Also, set the preparation parameters as below. When the standard samples are not prepared by using the ASC Clear a check mark of the [Mixing ON]. In this case, mixing is not performed and the [Total Vol] becomes the volume to be injected into the graphite tube. Enter the sample injection volume into the graphite tube in the [Standard] (You cannot input a value in the [Total Vol] directly). Leave all the [Diluent], [Reagent 1], [Reagent 2] and [Reagent 3] as 0. Then [Total Vol] becomes equal to [Standard]. Don't use a value larger than 100L for [Total Vol]. 20L is acceptable as an injection volume for usual measurements. When only sample is injected (all of the diluent and reagent parameters are set to "0" ), the instrument automatically judges that no mixing should be performed, even if the [Mixing ON] is checkmarked. When the standard samples are prepared by using the ASC Input each field of the [Diluent], [Reagent 1], [Reagent 2] and [Reagent 3]. Then the [Total Vol] will be automatically calculated. The following example shows a case in which the standard sample is diluted to make each concentration for calibration curve by using the ASC preparation function. NOTE The [Total Volume] must satisfy the following condition. When the mixing is performed (Injection Vol.)(Max. No. of Reps.)(No. of Boost Cycles)50L(Total Vol.) 600L The (Injection Vol.) is the value set in theMixing Setup dialog box, and the50Lis the dead volume of the mixing port. If furnace boost cycle is not performed, (No. of Boost Cycles) is 1. When the mixing is not performed (Injection Vol.) = (Total Vol.) 100L
AA-6800/6650
(EXAMPLE) 200L of 10ppb, 20ppb and 30ppb standard samples are prepared from the 100ppb standard sample solution. The 100ppb standard sample is regarded as the "Sample" here and the parameters are set as below. The total volume is automatically calculated. [Conc.] 10 20 30 [Pos.] 1 1 1 [Standard] 20 40 60 [Diluent] 180 160 140 [Reagent 1] 0 0 0 [Reagent 2] 0 0 0 [Reagent 3] 0 0 0 [Total Vol] 200 200 200
4
Basic Operation
If the "Sample Injection Volume" (set in the "Mixing Setup" dialog box or the "ASC Parameters" page) is "20L" and the "Max. Number of Repetition" (set in the "Repeat Measurement Conditions" dialog box) is "5 times" and furnace boost cycle is not performed (this means [Number of Boost Cycles] in "Coating and Boost Cycles" dialog box is "1"), the calculation for toatl volume condition is as follows: (20L) (5 times) (1 cycle) 50L 200L 600L This indicates that the settings are correct. (4) Weight Correction Factors Input the [Weight Correction Factors]. These factors are necessary for calculating the actual concentration. The [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factors] are used in the following equation. Actual concentration = (Conc.)[Volume Factor][Dilution Factor][Correction Factor] / [Weight Factor] The actual concentration is calculated with the above equation. Note that the unit is not converted automatically. Convert the unit using the [Correction Factor] factor if necessary (Refer to the example below). If the above calculation for actual concentration is not necessary, leave all the factors "1" . When the "Auto Dilution and Remeasurement" was performed, the dilution ratio used for the automatic dilution by the ASC is displayed in the [ASC DF] (ASC Dilution Factor) on the MRT work sheet, and the actual concentration is calculated as below. Actual concentration = (Conc.)[Volume Factor][Dilution Factor][ASC Dilution Fctor] [Correction Factor] / [Weight Factor] Each factor is expressed in MRT work sheet and data print as follows. [Volume Factor] [Dilution Factor] [ASC Dilution Fctor] [Correction Factor] [Weight Factor] [VF] [DF] [ASC DF] [CF] [WF]
4-27 AA-6800/6650
(EXAMPLE) If the reagents and diluent are added to 50L of the sample and filled up to 250L. The actual concentration is calculated from the measured [Conc.] with the factors; [Weight Factor]: 50 L, [Volume Factor]: 250L and [Correction Factor]: 1. From the above equation , Actual concentration = (Conc.) 250L 1 150L In the same example, if calculating the actual conc.(ppm) from the conc.(ppb) by converting the unit, use 0.001 for CF since 1ppb is 0.001ppm.
4
Basic Operation
4-28
Actual concentration ppm = (Conc. ppb) 250L 1 0.00150L If the actual concentration calculation is not necessary, set all the factors to "1". (5) [Unknown Samples] Preparation Parameters When the sample mixing is not performed by using the ASC Clear a check mark from the [Mixing ON]. In this case, the mixing is not performed and the [Total Vol] becomes the volume to be injected into the graphite tube. Enter the sample injection volume into the graphite tube in [Sample] (You cannot input a value in the [Total Vol] directly). Leave all the [Diluent], [Reagent 1], [Reagent 2] and [Reagent 3] as 0. The [Total Vol] becomes equal to the [Sample]. Don't use the value larger than 100L for [Total Vol]. 20L is acceptable as an injection volume for usual measurements. When only the sample is injected (all of the diluent and reagent parametes are set to "0"), the instrument automatically judges that no mixing should be performed, even if the mixing is set to "ON". When the sample mixing is performed by using the ASC Input each of the [Diluent], [Reagent 1], [Reagent 2] and [Reagent 3] (the unit is "L"). Then the [Total Vol] will be automatically calculated. The [Total Vol] must satisfy the following condition. When the mixing is performed (Injection Volume)(Max. No. of Reps.)(No. of Boost Cycles)50L(Total Volume)600L The (Injection Volume) is the value set in the "Mixing Setup" dialog box, and the "50L" is the dead volume of the mixing port. If furnace boost cycle is not performed, (No. of Boost Cycles) is 1. When the mixing is not performed (Injection Volume) = (Total Volume) 100L When the [Mixing ON] is checkmarked, the injection volume is set in the "Mixing Setup" dialog box (Figure 4.23).
AA-6800/6650
(6) [Blank Samples] Preparation Parameters Set up the periodic blank measurement here. The Periodic Blank Measurement is a function to create a measurement procedure on the MRT. to remove the influence of baseline drift by inserting a blank measurement in a fixed interval. When the [Periodic Blank] is not used Leave the [Periodic Blank] field "Off". When the [Periodic Blank] is used Click on [Periodic Blank] and click on the button at the right of "Off" to display the list for selecting "On" or "Off". Click on "On". Click on [Meas. Interval] and enter the numerical value to insert the blank measurement in
4
Basic Operation
every some samples. If "1" is entered, the sample and blank are measured alternately. [Pos.] indicates the blank position on the ASC turn table. Select the position from the list. Set the preparation parameters for blank sample in the same procedure as that for [Unknown Samples] preparation parameters. (7) After setting the parameters, click on <OK> to return to the "Preparation Parameters" page. In the case of multi-element analysis, click on the next row to highlight it, then click on <Edit> and set the parameters in the same way. (8) Loading/Saving the Preparation Parameters The standard samples preparation parameters, the unknown samples preparation parameters and the blank samples preparation parameters can be saved in a file together and used again for setting other element parameters. Press <Save> button and specify the file name and the place to save it. In a preparation parameter file(*.mix), the following parameters are saved together; Parameters (A) (B) (C) (D) Measurement Type (Calibration Curve Method or SMSA) Mixing ON/OFF Preparation Parameters (STD, Unknown, Blank) Reagent Name Reagent Position Intake Order (E) Coating and Boost Cycles Coating and Boost Cycles Dialog Box Reagent Setup Dialog Box Edit Preparation Parameters Dialog Box Edit Preparation Parameters Dialog Box Screens Edit Preparation Parameters Dialog Box
A file which was created under different conditions((A)Measurement Type and (B)Mixing ON/OFF) from the current setting cannot be loaded. (9) When completing all the settings, click on <Next>. Then the "Sample ID" page will appear.
4-29 AA-6800/6650
4.2.2.5 Sample ID
4
Basic Operation
4-30 AA-6800/6650

(1) In this "Sample ID" page, enter the sample number first. Then keyin the sample ID (sample name) in [Sample ID] one by one. (2) When using the same name with successive No. for all the samples, click on <Collective Setup> button. Then the "Sample ID Collective Setup" dialog box will appear.

Click the "Create Sample ID" check box to select it, and enter a common sample name in [Name]. Then names with successive number are automatically created and shown in the table (e.g. Sample001, Sample002, ). Entering the first sample position in [ASC Start Pos.] sets the sample positions of the second and after in the table automatically. Click on <OK> to return the "Sample ID" page. (3) You can input and change the name individually after the collective setup. (4) After completing the settings, click on <Next>. Then the "Sample Selection" page will appear.
4.2.2.6 Sample Selection
4
Basic Operation
Figure 4.26
"Sample Selection" Page
In this "Sample Selection" page, the samples to be measured for each element are selected. When all the samples are to be measured for all elements Confirm that each cell has a check mark and click on <Next> to proceed to "Instrument Connection/Send Parameters" page. When some of the samples are not to be measured for all elements (1) Click the check box of the sample that is not to be measured to clear it. To clear some check boxes together, drag the mouse cursor to select the range, and press the DEL key on the keyboard or select "Not Measure" by clicking the right mouse button. (2) After completing the settings, click on <Next> to proceed to "Connect to Instrument/Send Parameters" page.
4-31 AA-6800/6650
4.2.2.7 Connect to Instrument/Send Parameters
4
Basic Operation
Figure 4.27 "Connect to Instrument/Send Parameters" Page
After checking that the power switches of the AA main unit and peripheral equipments are already turned ON, click on <Connect/Send Parameters>. The "Initialize" dialog box is opened and the AA main unit is initialized. After completing the initialization, click on <OK> to close the "Initialize" dialog box. Then, click on <Next> in the "Connect to Instrument/Send Parameters" page to proceed to "Optics Parameters" page.
4-32 AA-6800/6650
4.2.2.8 Optics Parameters
4
Basic Operation

The wavelength, slit width, socket number, lamp current and lamp mode for the element to be firstly analyzed are set here. Note that these settings are only for the element to be firstly analyzed (the element that was specified in [Meas. Element] at the right lower on the "Element Selection" page or "Connect to Instrument/Send Parameters" page). (1) For the [Wavelength] and [Slit Width], you usually need not to change the value since the default values which are appropriate for each element are indicated. If you want to change them specially, enter the numeric value for wavelength and select a slit width from 6 levels from the list that is displayed by clicking on the button. (2) Click on <Lamp Pos. Setup> button. Then "Lamp Position Setup" dialog box will appear. Enter the "Element" and "Type" of the lamp actually mounted for each socket number. Select the element from the drop-down list. Select "Normal Lamp" or "SR Lamp" for "Lamp Type" from the drop-down list. Then select lamp ID in [Lamp ID] field. Click on <OK> to return to the "Optics Parameters" page. While "Lamp Position Setup" dialog box is displayed, you can turn the lamp turret manually and change the lamp.
4-33 AA-6800/6650
4
Basic Operation
4-34 AA-6800/6650

(3) In the [Socket #] field, set the socket number where the lamp of the selected element is set. If the same element lamps are set in two or more positions of the lamp turret, click on the button and select the socket # from the drop-down list. (4) In the [Lamp Mode], the appropriate mode according to the selected element and lamp type is indicated, so you need not to change it for most cases. If you want to change it specially, click on the button and select the mode from the drop-down list. (5) In the [Lamp ID], the lamp ID currently used (set at the time of lamp history data registration) is displayed. (6) In the [Lamp Status], a necessary message, for example, "Line Search is necessary" is indicated. (7) Putting a check mark in the check box of [Lamp ON] lights on the lamp. (8) In the [Lamp Current], the lamp current according to the selected element and lamp type is indicated, so you need not to change it for most cases. In the case of normal lamp, the numeric value is shown in the [Low] and "0" is in the [High]. The lamp current changed here is actually set on the unit at the following timings. when the extinguished lamp is lit on. when Line Search/Beam Balance is executed in the case of main lighting lamp. when <Warmup Lamp> in the "Optics Parameters" page of the main lighting element is clicked then <Apply> is clicked in the "Select Warmup Lamp" dialog box in the case of warmup lamp.
(9) <Warmup Lamp> button This is used to warm up the lamp of the next element to be analyzed after the current element. For details, refer to the section 5.5.6.2. (10) <Line Search> button If the <Line Search> is clicked on, the "Line Search/Beam Balance" dialog box appears. When the Line Search/Beam Balance is necessary, it is automatically executed. If the Line Search/Beam Balance has already finished, the result is displayed.
4
Basic Operation
Figure 4.30 "Line Search/Beam Balance" Dialog Box

When it is automatically executed, the line search (wavelength adjustment) is executed first, then the beam balance (gain adjustment for detector) is performed. If only the beam balance is necessary, only the beam balance is executed. After completed, click on <Close> to return to the "Optics Parameters" page. (11) After all the settings are completed, click on <Next> to proceed to the "Furnace Program" page. NOTE When measuring plural elements, you cannot set parameters for the elements other than the current measurement one on the Optics Parameters and Furnace Program page. If you use the ASC to measure plural elements automatically and you need to change the parameters for other elements than the current measurement one, you can change these parametrs by using the <Edit Parameters> button in theElement Selectionpage.
4-35 AA-6800/6650
4.2.2.9 Furnace Program
4
Basic Operation
Figure 4.31 "Furnace Program" Page
(1) Set the furnace program here. A default furnace program is automatically indicated in the table according to the selected element, so you may use it as it is. Make any changes to this program as required. (EXAMPLE) The default furnace program has the following basic steps. Table 4.1
STAGE# 1 2 3 4 5 6 7
Example of Furnace Program

Temp () 150 250 800 800 800 2300 2500 Time (sec) 20 10 10 10 3 2 2 Heat Mode Sensitivity RAMP RAMP RAMP STEP STEP STEP STEP GAS Type #1 #1 #1 #1 #1 #1 #1 Flow Rate (L/min) 0.1 0.1 1.0 1.0 0.0 0.0 1.0
The above furnace program is explained as below.
4-36 AA-6800/6650
In this program, water is vaporized and the sample is "Dried" at the stage #1, and coexisting organic substances are "Ashed" from the stage #2 to #5, then the target element is "Atomized" at stage #6. The stage #7 is a "Cleaning" stage to eliminate the residue in the graphite tube. For the "Ashing" stage, change the [Temp.] and [Time] according to the contained coexsisting substances (For example, if much amount of organic compounds are contained, set the [Temp.] higher and the [Time] longer). Set [Heat Mode] to "RAMP" (the temperature is increased gradually) during "Drying" stage and at the beginning of "Ashing" stage, and set it to "STEP" (heated directly to the set temperature) during "Ashing" and "Atomizing" stages. In the [Sensitivity] column, the "Atomizing" stage and its preceding stage are checkmarked to perform a high sensitivity measurement. At this time the inner gas is fixed to 0 (L/min).
4
Basic Operation
The [Sampling Stage No.] indicates a stage for data sampling. Usually, the atomizing stage is selected. The [Gas Type] is set to #1 for all the stages when a usual measurement is peformed. (2) When changing/creating a furnace program, you can save it so that you can use the same program next time. <Save> To save the furnace program, click on <Save> and enter the file name on the "Save As" dialog box. The extension for furnace program is ".fur" (For example, "copper.fur" ). Then click on <Save>. <Load> To open the furnace program file, click on <Load>. The "Open" dialog box will appear. Then click on the file name to be opened and click on <Open>. (3) When editing a ready-made furnace program, use the <Insert Row> or <Delete Rows> buttons to insert a row or delete rows. (4) The <Cleanig> button is used to heat the graphite tube to a high temperature for cleaning. Also, the <Test Meas.> button is used to perform the test measurement actually using the set furnace program. For details, refer to the section 5.5.9.2 and 5.5.9.3. (5) For details of the <Coating/Boost Cycle> <Change Graphite Tube> and <Temp. Search>, refer to 5.5.9.1, 5.5.9.4 and 5.5.9.5, resepectively. (6) After completing all the settings, click on <Finish>. The Wizard finishes and the main window will appear.
4-37 AA-6800/6650
4.2.3 Saving the Template

If you want to use the parameters set with the above procedures from the next time, you can save them as a template. Then you can load it in the "Wizard Selection" dialog box. (1) Click on [File] in the menu bar and select [Save As].
4
Basic Operation
Figure 4.32 "Save As" Dialog Box
(2) Select "template (*.taa)" for [Save as type]. The extension of the file name displayed in [File name] is changed to ".taa"."Save As" dialog box is closed and the template file is saved."Save As" dialog box is closed and the template file is saved."Save As" dialog box is closed and the template file is saved."Save As" dialog box is closed and the template file is saved."Save As" dialog box is closed and the template file is saved. (e.g.) If "notitle.aa" is displayed in [File name] when t he "Save As" dialog box is opened, selecting "template (*.taa)" changes the file name to "notitle.taa". (3) (4) Input the file name. Leave the extension as ".taa". (e.g.) Change the part "notitle" in the "notitle.taa" to a name you like. Press <Save> button. "Save As" dialog box is closed and the template file is saved.
4-38 AA-6800/6650
4.3
Measurement Procedures
After completing all the settings, prepare the samples. Perform the measurement following the procedure indicated on the MRT work sheet. The current row is highlighted and its [Action] field shows the type of measurement. When using the ASC, set the samples in proper positions. If no setting is made on the MRT work sheet, a message appears to indicate that no schedule exists. In this case, select [Parameters]-[Schedule Creation Wizard] from the menu and set the measurement procedures. NOTE If a menu or dialog box is kept opened during the measurement operation, the measurement operation may be interrupted. Be careful about it when checking the setup parameters during the operation.
4
Basic Operation
4.3.1 Measurement Operation (for Flame Method)

In the case of flame method, read the section "4.8 Igniting and Extinguishing the Flame" thoroughly before starting the measurement. Confirm that the gases are supplied at correct pressures and the burner head is mounted properly. Note that the ignition cannot be made for 10 minutes after the automatic gas leak check is started. If the lamp warmup time (unit:minute) is set, wait to start the measurement during the time after lighting on the lamp. Manual Measurement (1) Igniting the Flame Press the IGNITE button on the front of the AA main unit to ignite the flame. (2) Auto Zero At the [AUTO ZERO] row on the MRT work sheet, put the suction nozzle into vaporized water (or solvent) and spray it. When the signal of real time graph is stabilized, click on <START> at the bottom of the Main window (or press the F5/F6 key). Also, the Auto Zero can be executed by pressing <AUTO ZERO> (or F3 key), although the operation result of Auto Zero execution is not indicated on the MRT worksheet in this case. (3) Blank Measurement (if necessary) Spray the blank sample and click on <BLANK> at the bottom of the Main window (or press the F4 key). The "BLANK" row is inserted on the MRT work sheet and the measurement result is displayed. When the "BLANK" row is prepared on the MRT worksheet beforehand, press <START> (or F5/F6 key). If the standard or unknown samples are measured after executing the blank measurement, their measured values (absorbance or energy) are indicated after the measured blank value is subtracted from their actual measured values. The difference between this measured blank value and the actual measured standard or unknown sample value is displayed in [Abs] ( or [Energy]) on the MRT until the next blank measurement is executed.
4-39 AA-6800/6650
4.3 Measurement Procedures
(4) Standard Measurement Spray the standard sample. When the signal of real time graph is stabilized, click on <START> at the bottom of the Main window (or press the F5 or F6 key) according to the set order. Measure the standard sample while checking that it accords with the current row on the window. If the repeat measurement is selected, clicking on <START> inserts a new row for repeat measurement according to the set repeat parameters. Repeat the measurement following the row indication. (5) Checking the Calibration Curve After measuring the standard samples, check the calibration curve displayed on the right upper of
4
Basic Operation
4-40
the window. If the calibration curve graph display is too small, set the mouse cursor onto the border of the calibration curve graph to indicate an arrow with two directions. Drag it to specify the range ("drag" means moving the mouse while holding down the left mouse button). If the calibration curve is correctly made, proceed to the measurement of unknown samples. If you want to change the order or other parameters for calibration curve, click on <Type> above the calibration curve graph then make a change on the "Change Calibration Curve Condition" dialog box. (6) Unknown Sample Measurement Spray the unknown sample. When the signal of real time graph is stabilized, click on <START> at the bottom of the Main window (or press the F5 or F6 key). If the repeat measurement is selected, clicking on <START> inserts a new row for repeat measurement according to the set repeat parameters. Repeat the measurement following the row indication. Then continue to measure the unknown samples according to the specified order. Measure an unknown sample while checking that it accords with the current row on the window. If <START> key is pressed when all the rows on the MRT work sheet have been executed, a new "UNK" row (unknown sample row) is added and its measurement result is displayed. When the "Periodic Blank" is ON, "BLK" rows (blank measurement) are inserted in the specified interval. Spray the blank and measure it at the rows. If you want to make the size of MRT (Measurement Result Table) work sheet larger, set the mouse cursor onto the upper border of the table to indicate an arrow with two directions. Press down the mouse left button and drag it to specify the range. More number of rows can be displayed. For details on changing sizes or using a scroll bar, refer to the WindowsTM documentation. (7) Finishing the Measurement After finishing the measurement, put the suction nozzle in vaporized water and spray it for a while. Then press the EXTINGUISH button on the front of the AA main unit to extinguish the flame. Using the ASC NOTE When using the ASC, put a check mark in the check box of [Using ASC] in Sequencepage ofEdit Parameters.
AA-6800/6650
When using the ASC, verify that the position of each actual sample on the ASC turn table accords with the setting on the MRT work sheet. (1) Igniting the Flame Press the IGNITE buttons on the front of the AA main unit to ignite the flame. (2) Starting the ASC (Auto Sample Changer) Click on <START> at the bottom of the Main window (or press the F5 or F6 key) according to the set order. The automatic measurement is started with the ASC. (3) Extinguishing the Flame After finishing the measurement, press the EXTINGUISH button on the front of the AA main unit to extinguish the flame (A flame is automatically extinguished if the automatic flame extinction is selected). (4) Checking the MRT work sheet Check the measured results on the MRT work sheet. If a remeasurement is necessary, refer to the section 4.7.2. When printing or saving the data, proceed to the section 4.4.
4
Basic Operation
4.3.2 Measurement Operation (for Furnace Method)

(1) Mount the graphite tube correctly. (2) Verify that the argon gas is supplied at the specified pressure, and flow the cooling water. (3) Verify that the power switches on the rear of GFA-6500, both of the 100V switch (CONTROL) and 200V switch (HEAT), are set to ON. (4) Verify that the nozzle position adjustment is correctly completed. For details on the ASC nozzle position adjustment, refer to 5.8.16. Using the ASC When using the ASC, verify that the position of each actual sample on the ASC turn table accords with the setting on the MRT work sheet. (1) Starting the ASC (Auto Sample Changer) Click on <START> at the bottom of the Main window (or press the F5 or F6 key) according to the specified order. The automatic measurement is started with the ASC. Before starting the measurement, the temperature calibration is executed. Note that heating is performed when the temperature calibration is executed. (2) When the last row of the MRT work sheet is finished, the instrument becomes in the waiting condition.
4-41 AA-6800/6650
(3) Checking the MRT work sheet Check the measured results on the MRT work sheet. If a remeasurement is necessary, refer to the section 4.7.2. When printing or saving the data, proceed to the section 4.4.
4
Basic Operation
4-42 AA-6800/6650
4.4
Saving/Printing/Deleting the Data
4.4.1 Saving the Data

When all measurements are completed, save the data. Select [File]-[Save As] from the menu bar, and enter the file name in the "Save As" dialog box. File extension is limited to ".aa". NOTE A measurement data whose repeat measurement has not finished is not saved in the file. If the data is necessary although the repeat measurement cannot be completed, print it out before ending the AA software.
4
4.4.2 Printing the Data
Basic Operation
Select [File]-[Print Data/Parameters] or [Print Table Data] from the menu bar. Then "Select Schedule" dialog box will appear. Click on the elements ( "Summary Report" is also available for [Print Table Data]) to highlight it. Then click on <OK>. Printing will be executed. [Print Data/Parameters] The measurement parameters and measured data are printed. You can select the items to be printed in the [File]-[Print Style]-[Print Style Setup] page. [Print Table Data] The current MRT work sheet is printed. You can select or change the items to be printed by selecting [File]-[Print Style...]-[Table Show/Hide] page from Menu. In the case of [Summary Report], the columns shown in the MRT work sheet on the window are printed. For details on printing, refer to the sections 5.2.9 to 5.2.12.
4.4.3 Deleting the Data

If you want to use the same measurement conditions again, you can delete only the data with leaving the measurement sequence. Execute [Edit]-[Clear Measurement Result] from the menu bar. When deleting all of the measurement parameters, measured data and measurement sequence, select [File]-[New] from the menu bar to open a new file.
4-43 AA-6800/6650
4.5
Completing the Measurement
(1) When the measurement is completed, verify that the flame is extinguished and tighten the main valve of the gas cylinder and compressor in the case of flame method. Close the main valves of the cooling water and gas in the case of furnace method. (2) Quit the software. For example, select [File]-[Exit] from the menu bar. The communication with the instrument is shut off first, then the main window is closed. It takes approximately 30 seconds. (3) Turn off the power switch of AA main unit.
4
(4) Turn off the power switches for peripheral equipments such as the ASC and GFA. When using the GFA-6500, be sure to turn off the 200V power switch.
Basic Operation
4-44 AA-6800/6650
4.6
Explanation of Main Window
When the Wizard is completed, the following main window appears. Menu bar Standard tool bar Measurement element tool bar (Display and switch the current measurement element) Absorbance digital display Real time graph (and temperature program graph) Peak profile (latest four measurements and overlay display) Calibration curve tool bar (Selection of calibration curve and type) Calibration curve display MRT work sheet Function buttons Status bar
4
Basic Operation
Figure 4.33 Main Window
4-45 AA-6800/6650
4.6 Explanation of Main Window
NOTE
While the [Properties] is opened from the right mouse button menu on the graph or MRT work sheet, the measurement is stopped. In this case, the measurement can be continued again when the [Properties] is closed.
4.6.1 Menu bar

Place the mouse cursor onto the menu ([File],[Edit],[Parameters],etc.) and click on it. Then a drop-down menu appears. Select an item from the menu and click on it. For details on each item, refer to Chapter 5.
4
Basic Operation
4-46
4.6.2 Standard tool bar

The items frequently used are displayed in the tool bar. Quick selection is possible if you use this instead of selecting from the menu bar. Each tool function is described below. New Open : All the data and parameters are cancelled and parameters are set newly. (Same as [File]-[New] in the menu bar) : A file already created is opened. (Same as [File]-[Open] in the menu bar) Save As : Current data and parameters are saved in the file. (Same as [File]-[Save As] in the menu bar) Print : Data and parameters are printed. (Same as [File]-[Print Data/Parameters] in the menu bar)
AA-6800/6650
4.6.3 Measurement element tool bar

The element currently measured (or to be measured) is indicated. If you want to change the element, click on the and select one from the drop-down list. Then the page proceeds from "Optics Parameters" to "Atomizer/Gas Flow Rate Setup" (for flame method) or "Furnace Program" (for furnace method). Set the parameters if necessary and click on <Finish> (or <Cancel> to close the sheet without changes). The MRT work sheet is also changed to that for selected element.
4.6.4 Absorbance digital display

The current absorbance value (or emission intensity in emission mode) is displayed. When the instrument is BUSY, it is highlighted.
4
Basic Operation
4.6.5 Real time graph (and furnace program graph)

The changing absorbance value (or emission intensity in the case of emission mode) under measurement is displayed in analog. You can check the peak shape and baseline conditions with this graph. In the case of furnace, "Furnace Program" is also displayed. The abscissa indicates time and the ordinate indicates absorbance (left scale) and temperature (right scale). Right mouse button menu If you want to change the scale or print the graph, place the cursor in the graph area and click on the right button of the mouse. Then the pop-up menu shown in Figure 4.34 appears. Select an item and make settings.
Figure 4.34 Right Mouse Button Menu (Real Time Graph)
4-47 AA-6800/6650
(1) [Properties] [Real Time Graph Scale] (Flame) You can change the graph ordinate and abscissa scale. Enter the maximum value and minimum value in [Ordinate Max] and [Ordinate Min], respectively. Enter a numeric value in [Time Interval] (unit:second) for abscissa. Clicking on <Reset> sets them to the values specified in [Parameters][Default Parameters]-[Graph]. [Scale] (Furnace) You can change the scales for [Absorbance], [Time] and [Temperature]. Enter the maximum value
4
Basic Operation
4-48
and minimum value in [Max] and [Min], respectively. Clicking on <Reset> sets the absorbance scale to the values specified in [Parameters]-[Default Parameters]-[Graph], and sets the time and temperature scales according to the furnace program. [Color] You can select colors of [Data Line], [BG Line], [Background] and [Grid] (also [Furnace Program] for furnace method). Click on the and select the color from the list. [Grid] You can select grids to be displayed from [Major & Minor Grid], [Major Grid] or [None]. You can also select the line type of [Major Grid Line] and [Minor Grid Line]. (2) [Copy] Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor or other application and move the cursor to the location where you want to paste the graph. Select [Paste] command in the wordprocessor, etc., and the graph will be displayed at the cursor position. (3) [Cross Hair] (Furnace) This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] in the right button menu. When the mouse cursor is in the graph area, the coordinate values at the cross hair intersection position are displayed. While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock] condition. (4) [Radar] The display range is automatically set so as to display the entire graph selected by the mouse cursor. (5) [Print] Selecting this opens the "Print" dialog box. Check the printer name, copies, etc. and click on <OK>. The real time waveform currently displayed will be printed.
AA-6800/6650
4.6.6 Peak Profile (Latest four measurements and overlay display)

The latest four measurement signal profiles are displayed. Both standard samples and unknown samples are displayed here. The abscissa shows time and the ordinate shows absorbance value (emission intensity in EMISSION mode). The signal profile is displayed during the integral time in the case of flame method, and during the prestage time and sampling time in the case of furnace method. In the rightmost area, plural number of signal profiles can be overlapped and displayed. Specify their colors in the [Graph] on the MRT work sheet. Right mouse button menu If you want to change the scale or print the graph, place the cursor in the graph area and click on the right button of the mouse. Then the pop-up menu shown in Figure 4.35 appears. Select an item and make settings.
4
Basic Operation
Figure 4.35 Right Mouse Button Menu (Peak Profile)

(1) [Properties] [Scale] You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales. The scale setting is used commonly for the five graph. Clicking on <Reset> sets the Y-axis to the value specified in [Parameters]-[Default Parameters]-[Graph]. [Color] You can select colors of [Data Line], [BG Line], [Background] and [Grid]. Click on the and select the color form the list. [Grid] You can select grids to be displayed from [Major & Minor Grid], [Major Grid] or [None]. You can also select the line type of [Major Grid Line] and [Minor Grid Line].
4-49 AA-6800/6650
(2) [Draw BG Line] Selecting this displays a profile of background signal. The display is deleted by selecting this menu again (The check mark of [Draw BG Line] is deleted). (3) [Copy] Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor or other application and move the cursor to the location where you want to paste the graph. Select [Paste] command in the wordprocessor, etc., and the graph will be displayed at the cursor
4
Basic Operation
4-50
position. (4) [Cross Hair] This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the coordinate values at the cross hair intersection position are displayed. The graph area is divided into five areas, and the coordinate values can be read only in each area. If you want to read an coordinate value in another graph, erase the cross hair cursor once by clicking the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted), then set the mouse cursor to another area and select [Cursor]-[Display] again. While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock] condition. (5) [Radar] This automatically sets the display range so that the selected graph by the mouse cursor is displayed in an appropriate size. At the same time, other four data scales are also chanegd to the same scale. (6) [Print] Move the mouse cursor to the graph area to be printed. Then the "Print" dialog box appears. Check the printer name, copies, etc. and click on <OK>. Only the selected peak profile will be printed.
AA-6800/6650
4.6.7 Calibration Curve Display After the standard samples are measured, the calibration curve is created and displayed. (1) Calibration Curve Display If you want to check a calibration curve other than the currently displayed one, set the <Latest> button to OFF (the button is embossed) and enter the element name and calibration curve number (C#). The settings here are limited to display and recalculation is not executed.
(2) Changing the Calibration Curve Conditions If you want to change the calibration curve parameters after viewing the created calibration curve, use the <Type> button. Clicking on <Type> opens the "Change Calibration Curve Condition" dialog box where you can change order of calibration curve and permission of zero intercept.
4
Basic Operation
Figure 4.36 "Change Calibration Curve Condition" Dialog Box

Changing the condition and clicking on <OK> immediately recalculates the concentration of unknown samples based on the new calibration curve and renews the quantitation result on the MRT work sheet. The recalculation is only applied to the unknown sample using the same C# as changed calibration curve. The result is invalid when the element is different, or when the C# is different even if the element is same. In the case of furnace method, whether the absorbance is obtained from the peak height or from the peak area is switched in this window. NOTE After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept and signal processing mode settings cannot be changed after the measurement. For details on QA/QC setup, refer to the section 5.6.9.
Symbols in Calibration Curve Equation When a calibration curve is created, calibration curve equation is displayed above the graph. Symbols in a calibration curve equation mean as follows;
4-51 AA-6800/6650
Symbol Abs E Conc r e ^ Absorbance Energy (Only for EMISSION mode) Concentration Correlation Coefficient
Meaning
When a coefficient is very small, this symbol is used to express it by using index. "AeB" means "A 10 B" This symbol means power. "Conc^2" means the second power of concentration.
4
Basic Operation
4-52
(Example) Calibration curve equation means equation . Abs = -9.5e-005Conc^2 + 0.011636Conc + 0 Abs = -9.5 10-5 Conc2 + 0.011636 Conc + 0 Right mouse button menu If you want to change the scale or print the graph, place the cursor in the graph area and click on the right button of the mouse. Then the pop-up menu shown in Figure 4.37 appears. Select an item and make settings.
Figure 4.37 Right Mouse Button Menu (Calibration Curve Display)

(1) [Properties] [Scale] You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales. Enter the values. [Options] You can set the graph color and data point shape. Clicking on each of [Data Point], [Calibration Curve], [Background] and [Grid] displays the list from which you can select the color. The shape of [Data Point] can be selected from the list displayed by clicking on the .
AA-6800/6650
[Grid] You can select grids to be displayed from [Major & Miner Grids], [Major Grid] or [None]. You can also select the line type of [Major Grid Line] and [Minor Grid Line]. (2) [Copy] Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor or other application and move the cursor to the location where you want to paste the graph. Select [Paste] command in the wordprocessor, etc., and the graph will be displayed at the cursor position. (3) [Cross Hair] This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the coordinate values at the cross hair intersection position are displayed. To erase the cross hair, select [Cross Hair]-[Display] (then the check mark of [Display] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock] condition. (4) [Radar] This automatically sets the display range so that the entire graph can be displayed. (5) [Print] Move the mouse cursor to the graph area to be printed. Then the "Print" dialog box appears. Check the printer name, copies, etc. and click on <OK>. Then the calibration curve currently displayed is printed out. This menu is not displayed when no calibration curve exists.
4
Basic Operation
4.6.8 MRT work sheet

It is possible to create measurement sequence, execute measurement, display the result, and calculate the actual concentration in the MRT work sheet. If measurement of plural elements is required, the work sheet is prepared for each element and the work sheets can be changed over with the tab. In [Summary], the measurement result for sample can be displayed at one time. The tab title consists of the element name and comment. As the comment, only the first line is displayed when a line feed is included in the comment, and the first ten characters are displayed when the number of characters exceeds ten. The comment is inputted by selecting [Parameters]-[Edit Parameters]-[Comment] page from the Menu bar. For details on each item in MRT work sheet, refer to the section 4.7. NOTE The currently measured element (or the element about to be measured) can be changed not by the tab at the left lower of the main window but by the measurement element tool bar.
4-53 AA-6800/6650
4.6.9 Function buttons

Functions of Wizard selection, auto zero execution, blank measurement, starting sample measurement, test measurement, ASC rinse are assigned to the buttons at the left below the MRT work sheet. These correspond to function keys on the keyboard as follows. <AUTO ZERO> button <BLANK> button <START> button <TEST MEAS.> button <RINSE> button : {F3} key : {F4} key : {F5, F6} keys This switches to <STOP> button during measurement. : {F9} key : {F10} key
The relations between the current measurement mode and the available buttons are shown below.
Basic Operation
"Auto (using ASC)" means the status where the ASC is connected and the [Using ASC] check box is checkmarked in [Parameters]-[Edit Parameters]-[Sequence] page from the Menu bar.
Flame Manual <AUTO ZERO> <BLANK> <START> <TEST MEAS.> <RINSE>
Flame Auto(using ASC)
Furnace Manual
Furnace Auto(using ASC)
Available
Not available
Clicking on <AUTO ZERO> button executes the Auto Zero while rinsing the nozzle in the case of flame auto-measurement (using ASC). In other cases, only the Auto Zero is executed. When clicking on <RINSE> button, the nozzle and mixing port (mixing port is rinsed only when Mixing is ON) are rinsed in the case of furnace measurement. In the case of flame measurement, nozzle rinse is executed. The nozzle rinse time in flame measurement is set in [Configuration] dialog box opened by selecting [Instrument]-[Configuration] from Menu. If the setting is "0" , 10 seconds rinse is executed regardless the setting. Clicking on <STOP> stops the measurement. However, while acquiring the data, the measurement is stopped after the data acquisition is finished.
4-54 AA-6800/6650
4.6.10 Status bar
Figure 4.38 Status Bar

The current measurement mode, operating mode, operating status of instrument, and connecting status of peripheral equipments (ASC, GFA) are indicated here. Displays current operating status of the instrument and error messages. Displays the hollow cathod lamp which is currently lit and its socket number. While the lamp is lit, the pane pops up. Displays the hollow cathod lamp which is under warming-up and its socket number. While the lamp is lit, the pane pops up. Displays whether the deuterium lamp is lit or not. When the lamp is lit on, the pane pops up. The "Lamp Status" dialog box can be displayed from the [Lamp Status] menu displayed by clicking the right mouse button in the regions of . Displays whether the ASC is connected. When it is connected, "ASC" is displayed. Displays whether the GFA is connected. When it is connected, "GFA:n" is displayed. The "n" indicates the heating number of the graphite tube. When the current measurement mode is furnace, "Change Graphite Tube" dialog box can be displayed from the [Change Graphite Tube] menu displayed by clicking the right mouse button in this region. When the gas leak check is executed at the time of initialization or by selecting [Instrument]-[Gas Leak Check] menu from the menu bar, the countdown before the gas leak check completion and its result are displayed. When the current measurement is furnace, however, they are not displayed. "Gas Controller Status" dialog box can be displayed from the [Gas Controller Status] menu displayed by clicking the right mouse button in this region. Displays the current connecting status of the instrument. OFF BUSY The communication between the instrument and the PC is off. The instrument is executing a command. While this is displayed, another command cannot be executed. READY The instrument is ready to execute commands or conduct measurement.
4
Basic Operation
4-55
AA-6800/6650
4.7
Operating the MRT work sheet
In the MRT (Measurement Result Table) work sheet, the functions of setting of measurement sequence, execution of measurement, result display, actual concentration calculation, and setting of ASC sample position are integrated. For example, if you create a calibration curve by measuring three standard samples and measure eight unknown samples, the measurement is proceeded in the following procedure. Row 1 to 3 : Executes measurement of standard samples.
Row 4 to 11 : Executes measurement of unknown samples (SAMPLE001 to SAMPLE008)
4
Basic Operation
4-56
As the measurement procedure, prepare the sample shown in the [Action] column and click on <START>. You can proceed the measurement in the order from top row to down. When a repeat measurement is set, rows for repetition are inserted at the time of measurement.
4.7.1 Fields of MRT work sheet

This section explains about the fields of MRT work sheet.
Figure 4.39 MRT work sheet

(1) [Action] Clicking on the cell in this field opens the drop-down list, showing the following indications. This [Action] field contains the measurement operations, operation using the ASC, QA/QC operation, etc.. For details on QA/QC, refer to the section 5.6.9. NOTE 1. Executing "FILESAVE" overwrites and saves the file even if the file of the same name exists. 2. When the path name is not set at all in [FILESAVE] or [FILEEXPORT], a path name is created based on the setting in [File]-[Auto Save]. When only the file name is set, the file is saved in the folder that was used in the last time for "Open" or "Save as" screen. 3. To enable the QA/QC actions, it is necessary to put a check mark in the check box of each QC type in "QA/QC Setup" page.
AA-6800/6650
4.7 Operating the MRT work sheet
4
Basic Operation
Figure 4.40 Drop-down List of [Action]

BLK : Specifies the blank sample measurement. The measured value of blank sample is subtracted from the measured values of standard samples and unknown samples until a new blank measurement is done. STD UNK CAL-CHK : Specifies the standard sample measurement by calibration curve method. : Specifies the unkown sample measurement by calibration curve method. : Specifies the evaluation of calibration curve after the standard sample measurement (The correlation coefficient is checked). This is usually inserted to the row just after the last "STD" . This setting is not necessary in the case of standard addition method or simple standard addition method because the evaluation is done at "MSA-RES" row. QC SPIKE : Specifies the measurement and evaluation by LCS (Laboratory Control Sample/Standard substance). : Specifies the measurement and evaluation by SPK (Pre-Digestion Spike/ addition and recovery check without pretreatment). This is usually inserted to the row just after the objective "UNK" . RESLOPE : Specifies the measurement for sensitivity correction (Usually, the standard sample of highest concentration is used). After this, "A,B,C..." is added to C# on the MRT and a new calibration curve number (C#) is created. MSA SMSA MSA-RES : Specifies the measurement by standard addition method. : Specifies the unkown sample measurement by simple standard addition method. : Specified as the result of standard addition method. When the measurement of a set of standard addition samples is finished, the calibration curve is created and the result is indicated in this row at the same time. AUTOZERO : Shifts the current displayed value to zero. In the case of flame measurement using the ASC, the Auto Zero can be executed while aspirating the sample. The aspirating time in second unit can be specified in [Sample ID] field (0 to 600 seconds).
4-57 AA-6800/6650
RINSE
: In the case of furnace measurement, the nozzle and mixing port are rinsed (mixing port is rinsed only when Mixing is ON). In the case of flame analysis, the nozzle is rinsed when the ASC is used. The rinse time (0 to 600 seconds) in second unit can be specified in [Sample ID] field.
CLEANING : Specifies cleaning of the graphite tube PAUSE WAIT : Specifies temporary stop until the <OK> is selected. Input a message to be displayed on the message box in the [Sample ID] field. : Specifies a stop in a fixed time. Input waiting time in the unit of second in the [Sample ID] field (07200 seconds). COMMAND : Specifies execution of command line. Specify the command to be executed in the [Sample ID] field. FILESAVE : Specifies the file saving of the data collected so far. Specify the file name in the [Sample ID] field. FILE EXPORT : Specifies the text file saving of the data collected so far on the MRT work sheet. Specify the file name in the [Sample ID] field. (2) [Sample ID] In normal operation, sample ID is entered in this field. Sample name can be entered only when [Action] field indicates measurement of standard sample or unknown sample (STD, UNK, BLK, QC, SPIKE, RESLOPE, MSA, SMSA and MSA-RES). When the [Action] is CAL-CHK, the sample name cannot be entered. When the Element Selection Wizard or Schedule Creation Wizard was executed, the sample name set in the "Sample ID" page is entered when [Action] is unknown sample. When the [Action] is standard sample, the name automatically given in the "Edit Preparation Parameters" dialog box (STD1, STD2,...) is entered. In the following six cases, the [Sample ID] has a special meaning. a) When "RINSE" is set in flame auto-measurement (using ASC), enter the aspiration time in second unit (0 600 seconds) in this [Sample ID] . b) When "PAUSE" is set, enter the message to be displayed on the message box in this [Sample ID]. c) When "WAIT" is set, enter the wait time of second unit in this [Sample ID] (07200 seconds). d) When "COMMAND" is set, describe the command line in this [Sample ID]. e) When "FILESAVE" is set, enter the file name together with path to save the data measured so far (e.g. C:\AA\WATER CU.aa). Use ".aa" for extension. f) When "FILEEXPOPRT" is set, enter the file name together with path. Then the data on the MRT work sheet data of the currently measured element is saved in a text file (e.g. C:\AA\WATER_CU.txt). Use ".txt" for extension. (3) [Graph] When overlaying the peak profiles, click on the right part of the cell and select the color of data lines from the list. The overlayed profiles are displayed on the rightmost of peak profile area. On the other hand, the BG lines are overlayed by the same one color.
4
Basic Operation
4-58
AA-6800/6650
(4) [X] (Exclusion) Doubleclicking this excludes the data in the row. Doubleclicking again enables the data to be recovered. (5) [M] (Modified) Rewriting the absorbance data after measurement displays M mark (Modified). Once rewritten, this check mark is always displayed and the original data cannot be recovered. Only absorbance can be written. (6) [Q] When the control standard which is set by selecting [Parameters] - [Edit Parameters] - [QA/QC Setup] page from the menu bar is applied to the row, a check mark is indicated. Marked data cannot be excluded or modified.
4
Basic Operation
For details on "QA/QC setup" page, refer to the section 5.6.9 (7) [True Value (and unit)] The set concentration (and unit) of standard samples is indicated. This can be entered only when the [Action] is STD, SPIKE, RESLOPE, QC or MSA. In the case of "SPIKE" , enter the added concentration. (8) [Conc. (and Unit)] Displays the result of concentration obtained with measurement. As the [True Value] column heading, the unit specified in the "Preparation Parameters" page is automatically displayed. (9) [Abs.] Displays the measured absorbance. Energy intensity is displayed instead in the case of EMISSION mode. If a blank measurement is executed prior to this, the value is indicated after the measured blank value is subtracted from the actual measured value. (10) [BG] For measurement in BGC-D2 or BGC-SR mode, absorbance of background signal is displayed. This is not displayed in the lamp modes in which the background signal is not acquired. When "Peak Height" is selected for signal processing mode in furnace measurement, this field indicates the background value at the time of acquisition of the absorbance signal peak. (11) [Pos.] Indicates the sample position in the turn table of the autosampler (ASC). For details, refer to the instruction manual provided with the ASC. (12) [VOL] [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] [Total Volume] These are sample and reagent volume values necessary for sample mixing using ASC in furnace measurement. The values set in [STD Samples] or [Unknown Samples] preparation parameters table in the "Edit Preparation Parameters" dialog box are displayed here. The header row of the [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] displays the settings in [Diluent/Reagent Name & Position] which are set in [Parameters]-[Edit Parameters]-[ASC Parameters] page from the Menu bar.
4-59 AA-6800/6650
(13) [WF] [VF] [DF] [ASC DF] [CF] Each acronym means as follows. [WF] [VF] [DF] [ASC DF] [CF] [Weight Factor] [Volume Factor] [Dilution Factor] [ASC Dilution Factor] [Correction Factor]
4
Basic Operation
4-60
These are factors necessary for actual concentration calculation. The factors set in [Weight Correction Factors] in the "Edit Preparation Parameters" dialog box are displayed. For details on the equation of actual concentration calculation, refer to the section 5.5.2.1. The [ASC DF] is displayed only in the case of furnace auto-measurement using ASC. The dilution factor of automatic dilution is displayed when the automatic dilution and remeasurement is performed. (14) [Actual Conc.] Indicates the result of actual concentration calculation. For the calculation, the factors of WF, VF, DF and CF are used. (15) [Actual Conc. Unit] Enter the unit used for actual concentration of the sample. Clicking on the right part of the cell opens the drop-down list from which the unit can be selected. Note that changing this unit does not recalculate the actual concentration. It is necessary to change the factors used for calculation. (16) [%RSD] [SD] [%R] The [%RSD] and [SD] are calculated in repeat measurement. The [%R] is calculated when "QC" or "SPIKE" is measured. For details on these calculation equations, refer to the section 5.6.2 and 5.6.9. (17) [C#] Indicates calibration curve number. When plural calibration curves are created on the same sheet, number is put in the order of creation and indicated. If entering a changed number, in the case of standard sample, a calibration curve is created by the standard samples of the same curve number and in the case of unknown sample, the concentration is calculated using the calibration curve of the entered number. This can be enterd when the [Action] is STD, UNK, CAL-CHK, QC, SPIKE, RESLOPE, MSA or SMSA. This number is also used when selecting the calibration curve to be displayed (refer to 4.6.7). (18) [Out of Control Remark] A Note is displayed when QA/QC function judges that the acquired data is out of standard range. (19) [Date] Displays the date when the data was obtained by measurement. (20) [Time] Displays the time when the data was obtained by measurement. In the case of repeat measurement, the time displayed in the average row is the time of the first measurement.
AA-6800/6650
4.7.2 Right Mouse Button Menu

Clicking on the right mouse button on the MRT work sheet opens the pop-up menu as below (Figure 4.41).
4
Basic Operation
Figure 4.41 Right Mouse Button Menu (MRT work sheet)

(1) [Properties] [Table Show/Hide] You can select to show or hide each column on the MRT work sheet. Only checkmarked items are displayed. Click on the item you don't want to show, and erase the check mark. The show/hide selection for each column has no relation to the print items in the [File]-[Print Table Data]. To select the items to be printed in Table Print, select [File]-[Print Style] from the menu and select the items in "Table Show/Hide" page. When the ASC is set not to be used in the [Parameters]-[Edit Parameters]-[Sequence], the items related to ASC such as [Pos.], [VOL], [Diluent], [Reagent 1], [Reagent 2], [Reagent 3], [Total Volume] and [ASC DF] are not shown or printed, even if these items are set to be shown or printed in the "Table Show/Hide" page.
Figure 4.42 Table Show/Hide (MRT work sheet) 4-61 AA-6800/6650
[Row Style] Font (character style, size, etc.), color and ruled line type can be set for each row group (row and column header, basic style, current row, measurement result row and excluded row).
4
Basic Operation
Figure 4.43 Row Style (MRT work sheet)
(2) [Hide Repetition] When this is selected in the case of repeat measurement, only the row of average value is shown and the rows of repeating process are not shown. The repetition rows are not printed in the "Print Table Data", either. While this is selectd, a check mark is indicated in the drop-down menu. (3) [Hide Excluded Row] When this is selected, a row with a check mark in its [X](excluded) field is not shown. The excluded rows are not printed in the "Print Table Data", either. (4) [Hide Blank] When this is selected, a row of blank measurement is not shown. The blank rows are not printed in the "Print Table Data", either. (5) [Hide Command Row] When this is selected, a row whose [Action] field is "Command" is not shown. The command rows are not printed in the "Print Table Data", either. (6) [Keep Meas. Row Visible] When this is selected, the MRT work sheet is automatically scrolled as the measurement proceeds so that the row under measurement may be always displayed.
4-62 AA-6800/6650
(7) [Add Successive No. to Meas.] Selecting this puts successive numbers to "UNK" and "SMSA" of [Action]. This setting also has an effect on "Print Table Data". (8) [Remeasure Selected Range] When excluding measured rows and remeasuring the sample, the operation is as follows. First, select rows to be remeasured by using the mouse (Click the first row and drag to the last row while pressing the button). In the case of repeat measurement, the selected range must include the average row. A row (or sample) that is already excluded cannot be remeasured. If remeasuring the excluded row is necessary, doubleclick the [X] field to recover it once. Click the right mouse button and select [Remeasure Selected Range] from the displayed menu. The remeasurement rows are added below the last measured row on the MRT work sheet. The rows
4
Basic Operation
in the selected range are marked in the [X] fields and excluded. (9) [Collective Edit] To change the factors and unit for actual concentration calculation together which are already set on the MRT work sheet, follow the procedure described below. Select the cell range to be changed by using the mouse (Click the first row to be changed and drag to the last row with pressing the button). Click the right mouse button and select the [Collective Edit] from the displayed menu. Then the "Collective Edit" dialog box appears. Put a check mark to the check box of each item to be changed. Enter a new setup value to the item with the check mark.
Figure 4.44 "Collective Edit" Dialog Box

(In the case of flame measurement, [Volume] and [Coating] are not displayed.)
When completed, click on <OK> to close the "Collective Edit" dialog box. Settings are changed and the actual concentration is recalculated simultaneously and the work sheet is renewed. In rows already measured, however, [Volume] and [Coating] cannot be editted.
4-63 AA-6800/6650
4.7.3 Right Mouse Button on Summary Table

Clicking on the right mouse button on the Summary table displays the pop-up menu where you can select Show/Hide of Absorbance, Concentration, Actual Concentration and Concentration Unit. This Show/Hide selection is also used for the "Print Table Data".
4.7.4 Inserting and Deleting the Measurement Row

Only the row that has not been measured can be inserted or deleted for measurement. To insert the row: (1) Click on the number of row position to be inserted (a new row is added above the row). (2) Select [Edit]-[Insert Row] from the menu bar.
4
Basic Operation
4-64
To delete the row: (1) Select the number of row (or the range of plural rows) to be deleted. (2) Select [Edit]-[Delete Rows] from the menu bar.
NOTE
Insertion and deletion of a row next to current measuring row can't be done during measurement.
4.7.5 Active Cell Movement by Shortcut Key and Cell Selection 4.7.5.1 Moving an Active Cell
Clicking a cell with the mouse pointer displays a bold frame around the cell. The cell in this status is called an active cell. However, all the cells cannot be activated. Some cells can be activated but some cannot be. The active cell can be moved through the following key input. Home This key moves the active cell to the leftmost cell that can be active in the current row. End This key moves the active cell to the rightmost cell that can be active in the current row. Ctrl+Home These key move the active cell to the leftmost cell that can be active in the first row unexecuted. Ctrl+End These key move the active cell to the rightmost cell that can be active in the last measurement row. Tab This key moves the active cell to the right. After moving to the rightmost cell, it moves to the leftmost cell in the next row below. It skips a cell that cannot be activated and moves to the next cell. Shift+Tab These keys move the active cell to the left. After moving to the leftmost cell, it moves to the rightmost
AA-6800/6650
cell in the upper row. It skips a cell that cannot be activated and moves to the next cell. 4.7.5.2 Selecting Cells Using the mouse can select contiguous plural cells as described below. Cell range Click the cell in the upper left corner of the region to be selected and drag to the cell in the lower right corner. Column When selecting a column, click the column header of the column to be selected. When selecting contiguous plural columns, drag along the column header. Row When selecting a row, click the row header of the row to be selected. When selecting contiguous plural rows, drag along the row header. Whole table Click the upper left cell of the header. Then all of the rows entered on the table are selected.
4
Basic Operation
4.7.6 Copy and Paste

Numeric values and characters on the MRT worksheet and summary table can be copied to the clipboard. Also, text data can be pasted from the clipboard only to the sample ID column in the MRT work sheet. 4.7.6.1 Copy Select an area on the table to be copied using the mouse and select [Edit]-[Copy] menu or press "Ctrl+C" key. Then the values in the selected area are copied to the clipboard. These copied values can be pasted as text data to the word processor or spreadsheet software. NOTES 1. The contents of column header and row header are not copied. 2. Graph column is never copied. 3. Hidden column is not copied. 4. Hidden row included in the selected area is always copied. 4.7.6.2 Paste Text data can be pasted from the clipboard to the sample ID column. [Copy & Paste of Sample ID between MRT work sheets] 1. Select a cell area of sample ID as the copy source and copy it to the clipboard by [Edit]-[Copy] menu or "Ctrl+C" key. If hidden rows are included in the selected area, the contents of the sample ID cells in the hidden rows are also copied. Therefore, set all the rows displayed and check the contents to be copied before executing the copy.
4-65 AA-6800/6650
2. Click the top cell of the sample ID cell area in the paste destination. Note that paste is not applied to the rows already measured or rows under repeat measurement. 3. Select [Edit]-[Paste] menu or press "Ctrl+V" key in this status. Then the sample ID is overwritten on the cells from the top cell to down. 4. When the number of sample ID in the copy source is over the number of rows in the paste destination, the excess are added as new rows. NOTE 1. If a value other than numeric value is pasted to the items for which time should be set in the sample ID field (WAIT, AUTO ZERO or RINSE at the use of ASC), it is reset to "0". Numeric values out of the acceptable entry range are also ignored. 2. If the paste is applied to the items for which nothing can be entered in sample ID field (CAL-CHK, etc.), it is ignored. 3. Also, sample IDs created using a word processor or spreadsheet software can be pasted to the MRT worksheet. When creating sample IDs using a word processor, insert a line feed between the sample IDs. Also, the sample ID must not contain the tab code.
4
Basic Operation
work sheet.
4.7.7 Changing Column Width and Column Header Height of MRT Worksheet
The column width for an arbitrary column and the column header height can be changed in the MRT
Procedure for setting the column width (1) Position the mouse cursor on the column border line in the column header. The mouse shape changes to a two-direction arrow. (2) While the mouse cursor is in the two-direction arrow status, press the left mouse button down and drag to the right or left. The cell width of the column header is changed. (3) Release the left mouse button at the appropriate position. The column width is set at the position. Procedure for setting the column header height (1) Position the mouse cursor on the bottom line of the leftmost cell in the column header. The mouse shape changes to a two-direction arrow. (2) While the mouse cursor is in the two-direction arrow status, press the left mouse button down and drag upward or downward. The height of the leftmost cell is changed. (3) Release the left mouse button at the appropriate position. The column header height is set at the position.
4-66 AA-6800/6650
4.8
Igniting and Extinguishing the Flame
4.8.1 Operation Locations

Locations associated with igniting and extinguishing of the flame are described here. Firstly, the IGNITE buttons, EXTINGUISH button and BURNER SELECT switch are located on the front side of the AA main unit. In addition, operation panel of gas controller is located at the rear of the right side of AA main unit.
4.8.2 Safety Precautions Prior to Ignition

(1) Switch ON the power for the fan of the room exhaust duct. (2) Verify that the gas to be used is appropriate and that the gas pressure is set correctly. Gas type Supply pressure Setting pressure Air, N2O, Ar 0.35 MPa 0.25 MPa C2H2, H2 0.09 MPa 0.05 MPa
4
Basic Operation
Supply pressure" is a value indicated by the pressure regulator in the analysis room and "Setting pressure" is a value indicated by the pressure gauge in the gas controller panel of the AA main unit. (3) Confirm that the drain tank is filled with water. (4) Verify that there are no leaks in any of the gas lines (Refer to section 6.3). (5) Verify that the flame and burner head to be used are appropriately matched.
Table 4.2 Type of Burner Heads and Usable Flames Standard burner head High temperature burner head (optional)
Slot length Usable flame 10cm Air-acetylene Air-hydrogen Argon-hydrogen 5cm Air-acetylene Air-hydrogen Argon-hydrogen Nitrous oxide-acetylene CAUTIONS Before igniting a flame, check that the ignition buttons work properly. <Checking procedure> 1. Referring to section 4.1, turn on the power of the instrument. 2. Referring to section 4.2.1.7, initialize the instrument and wait until the 10minute gas leak check step after the initialization has finished. 3. Perform Element Selection Wizard of AA software or open a flame measurement file to set the instrument to flame measurement mode. 4. Press only the upper button (black) of the two buttons. When the ignition is not executed, it is normal. 5. Next, press only the lower button (white). When the ignition is not executed, it is normal. 6. If the above step 4 or 5 should ignite a flame, the switch system is broken. Stop using the instrument immediately.
4-67 AA-6800/6650
4.8 Igniting and Extingushing the Flame
NOTE
4
Basic Operation
4-68
If the power is turned on and the fuel gas is supplied at the time ofConnect to Instrument, a gas leak check is automatically conducted for 10 minutes. During this time, the flame cannot be ignited. On theInitializedialog box, press the EXTINGUISH button at the time of [Start Leak Check]. The fuel gas will be filled inside the pipe of the gas controller by this action. If the EXTINGUISH button is not pressed, buzzer can sound within 10 minutes even if there is no gas leak. If the buzzer sounds within 10 minutes after starting the gas leak check, stop using the instrument immediately and perform an inspection (Pressing the BUZZER OFF button in the gas controller to turn off the buzzer). In case that a gas leakage is detected, a buzzer sounds immediately after the gas leakage check is started. The time of 10 minutes is set as a sufficient value for safety, and there is no problem when a buzzer sounds after 10 minutes or later. Pressing the PURGE button during the gas leak check will purge the gas from the gas lines and cancel the gas leak check. To next perform the gas leak check, execute the [Instrument]-[Gas Leak Check] from the menu. However, if the PURGE button is pressed within 10 minutes after turning on the power and the gas leak check is to be performed again, press the EXTINGUISH button. When the PURGE button is pressed, an error message indicating that fuel gas pressure is too low may be displayed. This message, however, may be ignored.
4.8.3 Igniting and Extinguishing Air-C2H2, Air(Ar)-H2 flames

(1) Set the fuel gas flow rate in a range listed below. To set the fuel gas flow rate, click on the radio button of [Fuel Gas Flow Rate] on the "Atomizer/Gas Flow Rate Setup" page and enter a numeric value in [Fuel Gas Flow Rate] and clickon <Flame Setup> button. You can also use <Increase> or <Decrease> buttons. Acetylene gas Hydrogen gas 2.0 - 3.0 (L/min) at least 4.0 (L/min)
(2) Keep the PURGE button pressed, check the support gas (Air) flow rate and adjust it by using the support gas flow rate control knob so that the scale may indicate 8.0. CAUTION The support gas flow meter indicates both the scale for air and the scale for N2O. Read the proper scale when adjusting the support gas flow rate. Read the flow rate at the center of the ball. (3) In the case of Ar-H2 flame, it is necessary to invalidate the flame monitor safety device. Since the flame is colorless, the sensor cannot detect it and stops the gas supply. In the cases other than Ar-H2 flame, however, be sure to validate the flame monitor safety device. (When the instrument is initialized, the flame monitor safety device is always valid.)
AA-6800/6650
To invalidate the flame monitor safety device, select [Instrument]-[Gas Controller Status] menu to display "Gas Controller Status" dialog box and clear [Flame Monitor ON] check box. CAUTION When the [Flame Monitor ON] check box is cleared, the flame monitor safety device doesn't operate. Therefore, stay near the instrument and always check that the flame doesn't go out. If the flame should go out, press the EXTINGUISH button. (4) Press two IGNITE buttons at the same time. The pilot flame is ignited first, then the burner head is flamed. Keep pressing the IGNITE buttons until the flame is completely ignited. If the flame is not ignited even if the buttons are pressed for three seconds or more, stop igniting
4
Basic Operation
operation once, and retry after ten seconds or more. When the ignition has failed, the AA software may display an error message like "Flame has been extinguished". When such a message is displayed, the AA main unit is locked so that the ignition cannot be done. To release this lock, close all the error messages displayed on the software. (5) Set the fuel gas flow rate and support gas pressure and flow rate if necessary. (6) To extinguish the flame, press the EXTINGUISH button. NOTE 1. If the gas pressure decreases while the flame is burning, the flame is automatically extinguished. In that case, check the gas supply pressure before igniting the flame again. 2. If a momentar y AC supply power outage should occur, the flame is automatically extinguished. 3. In the following cases, an error message stating that the fuel gas pressure is too low will be displayed, but this message can be ignored. When the PURGE button is pressed When the flame out safety device is activated becasue the flame is extinguished due to an obvious reason (such as wind blowing out the flame, etc.). When the automatic measurement by ASC is completed and the flame is automatically extinguished according to the setup. When there is a momentary AC power outage. 4. After the error message of too low fuel gas pressure is displayed, the pilot flame is not ignited by pressing the IGNITE button even if the instrument condition is set ready for ignition. In this case, once press the EXTINGUISH button then press the IGNITE button. 5. If ignition is attempted when the support gas is not being supplied, or when the support gas pressure is low, the ignition spark is generated but the flame is not ignited (At this time, as the safety mechanism functions, the fuel gas does not flow through the burner slot). However, in this case, a low pressure error
4-69 AA-6800/6650
message will not be displayed. Therefore, if an error message will not be displayed in spite of impossible ignition, check the support gas pressure. 6. When the following error messages are displayed on the AA software, the AA main unit is locked so that the ignition cannot be done. To release this lock, solve the problems in the instrument settings then close all the error messages displayed on the software. While the error message is displayed, the ignition cannot be done. -Fuel gas leak detected. -Fuel gas pressure is too low. -Support gas pressure is too low. -Flame has been extinguished. -Drain tank water level is too low. -Momentary electric shutdown occurred in the gas controller. Forcibly support gas type is changed to Air and flame monitor is set to ON. 7. If the flame should not be extinguished even by pressing the EXTINGUISH button, do not panic and take action of following operation. Turn off the main unit POWER switch (on the left side of the main unit). This operation mechanically closes the solenoid valve of the gas controller, shutting off the gas supply safely. Close the gas main valve. Contact your service representative immediately. Do not operate the instrument until the repair by service person completes.
4
Basic Operation
4-70 AA-6800/6650
4.8.4 Igniting and Extinguishing N2O-C2H2 flame

(1) Take off the standard burner head (slot length 10cm) and mount the high temperature burner head (slot length 5cm) supplied as an optional accessory. (2) On the "Atomizer/Gas Flow Rate Setup" page, click on [Fuel Gas Flow Rate] radio button. Select "N2O-C2H2" for [Flame Type] and enter the flow rate (8.0 L/min) in the [Fuel Gas Flow Rate]. Also, the flow rate can be changed by the <Increase> and <Decrease> buttons. (3) Insert the burner recognizing key connected to the high temperature burner head with a wire into the hole of the BURNER SELECT switch. (4) Press two IGNITE buttons at the same time to ignite the flame. First, the Air-C2H2 flame will be ignited. Keep pressing the IGNITE buttons until the flame is completely ignited. If the flame is not ignited even if the buttons are pressed for three seconds or more, stop igniting operation once, and retry after ten seconds or more. When the ignition has failed, the AA software may display an error message like "Flame has been extinguished". When such a message is displayed, the AA main unit is locked so that the ignition cannot be done. To release this lock, close all the error messages displayed on the software. Approx. 10 seconds after the flame ignition is achieved, the C2H2 flow rate is automatically increased 5.0L/min and the flame emission intensity is increased. Then the support gas is automatically switched
from Air to N2O, changing the Air-C2H2 flame to N2O-C2H2 flame. NOTE Even if the [Flame Type] is set to N2O-C2H2, the flame will not be switched unless the BURNER SELECT switch is set to N2O-C2H2 with a key attached to the high temperature burner head. In this case, if the BURNER SELECT switch is changed from the Air-C2H2 to the N2O-C2H2 position while the Air-C2H2 flame is combusting, the support gas is automatically switched from Air to N2O, changing the Air-C2H2 flame to N2O-C2H2 flame.
4
(5) To extinguish the flame, press the EXTINGUISH button. The support gas is automatically switched from N2O to Air, changing the N2O-C2H2 flame to Air-C2H2 flame. Then the flame is extinguished.
Basic Operation
CAUTIONS Always use high temperature burner head when using a nitrous oxideacetylene flame. Using the standard burner head with this gas causes a danger of flashback. When the acetylene flow rate is high, carbon is deposited around the burner slot. When this occurs, use the provided large screwdriver to scrap off the carbon deposit while taking care about the following points. Insert the screwdriver at the center on the burner slot while keeping the top portion of the screwdriver lengthwise. Don't close a large part of the burner slot by keeping the top portion of screwdriver horizontally. While keeping the top portion of screwdriver lengthwise, slide it from the center to the outside (right or left side) and scrap off the carbon deposit gently. To prevent the flame from going out, don't slide the screwdriver from the outside to the center. Insert it at the center again and scrap off to the outside. Be careful not to scratch the burner head and slot. Remove the carbon deposit inside the burner slot using a piece of hard paper, after the flame is extinguished and the burner is completely cooled.
Carbon deposit
High temperature burner head
Figure 4.45 Removing Carbon Deposit in N2O-C2H2 Flame 4-71 AA-6800/6650
When using a nitrous oxide-acetylene, decreasing the acetylene or increasing the nitrous oxide will cause the pink portion of the flame (red feather) to gradually decrease. If this decreases to less than 2mm, the flame will split, and if the acetylene flow is further reduced, a flashback may occur.
4
Basic Operation
CAUTION connected.
Blue
Pink (Red Feather) Dark blue
Figure 4.46 N2O-C2H2 Flame
In case of flashback, set the safety valve at the back of the chamber as it was if it is out of place. Also, remove the spray unit to check it and if the disperser is separated, mount it as it was. Check the tube from the drain outlet is firmly
4-72 AA-6800/6650
4.8.5 Flame Conditions When Analizing Organic Solvent Samples

Since an organic solvent itself will burn in the flame, the flame will not be completely combusted using the normal flame conditions, as the result, the measurement accuracy will be decreased. To perform an accurate measurement, it is necessary to decrease the sample spray amount as well as decrease the acetylene gas flow rate, compared with the aqueous solution. The procedure for setting the flame conditions when using organic solvent is as follows. (1) Replace the suction nozzle with the provided polyethylene capillary tube. (2) While solvent is being sprayed into the flame, decrease the acetylene gas flow rate so that the color of the flame is from blue or slightly red (in the case of air-acetylene flame). Next, while organic sample is being sprayed, try various acetylene flow rates and burner heights until the maximum S/N ratio (signal to noise ratio) is achieved. (3) Overly decreasing the acetylene flow may cause the flame to go out when spraying of the organic sample is stopped. In this situation, increase the acetylene gas flow rate in 0.1L/min increments until the flame no longer goes out at the end of spraying the organic solvent sample, and then adjust the flame condition by increasing the support gas flow rate. When using a nitrous oxide-acetylene flame, be sure that the red feather (red portion of the flame) is more than 2 - 3 mm. If a stable flame is not achieved after performing the above procedure, continue with the steps (4) to (6) outlined below, and then search for the optimal flame conditions using steps (2) to (3) again. (4) Return the acetylene flow rate to its normal value. (5) Rotate the support gas pressure adjusting knob so that the support gas pressure is in the range of 0.1 to 0.25 MPa, and decrease the amount of sample sprayed. (6) Increase the support gas flow rate by rotating the support gas flow adjusting knob to approach the flow rate used prior to decreasing the support gas pressure.
4
Basic Operation
4-73
AA-6800/6650
4.9
Standard Addition Method and Simple Standard Addition Method
The standard addition method is used when there is interference by coexistent material (matrix) in the sample and its influence is given to the measured value. For the standard addition method, equal volumes of unknown sample solution are prepared, and a standard solution of different but known concentration is added to each of the unknown sample solutions. The absorbance is measured for each of these samples, and a calibration curve is created. The unknown sample concentration is obtained from the point at which the extended calibration curve intersects with the horizontal axis.
Absorbance
4
Basic Operation
4-74 AA-6800/6650
Standard addition concent Concentration of unknown sample
Figure 4.47 Standard Addition Method

When the coexistent material or matrix of plural unknown samples are similar, measure one of them by standard addition method, and you can use the slope of the same calibration curve to determine the concentrations of other unknown samples. This is called simple standard addition method.
Sample concentartion by simple standard addition method
Figure 4.48 Simple Standard Addition Method

When using these methods, the absorbance of standard addition samples must be within the range that has linearity of calibration curve. To check whether the result is valid or not, refer to the coefficient of correlation.
Absorbance
4.9
4.9.1 Setting the "Edit Preparation Parametrs" Dialog Box

Note that parameters for "MSA (Method of Standard Addition)" cannot be set using the Wizard. Follow the procedure below. First, set [Measurement Type] to "SMSA" and [Number of STD] to "1" and finish the settings. Then set necessary items on the MRT work sheet. In the case of furnace measurement using the ASC, settings of Preparation Parameters are also necessary. In the case of flame method When the Preparation Parameters page is displayed, first, click on the element row for setup to highlight it and click on <Edit>. Then "Edit Preparation Parameters" dialog box opens. (1) Select "SMSA" for the [Measurement Type]. (2) Setup of [Order] and [Zero Intercept] is not possible. The order is automatically set to the 1st (linear) and zero is not intercepted. (3) Select [Conc. Unit]. Click on the and select the unit from the list. (4) Entering [Number of STD] displays the table of [Conc]. Enter the concentrations of standard samples to be added. (5) Enter the [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the field of [Weight Correction Factors]. (6) When completing the setup, click on <OK>. Then "Preparation Parameters" page is displayed again. When measuring plural elements, make setup for other elements in the same procedure. In the case of furnace method When the "Preparation Parameters" page is displayed, first, click on the element row for setup to highlight it and click on <Edit>. Then "Edit Preparation Parameters" dialog box opens. (1) Select "SMSA" for [Measurement Type]. (2) Setup of [Order] and [Zero Intercept] is not possible. The order is automatically set to the 1st (linear) and zero is not intercepted. (3) Select [Conc. Unit]. Click on the and select the unit from the list. (4) Entering the [Number of STD] displays a table of [STD Samples] preparation parameters. Enter the concentrations of standard samples in [Conc.] fields and the volume of unknown sample in the [Unknown Samples]. When using the ASC to add the standard sample automatically for preparation, regard the standard sample as [Reagent 3] for setup. (5) In the case of "SMSA" , the [Pos.] in the table indicates the ASC position of unknown sample to which the standard is to be added. (6) Enter the [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the fields of [Weight Correction Factors]. (7) In the case of "SMSA", enter the [Unknown Sample] preparation parameters (sample volume, diluent, Reagent 1, etc.). In the case of "MSA" , this can be ignored. (8) When completing the setup, click on <OK>. Then "Preparation Parameters" page is displayed again. When measuring plural elements, make setup for other elements in the same procedure.
4
Basic Operation
4-75 AA-6800/6650
4.9 Standard Addition Method and Simple Standard Addition Method
(Example) In this example, the ASC is used to add the standard samples of 0ppb, 10ppb, 20ppb and 30ppb to the unknown samples which are being diluted 5 times. Standard sample of 100ppb is prepared for addition and is regarded as the Reagent 3. As other conditions, assume that [Mixing] is to be performed, [Injection Volume] is 20L, and [No. of repetition] is 3 ([Max No. of repetition] is 5). The [Sample] must be constant for all the concentrations. Here, assume it is 40(L). [Conc] 0 10 20 30 [Sample] 40 40 40 40 [Diluent] 160 140 120 100 [Reagent 1] [Reagent 2] 0 0 0 0 0 0 0 0 [Reagent 3] [Total Vol] 0 20 40 60 200 200 200 200
4
Basic Operation
4-76
This [Total Vol] must satisfy the following condition. [(Injection Volume)(Max. No. of repetition)(No. of Boost Cycles) + 50L] [Total Volume] 600 (L) In this equation, the [Injection Volume] means the [Volume] set in the "Mixing Setup" dialog box. The "50L" indicates the dead volume of mixing port. If furnace boost cycle is not performed, (No. of Boost Cycles) is 1. Based on settings made up to now, the calculation is as follows: [(20L)(5 times)(1 cycle) + 50L] [200L] 600 (L) This indicates that the settings are correct. Assume that unknown samples B and C which have similar matrix components to that of unknown sample A in the above setup example. These concentrations are calculated using the calibration curve created by unknown sample A (simple standard addition method). In this case, since the [Sample] is 40L and the [Total Vol] is 200L, the [Unknown Sample] preparation parameters are set as below. [Sample] 40 [Diluent] 160 [Reagent 1] [Reagent 2] 0 0 [Reagent 3] [Total Volume] 0 200
In the [Weight Correction Factors] fields, enter 40 (L) in [Weight Factor] and 200 (L) in [Volume Factor]. Then the actual concentration before dilution can be calculated.
AA-6800/6650
4.9
4.9.2
Measurement Procedures on MRT work sheet

The indication of [Action] on the MRT work sheet related to "SMSA (Simple Method of Standard
Addition)" and "MSA (Method of Standard Addition)" is described below. MSA MSA-RES SMSA : : : Indicates standard addition method. Indicates the concentration of unknown sample calculated from the result of measuring a set of standard addition samples. Indicates simple standard addition method. Unknown sample is measured using a calibration curve created by another sample for standard addition method. In the case of the "Simple standard addition method" setup example described above, the procedure is as
4
Basic Operation
follows. Table 4.3 Measurement Procedure of Simple Standard Addition Method [Action] 1 2 3 4 5 6 7 MSA MSA MSA MSA MSA-RES SMSA SMSA (Measures Sample A with standard 0ppb addition) (Measures Sample A with standard 10ppb addition) (Measures Sample A with standard 20ppb addition) (Measures Sample A with standard 30ppb addition) (Indicates concentration result of Sample A) (Measures Unknown Sample B) (Measures Unknown Sample C) C# 01 01 01 01 01 01 01
If the samples A, B and C are measured by "MSA" , the procedure is as follows. First, delete the raws No.6 and 7 in Table 4.3 by selecting [Edit]-[Delete Rows] from menu. Next, create the raws No.6 to 15 shown in Table 4.4 newly on the MRT work sheet.
4-77 AA-6800/6650
4.9 Standard Addition Method and Simple Standard Addition Method
Table 4.4
Measurement Procedure of Standard Addition Method [Action] C# (Measures Sample A with standard 0ppb addition) (Measures Sample A with standard 10ppb addition) (Measures Sample A with standard 20ppb addition) (Measures Sample A with standard 30ppb addition) (Indicates concentration result of Sample A) (Measures Sample B with standard 0ppb addition) (Measures Sample B with standard 10ppb addition) (Measures Sample B with standard 20ppb addition) (Measures Sample B with standard 30ppb addition) (Indicates concentration result of Sample B) (Measures Sample C with standard 0ppb addition) (Measures Sample C with standard 10ppb addition) (Measures Sample C with standard 20ppb addition) (Measures Sample C with standard 30ppb addition) (Indicates concentration result of Sample C) 01 01 01 01 01 02 02 02 02 02 03 03 03 03 03
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
MSA MSA MSA MSA MSA-RES MSA MSA MSA MSA MSA-RES MSA MSA MSA MSA MSA-RES
4
Basic Operation
4-78
In this case, three calibration curves are created. When "MSA" is added in the MRT work sheet, C# (calibration curve number) is automatically allocated. Check that C# corresponds properly to the series of standard addition samples.
AA-6800/6650
4.10
Conditions and Operation for Flame Emission Analysis
Flame emission quantitative analysis is described here. As the case of atomic absorption analysis, the Wizard can be used for setup. However, the setup procedures in the "Optics Parameters" and "Atomizer/Gas Flow Rate Setup" pages are different in some points. Other operations are the same as those of the flame method of atomic absorption analysis.
4.10.1 Optics ParametersPage
4
Basic Operation
Figure 4.49 Optics ParametersPage

(1) [Wavelength] For wavelength used for flame emission analysis, refer to Table 4.5. Enter the numeric value if the wavelength is different from that for atomic absorption analysis. (2) [Slit Width] It is recommended to set the slit width to "0.5 nm". (3) [Socket #] Although a lamp is not used, it is necessary to set an arbitrary socket number as a dummy. (Procedure for dummy setup) 1. Press the <Lamp Pos. Setup> button to display the "Lamp Position Setup" dialog box. 2. For an arbitrary [Socket #], select "*" in the [Element] and "Normal" in the [Lamp Type]. 3. Select "Emission" in [Lamp ID]. This lamp ID is a special ID of dummy lamp for flame emission analysis. 4. Press <OK> to close the "Lamp Position Setup" dialog box and return to the "Optics Parametrs" page. Then select the socket # in which the dummy lamp for flame emission analysis was set. When performing the line search using a lamp, set a proper lamp in "Lamp Position Setup" dialog box. (4) [Lamp Mode] Set the [Lamp Mode] to "EMISSION" . (5) [Lamp Current] Set the [Low] to "0" (zero). When the lamp mode is set to "EMISSION", the [High] is automatically
4-79 AA-6800/6650
4.10
set to "0" (zero) and cannot be entered. (6) <Line Search> In the case of flame emission analysis, a line search is performed when the flame has been ignited and the standard sample is being sprayed. So, the line search is not performed in this page. Proceeds to the next "Atomizer/Gas Flow Rate Setup" page first and set the parameters so that ignition may be possible. After that, return to this page perform the line search. It is also possible to perform a line search using the hollow cathode lamp. In this case, light on the hollow cathode lamp to perform the line search. If the lamp is lit on in the EMISSION mode, the lamp is automatically turned off when the <START> key is pressed to start the measurement. Don't forget to turn off the lamp, however, when observing a signal in the "Atomizer/Gas Flow Rate Setup" page while aspirating the sample. (7) Click on <Next> button to proceed to the "Atomizer/ Gas Flow Rate Setup" page first. Table 4.5 Element Ag Al As Au B Ba Be Bi Ca Cd Ce Co Cr Cs Cu Dy Er Eu Fe Ga Gd Ge Band spectrum Analysis Line Wavelength Table for Flame Emission Analysis Wavelength (nm) 328.1 396.2 193.7 267.6 518.0 455.4 234.9 306.8 422.7 326.1 494.0 345.4 425.4 455.5 324.8 404.6 400.8 459.4 372.0 417.2 622.0 265.1 Element Hf Hg In Ho Ir K La Li Lu Mg Mn Mo Na Nb Nd Ni Os Pb Pd Pr Pt Rb Wavelength (nm) 531.2 253.7 451.1 410.4 550.0 766.5 442.0 670.8 451.9 285.2 403.3 390.3 589.0 405.9 492.5 352.5 442.1 405.8 363.5 495.1 265.9 794.8 Element Re Rh Ru Sc Si Sm Sn Sr Ta Tb Te Ti Th Tl U V W Y Yb Zn Zr Wavelength (nm) 346.1 343.5 372.8 402.4 251.6 476.0 317.5 460.7 474.0 534.0 486.6 334.9 492.0 377.6 544.8 437.9 430.2 597.2 398.8 636.2 360.1
4
Basic Operation
4-80
AA-6800/6650
4.10
4.10.2 Atomizer/Gas Flow Rate SetupPage

The "Atomizer/Gas Flow Rate Setup" pages are different in AA-6800 and AA-6650. Refer to the description for your AA type. 4.10.2.1 AA-6800 (1) Firstly, select the [Fuel Gas Flow Rate] for [Operation Object] by clicking on the radio button.
4
Basic Operation
Figure 4.50 Atomizer/Gas Flow Rate SetupPage (in the case of [Fuel Gas Flow Rate])
[Flame Type] Since the flame used for atomic absorption analysis is indicated, click on the and select the flame type used for flame emission analysis. As a flame type used for flame emission analysis, generally, the high temperature N2O-C2H2 flame is good. However, in the cases of alkaline metals (Na, K, etc.), other flame (Air-C2H2) is also available for measurement of sufficiently minute quantities. The Air-H2 flame with low background can also be used effectively for flame emission analysis. [Fuel Gas Flow Rate] Since the flow rate for atomic absorption analysis is indicated by default, enter the flow rate value for flame emission analysis. It is necessary to check the optimum value for each element beforehand. In general, a low acetylene flow rate is best. When using the N2O-C2H2 flame, adjust the flow rate so that the red feather (pink portion of flame) is approx. 2 to 3 mm in height. To obtain the optimum gas flow rate, the function of <Gas Flow Auto> button is convenient. Use it after setting the ignition conditions and performing the line search.
4-81 AA-6800/6650
4.10
(2) Select the [Atomizer Position] for [Operation Object] by clicking on the radio button.
4
Basic Operation
Figure 4.51 Atomizer/Gas Flow Rate SetupPage (in the case of [Atomizer Position])
[Burner Height] Since the value for atomic absorption analysis is indicated by default, enter the optimum value for flame emission analysis. If the optimum value is not known, as a first step, set it to 7mm for Air-C2H2, 11mm for N2O-C2H2 and 15mm for Air-H2. Then, after setting the ignition conditions and performing the line search, obtain the optimum value again. To obtain the optimum burner position, the function of <Burner Position Auto> button is convenient. [Burner Lateral] This is used to change the position intentionally from the burner origin position set in Maintenance. For example, set a value here to lower the sensitivity of a particular element in full-automatic continuous measurement of plural elements (this is a substitute for changing a burner angle in manual measurement to lower the sensitivity). When simply setting the optimum position of burner lateral, select [Instrument]-[Maintenance]-[Burner Origin Position Adjustment] from the menu and set the "Burner Lateral" to zero. [Burner Angle] Set the angle of burner head according to the purpose. Generally, the S/N ratio is better when the angle is set at 0 degree for optical axis (parallel) than at 90 degrees, but its linearity may become worse. When the concentration of analysis element is relatively high, the burner head is used at 90 degrees.
4-82 AA-6800/6650
4.10
4.10.2.2 AA-6650 (1) Firstly, select the [Fuel Gas Flow Rate] for [Operation Object] by clicking on the radio button.
4
Basic Operation
Figure 4.52 "Atomizer/Gas Flow Rate Setup" Page (in the case of [Fuel Gas Flow Rate])
[Flame Type] Since the flame used for atomic absorption analysis is indicated, click on the and select the flame type used for flame emission analysis. As a flame type used for flame emission analysis, generally, the high temperature N2O-C2H2 flame is good. However, in the cases of alkaline metals (Na, K, etc.), other flame (Air-C2H2) is also available for measurement of sufficiently minute quantities. The Air-H2 flame with low background can also be used effectively for flame emission analysis. [Fuel Gas Flow Rate] Since the flow rate for atomic absorption analysis is indicated by default, enter the flow rate value for flame emission analysis. It is necessary to check the optimum value for each element beforehand. In general, a low acetylene flow rate is best. When using the N2O-C2H2 flame, adjust the flow rate so that the red feather (pink portion of flame) is approx. 2 to 3 mm in height.
4-83 AA-6800/6650
4.10
(2) Select the [Atomizer Position] for [Operation Object] by clicking on the radio button.
4
Basic Operation
Figure 4.53 Atomizer/Gas Flow Rate SetupPage (in the case of [Atomizer Position])
[Burner Height] Since the value for atomic absorption analysis is indicated, enter the optimum value for flame emission analysis and set the burner height using the knob for adjusting burner vertical position. The "Burner Height" indicates the distance from the optical axis down to the burner head by a positive value. If the optimum value is not known, as a first step, set it to 7 mm for Air-C2H2 and 11 mm for N2OC2H2. Then after setting the ignition conditions and performing the line search, obtain the optimum value newly. To obtain the optimum value, change the burner height while spraying the sample, and search the burner height so that the real time data profile shows a high and stable sensitivity. [Burner Angle] Set the angle of burner head according to the purpose. Generally, the S/N ratio is better when the angle is set at 0 degree for optical axis (parallel) than at 90 degrees, but its linearity may become worse. When the concentration of analysis element is relatively high, the burner head is used at 90 degrees.
4-84 AA-6800/6650
4.10
4.10.3
Line Search and Beam Balance
After completing the condition setup in the "Atomizer/Gas Flow Rate Setup" page, click on <Back> to return to the "Optics Parameter" page. Read the section 4.8 thoroughly and set the conditions so that a flame can be ignited. (1) Ignite the flame. (2) Start spraying the standard sample of the highest concentration. If the sample position of the highest concentration standard sample on ASC turn table is set to the [ASC Sample Pos. for EMISSION Line Search], the automatic spray using the ASC is possible. (3) While spraying the sample, click on <Line Search> button. Then the line search/beam balance is executed. Continue spraying the sample until the line search/beam balance operation is completely
4
Basic Operation
finished. When the ASC is used, the spray of the sample in the specified position on the ASC turn table is started before starting the line search/beam balance. The line search/beam balance is started when the pre-spray time set in the [Parameters]-[Edit Parameters]-[Measurement Parameters] is finished after starting the spray. (4) If the line search fails and the message stating insufficeint energy is displayed, prepare and spray a standard sample of even higher concentraion and try it again. (5) When the line search is completed, click on <Close> to return to the "Optics Parameters" page. Then click on <Next> button to proceed to the "Atomizer/Gas Flow Rate Setup" page again. While monitoring the real time graph on the "Atomizer/Gas Flow Rate Setup" page, spray vaporized water and check that the signal becomes almost zero. (6) If the signal does not become small, it is possible that the analysis line was not correctly detected. In that case, go back to the "Optics Parameters" page and perform the line search once again following the procedures (1) to (5).
4-85 AA-6800/6650
4.11
Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height(AA-6800)
In the atomic absorption analysis, the [Fuel Gas Flow Rate] and [Burner Height] affect the absorption sensitivity. Although standard values are automatically set as default values by selecting an element, the optimum condition may differ depending on the sample characteristics and matrix components. The "Optimum Burner Height Search" and "Optimum Gas Flow Rate Search" are the functions to search the optimum conditions by the measurement while changing the burner height or gas flow rate automatically. In this section, the operation procedures are described. For details on each item of the dialog box, refer to the section 5.5.7. In addition, read the section 4.8 thorougly and set the conditions for ignition. NOTE The <Burner Position Auto> and <Gas Flow Auto> cannot be used in the AA-6650.
4
Basic Operation
4-86
4.11.1
Setting the Optimum Condition of Burner Height
(1) Open the "Atomizer/Gas Flow Rate Setup" page in the Wizard. (2) Click on the radio button of [Atomizer Position] for operation object, then the <Burner Position Auto> button is available. The optimum condition of burner height is obtained in the procedure described below. Click on <Burner Position Auto>. Then the "Optimum Burner Height Search" dialog box appears.
Figure 4.54 Optimum Burner Height SearchDialog Box

Set the [Start] and [End] of the burner position search range. Although the available search range is within 0 to 25 (mm), you may set the range 5 to 10 (mm) for Air-C2H2 and 8 to 14 (mm) for N2OC2H2. Press the IGNITE button on the front side of AA main unit to ignite a flame. Start spraying the blank solution and click on <Blank Meas.> button. The measurement is performed while the burner height is changed by 1 mm step in the selected range. Continue to spray it until the measurement is completed. Next, start spraying the standard (or sample) solution and click on <STD Meas.> button. In the
AA-6800/6650
4.11 Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height(AA-6800)
same way as blank measurement, the measurement is performed while the burner height is changed. Continue to spray it until the measurement is completed. The dialog box displays the graph which is created by subtracting the measurement result of from the measurement result of . And the burner height with which the absorbance becomes the highest is also displayed in [Current Value]. If the result is acceptable, extinguish the flame and click on <OK>. The "Optimum Burner Height Search" dialog box is closed to return to the "Atomizer/Gas flow Rate Setup" page, and the obtained value is indicated and used as the [Burner Height]. If the <Cancel> is pressed, the burner height is returned to the original position.
4
Basic Operation
4.11.2
Setting the Optimum Condition of Fuel Gas Flow Rate
(1) Open the "Atomizer/Gas Flow Rate Setup" page in the Wizard. (2) Click on the radio button of [Fuel Gas Flow Rate] for operation object, then the <Gas Flow Auto> button is available. The optimum condition of fuel gas flow rate is obtained in the procedure described below. Click on <Gas Flow Auto>. Then the "Optimum Gas Flow Rate Search" dialog box appears.
Figure 4.55 Optimum Gas Flow Rate SearchDialog Box

Set the [Start] and [End] of the burner position search range. The range can be set within 0.6 4.9 L/min in the case of Air-C2H 2 and within 5.6 9.9 L/min in the case of N2O-C2H 2. It is recommended to set the range within the standard condition 0.5L/min. Press the IGNITE button on the front side of AA main unit to ignite a flame. Start spraying the blank solution and click on <Blank Meas.> button. The measurement is performed while the fuel gas flow rate is changed by 0.1 L/min step in the selected range. Continue to spray it until the measurement is completed.
4-87 AA-6800/6650
4.11 Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height(AA-6800)
Next, start spraying the standard (or sample) solution and click on <STD Meas.> button. In the same way as blank measurement, the measurement is performed while the fuel gas flow rate is changed. Continue to spray it until the measurement is completed. The dialog box displays the graph which is created by subtracting the measurement result of from the measurement result of . And the fuel gas flow rate with which the absorbance becomes the highest is also displayed in [Current Value]. If the result is acceptable, extinguish the flame and click on <OK>. The "Optimum Gas Flow Rate Search" dialog box is closed to return to the "Atomizer/Gas Flow Rate Setup" dialog box, and
4
Basic Operation
4-88
the obtained value is inidcated as the [Fuel Gas Flow Rate]. If the <Cancel> is pressed, the fuel gas flow rate is returned to the original position. If the [Fuel Gas Flow Rate] is changed, distribution of atoms in the flame changes, as the result, the optimum [Burner Height] also changes. On the other hand, changing the [Burner Height] also changes the optimum gas flow rate. Note that the optimum condition changes if the other condition is changed. To search the optimum condition precisely, for example, select several levels of burner height and search the optimum gas flow rate at each level of burner height. Then select the best combination that shows highest sensitivity. (Or you can also select several levels of gas flow rate and search the burner height at each flow rate). Although some elements (such as Cu) are not affected so much by these conditions, some elements (such as Cr) are affected greatly. If these settings are not appropriate, not only the sensitivity decreases, but also poor reproducibility of data may be caused by sensitivity fluctuation. Utilize these functions for setting the optimum conditions when required.
AA-6800/6650
Chapter 5 Functions of Operation Menu

This chapter explains items and functions displayed on the screen of PC software that controls the AA instruments.
5
Functions of Operation Menu
Contents 5.1 Wizard Selection dialog box 5-1
5.1.1 "Wizard" page 5-1 5.1.2 "Recent Files" page 5-2 5.1.3 "Recent Templates" page 5-2 5.2 [File] 5-3 [New] 5-3 [Open] 5-4 [Save] 5-4 [Save As...] 5-4 [Additional Load] 5-5 [File Export...] 5-6 [Export Items] 5-6 [Auto Save] 5-7 [Print Data/Parameters...] 5-9 [Print Table Data...] 5-10 [Print Style] 5-11 "Print Style Setup" page 5-11 "Table Show/Hide" page5-11 "Font" page 5-12 5.2.1 5.2.2 5.2.3 5.2.4 5.2.5 5.2.6 5.2.7 5.2.8 5.2.9 5.2.10 5.2.11
5.2.11.1 5.2.11.2 5.2.11.3
AA-6800/6650
5.2.12 5.2.13 5.2.14 5.3.1 5.3.2 5.3.3 5.3.4 5.3.5 5.3.6 5.3.7
[Print Setup] 5-13 Recent Files 5-13 [Exit] 5-13 [Insert Row] 5-14 [Delete Rows] 5-14 [Import Other Schedule] 5-14 [Collective Edit] 5-14 [Remeasure Selected Range] 5-14 [Clear Measurement Result] 5-14 [Copy]5-15 [Paste] 5-15
5.3 [Edit] 5-14
5
5.3.8
5.4 [Refer to Parameters] 5-16 5.5 [Parameters] 5-17 5.5.1 "Element Selection" Page 5-18 5.5.1.1 Cookbookpage 5-20 5.5.1.2 Templatepage 5-21 5.5.2 "Preparation Parameters" Page 5-22 5.5.2.1 5.5.2.2 5.5.2.3 5.5.2.4 5.5.2.5 5.5.2.6 5.5.2.7 Weight Correction Factors 5-24 Preparataion Parameters for Standard 5-24 Preparation Parameters for Unknown 5-25 Preparation Parameters for Periodic Blank 5-25 Mixing Setup and Reagent Setup 5-26 Coating/Boost Cycle (only for furnace method) 5-27 Repeat Measurement Conditions 5-28
5.5.3 "Sample ID" Page 5-29 5.5.4 "Sample Selection" Page 5-31 5.5.5 "Connect to Instrument/Send Parameters" Page 5-31 5.5.6 "Optics Parameters" Page 5-32 5.5.6.1 5.5.6.2 5.5.6.3 5.5.7.1 5.5.7.2 5.5.7.3 5.5.7.4 <Lamp Pos. Setup> button 5-35 <Warmup Lamp> Button 5-36 <Line Search> Button 5-37 Atomizer Position 5-38 <Burner Position Auto> Button 5-40 Fuel Gas Flow Rate 5-41 <Gas Flow Auto> Button 5-42
5.5.7 "Atomizer/Gas Flow Rate Setup" Page (for flame method by AA-6800) 5-38
5.5.8 "Atomizer/Gas Flow Rate Setup" Page (for flame method by AA-6650) 5-43 5.5.8.1 Atomizer Position 5-43 5.5.8.2 Fuel Gas Flow Rate 5-44
AA-6800/6650
5.5.9 "Furnace Program" Page (for furnace method) 5-46 5.5.9.1 5.5.9.2 5.5.9.3 5.5.9.4 5.5.9.5 5.6 <Coating/Boost Cycle> Button 5-48 <Test Meas.> Button 5-49 <Cleaning> Button 5-50 <Change Graphite Tube> Button 5-50 <Temp. Search> Button 5-52
[Edit Parameters] 5-54
5.6.1 "Measurement Parameters" page 5-54 5.6.2 "Repeat Measurement Conditions" page 5-57 5.6.3 "Weight Correction Factors" page 5-59 5.6.4 "Y-axis Print Range" page 5-60 5.6.5 "Analyst" page 5-60 5.6.6 "Comment" page 5-60 5.6.7 "Sequence" page 5-61 5.6.8 "ASC Parameters" page 5-62 5.6.9 "QA/QC Setup" page 5-63 5.6.10 "Calibration Curve Parameters" page 5-66 5.6.11 "Optics Parameters" page 5-67 5.6.12 "Atomizer/Gas Flow Rate Setup" page (Flame method) 5-67 5.6.13 "Furnace Program" page (Furnace method) 5-67 5.7 [Default Parameters] 5-68 [Flame] 5-68 [Furnace]5-68 [Graph] 5-68 [Analyst] 5-68 [Connect] 5-70 [Option Connect] 5-72 [Configuration] 5-72 [Lamp Position Setup] 5-76 [Lamp History] 5-77 [Maintenance] 5-79 [D2 Lamp Position] 5-79 [Wavelength Adjustment] 5-79 [Burner Origin Position Adjustment] (AA-6800) 5-80 [Furnace Origin Position Adjustment] (AA-6800) 5-81 [Furnace Origin Position Adjustment](AA-6650) 5-82 [ASC Maintenance] 5-83 [Set Syringe Volume] 5-83 5.7.1 5.7.2 5.7.3 5.7.4 5.8 5.8.1 5.8.2 5.8.3 5.8.4 5.8.5 5.8.6
5
[Instrument] 5-69
5.8.6.1 5.8.6.2 5.8.6.3 5.8.6.4 5.8.6.6 5.8.6.7
5.8.6.5 [Burner Origin Position Adjustment](AA-6650) 5-82
5.8.6.7.1
AA-6800/6650
5.8.6.7.2 5.8.6.8 5.8.7 5.8.8 5.8.9 5.8.10 5.8.11 5.8.12 5.8.13 5.8.14 5.8.15
[Change Syringe] 5-85
[Maintenance only for service engineer] 5-85
[Lamp Status] 5-86 [Change Graphite Tube] 5-88 [Gas Controller Status] 5-88 [Gas Leak Check] 5-89 [Remaining Gas Combustion] 5-89 [Execute Line Search] 5-91 [Cleaning] 5-91 [Rinse Nozzle] 5-91 [Flame Nozzle Position] 5-91 [Furnace Nozzle Position] 5-92 [Search for Help on...] 5-94 [About WizAArd...] 5-94
5
5.8.16 5.9 5.9.1 5.9.2
[Help] 5-94
AA-6800/6650
5.1
Wizard Selection dialog box
After the software is started, the "Wizard Selection" dialog box shown in Figure 5.1 is displayed. Clicking on <Cancel> closes this dialog box, and clicking on <Wizard> at left lower of the main window displays this dialog box again.
5
Figure 5.1 "Wizard Selection" dialog box 5.1.1 "Wizard" page

The following three icons are indicated on the "Wizard" page in the "Wizard Selection" dialog box. Each Wizard can be started by selecting one of the icons and clicking on <OK>. However, when you start newly, or when no element has been selected, the [Schedule Creation] and [Measurement Preparation] are not displayed. [Element Selection] The element selection Wizard is started. Selection of measurement elements, setup of measurement element order and selection of flame/furnace are performed here. You may close the Wizard in the element selection page only. Or you may also proceed to the pages of schedule creation and measurement preparation to set the parameters until the measurement can be performed in that conditions. This is equivalent to selecting [Parameters]-[Element Selection Wizard] from the menu. [Schedule Creation] Setup of calibration curve parameters, setup of sample preparation parameters, setup of the sample information, and input of factors for actual concentration calculation are performed here and the measurement sequence is created on the MRT Work sheet. This is equivalent to selecting [Parameters]-[Schedule Creation Wizard] from the menu.
5-1 AA-6800/6650
5.1 Wizard Selection Screen
[Measurement Preparation] This is applied for one element when the measurement sequence is already created. Lighting of hollow cathode lamp, line search/beam balance, and setup of the burner position and gas flow rate or setup of furnace temperature program are performed. This is equivalent to selecting [Parameters]-[Measurement Preparation Wizard] from the menu.
5.1.2 "Recent Files" page

A data file lately used can be selected from the list and opened.
5
5-2
5.1.3 "Recent Templates" page

A template lately used can be selected from the list and opened.
AA-6800/6650
5.2
[File]
This menu summarizes functions associated with WizAArd's file and print. In the WizAArd, two file types of "*.aa" and "*.taa" are handled. The "*.aa" refers to a data file and contains the measurement parameters, calibration curve, sample informations, measurement procedure and measured data. These informations for plural elements can be saved in one file. The "*.taa" refers to a template and is different from a data file in the following points. (1) Measured data is not included. The contents are the same as those of "*.aa" file before measurement. If a file is saved as a template file in [File]-[Save As] after measurement, the measured data is cleared and other contents are saved. (2) When a template file is loaded, it has no name. When a template file is loaded, the title bar displays "notitle - WizAArd". If selecting the [File]-[Save], the [Save As] dialog box always appear instead. (3) It can be utilized as a cookbook (standard parameters for each element).
5
When using the parameters, such as wavelength, lamp current and furnace program, which are different from the standard parameters built in the software, save them as a template file so that you can use it easily instead of the built-in standard parameters (refer to the section 5.5.1.2.["Template" page]).
Figure 5.2 Drop-down Menu of [File] 5.2.1 [New]

This command is used to create measurement parameters and measurement procedures. Execution of this command resets the data and parameters already existing on MRT Worksheet. When the data exists on MRT Worksheet, save the data with [Save] or [Save As...] command before executing [New].
5-3 AA-6800/6650
5.2 [File]
5.2.2 [Open]
This command is used to read the files already saved in the disk. Execution of this command opens the "Open" dialog box (Figure 5.3). Specify the [Look in], [Files of type] and [File name], and click on <Open>.
5
5-4 AA-6800/6650
Figure 5.3 "Open" Dialog Box

<Comment> If a comment has been written with the file to be opened, the comment can be read. Enter [File name] and click on <Comment>, then the comment is displayed.
5.2.3 [Save]
This command is used to save the parameters and data currently loading on the software, without changing the file name. When the file name does not exist (not named), same as [Save As...] is executed. NOTE A measurement data whose repeat measurement has not finished is not saved in the file. If the data is necessary when the repeat measurement cannot be completed, print it before ending the AA software.
5.2.4 [Save As...]

This command is used to save the parameters and data currently loading on the software with a new file name. When this command is executed, the "Save As" dialog box (Figure 5.4) opens. Specify the [Save in], [Save as type] and [File Name], and click on <Save>. If the "*.taa" is selected for file type, data is not saved. NOTE A measurement data whose repeat measurement has not finished is not saved in the file. If the data is necessary when the repeat measurement cannot be completed, print it before ending the AA software.
5.2 [File]
5
Figure 5.4 "Save As" Dialog Box

If a file is saved as "template.aa" in the same folder (default: C:\Program Files\WizAArd\") of the execution file ("Wizaa.exe"), the "template.aa" file is automatically loaded when starting AA software at next time or when newly creating file with [New] command. It is convenient to save a frequently used measurement parameter file in your routine as "template.aa". <Comment> This button is used to record your comment. Click on <Comment> button, then "File Comment" dialog box opens. Write your comment and click on <OK>. The comment is saved with the file.
5.2.5 [Additional Load]

Schedules of measurement element in a file saved in the disk are added to the end of the current schedule of measurement element. This function can be used for the following purposes. (1) A file for continuous measurement of plural elements can be created using several measurement files (or measurement template files) created for single element. (2) One summary report can be created from several files. When a schedule of the same element is added, it is not combined in one schedule but added as another schedule. When the total number of schedules exceeds 20, the schedules over it are not read in.
5-5 AA-6800/6650
5.2 [File]
5.2.6 [File Export...]

This command is used to create a text file from data on the MRT Worksheet of currently opened file. The text file can be read in wordprocessor software or spreadsheet software. Executing this command opens the dialog box (Figure 5.5) to indicate the selection items. From this list, select items to be converted to text data and click on <OK>. Then the "Save As" dialog box as shown in Figure 5.4 opens. Specify the [Save in], [Save as type] and [File name], and click on <Save>. NOTE Only the data on the MRT worksheet can be output to text file. Measurement parameters and waveform data cannot be output.
5
5-6 AA-6800/6650
Figure 5.5 "Select Schedule" Dialog Box 5.2.7 [Export Items]

This specifies output items to output the data on the MRT worksheet to the text file. This setting is valid to the following text file output functions. Output from [File]-[File Export...] menu. Output by setting the automatic output of text file in [File]-[Auto Save] menu Output by setting "FILEEXPORT" in [Action] field in the MRT worksheet
5.2 [File]
5.2.8 [Auto Save]
q w e t y u i r
5
o !3
!0 !1 !2
Figure 5.6 "File Auto Saving and Exporting" Dialog Box

Saving the backup file automatically Automatic saving of the backup of measurement file can be set up in the style of "every X samples are measured". This setting is valid both for automatic measurement using the auto-sampler and for manual measurement. [Auto Save] When saving a backup file automatically, select this check box. The saving interval and file name can be entered. [every X samples] Enter the interval for saving a backup file. The input range is 1 to 300. The number of measurement items (BLK, STD, UNK, MSA, SMSA, RESLOPE, QC and SPIKE) on the MRT is counted as the sample number. [File Name] Set a path name (drive name + folder name + file name) of backup file. A path name can be entered easily by using < Brows...> (). If a backup name is not entered, the default file name "autosave.aa" is automatically set. When the automatic saving is executed, the preceding backup file of auto-saving is renamed and
5-7 AA-6800/6650
5.2 [File]
Example: When the auto saving is set with a file of the name "autosave.aa", executing another auto saving creates "autosave.aa.sav." as a backup of the preceding file. Exporting the MRT worksheet data automatically in text file When performing an automatic measurement using the auto-sampler, the measurement result of the schedule and summary report can be exported in text style at the end of schedule of each element (or when the execution of the last row of each element on the MRT is finished). This setup is invalid for manual measurement. Also, only the data in the MRT worksheet can be exported in text file, but the measurement parameters and waveform data cannot be exported. NOTE To perform the text file auto export in manual measurement, set a "FILEEXPORT" row in the MRT worksheet. [One element text file at the end of schedule] Select this check box to export the measurement result of each element in text style. [Summary text file at the end of schedule] Select this check box to export the summary report in text style. [Folder Name] This sets a destination folder of the text file automatically exported. Selecting the checkbox or makes this entry possible. A destination folder name can be entered easily by using < Brows...> (). The AA software automatically gives a file name of the automatically exported text file. The measurement result of each element schedule is given a file name as "element name + measurement type (Flame:1, Furnace:2, HVG/MVU:3).txt". For example, when Pb is measured in furnace method, the text file name is "Pb2.txt". The file name of summary report is fixed to "summary.txt". These files are saved over the preceding one without any warning message. Therefore, "summary.txt" is overwritten whenever a measurement of each element is finished. Also, when the same element is measured in the same measurement method, note that firstly exported measurement result is overwritten. This automatic export function can be used for the automatic data collection by the host computer on the network, in a combination with the following "Executing a program by command line". Executing a program by command line In the automatic measurement using the auto-sampler, a command line can execute a program when the schedule of each element is finished (when the execution of the last row on the MRT work sheet of each element is finished, or immediately after the auto-export of text file is finished). A command line means a method to specify an execution file name and start/execute the program, as MS-DOS prompt or "Start"-"Run..." in Windows. When executing a program from the command line, specify a combination of the execution file name or batch file name and its argument. In this dialog box, a name of text file to be exported automatically can
5
5-8
AA-6800/6650
5.2 [File]
be set up as argument. NOTE When executing a program by command line in manual measurement, set up "COMMAND" row in the MRT worksheet. [Execute command after exporting text file] Select this check box to execute a program by command line. Then the command file name can be entered. [Command File Name] Enter the execution file name. A file name can be entered easily by using < Brows...> (). [Add the element file name to the command] When this check box is selected, the single element text file name is set up as argument of command. This check box is selectable when the check boxes and are selected. [Add the summary file name to the command] When this check box is selected, the summary text file name is set up as argument of command. This check box is selectable when the check boxes and are selected. A file name of text file automatically exported is enclosed by " " (double quotation marks) and added to the end of a specified command line with an intervening space between them. When the both file names of schedule measurement result and summary report are added in the setting, the file name of summary report is added to the end of the file name of measurement result with an intervening space between them. For example, when the command line is "C:\something.bat" and when the Pb furnace measurement result and summary report are to be automatically exported to the "C:\My Documents\AA Export" folder, and the both file names are to be added to the command line, the actual command line to be executed is as follows. C:\something.bat Export\summary.txt" If a special program is additionally prepared, this function can be utilized to give a notice of the measurement end to another room through a computer network or to collect or handle the measurement results outputted in text style. "C:\My Documents\AA Export\Pb2.txt" "C:\My Documents\AA
5
5.2.9 [Print Data/Parameters...]

This command is used to print the measurement parameters and data of the currently opened file. When this command is selected, the element symbols available for printing the data and parameters are displayed in the dialog box that is same as Figure 5.5. From this list, select items to be printed and click on <OK>. Then the dialog box shown in Figure 5.7 opens. Set the [Copies], and click on <Print>. In the Print
5-9 AA-6800/6650
5.2 [File]
dialog box invoked from [Print Data/Parameters] menu, only [All] can be selected at [Print range].
NOTE
When the parameters are changed in the middle of the measurement in one schedule, only the final parameters are printed out. To print the measured data and its parameters correctly on the report, create another schedule when measuring one element with different parameters.
5
5-10 AA-6800/6650
Figure 5.7 "Print" Dialog Box 5.2.10 [Print Table Data...]

This command is used to print out the contents of MRT Worksheet of currently opend file (For "Table Show/Hide", refer to 5.2.11.2). When this command is executed, items which can be printed out are displayed in the dialog box as Figure 5.5. From this list box, select "Summary" or elements you want to print and click on <OK>. Clicking on <OK> button opens the "Print" dialog box (Figure 5.7). Operate in the same way as section 5.2.9. The data is printed out according to the format displayed on each MRT Worksheet.
5.2 [File]
5.2.11 [Print Style]

This command is used to make settings related to printing data and parameters from [Print Data/Parameters] menu. You can set the print mode, items and font here. When printing a peak profile data (waveform), set the graph scale in the "Y-axis Print Range" page by selecting [Parameters]-[Edit Parameters] from the menu bar. 5.2.11.1 "Print Style Setup" page
5
Figure 5.8 "Print Style Setup" page

Put check marks to the items or contents you want to print. Clicking on <Details> displays more detail items. In the [Data Print Mode], you can select it from the following three. All Only Average 5.2.11.2 printed. : : All the data of repeat measurement with peak profile All the data of repeat measurement without peak profile Only the average value calculated from repeat measurement data
Without Profile :
"Table Show/Hide" page
When printing the data of MRT work sheet, select items in this page. Put checkmarks in the items to be
5-11 AA-6800/6650
5.2 [File]
5.2.11.3 "Font" page
5
5-12 AA-6800/6650
Figure 5.9 "Font" page

Set the font type, size, style and other items. A sample of the characters based on the settings are displayed in [Preview]. These settings are valid only for "Print Data/Parameters".
5.2 [File]
5.2.12 [Print Setup]

Set the items related to the printer. Executing this command opens the "Print Setup" dialog box shown in Figure 5.10.
5
Figure 5.10 "Print Setup]" Dialog Box

[Printer] Select the printer to be used from the drop-down list of [Name]. [Paper] Select [Size] and [Source]. [Orientation] Select [Portrait] or [Landscape] by clicking on radio button.
5.2.13 Recent Files

Maximum four measurement file names recently opened are displayed. Click on the file name to be opened.
5.2.14 [Exit]
When this command is executed, the communication with the instrument is shut off first and then the software is closed. Therefore, it takes approx. 30 seconds to exit the program. If the data has not been saved, a warning message to ask you whether you want to save the data before exiting the program or not.
5-13 AA-6800/6650
5.3
[Edit]
Functions to be used in editing the data row on MRT Worksheet are summarized.
5
Figure 5.11 Drop-down Menu of [Edit] 5.3.1 [Insert Row]
This command is used to insert one row just before the row selected in the table. However, a row cannot be inserted to the row already measured.

5-14
5.3.2 [Delete Rows]

This command is used to delete the selected rows in the table. However, the row already measured cannot be deleted. NOTE Insertion and deletion of a row next to current measuring row can t be done during measurement.
5.3.3 [Import Other Schedule]

A measurement procedure created in other element's schedule is copied to the currently displayed (active) MRT work sheet.
5.3.4 [Collective Edit]

The values of a specified item can be changed collectively in selected rows on the MRT work sheet. The available items are C# (Calibration Number), Actual Conc. Unit, Sample Volume, Diluent Volume, Reagent 13, Weight Factor, Volume Factor, Dilution Factor, Correction Factor and Coating Reagent.
5.3.5 [Remeasure Selected Range]

This is a function to perform a remeasurement on the data already measured. After selecting rows to be remeasured on the MRT work sheet, execute this. The rows already measured are excluded from the measruement result and new rows for the same measurement items are added on the MRT work sheet. In the case of repeat measurement, select a range including average rows to perform a remeasurement. A remeasuremnt cannot be executed for rows already excluded or rows with no data (RINSE, AUTOZERO, etc).
5.3.6 [Clear Measurement Result]

All the measurement data on the MRT work sheet currently displayed are cleared and the status before measurement is recovered. The setting of measurement procedure remains without a change.
AA-6800/6650
5.3 [Edit]
5.3.7 [Copy]
Numeric values and characters on the MRT worksheet and summary table can be copied to the clipboard. Refer to Section 4.7.6 for details.
5.3.8 [Paste]
Text data can be pasted from the clipboard only to the sample ID row in the MRT work sheet. Refer to Section 4.7.6 for details.
5
5-15 AA-6800/6650
5.4
[Refer to Parameters]
Clicking on [Parameters] in Menu Bar during the measurement opens a drop-down menu.
5
Figure 5.12 [Parameters] Drop-Down Menu
Selecting [Refer to Parameters] from this drop-down menu opens the property sheet, which is a dialog box to show the parameters for the element under measurement. The parameters can be shown but cannot be changed. To change the parameters, stop the measurement once and select [Parameters]-[Edit Parameters] from Menu Bar (Refer to section 5.6).

5-16
NOTE
If a dialog box ("Coating and Boost Cycles", etc.) is opened in the sheet for referring to the parameters, the measurement operation is stopped temporarily. Therefore, close the dialog box immediately after referering to the necessary parameters.
AA-6800/6650
5.5
[Parameters]
Functions on parameter setup are summarized here.
5
Figure 5.13 Drop-down Menu of [Parameters]
The following three Wizards are available. [Element Selection Wizard] Selection of measurement elements, setup of measurement element order and selection of flame/furnace are performed here. You may close the Wizard in the element selection page only. Or you may also proceed to the pages of schedule creation and measurement preparation to set the parameters until the measurement can be performed in that conditions. You can proceed to the next page only after selecting an element newly. Use the [Schedule Creation Wizard] or [Measurement Preparatin Wizard] for elements already selected. [Schedule Creation Wizard] Setup of calibration curve parameters, setup of periodic blank measurement, setup of the sample information, and input of factors for actual concentration calculation are performed here and the measurement sequence is created on the MRT work sheet. This menu is valid when the element has been selected on the MRT work sheet. [Measurement Preparation Wizard] This is used for an element currently selected. Lighting of hollow cathode lamp, line search/beam balance, and setup of burner position/gas flow rate or setup of furnace temperature program are performed. This menu is valid when an element exists on the MRT work sheet. Each Wizard is composed of the pages shown below. Clicking on <Next> in each page opens the next page. You can close the Wizard by clicking on <Finish> when the settings are completed on each page.
5-17 AA-6800/6650
5.5 [Parameters]
[Element Selection Wizard] Element Selection Preparation Parameters Sample ID Sample Selection Connect to Instrument/Send Parameters Optics Parameters Atomizer/Gas Flow Rate Setup (for flame method) Furnace Program (for furnace method) [Measurement Preparation Wizard]
[Schedule Creation Wizard] Element Selection Preparation Parameters Sample ID Sample Selection
5
5-18
Connect to Instrument/Send Parameters Optics Parameters Atomizer/Gas Flow Rate Setup (for flame method) Furnace Program (for furnace method) In the [Element Selection Wizard], the <Next> button is valid only when a newly selected element exists. In the [Measurement Preparation Wizard], the "Optics Parameters" is displayed first when the connection with instrument is already completed. The followings are description of each page in the Wizard.
5.5.1 "Element Selection" Page

Measurement elements are selected and their parameters are edited here.
Figure 5.14 "Element Selection" Page
AA-6800/6650
5.5 [Parameters]
<Select Elements> When adding an element to be measured, click on this button. ThenLoad Parametersdialog box opens. <Edit Parameters> Select an element row and click on this button. Then the measurement property sheet opens. For details, refer to section 5.6. NOTE After selecting an element row, click on the right mouse button. Then a selection of Stop/Continue at the end of measurement can be set up. <Up> Select an element row and click on this button. Then the row moves up one row upper. <Down> Select an element row and click on this button. Then the row moves down one row lower. <Delete> If you want to delete a row, click on the row to make its color reversed and then click on <Delete>. When the lamp of selected element is lit on, you can t delete it. Please turn off the lamp in "Optics Parameters" page for current measurement element or [Instrument]-[Lamp Status] menu and delete the element. <Connect> Communication between the personal computer and AA main unit is built. For details, refer to 5.8.1. [Measurement Element] Select the element to be measured first from the drop-down list. The measurement is started from this element and performed to the last row in order.
5
5-19
AA-6800/6650
5.5 [Parameters]
5.5.1.1 "Cookbook" page In theCookbookpage, select the target element from the drop-down list. Also, select the method from flame or furnace and select the hollow cathode lamp type from normal or SR in this page. At this time, description of each parameter to be set is displayed on the screen. Since the contents of this cookbook has been written in the program beforehand, you cannot make a change.
5
5-20 AA-6800/6650
Figure 5.15 "Cookbook" page

<Periodic Table> Click on this button, then you can select the target element from the periodic table or element list. [Using ASC] When using the autosampler, put a check mark in the check box. [HVG] and [MVU] Putting a check mark in the check box calls the parameters for using the hydride vaporizer unit (HVG) or the mercury vaporizer unit (MVU). This check box gets active when the element measured by the cold vapor mercury technique or the hydride vapor technique is specified.
5.5 [Parameters]
5.5.1.2
"Template" page
5
Figure 5.16
"Template" page
In the "Template" page, a template (*.taa) already created can be read. Click on <Browse> to open the "Open" dialog box. Then specify the [Look in] and [File name] and click on <Open>. When the template is opened, Figure 5.16 is displayed. Click on the element in [Element Selection] to highlight it, then the description of parameters for the element are displayed in the right side of the element. When the template contains plural elements, you can specify the element to read the parameters. Put a check mark in the check box next to the element name only for the element you need. Clicking on <OK> returns to the "Element Selection" page. You can check that the selected element name is added in the measurement order field. When using a wavelength or flame type which is different from that in the "Cookbook", it is convenient to create a template (*.taa) with the parameters beforehand. In WizAArd, "Cookbook.taa" (flames for Ca, Pb and Sn) and "HyperLamp.taa" (hyperlamps for As, Se, Sb and Pb) are already prepared.
5-21 AA-6800/6650
5.5 [Parameters]
5.5.2 "Preparation Parameters" Page

You can set the calibration curve parameters and the preparation parameters for standard / unknown / periodic blank samples.
5
5-22 AA-6800/6650
Figure 5.17 "Preparation Parameters" Page

Double-click on the element to be edited, or select the element row and click on <Edit> to open the "Edit Preparation Parameters" dialog box.
Figure 5.18 Edit Preparation ParametersDailog Box
5.5
[Parameters]
[Measurement Type] Select either of "Calibration Curve" (calibration curve method) or "SMSA (Simple Method of Standard Addition)". In this case, the "MSA (Method of Standard Addition)" cannot be selected. To set the calibration curve parameters for MSA (Method of Standard Addition), refer to 4.9. [Order] and [Zero Intercept] Select the order of calibration curve polynomial. You can select 1st, 2nd or 3rd. Putting a check mark to [Zero Intercept] will force the calibration curve to pass through the origin. When the simple standard addition method is selected, 1st order without Zero Intercept are automatically set, and these items are not displayed on the screen. [Conc. Unit] Set the concentration unit used for [True Value] and [Conc.] in MRT work sheet.
5
[Load] A preparation parameter file (*.mix) already saved can be loaded. Clicking this button opens the "Open" dialog box. Specify the [Look in] and [File name] and click on <Open>. In a preparation parameter file(*.mix), the following parameters are saved together; Parameters (A) (B) (C) (D) Measurement Type (Calibration Curve Method or SMSA) Mixing ON/OFF Preparation Parameters (STD, Unknown, Blank) Reagent Name Reagent Position Intake Order (E) Coating and Boost Cycles Coating and Boost Cycles Dialog Box Reagent Setup Dialog Box Edit Preparation Parameters Dialog Box Edit Preparation Parameters Dialog Box Screens Edit Preparation Parameters Dialog Box
A file which was created under different conditions((A)Measurement Type and (B)Mixing ON/OFF) from the current setting cannot be loaded. [Save] The current preparation parameters are saved in the file. Clicking this button opens the "Save As" dialog box. Specify the [Save in] and [File name] and click on <Save>. For contents to be saved, refer to the [Load] described above.
5-23 AA-6800/6650
5.5 [Parameters]
5.5.2.1
Weight Correction Factors
The factors used for calculating the actual concentration are set here. NOTE Actual concentration is calculated with the following equation. Actual Conc. = (Measured Conc.) [Volume Factor] [Dilution Factor] [ASC Dilution Factor][Correction Factor][Weight Factor] However, there is no particular function to set units for [Weight Factor] and [Volume Factor]. Note that the entered values are only calculated using the above equation. Use [Correction Factor] to convert the unit. [ASC Dilution Factor] is a value automatically set by the software to correct a change of the actual dilution factor when the preparation parameters are changed automatically by the software in the case of "Auto Dilution and Remaseurement" (refer to 5.6.9(4)). 5.5.2.2 [Preparataion Parameters]-[Standard Samples] The standard sample preparation parameters are set here. (when the ASC is not used, only the [Conc.] field on the table is set). [Number of STD] Enter the number of standard samples to be measured. Maximum 8 can be entered. The row number of the [Preparation Parameters]-[STD Samples] table displayed on the screen is set by this number. [Conc.] Enter the concentrations of standard samples in the order of measurement. [Pos.] In the case of calibration curve method, enter the position (1 to 60, R1 to R8) of standard sample. In the case of simple standard addition method ("SMSA"), enter the position (1 to 60, R1 to R8) of unknown sample to which the standard sample is added. [Standard(L)] Enter the volume of standard sample. In the case of simple standard addition method ("SMSA"), the indication in this field becomes [Sample]. Enter the volume of unknown sample to which the standard sample is added. When performing the sample preparation using the connected autosampler in furnace method, set the following items in addition. [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] Enter the volume to be used for mixing. The titles of these fields are changed depending on the settings in the "Reagent Setup" dialog box and "Coating and Boost Cycles" dialog box. The upper line indicates the reagent name and the lower indicates the position on the ASC. When a reagent is set to be used for coating, the position is enclosed by [ ] (brackets). This indication is common for [Preparation Parameters]-[Unknown Samples] and [Preparation Parameters]-[Blank Samples].
5
5-24
AA-6800/6650
5.5 [Parameters]
[Total Vol(L)] Total volume of solutions to be mixed is calculated and indicated. The reagent volume used for coating is not included in this total volume. NOTE When using the ASC, put a check mark in the check box of [Using ASC] in "Sequence" page of "Edit Parameters" dialog box. 5.5.2.3 [Preparation Parameters]-[Unknown Samples] [Sample(L)] Enter the sample volume to be used for mixing. [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] Enter the volume to be used for mixing. [Total Vol(L)] Total volume of solutions to be mixed is calculated and indicated. The reagent volume used for coating is not included in this total volume. 5.5.2.4 [Preparation Parameters]-[Blank Samples] Set how many every samples the periodic blank is inserted at the time of automatic creation of measurement schedule. When using the ASC in furnace method, set the preparation parameters for blank sample in addition. [Periodic Blank] Selecting "On" will insert a blank measurement periodically at the time of automatic creation of measurement schedule. [Meas. Interval] For example, entering "5" will insert the blank measurement row after every five unknown sample rows. [Pos.] Set the position (1 to 60, R1 to R8) of blank sample when using the ASC. In furnace method, set the following items in addition. [Sample(L)] Enter the sample volume to be used for mixing. [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] Enter the volume to be used for mixing. [Total Vol(L)] Total volume of solutions to be mixed is calculated and indicated. The reagent volume used for coating is not included in this total volume.
5
5-25 AA-6800/6650
5.5 [Parameters]
5.5.2.5
Mixing Setup and Reagent Setup
When the [Using ASC] is checkmarked and the furnace method is selected at the [Element Selection] page, you can use the <Mixing>, <Reagent> and <Coating> buttons. First, put a check mark in the check box of "Mixing ON" then click on <Mixing> button. Then the "Mixing Setup" dialog box will open.
5
5-26 AA-6800/6650 Figure 5.19 "Mixing Setup" Dialog Box
[Rinse with Sample] This sets the type of rinsing to be conducted in this mixing port prior to mixing. Rinsing with sample refers to the use of sample to rinse the mixing port based on the set mixing conditions, after first rinsing with rinse liquid. This sample liquid is discarded and is not used for measurement. This method is used in high accuracy measurement to prevent the diluting of measurement sample with the very small amount of rinse liquid remaining after rinsing with rinse liquid. With this method, however, the rinse time is doubled and the amount of sample required is increased. [Volume] When mixing is set to ON, the volume of mixed sample set here is drawn into the ASC nozzle and injected into the graphite tube. Determine the injection volume in consideration of the total volume of mixed sample in the mixing port and the maximum number of repeat measurement. When mixing is set to OFF, the [Total Vol] in the sample preparation parameters becomes the volume to be injected into the graphite tube. [Speed] This sets the speed at which the sample is injected into the furnace. The default value is 25 (L/sec).
5.5 [Parameters]
Clicking on <OK> after completing the setup returns to "Edit Preparation Parameters" dialog box. Clicking on <Reagent> opens "Reagent Setup" dialog box.
5
Figure 5.20 Reagent SetupDialog Box
[Reagent Name], [Reagent Position] and the intake order of sample and reagents can be set here for four kinds of reagents. 5.5.2.6 Coating and Boost Cycles (only for furnace method)
Pressing <Coating> button opens the "Coating and Boost Cycles" dialog box.
Figure 5.21 "Coating and Boost Cycles" Dialog Box.
5-27 AA-6800/6650
5.5 [Parameters]
Coating means injecting a specified reagent into the furnace and drying it prior to the sample injection (coating the tube surface). First, the checkmarked reagent is injected in the furnace, and heating is executed up to the furnace program stage specified in [Last Coating Cycle]. After this, the sample is injected. Furnace boost cycle refers to the repetitive cycle of sample injection into the furnace, and drying and ashing of the sample in order to raise the concentration of the target element in the sample. Repeating this boost cycle enables measurement of the sample whose concentration is lower than the quantitation range by concentrating it and raising its absorbance to the quantitative range of the calibration curve. For details on the setting items, refer to 5.5.9.1.
5
5-28
NOTE
When "NONE" is selected for the reagent position, the reagent is not used in the setting and not displayed on the MRT, and it is excluded from the calculation of total volume of the preparation. This change has an effect on the entire one schedule. If the reagent position is changed to or from NONE in the middle of the schedule measurement, the displayed/printed total volume in the sample data already measured is also changed to be different from the actual volume. Therefore, when quitting a use of the reagent in the middle of one schedule, do not use NONE but set the reagent volume to zero.
5.5.2.7
Repeat Measurement Conditions
Pressing <Repeat Conditions> button opens the "Repeat Measurement Conditions" dialog box.
Figure 5.22 "Repeat Measurement Conditions" Dialog Box.

Repeat measurement conditions are set here. For details on the setting items, refer to 5.6.2. The maximum number of repetition set here has a relation to the preparation parameters setup.
AA-6800/6650
5.5
[Parameters]
5.5.3 "Sample ID" Page

Number of unknown samples to be measured, sample names and sample positions for connected autosampler are set in the screen.
5

[Number of Samples] Enter number of unknown samples here. Then the rows as much as the sample number are created in the table. For each sample, the following setup are available. [Sample ID] Enter the name to identify the sample. In theSummaryof MRT work sheet, concentration result of each element is listed based on this sample ID, then the summary report of plural elements are created for each sample. NOTE In the case of simple standard addition method, the position setting for the 1st sample is ignored because the 1st unknown sample is measured by the method of standard addition. The 1st sample position is set as the item of [STD Samples] preparation parameters inEdit Preparation Parametersdialog box. [Pos.] When using the autosampler, set the sample position on the sampler turn table. <Collective Setup> Clicking on this button opensSample ID Collective Setupdialog box. In this dialog box, the sample ID described above can be easily entered.
5-29 AA-6800/6650
5.5 [Parameters]
5
5-30 AA-6800/6650

This dialog box is used to set sample ID with successive No. automatically and ASC start position for the autosampler. When completing the settings, click on <OK>. [Number of Samples] Enter the number of unknown samples. [Create Sample ID] Marking a check in this box allows to enter sample ID automatically. [Name] Enter a common sample name here. [Start No.] Enter the first number of successive number. [ASC Start No.] Enter the measurement start position on the autosampler turn table when using the ASC. Successive numbers are set as much as the number of samples.
5.5 [Parameters]
5.5.4 "Sample Selection" Page

Specify the elements to be measured for each sample.
5
Figure.5.25 "Sample Selection" Page

Place a mark in the cell of element to be measured and delete a mark from the cell of element not to be measured. When selecting plural cells, drag them and click on the right mouse button to select "Measure/Not Measure".
5.5.5 "Connect to Instrument/Send Parameters" Page
Figure 5.26 "Connect to Instrument/Send Parameters" Page 5-31 AA-6800/6650
5.5 [Parameters]
<Connect/Send Parameters> Communication between the personal computer and AA main unit is connected. If the communication connection has been already completed, this button is invalid. For details, refer to the section 5.8.1. <Connect Options> If the power of ASC or GFA is not ON when connected to the instrument, these options are not recognized. At that time, turn on the power of ASC and GFA then click on this button. [Meas. Element] Select an element whose parameters are to be set in the following "Optics Parameters" page and "Atomizer/Gas Flow Rate Setup" or "Furnace Program" page.
5
5-32
5.5.6
"Optics Parameters" Page
Wavelength, slit width, socket number, lamp current, lamp mode, lamp ON/OFF are set for the selected element. Since the default values in the "Element Selection" page of Wizard are automatically set, you don t have to change wavelength, slit width or lamp current. Select lamp mode according to the sample to be analyzed.
AA-6800/6650
5.5 [Parameters]
[Wavelength] The analysis wavelength is selected. As the default value, the wavelength of first resonance line (analysis line of the highest absorption sensitivity) is displayed. To use another wavelength, enter the value in the range of 190.0 to 900.0 (nm). When Line Search is executed, the wavelength is automatically set to this value. [Slit Width] The slit width of monochromator is set. A slit width used ordinarily is displayed. If the light intensity of hollow cathode lamp is weak and if there is too much baseline noize, widen the slit width slightly. Note that in the BGC-D2 mode, it is necessary to consider the balance between the light intensities of the deuterium lamp and the hollow cathode lamp. If the light intensity of the deuterium lamp is too great, narrow the slit width slightly. Conversely, if the light intensity of the hollow cathode lamp is too great, widen the slit width slightly.
5
NOTE
When a neighboring line exists, note that the neighboring line may not be separated if the slit width is widened.
[Socket #] Enter the socket number to which the hollow cathode lamp of the selected element is mounted. [Lamp Current (Low, High)] The lamp current is entered here. A recommended current has been entered already. If you want to change the lamp current, enter the current value not exceeding the maximum lamp current value according to the instruction manual of the hollow cathode lamp. Lamp is automatically lit with the specified current value when executing <Line Search>. The [Lamp Current (High)] is valid only when the [Lamp Mode] is "BGC-SR". When the lamp current is changed, it is actually reflected on the instrument in the following cases. When the line search/beam balance is executed. When the Parameters sheet or Wizard is closed with "OK"/"Finish" (except when a necessary line search is cancelled). The lamp current of warmup lamp is changed only when <Apply> is clicked in the [Select Warmup Lamp] dialog box after <Warmup> is clicked in the [Optics Parameters] page of the main element lamp. [Lamp Mode] The following five modes are available (Also refer to the section 3.1.8). EMISSION mode This mode is used in flame emission analysis or when performing lamp or burner positioning adjustment. A value proportinal to the intensity of light incident upon the detector is displayed. In flame emission analysis, energy intensity of emission spectrum of the target element generated in flame is measrued without using the hollow cathode lamp.
5-33 AA-6800/6650
5.5 [Parameters]
NON-BGC mode This mode is used for atomic absorption analysis that does not require background correction, or atomic absorption analysis in the long wavelength range (430 to 900nm) where background correction by deuterium lamp cannot be used. The deuterium lamp does not light, so only the light of hollow cathode lamp is used. Transmission amount of lamp energy that passed the atomizer unit is detected and then is converted into absorbance. If molecular absorption other than the atomic absorption exists on the same wavelength of the target element, such absorption is simultaneouly observed. In such case, use BGC-D2 mode or BGC-SR mode. BGC-D2 mode This mode is used for atomic absorption with background correction by deuterium lamp. If
5
5-34
molecular absorption other than the atomic absorption exists on the same wavelength of the target element, true absorbance cannot be obtained in NON-BGC mode. In such case, make the light of deuterium lamp together with the light of hollow cathode lamp pass through the atomizer unit. Though the light of deuterium lamp cannot detect atomic absorption of narrow band, it can detect absorption of wide band such as the molecular absorption. Accordingly, it is possible to get true absorbance by taking difference of absorbances at the both lamps. BGC-SR mode Background correction is performed using the phenomenon of Self-Reversal of the spectrum when a hollow cathode lamp is used at a high current value. This mode is effective for a measurement of sample causing a spectral interference or in long-wavelength range (430nm900nm) in which the deuterium lamp cannot be used. CAUTION To use the BGC-SR mode, the SR lamp (L2433 series) is necessary. If a normal lamp is lit on in the BGC-SR mode, it may be damaged. D2 mode The absorbance measured by using the deuterium (D2) is displayed. Generally, this lamp is used to measure absorbance value of molecular that gives a broad absorbance spectrum. [Lamp Status] When the Line Search is not finished or when wavelength or slit width is changed after execution of Line Search, "Line Search is necessary" is indicated. When lamp current or lamp mode is changed after executuion of Beam Balance, "Beam Balance is necessary" is indicated. If the <Line Search> button is pressed while these are indicated, the Line Search/Beam Balance is appropriately executed. When closing the "Optics Parameters" page with <Next> or <Finish> button, a message appears to ask whether to execute the Line Search/Beam Balance or not. Execute it, if necessary. [Lamp ON] Click on the check box to put a mark in it. Then the hollow cathode lamp of specified socket number is lit on. When a check mark is already indicated, clicking on the check box will delete the check mark and the lamp is turned off. The lamp will be automatically lit on when the <Line Search> is executed even if
AA-6800/6650
5.5
[Parameters]
the this [Lamp ON] is OFF. [ASC Sample Pos. for EMISSION Line Search] In flame emission analysis, <Line Search> can be performed while spraying a sample automatically using the ASC. Set the position of the sample (ordinarily, the standard sample of the highest concentration) on the ASC turntable. This setting is valid only when the lamp mode is EMISSION and [Lamp Current (Low)] is "0". 5.5.6.1 <Lamp Pos. Setup> button It is necessary to set the hollow cathode lamp to be used and its socket No. beforehand. Clicking on this button opens the "Lamp Position Setup" dialog box in Figure 5.28. Enter the element symbol of the lamp to be set in each socket No. The "*" mark is used as a wild card. When using a multi-element lamp, enter "*" instead of element symbol. Also, an element can be selected from the drop-down list displayed by clicking [Element]. In [Lamp type], select the correct type of hollow cathod lamp to be used.
5

While this dialog box is displayed, you can turn the lamp turret and change the lamp.
5-35 AA-6800/6650
5.5 [Parameters]
5.5.6.2 <Warmup Lamp> Button Set the items to warm up the hollow cathode lamp of the element to be measured next. Clicking on this button opens the " Select Warmup Lamp" dialog box. First, select an element in [Schedule].
5
5-36 AA-6800/6650
Figure 5.29 "Select Warmup Lamp" Dialog Box

Next, click on <Aplly>, then the parameters, [Socket #] and [Lamp Current], loaded in the element selection are automatically set and the lamp is lit ON. If you don't want to light on the lamp here, select [Schedule] then click on <OK>. NOTE Be sure to combine appropriately odd/even or even/odd socket numbers in "Optics Parameters" and "Warmup Lamp Setup". If odd/odd or even/even socket numbers are combined, the lamp warmup cannot be executed. When plural elements are selected in "Element Selection" page and autosampler is used, the instrument automatically judge and light on the warm-up lamp if no setting is made in this "Warmup lamp Setup" dialog box. In addition, according to the setting [Lamp Warmup Time] in "Sequence" page, the ending time is estimated and warming up of the hollow cathode lamp of the next measurement element is started. Therefore, when starting a measurement, the lamp of the next measurement element may not be lit on.
5.5 [Parameters]
5.5.6.3
<Line Search> Button
Clicking on this button opens the "Line Search/Beam Balance" dialog box. When the <Line Search> button is pressed in the "Optics Parameters" page of the currently measured element, the Line Search/Beam Balance is automatically executed, if necessary. If the Line Search/Beam Balance is already finished, only the result is displayed. When the element is not the currently measured element, only the result of the Line Search/Beam Balance execution is displayed.
5
Figure 5.30 Line Search/Beam BalanceDialog Box

<Close> When this button is clicked on, this dialog box is closed to return to previous screen. <Stop> If this button is clicked on during execution of line search, beam blance execution stops. <Do Line Search> Clicking on this button lights the lamp, scans wavelength near the set wavelength, and detects the highest peak in the emission profile according to the parameters set on [Optics Parameters] page. Scanning wavelengh is performed within the range of the set wavelength 0.5nm. When the correct peak is detected, "Line Search: OK" is indicated. Successively setup of lamp mode and optimization of detector sensitivity (beam balance) are performed. When the sensitivity setup is finished, "Beam Balance: OK" is indicated. NOTE When the Beam Balance is performed, in some cases, an error message indicating that hollow cathode lamp emission is too high or too low compared with D2 lamp emission. Change [Lamp Current (Low)] to a smaller value when it is too high, and change [Lamp Current (Low)] to a larger value when it is too low.
5-37 AA-6800/6650
5.5 [Parameters]
<Print> The result of Line Search is printed out.
5.5.7 "Atomizer/Gas Flow Rate Setup" Page (for flame method by AA-6800)
Parameters related to burner (burner height and fuel gas flow rate) are set in this screen. In the graph displaying real time data, the right mouse button menu can be used as in the real time graph of the main window (refer to section 4.6.5). (Only the [Properties], [Copy] and [Rader] are available.) 5.5.7.1 Atomizer Position
5
Figure 5.31 "Atomizer/Gas Flow Rate Setup" Page
When adjusting the burner position, select [Atomizer Position] by the radio button of [Operation Object]. Ignite a flame and introduce the sample. While monitoring the [Measured Data] indication or real time data, change the burner position upward and downward to search the optimum position. After entering the [Burner Height], click on the [Set Position]. Then the burner moves to the position. The distance from the optical path down to the burner is indicated in a positive value. Clicking on <Up> or <Down> moves the burner 1mm upward or downward. Since the [Burner Lateral] position has been adjusted prior to shipping, set it to zero ordinarily. If the lateral position should move with some reason, execute [Instrument]-[Maintenance]-[Burner Origin Position Adjustment] from the menu bar (Refer to the sections 5.8.6.3 and 6.1.1.1). [Burner Lateral] is used to lower the sensitivity of a particular element intentionally in the continuous measurement of plural elements. After clicking on <Fore>/<Back> or entering a numeric value directly, click on <Set Position>. Then the burner is moved forward or back. Search an appropriate lateral position to lower the sensitivity of the element while spraying the sample.
5-38 AA-6800/6650
5.5
[Parameters]
The data reproducibility is better when lowering the sensitivity by the burner angle setting instead of the burner lateral position setting. [Operation Object] Select the item to be adjusted. Select [Atomizer Position] when adjusting the burner position. Select [Fuel Gas Flow Rate] when adjusting the fuel gas flow rate. [Measured Data] The current measurement data is displayed. In the background correction modes, the indicated value as this [Measured Data] is the result calculated by subtracting the background data from the original measued data. [Background Data] In the background correction mode, the background data is displayed. [Burner Height] When the burner is below the optical path, the value is positive. You can enter the value in 1mm increments. This is automatically set when the parameters are called. [Burner Lateral] This is used to shift the position intentionally from the burner origin adjusted in Maintenance. For example, when lowering the sensitivity of a particular element intentionally in the full-auto continuous measurement of plural elements, enter a numeric value here. [Burner Angle] The burner angle may be entered as a comment. The burner angle can be adjusted manually by using the burner head angle adjustment lever. Usually, the burner angle is zero for ordinary use. Change the burner angle only when decreasing the sensitivity by changing the burner angle, for example, in the case of high-concentration sample. <Set Position> Enter the value to [Burner Height] or [Burner Lateral] and click on this button. Then the burner moves to the set position. <Auto Zero> The current indicated value is shifted to zero. <Up> This moves the burner upward. Each time this button is clicked on, the burner height value is decreased by 1mm. <Down> This moves the burner upward. Each time this button is clicked on, the burner height value is increased by 1mm. <Fore> This moves the burner forward. Each time this button is clicked on, the burner moves by 1 pulse of the pulse motor. <Back> This moves the burner backward. Each time this button is clicked on, the burner moves by 1 pulse of the pulse motor.
5
5-39 AA-6800/6650
5.5 [Parameters]
5.5.7.2 <Burner Position Auto> Button Clicking on this button opens the dialog box in Figure 5.32.
5
5-40 AA-6800/6650
Figure 5.32 "Optimum Burner Height Search" Dialog Box

This automatically searches for and sets the burner height which provides the maximum sensitivity based on the current gas flow rate setting. [Search Range] This sets the search range. Set the range within 0 to 25 mm. [Current Value] During the search, this displays the current burner height. After the search, the optimum position is displayed. <OK> After completing the search, click on this button to validate the burner height search result for use in measurement. The value displayed for [Current Value] will be set. <Cancel> This ignores the burner height search result, and returns to the previous setting. <Blank Meas.> This executes the measurement of blank sample. Set a blank sample, then click on this button. <STD Meas.> This executes the measurement of standard sample. Set a standard sample, then click on this button. <Stop> This interrupts and stop the search.
5.5
[Parameters]
5.5.7.3
Fuel Gas Flow Rate
5

When setting the flame type and the fuel gas flow rate, select [Fuel Gas Flow Rate] by the radio button of [Operation Object]. Ignite a flame and introduce the sample. While monitoring the [Measured Data] indication or real time waveform, change the fuel gas flow rate to search the optimum flow rate. After entering the [Fuel Gas Flow Rate], click on the <Flame Setup>. Then the gas flow rate is set to the value. [Flame Type] This is for selecting the type of support gas and fuel gas. Select the appropriate one from the dropdown list. [Fuel Gas Flow Rate] This is for entering the fuel gas flow rate. Enter the gas flow rate and click on <Flame Setup>. Then the gas flow rate is set to the value. Note that the setting range of fuel gas flow rate differs depending on the type of support gas. <Flame Setup> Click on this button after entering a value in [Fuel Gas Flow Rate], then the flow rate is set to the entered value. <Auto Zero> The current indicated value is shifted to zero. <Increase> Each time this button is clicked on, the fuel gas flow rate increases by 0.1L/min. <Decrease> Each time this button is clicked on, the fuel gas flow rate decreases by 0.1L/min.
5-41 AA-6800/6650
5.5 [Parameters]
5.5.7.4 <Gas Flow Auto> Button Clicking on this button opens the dialog box in Figure 5.34.
5
5-42 AA-6800/6650
Figure 5.34 "Optimum Gas Flow Rate Search" Dialog Box

This automatically searches for and sets the fuel gas flow rate which provides the maximum sensitivity based on the current burner height setting. [Search Range] This sets [Start] and [End] of search range. The setting range of fuel gas flow rate differs depending on the type of support gas. Set the range within 0.6 to 4.9 L/min for Air-C2H2, and 5.6 to 9.9 L/min for N2O-C2H2. [Current Value] During the search, this displays the current fuel gas flow rate. After the search, the optimum flow rate is displayed. <OK> After completing the search, click on this button to validate the fuel gas flow rate result for use in measurement. The value displayed for [Fuel Gas Flow Rate] will be set. <Cancel> This ignores the search result, and returns to the previous setting. <Blank Meas.> This executes the measurement of blank sample. Set a blank sample, then click on this button. <STD Meas.> This executes the measurement of standard sample. Set a standard sample, then click on this button. <Stop> This interrupts and stop the search.
5.5
[Parameters]
5.5.8 "Atomizer/Gas Flow Rate Setup" Page (for flame method by AA-6650)
Parameters related to burner (burner height and fuel gas flow rate) are set in this screen. In the graph displaying real time data, the right mouse button menu can be used as in the real time graph of the main window (refer to section 4.6.5). (Only the [Properties], [Copy] and [Radar] are available.) 5.5.8.1 Atomizer Position
5

When adjusting the burner position, select [Atomizer Position] by the radio button of [Operation Object]. Ignite a flame and introduce the sample. While monitoring the [Measured Data] indication or real time data, change the burner position upward and downward to search the optimum position. To change the burner height, use the knob for adjusting burner vertical position. Usually, the burner forward-back position is not changed. However, if the forward-back position is moved with some reason, adjust the forward-back position referring to 6.1.1.2. [Operation Object] Select the item to be adjusted. Select [Atomizer Position] when adjusting the burner position. Select [Fuel Gas Flow Rate] when adjusting the fuel gas flow rate. [Measured Data] The current measurement data is displayed. In the background correction modes, the indicated value as this [Measured Data] is the result calculated by subtracting the background data from the original measured data. [Background Data] In the background correction mode, the background data is displayed.
5-43 AA-6800/6650
5.5 [Parameters]
[Burner Height] When the burner is below the optical path, the value is positive. You can enter the value in 1mm increments. Use the knob for adjusting burner vertical position to adjust the burner height. [Burner Angle] The burner angle may be entered as a comment. The burner angle can be adjusted manually by using the burner angle adjustment lever. Usually, the burner angle is zero for ordinary use. Change the burner angle only when decreasing the sensitivity by changing the burner angle, for example, in the case of high-concentration sample. <Auto Zero> The current indicated value is shifted to zero.
5
5.5.8.2 Fuel Gas Flow Rate

When setting the flame type and the fuel gas flow rate, select [Fuel Gas Flow Rate] by the radio button of [Operation Object]. Ignite a flame and introduce the sample. While monitoring the [Measured Data] indication or real time waveform, change the fuel gas flow rate to search the optimum flow rate. After entering the [Fuel Gas Flow Rate], click on the <Flame Setup>. Then the gas flow rate is set to the value. [Flame Type] This is for selecting the type of support gas and fuel gas. Select the appropriate one from the dropdown list.
5-44 AA-6800/6650
5.5 [Parameters]
[Fuel Gas Flow Rate] This is for entering the fuel gas flow rate. Enter the gas flow rate and click on <Flame Setup>. Then the gas flow rate is set to the value. Note that the setting range of fuel gas flow rate differs depending on the type of support gas. <Flame Setup> Click on this button after entering a value in [Fuel Gas Flow Rate], then the flow rate is set to the entered value. <Auto Zero> The current indicated value is shifted to zero. <Increase> Each time this button is clicked on, the fuel gas flow rate increases by 0.1L/min. <Decrease> Each time this button is clicked on, the fuel gas flow rate decreases by 0.1L/min.
5
5-45 AA-6800/6650
5.5 [Parameters]
5.5.9 "Furnace Program" Page (for furnace method)

This is used to display or edit the conditions such as furnace heating temperature, furnace coating with reagent and concentration boost cycle. The furnace program may be displayed graphically in the screen. In the graph displaying real time waveform, the right mouse button menu can be used.
5
[Temp.] and [Time] Enter the furnace target temperature (0 to 3000) and heating time (0 to 300 seconds). [Heat Mode] SelectRAMP" or "STEP" by doubleclicking. When [RAMP] is set, the target temperature is attained at the end of this stage using fixed uniform heating throughout the stage. When [STEP] is set, heating is conducted so as to attain the target temperature immediately and maintain that temperature until the end of the stage. [Sensitivity] A high-sensitivity measurement is enabled by controlling the inner gas flow during the sample atomization. [Sensitivity] is a switch to set a high-sensitivity mode. To perform a high-sensitivity measurement, put a checkmark to the sensitivity field of atomization stage (at this time, the [Flow Rate] is fixed to 0 L/min) and delete checkmarks from other stages. In the report printing, this sensitivity switch status may be indicated as "HIGH" when it is "On", and as "REGULAR" when it is "Off".
Figure 5.37 "Furnace Program" Page
5-46 AA-6800/6650
5.5 [Parameters]
[Gas Type] Select "#1" or "#2" by doubleclicking. The GFA-6500 incorporates 2 gas line systems. Select the gas line system which you are going to use. Heating may be conducted by switching the gases at each stage. For example, when analyzing samples in an organic solvent, connecting oxygen to the Gas #2 line will allow you to use oxygen during the ashing stage to completely combust the organic materials. The gas lines are specified as follows. #1 #2 used for #1. [Flow Rate] This sets the inner gas flow rate in the range of 0 to 1.5 L/min (0.1 L/min increments). When [Sensitivity] is checkmarked, this is fixed at 0 L/min, this is fixed at 0 L/min. The outer gas flow rate is fixed. [Sample] Select "ON" or "OFF" by doubleclicking. When set to "ON", data is acquired during the heating time of that stage. Normally, this is set to "ON" in the atomization stage. Note that the "ON" setting can be used for only one stage. [Max. No. of Stages] Enter a numeric value (up to 20). The heating stages as many as the number can be programmed. [Sampling Stage No.] The data sampling is performed during the heating time of the stage specified here. Usually, the atomization stage is specified. [Graphite Tube Type] Select a type of Graphite tube. Note, however, that the setting here has no effect on acutal instrument operation. This is used only to be printed as a measurement parameter on the report. <Load> A furnace program file (*.fur) which has been already created can be loaded. Clicking on this opens "Open" dialog box. Specify [Look in] and [File name] and click on <Open>. <Save> The furnace program created in "Furnace Program" page is saved with a new file name. Clicking on this opens "Save As" dialog box. Specify [Save in] and [File name] and click on <Save>. <Insert Row> A row is inserted just before the selected row in the furnace program. <Delete Rows> The selected row in the furnace program is deleted. : : Ar on GFA rear panel ALT on GFA rear panel
When #2 is to be used, verify that gas tubing is connected to the ALT connector. Only Ar can be
5
5-47 AA-6800/6650
5.5 [Parameters]
5.5.9.1 <Coating/Boost Cycle> Button Clicking this button opens the "Coating and Boost Cycles" dialog box.
5
5-48
Figure 5.38 "Coating and Boost Cycles" Dialog Box.

Coating refers to injecting a specified reagent into the furnace and drying it prior to the sample injection (coating the tube surface). First, the checkmarked reagent is injected in the furnace, and heating is executed up to the furnace program stage specified in [Last Coating Cycle]. After this, the sample is injected. Furnace boost cycle refers to the repetitive cycle of sample injection into the furnace, and drying and ashing of the sample in order to raise the concentration of the target element in the sample. Repeating this boost cycle enables measurement of the sample whose concentration is lower than the quantitation range by concentrating it and raising its absorbance to the quantitative range of the calibration curve. [Coating by Reagent] This specifies a reagent to be injected into the furnace and dried prior to the sample injection. The reagent volume used for coating is displayed/printed in parentheses on the MRT or data print to show that this volume is not used for sample preparation. NOTE The coating setup is saved for each row on the MRT. This setup is reflected on the row when a new row is added on the MRT or when the sample or reagent volume is editted on the MRT. To change the coating setup for each row directly, use [Collective Edit] from [Edit] menu. [Last Coating Cycle] This specifies the stage to which the injected preceding reagent is heated and dried up in the furnace program.
AA-6800/6650
5.5
[Parameters]
[Number of Boost Cycles] This specifies the number of boost cycles. In normal analysis without boost cycles, set this value to "1". [Last Boost Cycle] Enter the last stage number of boost cycle. From the sample injection stage #1 to the last stage specified here, the concentration is boosted by the heating process for the specified number of sample injections. Note that a data sampling stage cannot be included during the concentration boost cycles. [Coating] This displays reagents to be precedently injected for coating and their intake order to the ASC if plural reagents are used. [Sample] This displays reagents to be injected together with the sample and their intake order to the ASC.
5
(Setup Example) Coating by Reagent Last Coating Cycle Last Boost Cycle Sampling Stage # : Reagent 1, Reagent 2 :2 :4 :6
Number of Boost Cycles : 3
With the above setting, the furnace program proceeds as below. Injection of Reagent 1 and Reagent 2 Stage 1 Stage 2 Injection of Sample, Dilutant and Reagent 3 Stage 1 Satge 2 Stage 3 Stage 4 Injection of Sample, Dilutant and Reagent 3 Stage 1 Satge 2 Stage 3 Stage 4 Injection of Sample, Dilutant and Reagent 3 Stage 1 Satge 2 Stage 3 Stage 4 Stage 5 Stage 6 (Measurement) 5.5.9.2 <Test Meas.> Button
Clicking on this button opens the "Test Measurment" dialog box.
Figure 5.39 "Test Measurement" Dialog Box 5-49 AA-6800/6650
5.5 [Parameters]
A test measurement is conducted in the "Test Measurement" dialog box to check whether the furnace program is appropriate or not. A peak profile of measurement result is displayed in the graph on the screen, but the data is not acquired. In the "Test Measurement" dialog box, you can select either of manual measurement or autosampler (measurement) by clicking on the radio button. When selecting the autosampler (measurement), enter the position of test sample and the preparation parameters. When completing the settings, click on the <Measure>. To rinse the mixing port, press <Rinse> button. The <Rinse> button is displayed only when the Mixing is set to On in the ASC parameters. 5.5.9.3 <Cleaning> Button
Clicking on this button opens the "Cleaning" dialog box.
5
5-50 AA-6800/6650
Figure 5.40 "Cleaning" Dialog Box

When the <Start> is pressed, the graphite tube is baked for cleaning according to the built-in heating program. Use "Test Measurement" together, if necessary. 5.5.9.4 <Change Graphite Tube> Button
Clicking on this button opens the Change Graphite Tube dialog box.
Figure 5.41 "Change Graphite Tube" Dialog Box.
5.5
[Parameters]
[Graphite Tube Heat Cycle Count] This indicates the heating times of the graphite tube. This number increases every after the tube is heated. After changing the graphite tube, reset it to "0". <Change Graphite Tube> This starts the procedure for changing the graphite tube and adjusting the sample injection position of ASC nozzle. Refer to the section 6.5.3 for details. <Graphite Tube Conditioning> A new pyrolytic coating graphite tube and a new platform tube must be heated repeatedly for conditioning. Be sure to perform the conditioning after a replacement for a new pyrolytic coating graphite tube(or a new platform tube). This conditioning is not necessary for high density graphite tube. After the conditioning, 10 is added to the furnace heating number.
5
<Stop Tube Conditioning> This stops the heating cycle of conditioning. Note, however, that 10 is added to the furnace heating number even if the conditioning is quitted halfway. <Auto Temp. Calib.> To obtain a precise temperature control in low temperature range, the heating temperature of the graphite tube is calibrated using a optical temperature sensor. Execute the temperature calibration immediately after replacing the graphite tube, or after executing the conditioning of pyrolytic coating graphite tube(or platform tube).
5-51 AA-6800/6650
5.5 [Parameters]
5.5.9.5 <Temp. Search> Button Clicking on this button opens the dialog box in Figure 5.40. Here, the measurement is automatically performed while changing the heating temperature condition little by little, and the data is automatically plotted in the graph on the screen. With this function, optimum atomization and ashing temperatures can be searched. In both of the right and left graphs on the screen, the right mouse button can be used.
5
[Step Width] Enter the increment step for search to change the heating temperature. [Current Value] Current temperature of the objective stage in the furnace program is indicated.
Figure 5.42 "Optimum Furnace Program Search" Dialog Box

[Objective Stage] Enter the stage No. for searching the heating temperature. [Single Stage] [2-Stage link] [3-Stage link] Successive stages up to 3 can be selected for search. Use the radio button for selection. This is used, for example, to set an ashing temperature when using a RAMP heating stage to raise it to a particular temperature and using a STEP heating stage to maintain the temperature. [Start] and [End] Set the search range.
5-52 AA-6800/6650
5.5 [Parameters]
In the temperature search measurement, you can select either of [Manual Measurement] or [Autosampler] (measurement) by clicking on the radio button. When selecting the [Autosampler] (measurement), enter the position of test sample and the preparation parameters. When completing all the settings, execute the measurement. The measurement result is plotted in the right graph on the screen. Judge the optimum heating temperature from this graph. The peak profiles are overwritten in the graph in center. <Measure> Before starting the measurement, the temperature calibration is executed. Note that heating is performed when the temperature calibration is executed, After setting the sample, click on this button. <Stop> This stops the search. NOTE After finding the optimum heating temperature, it is necessary to set and edit the table in "Furnace Program" page.
5
5-53 AA-6800/6650
5.6
[Edit Parameters]
Executing this opens the Edit Parameters dialog box . This is used to set each parameter individually without using Wizard. In this case, you can change the settings for the element of the MRT work sheet which you can select by clicking on the tab in the left lower of the main window. NOTE In the Edit Parameters, you can make a change or refererence only for the element selected on the MRT work sheet. When completing the setup for all the pages, click on <OK>. To cancel the setting halfway, click on <Cancel>. Then the settings return to the previous conditions before changed.
5.6.1 "Measurement Parameters" page
5
Figure 5.43. is displayed. The displayed contents are different according to the selection of flame/furnace.
Figure 5.43 "Measurement Parameters" page

(The upper figure is for flame measurement and the lower one is for furnace measurement.)
5-54 AA-6800/6650
5.6 [Edit Parameters]
Flame At the start of sample aspiration, the signal is not stable. The time required for introducing sample to the flame until the signal becomes stable is refferred to as pre-spray time.
Pre-Spray (Time)
Integration Time
5
Figure 5.44 Pre-Spray and Integration Time.
[Repetition Sequence] This will set whether pre-spray is conducted during repeat measurement. There are 2 types of settings. (S:Spray, M:Measure) SM-SM-.. measurement. In repetition sequence, pre-spray is conducted prior to each repetition of sample
Figure 5.45 Repetition Sequence (SM-SM-...)
5-55 AA-6800/6650
SM-M-M-... In repeat measurement, pre-spray is conducted only prior to the first repetition of sample measurement. Select this type when it is appropriate to continue spraying sample throughout the repeat measurements.
5
Figure 5.46 Repetition Sequence (SM-M-M-...)

5-56
NOTE
In the case of automatic measurement with the ASC, the instrument always operates as "SM-M-M-..." even if "SM-SM..." is selected as the repetition sequence.
[Pre-Spray Time] and [Integration Time] Enter the time interval to be used for pre-spraying and for signal integration (measurement time). The integration time (measurement time) will start directly after elapse of the pre-spray time. There is no integration of the signal during the pre-spray. [Response Time] This selects the time constant of signal response. The time constant of signal response corresponds to time constant in the Real Time Graph Monitor. That is to say, the signal profile displayed on the graph is affected by the response. In the case of #1, the profile is close to the actual signal profile. As the value increases from #1 to #4, the profile becomes more and more processed, as if a filter is applied. When excessive noise is a problem, settings in the direction of #4 will provide better repeatability.
AA-6800/6650
NOTE
[Pre-Spary Time] must be changed depending on the property of the sample. For example, take long [Pre-Spray Time] for sample with viscosity. If the absorbance of the sample is low, and liable to be affected by noise, take long [Response time]. In this case also, since it takes long time to become stable after spray of the sample, set the following time as [Pre-Spray Time] in standard operation.
Time until stabilization Response Time 1 : 3 sec. Response Time 2 : 5 sec. Response Time 3 : 10 sec. Response Time 4 : 20 sec.
5
Furnace [Signal Processing] As a measured value, you can select the peak height or peak area of the obtained waveform.
5.6.2 "Repeat Measurement Conditions" page

Number of repeat measurements is set here.
Figure 5.47 "Repeat Measurement Conditions" page
5-57 AA-6800/6650
[Blank] This row is for setting the repeat conditions for blank measurement. [Standard] This row is for setting the repeat conditions for standard measurement and standard addition measurement. [Sample] This row is for setting the repeat conditions for unknown sample measurement and simple standard addition measurement. [Reslope] This row is for setting the repeat conditions for sensitivity correction measurement. [Num. of Reps.] and [Max. Num. of Reps]
5
5-58
The number of repetition refers to the minimum number of measurement repetitions to be used in acquiring data. After completing this set number of measurement repetitions, the average value, relative standard deviation (RSD) and standard deviation are calculated. Then, the measurement repetitions will continue until (1) the RSD value limit is satisfied, (2) the standard deviation limit is satisfied, or (3) the maximum number of repetition is reached. Setup is possible up to 20 for each item. [RSD Limit] and [SD Limit] Both the RSD (Relative Standard Deviation) limit and the SD (Standard Deviation) limit are indicators of data scattering. If these values are small enough, the data is considered to be stable and the measurement results reliable. Normally, set the SD limit value to 0 and use only the RSD limit. However, since the average value is used as the denominator for the RSD limit, as shown in the following equations, a small value is difficult to attain when samples of low concentration are measured. In such cases, use the SD limit in addition to the RSD limit. After the set repetition number (Num. of Reps) is over, the average value, RSD and SD are calculated using the combination of set number of measured data which provides the smallest amount of data scattering. n Xi : Number of measurement data : Measured data (i=1 to n)
Average value : = Xi
n
SD RSD
: =
nXi2-(Xi)2 n(n-1)
: RSD= 100(%)
AA-6800/6650
5.6.3 "Weight Correction Factors" page

The following are set here. Factors used in actual concentration calculation. Actual concentration unit Decimal place of the factors and actual concentraion to display and print
5
Figure 5.48 "Weight Correction Factors" page

NOTE Actual concentration is calculated with the following equation. Actual Conc. = (Measured Conc.) [Volume Factor] [Dilution Factor] [ASC Dilution Factor][Correction Factor][Weight Factor] However, there is no particular function to set units for [Weight Factor] and [Volume Factor]. Note that the entered values are only calculated using the above equation.Use [Correction Factor] to convert the unit. [ASC Dilution Factor] is a value automatically set by the software to correct a change of the actual dilution factor when the preparation parameters are changed automatically by the software in the case of "Auto dilutin and Remeaseurement" (refer to 5.6.9(4)). [Weight Factor] Enter the sampling weight or sampling volume. [Volume Factor]] Enter the weight or volume after the sample is dissolved or processed and brought up to a specific volume.
5-59 AA-6800/6650
[Dilution Factor] Enter the dilution factor when the sample solution is diluted after brought up to the above specific volume. [Correction Factor] Arbitrary factor necessary for unit conversion can be set. [Actual Conc. Unit] Enetr a unit for actual concentartion. [Decimal Place] Set a decimal place for displaying and rounding the Weight Factor, Volume Factor, Dilution Factor, Correction Factor and Actual Conc. This decimal place is used for actual concentration calculation, the display on the screen and data print.
5
5-60
In the case of [Auto Dilution] (Dilution factor for automatic dilution and remeasurement), the decimal place is fixed to 6 for both for the display and actual concentration calculation.
5.6.4 "Y-axis Print Range" page

Enter the graph scale to print the peak profile with [File]-[Print Data/Parameters...].
5.6.5 "Analyst" page

Enter the analyst name and file comment. They are output when printing the parameter, and saved together with the file.
5.6.6 "Comment" page

Comment is added to the element name. When the same element is measured with different parameters, you can identify them with this comment. This comment is displayed in the element combo box on the main window and on the MRT work sheet tab together with the element name. Characters up to 10 can be displayed on the tab. If a line feed is included, however, only the characters before the line feed are displayed.
AA-6800/6650
5.6.7 "Sequence" page
5
Figure 5.49 "Sequence" page
[Using ASC] Put a check mark in the check box when using the ASC. [At the End of Measurement] When measuring plural elements successively, you can select to stop the measurement once at the end of each element or to continue the measurement. [Lamp Warmup Time] Set the hollow cathode lamp warmup time, which is a waiting time after lighting on the lamp and before starting the measurement, in the unit of minute. To select the lamp warmup time, check the time from lighting the lamp to stabilizing the signal while observing the real time graph in the flame measurement. Usually it is set to 5 to 30 minutes depending on the element and the lamp condition such as deterioration degree.
5-61 AA-6800/6650
5.6.8 "ASC Parameters" page

This page is displayed only for the furnace method.
5
5-62 AA-6800/6650
Figure 5.50
"ASC Parameters" page[Rinse with Sample]
This sets the type of rinsing to be conducted in this mixing port prior to mixing. Rinsing with sample refers to the use of sample to rinse the mixing port based on the set mixing conditions, after first rinsing with rinse liquid. This sample liquid is discarded and is not used for measurement. This method is used in high accuracy measurement to prevent the diluting of measurement sample with the very small amount of rinse liquid remaining after rinsing with rinse liquid. With this method, however, the rinse time is doubled and the amount of sample required is increased. [Mixing ON] If a check mark is put in the check box, the sample and reagent are mixed after being introduced into the mixing port. [Intake Speed] and [Discharge Speed] When the ASC-6100 is connected, the setting of [Intake Speed] is ignored. Mixing strength is set by [Discharge Speed]. Change the setting if necessary while considering the sample viscosity. Ordinarily, "150" is appropriate. This parameter is valid only when the [Mixing ON] is checkmarked. [Volume] When the mixing is ON, the volume of mixed sample set here is drawn into the ASC nozzle and injected into the graphite tube. Determine the injection volume in consideration of the total volume of mixed sample in the mixing port and the maximum number of repeat measurement. When mixing is set to OFF, the [Total Vol] (L) in the sample preparation parameters becomes the volume to be injected into the graphite tube. [Speed] This sets the speed at which the sample is injected into the furnace. The default value is 25 (L/sec). [Diluent/Reagent Name and Position] The ASC-6100 can mix one diluent and three reagents automatically. Set the prepared reagents on the
turntable and enter the position number. NOTE When "NONE" is selected for the reagent position, the reagent is not used in the setting and not displayed on the MRT, and it is excluded from the calculation of total volume of the preparation. This change has an effect on the entire one schedule. If the reagent position is changed to or from NONE in the middle of the schedule measurement, the displayed/printed total volume in the sample data already measured is also changed to be different from the actual volume. Therefore, when quitting a use of the reagent in the middle of one schedule, do not use NONE but set the reagent volume to zero. [Intake Order] This specifies the intake order of sample and reagents to the ASC nozzle. The order can be changed using the upward/downward arrow keys. The upper one is taken in (to the ASC earlier and injected later. Set the order considering the mixing of the reagents and sample.
5
5.6.9 "QA/QC Setup" page

In this page, select the ON/OFF of checking with each QC type, set the standard value, and select the action when the result is out of standard range. NOTE After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept and signal processing mode settings cannot be changed after the measurement. When these settings are expected to be changed after the measurement, set all the check boxes to OFF before starting the measurement.
Figure 5.51 "QA/QC Setup" page
5-63 AA-6800/6650
(1) The followings are the QC types. Correlation coefficient (= r) This factor indicates the degree of agreement of the measured point (data) with the calibration curve obtained by the least squares method. A value closer to "1" is desirable. The "r" is calculated using the following equation. r= Nxiyixiyi [Nxi2(xi)2] [Nyi2(yi)2]
1 2 1 2
Put a check mark in this check box, and set "CAL-CHK" in [Action] field after a series of STD measurements on the MRT work sheet to execute the evaluation by correlation coefficient. NOTE "CAL-CHK" setting is necessary only in the calibration curve method. In standard addition method and simple standard addition method, this setting is not necessary because the evaluation is done atMSA-RES .
5
5-64
LCS (QC Standard) (Laboratory Control Sample: Evaluation by standard sample) This is the evaluation using a standard sample with known concentration. The ratio between certified value and obtained value is calculated for evaluation. %R= Concentration 100 True Value In this case, "True Value" means a certified value. Set this value in [True Value] field on the MRT work sheet. Put a check mark in this check box, and set "QC" in [Action] field on the MRT work sheet to execute the evaluation by LCS. SPK (Spike) (Pre-Digestion Spike: Addition and recovery without pretreatment This evaluates the recovery degree of the amount added to the sample. It is calculated by the following equation. %R= SR SSRSR SA 100
: Measured result of sample without addition ([Conc.] value of UNK on the MRT work sheet)
SSR : Measured result of sample with addition ([Conc.] value of SPIKE on the MRT work sheet) SA : Amount of addition (Calculated value) (Enter this value in [True Value] field of SPIKE on the MRT work sheet) Mark a check in this check box, and set "SPIKE" in [Action] field after "UNK" whose recovery degree you wish to get on the MRT work sheet. It executes the evaluation by SPK. Sample Upper Limit Put a check mark in the "Sample Upper Limit" check box, the software evaluates whether the concentration of each sample is within the standard value. %RSD (Relative Standard Deviation) Put a check mark in the "%RSD" check box, the software evaluates whether the deviation of repeat
AA-6800/6650
measurement results of each sample is within the standard value. NOTE RSD Limit and SD Limit on the Repeat Measurement Conditions page are used as the standard value of %RSD. (2) The default (initial) standard values displayed on the screen are the values recommended by EPA (United States Environmental Protection Agency) method. However, the values can be changed. (3) Also, in the [Out of Control Remark], you can set " Stop Measurement " or " Mark and Continue" when each QC type value exceeds the range of standard value. Only for the [Sample Upper Limit], you can select "Auto Dilution and Remeasurement" in addition to "Stop Measurement" or "Mark and Continue".
5
NOTE
"Auto Dilution and Remeasurement" is valid only in furnace measurement.
(4) Auto Dilution and Remeasurement The function of Auto Dilution and Remeasurement is described here. The Auto Dilution and Remeasurement is a function to change the ASC preparation parameters automatically and perform a remeasurement so that the concentration may be near the center of the calibration curve (mean value of the highest and lowest concentrations of the standard sample). The change of preparation parameters at this time is automatically reflected on the [Auto DF] value in the MRT to correct the actual concentration calculation value. The actual functions are as below. 1) The ratio of the current value to the concentration of calibration curve center is obtained as an integral number. 2) When the order of the calibration curve is 2nd, and if the absorbance exceeds the top of the 2nd order equation and the concentration cannot be calculated, the above integral number is set to 10. 3) The sample volume is reduced according to the auto-dilution ratio. When the sample volume is reduced to the minimum value 2L, (A) the value is used as it is when the Mixing is Off. (B) the diluent volume and reagent volume are increased when the Mixing is On. In addition to the limitation that the minimum sample volume is 2L when the Mixing is Off, the following items are also limited. (1) The maximum auto-dilution factor is 100. (2) When the solution of the 2nd-order calibration curve equation is not found, the 10-time dilution is not repeated.
5-65 AA-6800/6650
5.6.10 "Calibration Curve Parameters" page
5
5-66 AA-6800/6650
Figure 5.52 "Calibration Curve Parameters" page

[Order] Select an order of calibration curve equation. You can select 1st, 2nd or 3rd. [Zero Intercept] Putting a check mark in the check box will create the calibration curve equation that forcibly intercepts the origin. When the standard addition method or simple standard addition method is selected, setup is made automatically to "1st" and "no zero intercept", and these items are not displayed. Correlation Coefficient calculation of calibration curve when Zero Intercept is selected When the order of the calibration curve is 1st, the correlation coefficient of the calibration curve is not changed by changing the selection of zero intercept. This may seem unnatural, but can be understood as follows. The correlation coefficient shows the relation of "increasing way" of two quantities. When the order of the calibration curve is 1 st, the increase is linear whether the zero is intercepted or not. Therefore, the relation of increasing way is also not changed (the slope of linear line has no relation with "Correlation").
[Conc. Unit] Unit of concentration used in MRT work sheet is set here.
5.6.11 "Optics Parameters" page

The contents are the same as the "Optics Parameters" page in Wizard (Refer to 5.5.6).
5.6.12 Atomizer/Gas Flow Rate Setup" page (Flame method)

The contents are the same as the "Atomizer/Gas Flow Rate Setup" page in Wizard (Refer to 5.5.7, 5.5.8).
5.6.13 "Furnace Program" page (Furnace method)

The contents are the same as the "Furnace Program" page in Wizard (Refer to 5.5.9).
5
5-67 AA-6800/6650
5.7
[Default Parameters]
This sets the parameters which are read in as initial values when creating a new file. The parameters for QA/QC setup, calibration curve parameters, repeat measurement conditions, measurement parameters and sequence can be set here. Contents and operation of each page are completely the same as those of the property sheet. Refer to the section 5.6.
5.7.1 [Flame]
The property sheet for flame default parameters is opened.
5.7.2 [Furnace]
The property sheet for furnace default parameters is opened.
5
5.7.3 [Graph]
"Graph Default Scale" dialog box is opened. The ordinate scale and the time width for real time graph can be set here.

5-68
Figure 5.53 "Graph Default Scale" Dialog Box 5.7.4 [Analyst]

"Default Analyst" dialog box opens. Enter [Analyst] and [File Comment] newly, then the entered contents are used when creating a new file next time.
AA-6800/6650
5.8
[Instrument]
The functions related to instrument hardware are summarized in this menu.
5
Figure 5.54 "Instrument" Drop-Down Menu
5-69 AA-6800/6650
5.8 [Instrument]
5.8.1 [Connect]
If this menu is selected, communication between the instrument and personal computer will be performed. After starting communication, first "Initialize" screen is displayed, where the instrument information (model, ROM version, serial No.) of AA/ASC/GFA and the progress of hardware initialization is sequentially displayed. Item under check is indicated in yellow, items successfully completed are indicated in green, items with failure are indicated in red. In takes several minutes to finish the initialization. The item "Start Leak Check" is displayed on the "Initialize" screen when the instrument applicable to a flame measurement (AA-6800F/AA-6650F) is initialized. Since a message prompting to check the fuel/support gas set pressure and the fuel gas flow rate is displayed before executing this item, check them when a flame measurement is to be used (refer to section
5
5-70
3.1.6). If all items are indicated in green, the initialization is correctly completed. Click on <OK> buttotn to close the screen. The items of [ASC Check] and [GFA Check] are indicated in red even if they are not connected with the AA main unit. When the ASC or GFA is not used from the first, it doesn't mean an abnormal status. When the communication is performed again while the power of instrument is ON, the slit, turret, burner up/down, burner fore/back and C2H2 valve are not checked. Also, when the gas leak check has been already finished, the gas leak check is not started and the item is indicated in green. In the case of AA-6800G or AA-6650G, the inidications of C2H2 valve origin search, gas leak check start, gas pressure monitor ON and flame monitor ON are not displayed. In the case of AA-6650, the items "Atomizer Up/Down" and "Atomizer Fore/Back" are not displayed.
Figure 5.55 "Initialize" Screen
AA-6800/6650
5.8 [Instrument]
After the "Initialize" screen is closed, "Instrument Check List for Flame Analysis" is displayed.
5
Figure 5.55_2 Instrument Check List for Flame Analysis

This screen is always displayed when the instrument applicable to a flame measurement (AA-6800F/AA6650F) is used (except when the GFA is connected and the gas leak check was not started). To use the instrument safely, always check these items displayed on this screen before igniting a flame. Put a check mark to the item already checked. When all the items have been checked, <OK> can be selected.
5-71 AA-6800/6650
5.8 [Instrument]
5.8.2 [Option Connect]

This indicates the connection status between the AA main unit and the peripheral attachments (ASC, GFA).
5
Figure 5.56 "Option Connect" Screen
<Connect> Click on this button when turning on the power of peripheral attachment (ASC, GFA) after the communication between the personal computer and AA main unit are completed.

5-72
5.8.3 [Configuration]
The PC communication port and the type of AA main unit are set here. Selecting this menu opens "Configuration" dialog box.
Figure 5.57 "Configuration" Dialog Box
AA-6800/6650
5.8 [Instrument]
[COM Port] The communication port on the PC is set here. Set the number of port to which the communication cable with the AA main unit is connected. [Instrument Type] This indicates the AA main unit model with which this software can be connected. [Instrument type is checked when connected] Putting a check mark in the check box will give an alarm if the connected instrument is different from [Instrument Type]. [Flame ASC Rinse Time] Enter a numeric value from 0 to 600 (seconds). When a numeric value except "0" is entered, the ASC executes the rinse for every sample. [Flame ASC Autozero in Rinsing] This function is used to set the baseline to zero frequently in the flame measurement with ASC. When this check box is set to ON, the auto zero is executed every after the rinse for each sample while keeping the rinse liquid aspirated. For example, when [Flame ASC rinse time] is set to "10 seconds", the auto zero is executed (for 10 seconds) after executing the rinse for 10 seconds. So the rinse liquid is aspirated for approx. 20 seconds in total. NOTE If the auto zero is executed with an insufficient rinse, the zero set is executed before the signal has not go back to the base, as the result, the measurement cannot be performed properly after that. Before using this function, check that the signal in the real time graph goes down to the base within the time set in [Flame ASC rinse time]. [Action setup when measurement is finished] This sets the Automatic Flame Extinction Yes/No and Automatic Lamp Extinction Yes/No when the measurement is finished. This action is also applied when "Stop" is selected for switching the element in measuring plural elements. This is valid only when using ASC. [Action setup when measurement is stopped] The measurement is stopped by QA/QC judging process. In this case, you can set "Automatic Flame Extinction YES/NO" and "Automatic Lamp Extinction YES/NO". These are valid only when using ASC. [Automatic Flame Extinction] Put a check mark in the check box to extinguish the flame automatically. [Wait Time] Enter a numeric value (minute) to wait before extinguishing the flame. In the automatic continuous measurement using the ASC and HVG, the hydrides are generated for a while after the measurement. If these hydrides are left in the absorption cell, the life of the absorption cell will be shortened. In order to purge the hydrides remaining in the cell, it is necessary to heat the absorption cell for a while after the measurement. Usually, 3 minutes is sufficient.
5
5-73 AA-6800/6650
5.8 [Instrument]
[Automatic Lamp Extinction] Put a check mark in the check box to turn off the lamp automatically. [Show Instrument Check List for Furnace Analysis] When this check box is set to ON, the list of the items to be noted before the furnace measurement is displayed at the start time of the software.
5
5-74 AA-6800/6650
Figure 5.58 Instrument Check List for Furnace Analysis

[Show performing temp. calib. warning message at start of furnace measurement] The temperature calibration is executed when starting the furnace measurement with <Start> button in the Main window or when starting the optimum furnace prorgram search. When this check box is checkmarked, a message appears to indicate a caution on executing this temperature calibration program or heating the furnace. When the check mark is deleted, the message is not displayed, but the temperature calibration itself is always executed. [Show lamp used time over operating life message] Put a check mark in the check box to check whether the lamp used time is over the specified lamp life or not. [Use Rounded ABS for calculation] The absorbance data is displayed or printed down to the fourth decimal place. The absorbance data kept in the internal memory is a little more precise. When this "Use Rounded ABS for calculation" is checkmarked, the displayed rounded value is used for the calculations such as "Average", "% RSD value", "Standard deviation", "Calibration curve polynomial expression" and "Quantitation of unknown sample". When the check mark is deleted, the value kept in the internal memory is used for these calculations. Although the calulation is performed more precisely when the check mark is deleted, the value kept in
5.8 [Instrument]
the internal memory cannot be known instead. As the result, the WizAArd software processing is like a black box, and the calculation process cannot be verified from the outside. If the "Use Rounded ABS for calculation" is checkmarked, the processing contents in the WizAArd software can be verified by a manual calculation with a calculator.
CAUTION
If this setting is changed, the calibration curve and quantitation result of the measured data are also changed. Take note of this when changing the setting. When [Rounded absorbance is used for calculation] and [Decimal place] are changed, the calibration curve and quantitation results of the data measured before will be changed. Also, if the QA/QC judgement is already executed at the time of data acquisition, the file of the data cannot be read in. Note this when changing these settings. In both cases, to recover the data at the time of the measurement, read in the file after changing the rounding settings back to the original ones used at the time of measurement.
5
[Decimal place] This sets a decimal place to which the absorbance is rounded. The rounding method is as follows. When the figure below the specified place is just 5, it is rounded down if the specified figure is even and rounded up if the specified figure is odd. In other cases, it is rounded off normally. Example: When the specified decimal place is 4 Average between 0.1234 and 0.1235 is calculated as follows. (0.1234 0.1235) 2 0.12345000.... 0.1234 Average between 0.1233 and 0.1234 is calculated as follows. (0.1233 0.1234) 2 0.12335000.... 0.1234 [Show meas. file created by older version WizAArd message] When an old measurement file created in old version WizAArd (ver.1.x) is opened, the values such as absorbance and concentration on the MRT worksheet are not completely compatible and may have some differences in decimal fraction. To keep a complete compatibility, it is necessary to open the measurement file from the old version WizAArd in which the file was created. To check whether the measurement file was created in old version WizAArd or not, set the [Show meas. file created by older version WizAArd message] check box to ON. Then a message appears when an old measurement file is opened.
5-75 AA-6800/6650
5.8 [Instrument]
5.8.4 [Lamp Position Setup]

Selecting this menu opens "Lamp Position Setup" dialog box. Enter the element symbol to be set to each socket number. "*" is used as a wild card. When using multi-element lamp, enter "*" instead of the element symbol. Clicking on the cell of the [Element] opens the drop-down list, from which you can select the element. Set the correct type of hollow cathode lamp to be used in [Lamp Type]. Setting the element and lamp type allows you to select a lamp ID in [Lamp ID] field. Select the lamp to be used. Selecting the lamp displays the judgement whether the lamp life is over or not, lamp life, used time and unit of used time. When the unit of the used time is mA*hrs, the use degree is calculated by the lamp current and the lighting time. When the lamp is lit at 10 mA for 10 hours for example, the used time is as follows.
5
5-76
10 (mA) 10 (hrs) 100 (mA*hrs) When the unit of used time is hrs, the lighting hour is directly used, and the use degree is 10 (hrs) in this example. If there is no item to select in [Lamp ID] field after you specify the element and lamp type, register the data for the lamp in "Lamp History" dialog box(Refer to the section 5.8.5). To clear the selected lamp, select "None" at the top of the drop-down list. Editting is not available for the lamp which is lit on. Turn off the lamp before editting. [OK] This closes the dialog box after changing and saving the lamp position setting. At this time, if the lamp whose use time exceeds the lamp life is selected, a warning message for checking appears. [Cancel] This cancels changing the lamp position setup and closes the diaolog box. [Print] This prints the table of lamp position setup.
AA-6800/6650
5.8 [Instrument]
5
5.8.5
[Lamp History]
Selecting this menu opens the "Lamp History" to register/delete/edit the lamp informations for the lamp life management in the data base.
Figure 5.60 "Lamp History" Dialog Box 5-77 AA-6800/6650
5.8 [Instrument]
A new lamp can be registered by entering a new lamp ID in [Lamp ID]. Firstly, set the element of the lamp in [Element]. The "*" mark is used as a wild card. When using a multi-element lamp, enter "*" instead of element symbol. Also, an element can be selected from the drop-down list opened by clicking [Element]. In [Lamp Type], select the correct type of the hollow cathod lamp to be used. Next, set [Lamp Life] and [Unit] referring to the manuals provided with the lamp to be used. The unit can be selected from "mA*/hrs" and "hrs". In the case of SR lamp, however, the unit is fixed to "hrs". Use [Comment] freely for anything such as date. When the unit of the used time is "mA*hrs", the use degree is calculated by the lamp current and the lighting time. When the lamp is lit at 10 mA for 10 hours for example, the use degree is as follows.
5
5-78
10 (mA) 10 (hrs) 100 (mA*hrs) When the unit of used time is "hrs", the lighting hour is directly used, and the use degree is 10 (hrs) in this example. Then the registered lamps can be selected in the "Lamp Position Setup". When the lamp is selected in the "Lamp Postion Setup", the used time of the lamp is accumulated. Once the accumulation of use time is started, the [Lock] is checkmarked for the lamp, and editting the fields except [Comment] is prohibited. For an edit, delete the check mark from the [Lock] or use [Clear] button to clear the accumulation content. For the lamp set to be used in "Lamp Position Setup", the accumulation cannot be cleared with [Clear] button, and the setting cannot be deleted with [Delete] button. To clear or delete the setting, delete the lamp from the "Lamp Position Setup". [OK] This saves the changed contents of the database and closes the dialog box. [Cancel] This cancels the changed contents of the database and closes the dialog box. [Clear] This clears the accumulation records of the lamps in the selected range, then the lamp information can be editted. The data of the lamp selected in the "Lamp Position Setup" cannot be deleted. [Print] This prints a table of the lamp registration data base.
AA-6800/6650
5.8 [Instrument]
5.8.6 [Maintenance]
Selecting this menu allows you to use the functions for maintenance of the instrument. 5.8.6.1 [D2 Lamp Position] This is used to adjust the position of deuterium lamp when replaced. For the replacing procedures, refer to the section 6.4.2. Selecting this menu displays the message "Adjust D2 lamp. First, adjust D2 lamp position roughly.". Set the D2 lamp approximately to the center position using the adjusting screw. Then the deuterium lamp is lit and "D2 Lamp Adjustment" Dialog Box opens.
5
Figure 5.61 "D2 Lamp Adjustment" Dialog Box

The bar graph and [Current] indicate the current absorbance value of D2 lamp. Adjust the D2 lamp position so that the absorbance value may become minimum. <Reset Max Min> Clicking on this button resets the values of [Max] and [Min]. 5.8.6.2 [Wavelength Adjustment] This executes the wavelength correction of monochromator automatically. It takes several minutes to execute this correction. Before execution, a message is displayed to check whether there is nothing interrupting the light beam in the atomizer unit. Click on <OK> to execute.
5-79 AA-6800/6650
5.8 [Instrument]
5.8.6.3
[Burner Origin Position Adjustment] (AA-6800)
This menu is used to adjust the burner up/down and fore/back positions. For the actual procedures, refer to the section 6.1.1.1.
5
Figure 5.62 "Burner Origin Position Adjustment" Dialog Box
[Moving Rate] This indicates pulse number for one movement. Select [Fast], [Middle] or [Slow]. <Fore> and <Back> Clicking on this button moves the burner by the pulse number set in [Moving Rate]. 1 pulse = 0.024mm <Up> and <Down> Clicking on this button moves the burner by the pulse number set in [Moving Rate]. 1 pulse = 0.012mm <Origin Memory> The current burner position is memorized as "fore/back=0, up/down = 0" in the AA main unit. <Autozero> This shifts the current indicated value to zero.
5-80 AA-6800/6650
5.8 [Instrument]
5.8.6.4
[Furnace Origin Position Adjustment] (AA-6800)
This menu is used to adjust the furnace up/down and fore/back positions. For the actual procedures, refer to the section 6.1.2.1.
5
Figure 5.63 "Furnace Origin Position Adjustment" Dialog Box

[Moving Rate] This indicates pulse number for one movement. Select [Fast], [Middle] or [Slow]. <Fore> and <Back> Clicking on this button moves the burner by the pulse number set in [Moving Rate]. 1 pulse = 0.024mm <Up> and <Down> Clicking on this button moves the burner by the pulse number set in [Moving Rate]. 1 pulse = 0.012mm <Origin Memory> The current furnace position is memorized as "fore/back=0, up/down=0". <Autozero> This shifts the current indicated value to zero.
5-81 AA-6800/6650
5.8 [Instrument]
<Line Search> This executes Line Search. [Move the furnace down to the lower position at the time of Line Search] Checkmarking the check box will move down the furnace beforehand at the time of Line Search so that the optical path may not be obstructed. Use this function when the furnace is out of position too much to execute Line Search. When the "Line Search/Beam Balance" dialog box is closed, the furnace position returns to the origin. 5.8.6.5 [Burner Origin Position Adjustment](AA-6650) In the case of AA-6650, the "Burner Origin Position Adjustment" dialog box cannot be used. Use
5
5-82
"Atomizer/Gas Flow Rate Setup" page when adjusting the burner position by observing the photometric value (refer to 6.1.1.2). 5.8.6.6 [Furnace Origin Position Adjustment](AA-6650) This menu is used to adjust the furnace up/down and forward/back positions. For the actual procedures, refer to the section 6.1.2.2.
Figure 5.64 "Furnace Origin Position Adjustment" Dialog Box
AA-6800/6650
5.8 [Instrument]
<Autozero> This shifts the current indicated value to zero. <Line Search> This executes Line Search. 5.8.6.7 [ASC Maintenance] This menu is used for maintenance related to the ASC. The maintenance related to the ASC is also described in the instruction manual for ASC-6100. 5.8.6.7.1 [Set Syringe Volume] After replacing the syringe, set the upper and lower position limits of the syringe plunger and the syringe volume.
5
Figure 5.65 "Set Syringe Volume" Dialog Box
5-83 AA-6800/6650
5.8 [Instrument]
Setting Procedures (1) Setting the upper position Move the plunger by using <Up> or <Down> button of [Move Plunger] so that it is set near 0L, as seen by the eye. Click on <Set Upper Limit> button to set the upper limit position. Note that the last position step must be finish on an up-stroke before clicking on <Set Upper Limit> button. This is to prevent backlash. (2) Setting the lower position Move the plunger by using <Up> or <Down> button of [Move Plunger] so that it is set near 230L, as seen by the eye. Click on <Set Lower Limit> to set the lower limit position. Note that the last position step
5
5-84 AA-6800/6650
must be finish on an up-stroke before clicking on <Set Lower Limit> button. This is to prevent backlash. (3) Volume Setting Enter the syringe volume in [Volume]. Enter a value determined by reading the syringe scale to find the difference between the plunger upper and lower limit positions. After entering the value in [Volume], click on <Set Volume> to fix the set syringe volume. Note that the volume setting is not executed if this button is not pressed. NOTE If the plunger is moved beyond the syringe upper and lower limits, the syringe motor gets out of step and as the result the syringe volume cannot be set properly after then. In this case, close this screen and power on the ASC again. After completing the option connection, set the syringe volume setup again. [Move Plunger] Select the plunger moving rate from [Fine (10 pulses)], [Coarse (600 pulses)] and [Specified Pulse]. When [Specified Pulse] is selected, you can enter and set the pulse number for one moving step. <Go to Upper Limit> This moves the plunger to the set upper limit position. After setting the upper limit position, you can use this to check whether the upper limit position is correctly set. <Go to Lower Limit> This moves the plunger to the set lower limit position. After setting the lower limit position, you can use this to check whether the lower limit position is correctly set.
5.8 [Instrument]
5.8.6.7.2
[Change Syringe]
5
Figure 5.66 "Change Syringe" Dialog Box
<Change> This is used to replace the syringe. Replace the syringe following the messages displayed on the screen sequentially. "Remove the syringe." "Fill the syringe with water and mount it to the instrument." <Fill> This is used to fill the rinse liquid in the syringe. Use this function after replacing the syringe or when bubbles are present in the syringe. Follow the messages displayed on the screen sequentially. The message "Is the tube tip soaked in the rinse bottle liquid?" appears. After checking, click on <OK>, then the plunger moves upward to finish filling. 5.8.6.8 [Maintenance only for service engineer]
Only the service engineers can use this menu.
5-85 AA-6800/6650
5.8 [Instrument]
5.8.7 [Lamp Status]

Selecting this menu opens "Lamp Status" dialog box and the status of the lamp currently used is displayed. This dialog box indicates how long the lamp has been lit on.
5
5-86 AA-6800/6650
Figure 5.67 "Lamp Status" Dialog Box

[Lamp Status] The lighting ON/OFF of the lamp is displayed. If the checkmark is deleted, the hollow cathode lamp can be turned off but cannot be lit on. D2 lamp can be lit on or turned off. [Lighting Time] Elapsed time of the lamp lighting is displayed. Once the lamp is turned off, it resets to 0. [Wait Time] When the warmup time is set, the rest of warmup time is displayed. If the measurement is started before the wait time becomes "0", the "Hollow Cathode Lamp Warmup Waiting" dialog box is opened to indicates the wait time. Clicking on <Start Measurement> in this dialog box ignores the waiting time and starts measurement.
Figure 5.68 "Warmup Waiting" Dialog Box
5.8 [Instrument]
[Warmup Lamp Status] When the rest waiting time becomes "0", "Completed" is displayed to indicate that warmup of the lamp is completed. When the lamp is not lit or when the specified warmup has not been completed, "Not Completed" is displayed. [D2 Lamp Warmup Time (min)] Enter the time necessary for warming up the D2 lamp in the unit of minute. Since the D2 lamp is once turned off when the line search is executed, the wait time set here is started after the line search/beam balance at the measurement start time is finished. During the wait time, the "Hollow Cathode Lamp Warmup Waiting" (or "D2 Lamp Warmup Waiting") dialog box is displayed. The sequence of the lamp warmup and line search/beam balance at the measurement start time is as follows.
5
Hollow cathode lamp and D2 lamp are lit on. Hollow cathode lamp is warmed up. Line search/beam balance is executed. D2 lamp is warmed up. Measurement is started.
NOTE
The warmup time of the hollow cathode lamp is set by selecting [Parameters]-[Edit Parameters]- "Sequence" page from the menu.
5-87 AA-6800/6650
5.8 [Instrument]
5.8.8 [Change Graphite Tube]

The "Change Graphite Tube" dialog box is opened. For details, refer to the section 5.5.9.4 for explanation of the dialog box and to the section 6.5.3 for procedure to exchange graphite tube.
5
Figure 5.69 "Change Graphite Tube" Dialog Box

5-88
5.8.9 [Gas Controller Status]

This displays the state of the gas leak check, the drain level and the fuel gas pressure.
Figure 5.70 "Gas Controller Status" Dialog Box

[Gas Leak Check] Displays the result of gas leak check. [Drain Level] Displays the status of drain tank level. [Fuel Gas Pressure] Displays whether the fuel gas pressure is appropriate or not. [Flame Monitor ON] When the check box is checkmarked, the extinguished flame safety device is valid. Normally, set the flame monitor "ON". Only in the case of Ar-H2 flame, however, set it off because the flame has no color and cannot be detected. When the AA software and the AA main unit are connected, the flame monitor is always set to ON at the time of initialization. Therefore, if you wish to invalidate the flame monitor safety device, set the flame monitor to OFF in this dialog box at every time of using the instrument.
AA-6800/6650
5.8 [Instrument]
NOTE
When the flame monitor is "OFF", the extinguished flame safety device doesn't operate. Stay near the instrument and always check that the flame is not extinguished. If the flame should be extinguished, press the EXTINGUISH button.
5.8.10 [Gas Leak Check]

This checks a gas leakage of the piping inside the gas controller. The gas leak check is usually performed at the initialization time of instrument, but can be performed by selecting this menu at any time if necessary. The message "Gas leak check will be started. Press the EXTINGUISH button on the instrument." is displayed. Following this instruction, press the EXTINGUISH button at the right of the combustion chamber, then click on <OK> on the message box to close the message. The instrument automatically starts the gas leak check of 10 minutes. After 10 minutes, the check result is indicated in a pop-up message box. If the gas leak check is finished before this, however, you can always ignite a flame within 10 minutes by pressing IGNITE button.
5
5.8.11 [Remaining Gas Combustion]

This menu is used to burn up acetylene gas in the piping from the gas main valve to the instrument by closing the main valve of acetylene gas during the combustion of Air-C2H2 flame. If the flame type is set to N2O-C2H2, you can't execute this procedure. Change the flame type to Air-C2H2 and retry it. CAUTION Be sure to follow the procedure below to perform the remaining gas combustion. If the procedure is compromised, a flashback may occur. (Procedure of Remaining Gas Combustion) (1) Set the supply pressure and setting pressure of the acetylene gas and air properly (refer to 4.8). (2) Select [Parameters]-[Edit Parameters] menu to open "Atomizer/Gas Flow Rate Setup" page when the measurement type of the current measurement element is set to flame in AA software. Select [Fuel Gas Flow Rate] radio button here, set "Air-C2H2" for [Flame Type] and click on <OK> to close the page. When using the high temperature burner, change the burner select key switch back to [AIR-C2H2] in the AA main unit. CAUTION Be sure to use Air-C2H2 flame to perform the remaining gas combustion. Using N2O-C2H2 flame may cause a flashback . (3) Press the IGNITE button to ignite a flame. (4) Select [Instrument]-[Remaining Gas Combustion] menu. The message in Figure.5.71 appears. Click on <OK>.
5-89 AA-6800/6650
5.8 [Instrument]
Figure 5.71 Remaining Gas Combustion - Message 1

(5) Next, the message shown in Figure 5.72 is displayed. Click on <OK> and close the main valve of the acetylene gas cylinder. At this time, don't stop the support gas (air) and continue to supply it in
5
5-90
the proper pressure. As the acetylene gas decreases, the gas pressure lowering alarm sounds (stop the gas pressure lowering alarm in the next (6)). Also, the AA software displays the message "Fuel gas pressure is too low". Click on <OK> to close it. NOTE When stopping the remaining gas combustion, click on <Cancel> in the message of Figure 5.72 without closing the main valve of the acetylene gas cylinder.

(6) Next, the message shown in Figure 5.73 is displayed. Since the support gas (air) flows out after the flame goes out, press the EXTINGUISH button of the AA main unit to stop the support gas (air). Also, press [BUZZER OFF] button on the gas controller panel to stop the gas pressure lowering alarm.
AA-6800/6650
5.8 [Instrument]
(7) Click on <OK> in the message of Figure 5.73 to close the message. With the above procedure, the remaining gas combustion is finished.
5.8.12
[Execute Line Search]
This is used to execute the line search for the element currently set. This function is the same as that of <Line Search> button in the "Optics Parameters" page.
5.8.13 [Cleaning]
By selecting this menu, cleaning of the graphite tube is performed. This function is the same as that of <Cleaning> button in the "Furnace Program" page.
5
5.8.14 [Rinse Nozzle]
The ASC nozzle rinse is executed in furnace measurement. This menu is disabled when current measurement is flame measurement.
5.8.15 [Flame Nozzle Position]

This is used to adjust the sample uptake position. Adjust the position of suction nozzle following the messages displayed step by step. To quit the position adjustment halfway, press the <Cancel>. Note, however, that the proper adjustment cannot be performed when the nozzle position adjustment is quitted halway. "Please set the ASC turn table for flame measurement and remove the sample suction nozzle from the arm. The ASC nozzle moves to sample intake position if you press OK button." "Please mount the sample suction nozzle and adjust the nozzle vertical position. Please press OK button after you finish the adjustment."
5-91 AA-6800/6650
5.8 [Instrument]
5.8.16
[Furnace Nozzle Position]
Firstly, the sample uptake position is adjusted. Adjust the position of suction nozzle following the messages displayed step by step. To quit the position adjustment halfway, press the <Cancel>. Note, however, that the proper adjustment cannot be performed when the nozzle position adjustment is quitted halway. "Please set the ASC turn table for furnace measurement and remove the sample suction nozzle from the arm. The ASC nozzle moves to sample intake position if you press OK button." "Please mount the sample suction nozzle and adjust the nozzle vertical position. Please press OK button after you finish the adjustment. The ASC arm moves to furnace position."
5
5-92
"Loosen the arm guide screw mounted onto the furnace and release the arm guide. Be careful not to change the arm guide position too much." Next, the "ASC Furnace Nozzle Position Adjustment" dialog box is displayed. The injection position is adjusted here.
Figure 5.74 "ASC Furnace Nozzle Position Adjustment" Dialog Box

Lower the nozzle to near the injection hole of the graphite tube, using the Up or Down button. Then, adjust the horizontal position forward,back, rightward and leftward using the injection position adjusting knob of the ASC table so that the tip of the nozzle comes almost to the center of the injection hole. After adjusting the horizontal position in every direction, move the nozzle to a proper injection position using the
AA-6800/6650
5.8 [Instrument]
Up or Down button then click on <OK> button. The position is set as the injection position. Clicking on <Cancel> button cancels setting the injection position. When quitting the setting at this step, note that the injection position is not set although the suction position is set. The message "Tighten the fixing screw of the arm guide" is displayed before this screen is closed. Tighten the screw of the arm guide previously loosened carefully so that the arm is not moved. [Fine (1 pulse)] [Coarse (30 pulses)] [Specified Pulses] Select a moving rate from these. When [Specified Pulses] is selected, a value 1 to 30 can be entered. [Current Pos.] The current nozzle position is displayed.
5
[Injection Pos.] The sample injection position currently selected is displayed. <Move Near to Tube> The nozzle is moved straight to the vicinity of graphite tube. When the injection position is largely shifted by a change of the furance position, care must be taken so that the tip of the nozzle may not be damaged. <Move Upward> <Move Downward> The nozzle is moved up or down at a specified rate.

5-93
AA-6800/6650
5.9
[Help]
Select this menu when using the help function.
5.9.1 [Search for Help on...]

By entering a key word in "Search for Help on..." dialog box, the help of a specified item can be searched.
5.9.2 [About WizAArd...]

Version and system information of this software are displayed.
5
5-94 AA-6800/6650
Chapter 6 Maintenance
6
Contents
Maintenance
6.1
Atomizer Positioning Adjustment 6-1 Burner Positioning Adjustment 6-1 AA-6800 6-1 AA-6650 6-2 AA-6800 6-3 AA-6650 6-3 6.1.1.1 6.1.1.2
6.1.1
6.1.2
Furnace Position Adjustment 6-3
6.1.2.1 6.1.2.2 6.2 6.2.1 6.2.2
Burner Maintenance 6-4 Cleaning the Burner Head 6-4 Nebulizer Maintenance 6-5 Cleaning the Nebulizer 6-5 Replacing the Polyethylene Tube 6-6
6.2.2.1 6.2.2.2 6.2.3 6.3 6.4
Cleaning the Chamber 6-7
Checking for Gas Leaks in Tubing 6-8 Replacing the Deuterium Lamp 6-9 Specifications of Deuterium Lamp 6-9 Replacing Procedures of Deuterium Lamp 6-9 High Density Graphite Tube 6-11 Pyrolytic Coating Graphite Tube 6-11 Replacing Procedure Using the ASC 6-11
6.4.1 6.4.2 6.5 6.5.1 6.5.2 6.5.3 6.6 6.7
Replacing Graphite Tube (GFA-6500) 6-11
Cleaning Graphite Cap, Holder, Window Plate Sockets and Window Plates (GFA-6500) 6-13 Cleaning the Temperature Sensor (GFA-6500) 6-16
AA-6800/6650
6.8 Cleaning the Slide Mechanism (GFA-6500) 6-17 6.9 Cleaning the Seal (GFA-6500) 6-18 6.10 6.11 GFA Performance Check (GFA-6500) 6-19 Maintenance Parts 6-21 AA-6800/6650 Maintenance Parts 6-21 GFA-6500 Maintenance Parts 6-22 For Flame Analysis 6-23 For Furnace Analysis (for GFA-6500) 6-23 For Furnace Analysis (for GFA-EX7) 6-23 Autosampler 6-23 Hollow Cathod Lamps (Single Element Lamps) 6-24 Hollow Cathode Lamps (Single Element Lamps, Usable for SR method) 6-26 Hollow Cathod Lamp (Multi-element Lamps) 6-27 Other Accessories 6-27
6.11.1 6.11.2 6.12 6.12.1 6.12.2 6.12.3 6.12.4 6.12.5 6.12.6 6.12.7
Special Accessories 6-23
6
Maintenance
6.12.8
AA-6800/6650
6.1
Atomizer Positioning Adjustment
6.1.1 Burner Positioning Adjustment 6.1.1.1 AA-6800

In the case of flame method, the burner moves automatically so that the burner head slot is positioned directly beneath the optical path. However, when the burner is dismantled for cleaning etc., the burner position must readjusted. The procedure is described below. (1) (2) Select an element which you usually use in flame method. In theOptics Parameterspage, set the lamp mode toEMISSIONand light on the lamp to perform the line search. (3) Returning to the main window displays the current measured photometric value. Rotate the lamp mounted in the turret and adjust the rotating position so that the indicated value may become maximum. (4) Select [Instrument]-[Maintenance]-[Burner Origin Position Adjustment] from the menu. Then Burner Origin Position Adjustmentdialog box opens. (5) Verify that the burner head is securely mounted. Then click on <Down> to lower the burner so that the burner may not interrupt the light beam. In addition, set the burner angle to 0. (6) Set the provided burner positioning jig at the center of the burner head so that the scale is facing the lamp. By using <Fore> and <Back> buttons, adjust front/back position of the burner so that the photometric data is at its maximum. (7) Without changing the direction of the adjustment jig, move it to the right end of the burner head and fix it in place. Then using the burner head angle adjustment lever, gradually rotate the burner head until you obtain the position where the displayed photometric value is at its maximum. (8) Once again, secure the positioning jig at the center of the burner head, and move the burner head front and back by <Fore> and <Back> buttons to determine the position where the photometric data is at its maximum. (9) Click on <Up> to set the burner height to 0 mm. Set a white paper on the burner facing the lamp. Adjsut the burner height so that the beam spot on the paper is semicircular (Figure 6.2). (10) Click on <Origin Memory>. Then the current burner position is memorized asFore/back = 0, Up/down = 0.
Burner head positioning jig Burner head
6
Maintenance
Burner head angle adjusting lever
Figure 6.1
Burner Position Adjustment 6-1 AA-6800/6650
6.1 Atomizer Positioning Adjustment
White paper Beam spot
Burner head
6
6.1.1.2 AA-6650
Figure 6.2
Burner Height Adjustment
The adjustment procedure, searching the most sensitive position of the burner front/back direction by using knobs for adjusting burner position (Refer to the section 3.1.4.2), is described below. (1) Select an element which you usually use in flame method. (2) In the "Optics Parameters" page, set the lamp mode to "EMISSION" and light on the lamp to perform the line search. (3) Returning to the main window displays the current measured photometric value. Rotate the lamp mounted in the turret and adjust the rotating position so that the indicated value may become maximum. (4) Select [Parameters] - [Edit Parameters...] from the menu, open [Atomizer / Gas Flow Rate Setup] page, and select [Atomizer Position] radio button. (5) Verify that the burner head is securely mounted. Then turn the knob for adjusting burner vertical position to lower the burner so that the burner may not interrupt the light beam. In addition, set the burner angle to 0. (6) Set the provided burner positioning jig at the center of the burner head so that the scale is facing the lamp. By using knob for adjusting burner horizontal position, adjust front/back position of the burner so that the photometric value is at its maximum. (7) Without changing the direction of the adjustment jig, move it to the right end of the burner head and fix it in place. Then using the burner head angle adjustment lever, gradually rotate the burner head until you obtain the position where the displayed photometric value is at its maximum. (8) Once again, secure the positioning jig at the center of the burner head, and move the burner head front and back by the knob for adjusting burner horizontal position to determine the position where the photometric value is at its maximum. (9) At this time, the most sensitive position of the burner front/back direction is specified. And adjust the burner height in accordance with each measurement parameter.
Maintenance
6-2
AA-6800/6650
6.1 Atomizer Positioning Adjustment
6.1.2
Furnace Position Adjustment

AA-6800
6.1.2.1
(1) Select an element which you usually use in furnace method. (2) In the "Optics Parameters" page, set the lamp mode to "EMISSION". Although the message "Line Search/Beam Balance is necessary" appears, press <Cancel>. (3) From the Menu, execute [Instrument]-[Maintenance]-[Furnace Origin Position Adjustment]. Then the "Furnace Origin Position Adjustment" dialog box is opened. (4) Next, after checkmarking the "Move the furnace down to the lower position at the time of Line Search." check box, click on <Line Search>. (5) After the furnace gets out of the optical axis position, the "Line Search/Beam Balance" dialog box is opened and the line search is executed. (6) When both line search and beam balance results are indicated as "OK", click on <Close>. (7) Using <Fore>, <Back>, <Up> and <Down> buttons, adjust the vertical and horizontal position so that the photometric data indicates the maximum value. (8) After adjusting the position, click on <Origin Memory>. Then the current furnace position is memorized as "Lateral = 0, Height =0".
6
Maintenance
6.1.2.2 position.
AA-6650
When changing the atomizer from the burner to the graphite furnace, it is necessary to adjust the furnace First, start the following procedure before mounting the graphite furnace on the optical path. (1) Select an element that you usually use. It doesn't matter which of the furnace method or flame method is selected. (2) In the "Optics Parameters" page, set the lamp mode to "EMISSION". Although the message "Line Search/Beam Balance is necessary" appears before returning to the main screen, press <Cancel>. (3) From the Menu, execute [Instrument]-[Maintenance]-[Furnace Origin Position Adjustment]. Then the "Furnace Origin Position Adjustment" dialog box is opened. (4) Next, click on <Line Search>. The "Line Search Beam Balance" dialog box is opened and the line search is executed (5) When both line search and beam balance results are "OK", click on <Close>. Then mount the graphite furnace (equipped with the graphite tube) on the light path. (6) Adjust the vertical and horizontal positions with the knobs manually so that the photometric data in the "Furnace Origin Position Adjustment" dialog box may indicates a maximum value. (7) Then the furnace position is adjusted properly. When only the graphite furnace is used without switching between the burner and the graphite furnace, the furnace position is not changed so much. Therefore, the procedure from (1) to (6) may be performed while keeping the graphite furnace mounted.
6-3 AA-6800/6650
6.2
Burner Maintenance
When foreign objects such as dirt and contaminants adhere to the burner head, nebulizer or chamber interior, the indicated value becomes unreliable and absorbance sensitivity is decreased. It is recommended that these burner components be periodically cleaned. The various O-rings at the joints connecting the burner head, nebulizer and disperser, etc. should also be replaced with new ones when they get deformed or decomposed. The procedure for cleaning components is shown below. CAUTION There are O-rings in all of the joints connecting the burner head, nebulizer and disperser, etc. Consequently, when you disassemble and then reassemble these components, make sure that the O-rings are in place and thoroughly check for leaks.
6.2.1 Cleaning the Burner Head
6
Maintenance
6-4
If the slot of burner head is clogged by carbide or salts etc., the reduction flame will have fine irregularities when the degree of blockage is small. When the slot is clogged more heavily, the flame splits as the left figure in Figure 6.3 (The figure is exaggerated to illustrate). Before the flame shows above state, extinguish the flame and rub the slot inner wall with thick paper or thin plastic plate to remove the stain.
Clogged
Normal
Figure 6.3
Flame Symptoms due to Clogged Slot
In some cases, orange colored flame may flicker when the burner is ignited again after above work. In such cases, spray pure water until flickering is not generated. If flickering does not easily disappear, remove the burner head from the chamber, wash the inside with pure water. If it is extremely dirty, soak it in acid or appropriate detergent over night then brush the slot inner wall. When measuring samples with high concentrations of coexistent components, such as salts etc, these will adhere to the slot inner wall. After measurement of such samples, be sure to perform cleaning described above. CAUTION Don't use metal brushes that may scratch the burner head.
AA-6800/6650
6.2 Burner Maintenance
6.2.2 Nebulizer Maintenance 6.2.2.1 Cleaning the Nebulizer

If the indication value fluctuates or the absorbance sensitivity decreased during measurement, the capillary of the nebulizer may be clogged by some contaminant. Clean the nebulizer in the following procedure. (1) Check that the flame is extinguished. Loosen the nebulizer fixing screw, pull the nebulizer retaining plate to upper right, and remove the SPRAY joint which is inserted into the nebulizer and then remove the nebulizer from the chamber. (2) Insert the provided cleaning wire into the capillary and brush out the inside. (3) After mounting the nebulizer by reversing the procedure (1), spray pure water. If no improvement is seen after performing the above operations (1) through (3), contaminants may stick between the capillary and the plastic jacket at the tip of the nebulizar. In this case, perform the following procedure. (4) After removing the nebulizer, dip the nebulizer tip into hydrochloric acid (1:1). At this time, hold the nebulizer so that only the jacket is immersed and make sure that the metal part is not immersed in the hydrochloric acid (see Figure 6.4). CAUTION 1. Do not remove the disperser unit. 2. The ceramic ball (impact bead) in the disperser unit is fragile; be careful not to accidentally hit it. If the ceramic ball is taken off, remount it to the support. 3. Don't apply the ultrasonic cleaner to the nebulizer. Otherwise, the adhesion between the capillary and the main body may be damaged. (5) Mount the nebulizer and then spray pure water. Then check the absorbance sensitivity using standard solution.
Body (Metal part) O-ring Disperser unit Jacket
6
Maintenance
Cap
Polyethylene tube
Ceramic ball
Capillary
Figure 6.4
Nebulizer 6-5 AA-6800/6650
6.2.2.2
Replacing the Polyethylene Tube
A polyethylene tube is sandwiched into the nebulizer capillary so as to firmly hold the Teflon sampling tube used for sample suction in place. If this polyethylene tube deteriorates or comes loose, it becomes unable to wedge the Teflon sampling tube in place or cannot be firmly held. In this case, use the following procedure to replace the polyethylene tube while referring to Figure 6.4. (1) Rotate the cap shown in Figure 6.4 counterclockwise. (2) If the old polyethylene tube is still in the capillary, remove it. sure that the capillary does not bend. If difficult to insert, enlarge the opening by inserting a drawing pin etc. (4) When you have completed inserting the polyethylene tube, mount the cap as before. (3) Cut the provided polyethylene tube to the appropriate size and insert it into the capillary, making
6
Maintenance
6-6 AA-6800/6650
6.2.3
Cleaning the Chamber

The procedure for disassembling the chamber and cleaning its components is explained below (refer to
Figure 6.5). (1) Remove the burner head and the nebulizer (refer to 6.2.1 and 6.2.2). (2) Pull out the nylon FUEL (red) and AUX (black) from the Y bend are connected to the sprayer. (3) Remove the spray fixing screws to remove the acetylene jacket. Then you can take the mixer out from the chamber inside. (4) Remove the cover mounting screws to remove the cover (stainless-steel plate) of the chamber. (5) Remove the chamber fixing screws and remove the chamber. Then loosen the strap of the joint at the lower chamber floor and remove the drain tube. CAUTION 1. When assembling the chamber after cleaning it, be sure to check the direction of the mixer. Since the outer diameter of the mixer is slightly tapered, push it in the direction which fits the taper of the chamber inside. 2. Before pouring water or alcohol from the burner fixing port, be sure to remove the nebulizer. Otherwise, the nebulizer may sink in the liquid and the adhesive may be damaged.
6
Maintenance
Y bend (FUEL/AUX connecting joint)
Cover
Mixer
Spray fixing screws
Acetylene jacket L bend Chamber fixing screw Cover mounting screws Joint
Figure 6.5 Burner Unit
6-7 AA-6800/6650
6.3
Checking for Gas Leaks in Tubing
Regular checks are automatically conducted for gas leaks in the fuel gas tubing within the gas controller. Gas leaks at other locations may also be conducted using the following procedure. This procedure should be performed regularly at monthly intervals. (1) Disconnect the three tubes from the Y bend and L bend of the burner unit. (Refer to the left in Figure 6.5) (2) Connect these tubes to the provided leak check seal joint and supply air 0.35MPa and acetylene at 0.09MPa.
6
Maintenance
6-8 AA-6800/6650 Figure 6.6 Seal Joint for Gas Leak Check
(3) Execute [Instrument]-[Gas Controller Status] from the menu. Then the "Gas Controller Status" dialog box is displayed. Click on "Flame Monitor ON" check box to delete the check mark. (4) Press the IGNITE button on the front of the instrument for 2 or 3 seconds. Since the burner is not supplied with the gas, a flame is not ignited. However, the instrument gets in a dummy combustion status becasue the flame monitor is set to OFF. As the result, all the solenoid valves in the gas controller open. (5) Close the main valve of the cylinder and turn the secondary pressure control handle of the air compressor sufficiently counterclockwise and close it. (6) Confirm the pressure drop in 30 minutes is less than 0.015MPa for fuel gas and less than 0.03MPa for support gas, viewing the gas control gauges. If the drop in pressure exceeds these values, it should be concluded that gas is leaking. (7) If gas is judged to be leaking, apply soapy water or commercial leak check liquid to each of the connecting joints of the cylinder, compressor, gas controller and burner to ascertain the location of the leak. (8) Reconnect any joints where a gas leak is discovered. If it is concluded that gas is leaking inside the gas controller, contact your service representative immediately. (9) Check for leaking in the drain tube by filling water inside and checking visually. (10) When the gas leak check is finished, press EXTINGUISH button. Then detach the three tubes from the seal joint and reconnect them to the burner as described under 2.4.4. NOTE To stop this gas leak check halfway, press the EXTINGUISH button at the front of instrument.
6.4
Replacing the Deuterium Lamp
6.4.1 Specifications of Deuterium Lamp

Table 6.1 Specifications of Deuterium Lamp Part No Type Average Characteristics 062-65063-01 L6382 500 hours Discharge voltage Discharge current 70 90V 300 mA
Discharge starting voltage 300 600V
6.4.2 Replacing Procedures of Deuterium Lamp

WARNING : HIGH TEMPERATURE The deuterium lamp and deuterium lamp house are very hot. Before replacing the lamp, turn OFF the power and check that the lamp has cooled sufficiently.
6
Maintenance
CAUTIONS
1. Handle the new lamp using gloves so as not to leave fingerprints on the light beam window. Otherwise, the window is stained with the fingerprints when it is hot, and as the result the light transmission will be reduced. If contaminated, clean it with alcohol or the like. 2. When detaching or attaching the cover of the deuterium lamp house, be very careful not to hit the protrudent upper edge of the deuterium lamp against the cover rear side. It may cause a vacuum leak of the bulb.
Protrudent part on upper edge
Light beam window
Figure 6.7
Interior of Deuterium Lamp House Unit 6-9 AA-6800/6650
6.4 Replacing the Deuterium Lamp
(1) As shown in Figure 6.8, remove the two screws to detach the lamp cover. When the cover is removed, the deuterium lamp will appear as shown in Figure 6.7.
Deuterium lamp cover
Hole for adjustment
6
Figure 6.8 Deuterium Lamp Cover
(2) Pull the deuterium lamp slowly upward and out of its socket. (3) Insert a new deuterium lamp into the socket. At this time check that the lamp is fully seated in the socket. (4) Turn on the power of the instrument. Start up the PC software and select [Instrument]-[Connect] from the menu to make the connection for communication with the instrument. (5) Select [Instrument]-[Maintenance]-[D2 Lamp Position] from the menu. The messageD2 lamp position adjustment procedure is going to start. Please adjust D2 lamp position roughly first..is displayed. Set the deuterium lamp to almost center with the adjusting screw. (6) Click on <OK> and close the lamp cover. (7) Next, the deuterium lamp intensity in absorbance is displayed inD2 Lamp Adjustmentdialog box. Adjust the position using the adjusting knob so that the indicated value may become minimum. (8) After completing the deuterium lamp adjustment, click on <OK> to closeD2 Lamp Adjustment dialog box.
Maintenance
6-10
AA-6800/6650
6.5
Replacing Graphite Tube (GFA-6500)
When the same tube is reheated many times, its surface oxidizes and becomes rough. Moreover, as oxidation continues, the tube wall becomes thinner in the vicinity of the injection hole, and the tube will finally bend and break. As wear in the tube due to oxidation progresses, reproducibility of the data declines and in some cases the absorption peak may divide into two peaks. In those cases, replace the graphite tube.
6.5.1 High Density Graphite Tube

Refer to the section 2.5.4.1 and replace the tube in the same procedure.
6.5.2 Pyrolytic Coating Graphite Tube

Refer to the section 2.5.4.2 and replace the tube in the same procedure.
6.5.3 Graphite Tube Replacement and ASC Nozzle Position Adjustment

This section describes the procedure for replacing the graphite tube and adjusting the ASC nozzle position when a replacement of graphite tube is necessary during the measurement linked with the ASC.
6
(1) Execute [Instrument]-[Change Graphite Tube] to open the "Change Graphite Tube" dialog box. Click <Change Graphite Tube> button. (2) The message dialog box for prompting the tube replacement is opened. Follow the message and replace the tube. When setting a new graphite tube in the furnace, the positioning is easily performed by using a pipet tip provided with the ASC. First, release the lock of the furnace unit and slide the right-hand furnce block rightward then remove the old tube. Next, insert a new tube in the graphite cap. Adjust the tube position using a pipet tip so that the injection hole comes upper. Then close the right-hand furnce block and lock the furnace unit. When the replacement is finished, click on <OK>. (3) Next, the dialog box shown in Figure 6.9 is opened. Before performing the items 1 to 3, loosen the arm guide screw mounted onto the furnace and release the arm guide. Be careful not to change the arm guide position too much.
Maintenance
Figure 6.9 ASC Furnace Nozzle Position Adjustment 6-11 AA-6800/6650
6.5 Replacing Graphite Tube (GFA-6500)
(4) Click on <Move Near to Tube> to move the nozzle near to the tube. Check that the horizontal injection position is appropriatetly adjusted. If not, adjust the ASC horizontal position forward, backward, rightward and leftward, using the knob of the ASC table. (5) Next, move the nozzle position with <Move Upward> and <Move Downward> buttons to the optimum injection position, while monitoring the [Injection Position] and [Current Position]. At this time, also check that the horizontal position of injection is appropriatetly adjusted. If not, adjust the position forward, backward, leftward and rightward. Obtain the optimum vertical position while checking the gap between the nozzle tip and tube inside bottom using the furnace monitoring mirror provided with the ASC. (6) After setting the optimum position, carefully tighten the fixing screw of the arm guide. Then click on <OK>. The current nozzle position is memorized as the sample injection position. If <Cancel> is clicked, the injection position is not memorized. When this dialog box is closed, the ASC arm moves to the discharge position. (7) Lastly, the dialog box prompting the conditioning and temperature calibration is opened. Check the
6
Maintenance
6-12
instructions on the screen and close it with <OK>. In the cases of pyrolytic coating graphite and platform tube, execute the [Graphite Tube Conditioning] and [Temp. Calib.]. In the case of high density graphite tube, execute only the [Temp. Calib.].
CAUTIONS When the high density graphite tube is loaded to the furnace and used at temperature set to 2700 or higher, carbon coming from the tube may deposit the emission detecting hole for temperature sensor made on the graphite cap. For this reason, the amount of light reaching the temperature sensor may decrease and as the result the actual temperature may be higher than the programmed temperature. So when using the high density graphite tube in the above setting, clean the emission detecting hole of the graphite cap periodically. Although the amount of carbon coming from the pyrolytic coating graphite tube is remarkably less compared with that coming from the high density graphite tube, periodical cleaning of the emission detecting hole of the graphite cap is recommended for the same reason of above 1.
AA-6800/6650
6.6
Cleaning Graphite Cap, Holder, Window Plate Sockets and Window Plates (GFA-6500)
WARNING
: RISK OF ELECTRIC SHOCK Before attaching or detaching the graphite furnace or heating cables, make sure that the power is off.
After repeated measurements, the inner surfaces of the graphite cap, graphite holder and window plate sockets and the quartz window plates become contaminated with graphite powder or smoke generated from samples. If the contamination becomes severe, reproducibility will be adversely affected or baseline noise will increase. In this case, clean these parts according to the following procedure. NOTE 1. Clean the graphite cap and graphite holder before measurement and after graphite tube replacement. 2. Clean the window plate sockets and window plate weekly when using the instrument daily. If measurement is performed only intermittenly, clean them before measurement.
6
Maintenance
(1) Press in the knurled lock knob and turn it counterclockwise to release the lock, then slide the righthand cooling block to the right and take out the graphite tube. (2) Remove the window plate socket from the socket adapter. (3) Remove the socket adapter by turning it counterclockwise. Also, remove the coil spring. (4) Remove the graphite cap and graphite holder. (5) Wipe off soot deposited on the inside of the sample injection hole and emission detection hole (2mm i.d.) on the side of graphite cap completely with wadded-up tissue paper. In the same way, clean the inside surface of graphite holder. (6) Soak the socket adapter in distilled water or alcohol to remove dirt, and then wipe away all moisture using tissue paper or gauge. (7) Mount the graphite cap so that the indicator line is aligned with the line on the left-hand cooling block and insert the coil spring. Then screw the socket adapter into the cooling block and fix it securely. (8) Next, remove the fluororubber tube connected to the window plate via the coupling. (9) Remove the O-rings with tweezers and then remove the window plates. (10) Soak the window plate sockets and window plates in distilled water or alcohol to remove dirt, and then wipe away all moisture using tissue paper or gauze. (11) Fit the window plate into the window plate socket and secure it with the O-ring. (12) Reconnect the fluororubber tube to the window plate socket coupling which was disconnected in step (8).
6-13 AA-6800/6650
6.6 Cleaning Graphite Cap, Holder, Window Plate Sockets

and Window Plates (GFA-6500)
(13) Mount the window plate socket with the attached window plate and fluororubber tube to the cooling block using the socket adapter. While turning the window plate socket clockwise, push it all the way in so that there is no play. If there is any play between the window plate socket and the cooling block, the gap may cause an electrical discharge, possibly melting the screws. The window plate socket must be installed so that the fluororubber tube is directed toward the GFA-6500 power supply unit. If the above procedure does not result in sufficiently improved reproducibility of data, replace the graphite cap and holder. After replacement, create a temperature program as Table 6.2 and run the program twice to heat the graphite furnace and remove contamination from the graphite cap and holder. After running the program, once again remove the graphite cap and holder and perform cleaning according to steps (1) to (12). Table 6.2 Temperature Program for Cleaning
Stage# 1 Temp() 1800 0 2500 0 3000 0 3000 0 3000 0 3000 0 3000 0 3000 0 3000 0 3000 0 Time (sec) 5 25 5 25 5 25 5 25 5 25 5 25 5 25 5 25 5 25 5 25 Heat Mode RAMP STEP RAMP STEP RAMP STEP RAMP STEP RAMP STEP RAMP STEP RAMP STEP RAMP STEP RAMP STEP RAMP STEP Sensitivity Gas Type Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular Regular #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 #1 Flow Rate (L/min) 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5
6
Maintenance
6-14
2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
AA-6800/6650
6.6 Cleaning Graphite Cap, Holder, Window Plate Sockets

and Window Plates (GFA-6500)
CAUTION
Pay careful attention to the following points when assembling the cooling block, graphite cap and holder, and socket adapter.
(1) Screw down the socket adapter tightly enough that the graphite cap and holder are firmly secured between the cooling block and socket adapter. The electrical current supplied by the power source flows in the following loop: Right cooling block Graphite holder
Power source
Graphite tube
Left cooling block
Graphite cap
6
Maintenance
Unless the socket adapters are sufficiently tightened down, contact between the parts will be poor. As the result, current may not flow, or a discharge may occur between the cooling blocks and socket adapters, possibly melting down the screws. Therefore, after assembly, move the cap and holder from the inside to check that they are not loose. (2) When the tube is heated, the light from the tube emitted through the emission detection hole on the surface of the graphite cap must properly enter the light inlet of the photosensor. This requires alignment of the two corresponding marks on the surface of the cap and the surface of the left-hand cooling block. Secure the cap when it is positioned with these marks aligned (Refer to Figure 6.10).
6-15 AA-6800/6650
6.7
Cleaning the Temperature Sensor (GFA-6500)
The light radiated from the surface of the graphite tube during heating of the sample passes through the emission detection hole of the graphite cap and enters the temperature sensor. It then passes through a filter to irradiate a photocell. A constant relation exists between the temperature of the graphite tube and the output signal of the silicon photocell, and this relation has been stored in instrument memory. In the range of the temperature control system, the current that flows to the tube is automatically controlled so that the output signal of the silicon photocell corresponds to the temperature setting. Therefore, in cases such as indicated below, even if the tube reaches the set temperature, the output signal of the photocell will be smaller than normally, and the current flowing to the tube will increase, with the tube ultimately being heated to an extremely high temperature compared with the temperature setting. Excessive increase in temperature may occur when: (a) The light path from the tube to the photocell is obstructed by soot, etc. (b) The graphite cap is misaligned so that emission detection hole in the surface of the cap is not properly facing the light inlet of the photosensor unit.
6
During heating of the sample, argon gas flows to the light inlet at a rate of about 0.5L/min to prevent intrusion of soot and smoke expelled from the tube. But when the graphite furnace is used every day, perform cleaning once a month, or when it is used only every few days, perform cleaning before measurement using the following procedure. (1) Remove the graphite cap. (2) Clean the emission detection hole of the graphite cap. (3) Loosen the set screw and remove the nozzle. Then take out the filter and clean it. (4) Assemble the temperature sensor unit and graphite furnace. (5) Secure the cap so that the mark on the surface of the graphite cap is aligned with that on the left-hand cooling block.
Maintenance
6-16
Window plate socket Cooling block Cap Mark
Graphite cap Graphite tube Filter Light Nozzle Argon gas Setscrew Mirror
Photocell
Tube Left-hand block
Figure 6.10
Temperature Sensor Unit
AA-6800/6650
6.8
Cleaning the Slide Mechanism (GFA-6500)
The right-hand block moves right and left along two guide rods. If soiled guide rods prevent smooth sliding of the cooling block, wipe off the guide rods and apply lubricant so that it moves smoothly. During heating of the sample, the graphite tube expands, causing the right-hand block to move slightly in opposition to the force of the spring but if soiled guide rods prevent smooth sliding of the block, excessive force will be applied to the tube, possibly causing it to break. In addition, when the surfaces of the slide rods become too dirty, the tube may not be secured properly. In this case, clean and lubricate the guide rods to obtain smooth movement. When the graphite furnace is used every day, perform cleaning once a month, or when it is used only every few days, perform cleaning before measurement.
Right-hand block
6
Maintenance
Guide rod
Figure 6.11
Opened Graphite Furnace
6-17 AA-6800/6650
6.9
Cleaning the Seal (GFA-6500)
After measurements are repeated many times, the seal (Teflon ring) may be contaminated with soot or smoke generated from samples. If the contamination becomes severe, the sample itself may be contaminated. In this case, clean the seal before measurement or when replacing the graphite tube. Remove the seal from the graphite holder and soak the seal in distilled water or alcohol to remove dirt, and then wipe away all moisture using tissue paper or gauze. With the wide surface of seal directed toward the graphite holder (right-hand cooling block), open it slightly to mount it the graphite holder.
6
Maintenance
6-18 AA-6800/6650
6.10
GFA Performance Check (GFA-6500)
The standard method for checking GFA function after installing the GFA or during daily measurement operations will be explained below. (1) Tools to prepare a) Micropipette (20L) (This is not necessary when using the auto-sampler.) b) Whole pipette (1mL) c) Volumetric flask (100mL) d) Distilled water e) Mn 1ppb test solution f) Hollow cathode lamp (Mn) g) Pyrolytic coating graphite tube (for GFA-6500) Mn 1ppb Test Solution Preparation Procedure Use reagent grade 1000ppm Manganese standard solution to prepare the test solution. i) Precisely measure 1mL of the Mn 1000ppm base solution into the volumetric flask, add 0.5mL hydrochloric acid (reagent grade), then add distilled water to make a total volume of 100mL, yielding a 10ppm standard solution. ii) Precisely measure 1mL of the 10ppm standard solution prepared in the above i) into the volumetric flask, add 0.5mL hydrochloric acid (reagent grade), then add distilled water to make a total volume of 100mL, yielding a 0.1ppm standard solution. iii) Precisely measure 1mL of the 0.1ppm standard solution prepared in the above ii) into the volumetric flask, add 0.5mL hydrochloric acid (reagent grade), then add distilled water to make a total volume of 100mL, yielding a 1ppb standard solution. (2) Setting the sample measurement parameters Using the element selection Wizard, select Mn and furnace method, and set the analysis parameters as below. Element Socket # Current Wavelength Slit Width Lamp Mode : : : : : : Mn 1 (When the Mn hollow cathode lamp is set to socket #1) 10mA 279.5nm 0.2nm NON-BGC 4 4
6
Maintenance
No. of Repetitions : Max. No. of Reps. :
Standard temperature program for Mn is shown in Table 6.3.
6-19 AA-6800/6650
6.10 GFA Performance Check (GFA-6500)
Table 6.3 Temperature Program for GFA Performance Check (Mn)

STAGE# 1 2 3 4 5 6 7 Temp () 150 250 800 800 800 2200 2500 Time (sec) 20 10 10 10 3 2 2 Heat Mode Sensitivity RAMP RAMP RAMP STEP STEP STEP STEP GAS Type #1 #1 #1 #1 #1 #1 #1 Flow Rate (L/min) 0.1 0.1 1.0 1.0 0.0 0.0 1.0
Sampling Stage No. : 6 When using the ASC for measurement, set the parameters as below.
6
[Order]
(a) Preparation Parameters [Measurement Type] Calibration Curve Method 1st ppb 1.000 R1 20 20 (b) Mixing Setup [Mixing] [Volume] [Speed] OFF 20 25
Maintenance
6-20
[Conc. Unit] [Conc.] [Pos.] [Sample (L)] [Total Vol (L)]
(3) Measurement Wait 30 minutes or longer after the hollow cathode lamp is lit on, then inject 20L of the 1ppb Mn test solution with micro-pipette or auto-sampler and measure it as a standard. Check the average of absorbance and reproducibility (%RSD) after 4 repetitions. Absorbance Reproducibility : : 0.18 Abs or greater Within 7% RSD
AA-6800/6650
6.11
Maintenance Parts
6.11.1 AA-6800/6650 Maintenance Parts

Part Name Lamp, D2 L6382 Nebulizer ASSY Ceramic ball 5/16 Chamber ASSY Burner head ASSY Burner socket ASSY O-ring, AS568-116-4D O-ring, 4D P16 O-ring, 4D P22 O-ring, 4D P14 O-ring, 4D P35 Cleaning wire Sampling tube Sampling tube ASSY Drain ASSY Gas tube ASSY Hose, 82B-BK Hose, 82B-R Hose, 82B-G Wire bands, for 16mm Tube, super cornace 913 Vinyl tube, R3603 3/81/16 Si rubber tube, 912 Fuse, 313.250 0.25A Fuse, 189100 Fuse, ULCS-61ML6 Fuse, 313.003 Burner positioning jig Seal joint ASSY Polyethylene capillary No.3 Retaining plate Vinyl cover Mixer Wiring band Part No. 062-65063-01 206-50226-91 031-65802-09 206-50363-91 206-50370-92 206-50762-91 036-15551-16 036-11217 036-11222 036-11215 036-11237 201-79229-01 204-05899-01 206-50772-91 206-80771-91 206-65112 016-02101-04 016-02101-03 016-02101-01 037-61019 016-43200-08 016-31409 016-31350-22 072-01664-11 072-01667-12 072-01661-24 072-01664-30 202-38757-02 204-27570-02 200-31328-01 206-50318 206-64902 206-50486 072-60315-01 For fixing the drain hose For checking for gas leaks For sealing the capillary For securing the nebulizer Vinyl cover for main unit Used in burner socket (burner side) Used in nebulizer, chamber plug Used in burner socket (chamber side) Used in drain-joint Used in jacket mounted on chamber For cleaning the capillary Teflon* tube for sample uptake Polyethylene tube for sample uptake Impact bead Polypropylene Titanium, 10cm Remarks Nebulizer (with impact bead)
6
Maintenance
Overflow-type drainage trap Nylon tube set for gas supply For support gas (Air), Black For fuel gas, Red For support gas (N2O), Green Hose band Drain hose (below chamber) Taigon Tube, connects to drain bottle (for water-soluble samples) Silicone rubber tube, connects to drain bottle (for organic solvent samples except petroleum group) For HC lamp For D2 lamp For 6A, 100V system For 3A, 200V system
6-21 AA-6800/6650
6.11 Maintenance Parts
6.11.2 GFA-6500 Maintenance Parts

Part Name High density graphite tube Pyrolytic coating graphite tube Graphite cap 6000 Graphite holder 6000 Seal Window socket ASSY Socket adapter Window plate, W(16)-Q O-ring, 4CP14 Hose, 82B-BK Wire band, for 14mm Part No. 206-80153-03 206-69984-02 206-80165 206-80164 206-69215 206-69949 206-69814-01 205-82654-02 036-11015 016-02101-04 037-61018 037-61019 016-35764-11 016-02401-01 016-31351-35 035-60374 016-35761 018-31506 072-01214-07 072-01214-08 206-65236 206-69790 Black, i.d.3, for gas Black, i.d.3, for cooling water For temp.sensor nozzle For fixing fluorine rubber tube Black, i.d.4, for cooling water For cooling water PHASE CONTROL For protecting furnace For preventing loosening of socket adapter Remarks
6
Maintenance
6-22
Wire band, for 16mm Nylon T, N5-4-43 Fluorine rubber tube, 104-0030 Silicone rubber tube, 01510 Sleeve, 40-13 Nylon T, N5-4-6 Tetron sleeve for cooling 1016 Fuse, FGBO 250V 1A Fuse, FGBO 250V 2A Protective plate Coil spring
AA-6800/6650
6.12
Special Accessories
6.12.1 For Flame Analysis

Part Name Flame conversion unit ACF-6800 Cover, flame High temperature burner head Air compressor (50Hz) Air compressor (60Hz) Silent-type air compressor Drain separator Precision gas pressure regulator YR-71 Precision gas pressure regulator MAF-85S Precision gas pressure regulator MAF-76S Precision gas pressure regulator MAF-106S Hose ASSY Hose ASSY Part No. 206-64843-92 206-50554 206-50300-92 200-33897-01 200-33897-02 200-64051 200-64020 040-72020-01 040-72019-11 040-72019-01 040-72019-21 206-50389-91 206-50389-92 For acetylene gas For nitrous oxide gas For hydrogen gas For argon gas For argon gas For hydrogen gas Titanium For AC100V, 50Hz For AC100V, 60Hz For both 50Hz/60Hz Remarks Required when mounting ACF-6800 on AA-6650G
6
Maintenance
6.12.2
For Furnace Analysis (for GFA-6500)

Part No. 206-80208-xx 206-80153-03 206-69984-02 206-82541 Remarks
Part Name Graphite Furnace Atomizer GFA-6500 High-density graphite tube Pyrolytic coating graphite tube Platform tube
6.12.3
For Furnace Analysis (for GFA-EX7)

Part No. 206-51000-xx 206-51141 206-50587 206-50588 206-50887-02 Remarks Required when mounting GFA-EX7 on AA-6650F
Part Name Graphite Furnace Atomizer GFA-EX7 Furnace base High-density graphite tube Pyrolytic coating graphite tube Platform tube
6.12.4
Autosampler
Part No. 206-50100-xx 206-50200-91 206-67563 Required when using ASC-6100 with HVG-1 Remarks
Part Name Autosampler ASC-6100 Unit for furnace ASK-6100 Nozzle ASSY, HVG
6-23 AA-6800/6650
6.12 Special Accessories
6.12.5 Hollow Cathod Lamps (Single Element Lamps)

HAMAMATSU PHOTONICS Co.LTD L233 Series (Not usable for SR method) Element Symbol Ag Al As Au B Ba Be Bi Ca Cd Co Cr Cs Element Name Silver Aluminum Arsenic Gold Boron Barium Beryllium Bismuth Calcium Cadmium Cobalt Chromium Cesium Copper Dysprosium Erbium Europium Iron Gallium Gadolinium Germanium Hafnium Mercury Holmium Indium Iridium Potassium Lanthanum Lithium Lutetium Magnesium Manganese Molybdenum Sodium Niobium Neodymium Part No. 200-38422-02 200-38422-01 200-38422-42 200-38422-25 200-38422-39 200-38422-03 200-38422-04 200-38422-43 200-38422-05 200-38422-06 200-38422-09 200-38422-07 200-38422-27 200-38422-08 200-38422-60 200-38422-61 200-38422-62 200-38422-10 200-38422-40 200-38422-63 200-38422-11 200-38422-64 200-38422-28 200-38422-65 200-38422-48 200-38422-66 200-38422-22 200-38422-29 200-38422-30 200-38422-67 200-38422-12 200-38422-13 200-38422-31 200-38422-14 200-38422-32 200-38422-68 Product Name L233-47NQ L233-13NB L233-33NQ L233-79NQ L233-5NQ L233-56NB L233-4NQ L233-83NQ L233-20NU L233-48NQ L233-27NU L233-24NB L233-55NB L233-29NB L233-66NB L233-68NB L233-63NB L233-26NB L233-31NU L233-64NB L233-32NU L233-72NU L233-80NU L233-67NB L233-49NB L233-77NQ L233-19NB L233-57NB L233-3NB L233-71NB L233-12NU L233-25NU L233-42NB L233-11NB L233-41NB L233-60NB
6
Maintenance
6-24
Cu Dy Er Eu Fe Ga Gd Ge Hf Hg Ho In Ir K La Li Lu Mg Mn Mo Na Nb Nd
AA-6800/6650
Element Symbol Ni Os Pb Pd Pr Pt Rb Re Rh Ru Sb Sc Se Si Sm Sn Sr Ta Tb Te Ti Tl Tm V W Y Yb Zn Zr
Element Name Nickel Osmium Lead Palladium Praseodymium Platinum Rubidium Rhenium Rhodium Ruthenium Antimon Scandium Selenium Silicon Samarium Tin Strontium Tantalum Terbium Tellurium Titanium Thallium Thulium Vanadium Tungsten Yttrium Ytterbium Zinc Zirconium
Part No. 200-38422-15 200-38422-69 200-38422-21 200-38422-41 200-38422-70 200-38422-20 200-38422-33 200-38422-44 200-38422-49 200-38422-45 200-38422-24 200-38422-71 200-38422-46 200-38422-16 200-38422-72 200-38422-18 200-38422-34 200-38422-35 200-38422-73 200-38422-47 200-38422-17 200-38422-74 200-38422-75 200-38422-19 200-38422-36 200-38422-76 200-38422-77 200-38422-23 200-38422-37
Product Name L233-28NQ L233-76NU L233-82NQ L233-46NQ L233-59NB L233-78NU L233-37NB L233-75NB L233-45NB L233-44NB L233-51NB L233-21NB L233-34NB L233-14NU L233-62NB L233-50NQ L233-38NB L233-73NU L233-65NB L233-52NQ L233-22NB L233-81NU L233-69NB L233-23NB L233-74NU L233-39NB L233-70NB L233-30NQ L233-40NB
6
Maintenance
6-25
AA-6800/6650
6.12.6 Hollow Cathode Lamps (Single element lamps, Usable for SR method)
HAMAMATSU PHOTONICS Co.LTD L2433 Series Element Symbol Ag Al As Au B Ba Be Bi Ca Cd Co Cr Cu Element Name Silver Aluminum Arsenic Gold Boron Barium Beryllium Bismuth Calcium Cadmium Cobalt Chromium Copper Dysprosium Erbium Europium Iron Gallium Germanium Hafnium Holmium Potassium Lanthanum Lithium Magnesium Manganese Molybdenum Sodium Nickel Lead Palladium Platinum Ruthenium Antimon Selenium Silicon Part No. 200-38456-01 200-38456-02 200-38456-03 200-38456-04 200-38456-05 200-38456-06 200-38456-07 200-38456-08 200-38456-09 200-38456-10 200-38456-11 200-38456-12 200-38456-14 200-38456-15 200-38456-16 200-38456-17 200-38456-18 200-38456-19 200-38456-21 200-38456-22 200-38456-24 200-38456-26 200-38456-27 200-38456-28 200-38456-30 200-38456-31 200-38456-32 200-38456-33 200-38456-35 200-38456-37 200-38456-38 200-38456-40 200-38456-43 200-38456-44 200-38456-46 200-38456-47 Product Name L2433-47NB L2433-13NB L2433-33NQ L2433-79NQ L2433-5NB L2433-56NB L2433-4NQ L2433-83NQ L2433-20NU L2433-48NQ L2433-27NU L2433-24NB L2433-29NB L2433-66NB L2433-68NB L2433-63NB L2433-26NQ L2433-31NU L2433-32NU L2433-72NU L2433-67NB L2433-19NB L2433-57NB L2433-3NB L2433-12NU L2433-25NU L2433-42NB L2433-11NB L2433-28NQ L2433-82NQ L2433-46NQ L2433-78NU L2433-44NB L2433-51NQ L2433-34NQ L2433-14NQ
6
Maintenance
6-26
Dy Er Eu Fe Ga Ge Hf Ho K La Li Mg Mn Mo Na Ni Pb Pd Pt Ru Sb Se Si
AA-6800/6650
Element Symbol Sm Sn Sr Te Ti V Y Yb Zn
Element Name Samarium Tin Strontium Tellurium Titanium Vanadium Yttrium Ytterbium Zinc
Part No. 200-38456-48 200-38456-49 200-38456-50 200-38456-53 200-38456-54 200-38456-56 200-38456-58 200-38456-59 200-38456-60
Product Name L2433-62NB L2433-50NQ L2433-38NB L2433-52NQ L2433-22NB L2433-23NB L2433-39NB L2433-70NB L2433-30NQ
6.12.7 Hollow Cathod Lamp (Multi-element Lamps) (Not usable for SR method)
Element CaMg FeNi NaK SiAl SiBa Part No. 200-38422-51 200-38422-53 200-38422-50 200-38422-52 200-38422-54 Product Name L733-202NU L733-204NQ L733-201NB L733-203NU L733-205NU
6
Maintenance
6.12.8 Other Accessories

Part Name Mercury vaporizer unit MVU-1A Gas flow cell Cell holder for gas flow cell Hydride vaporizer unit HVG-1 Cooling water circulating unit CA-1111 Cooler connection kit Regulator ASSY Part No. 204-21932-01 201-98687 202-35867 206-17143 044-01809-02 206-84373-91 206-86147-91 Working temperature range: -10 +40 Required when the GFA-6500 is connected with CA-1111. Pressure reducing valve for GFA-6500 cooling water Remark
6-27 AA-6800/6650
Chapter 7 Appendix
Contents 7.1 7.2 7.3 Measurement Conditions Table for Flame Atomic Absorption Analysis 7-1 Analysis Line Wavelength Table for Flame Emission Analysis 7-4 Graphite Tube Type Selection in Furnace Method 7-5 When Using a High Density Graphite Tube 7-5 When Using a Pyrolitic Coating Graphite Tube 7-6 When Using the Platform Type Tube 7-6
7
Appendix
7.3.1 7.3.2 7.3.3 7.4
Error Messages 7-9
AA-6800/6650
7.1
Measurement Conditions Table for Flame Atomic Absorption Analysis
Element Ag Al As (H) As Au B Ba Be Bi (H) Bi Ca (1) Ca (2) Cd Co Cr Cs Cu Dy Er Eu Fe Ga Gd Ge Hf Hg Ho Ir K La Li Lu Mg Mn Mo Na Nb Ni Os
Wave length (nm) 328.1 309.3 193.7 193.7 242.8 249.7 553.5 234.9 223.1 223.1 422.7 422.7 228.8 240.7 357.9 852.1 324.8 421.2 400.8 459.4 248.3 287.4 368.4 265.2 307.3 253.7 410.4 208.8 766.5 550.1 670.8 360.0 285.2 279.5 313.3 589.0 334.9 232.0 290.9
L233 (mA) 10 10 12 12 10 16 16 16 10 10 10 10 8 12 10 16 6 14 14 14 12 4 12 18 24 4 14 20 10 18 8 14 8 10 10 12 24 12 14
L2433 (mA) 10/400 10/600 12/500 12/500 10/400 10/500 12/600 10/600 10/300 10/300 10/600 10/600 8/100 12/400 10/600 10/500 15/600 15/500 10/600 12/400 4/400 20/500 20/600 10/600 8/600 18/600 8/500 8/500 10/600 10/500 8/600 10/400
Slit (nm) 0.5 0.5 1.0 1.0 0.5 0.2 0.2 1.0 0.5 0.5 0.5 0.5 1.0 0.2 0.5 1.0 0.5 0.2 0.5 0.5 0.2 0.2 0.2 0.2 0.2 1.0 0.2 0.2 0.5 0.5 0.5 0.5 0.5 0.2 0.5 0.2 0.2 0.2 0.2
Flame Type Air-C2H2 N2O-C2H2 Air-C2H2 Ar-H2 Air-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2
Flow (l/min) 2.2 7.0 2.0 [3.7] 1.8 7.7 6.7 7.0 2.0 2.2 2.0 6.5 1.8 1.6 2.8 1.8 1.8 7.0 7.0 7.0 2.2 1.8 7.0 7.8 7.0 7.0 2.2 2.0 7.5 1.8 7.0 1.8 2.0 7.0 1.8 7.0 1.6 7.0
Burner. H (mm) 7 11 <HVG-1> 15 7 11 11 11 <HVG-1> 7 7 11 7 7 9 7 7 11 11 11 9 7 11 11 11 11 7 7 11 7 11 7 7 11 7 11 7 11
7
Appendix
By the cold vapor mercury technique
7-1 AA-6800/6650
7.1 Measurement Conditions Table for Flame Atomic Absorption Analysis
Element Pb (1) Pb (2) Pd Pr Pt Rb Re Ru Sb (H) Sb Sc Se (H) Se Si Sm Sn (H) Sn (1) Sn (2) Sn (3) Sn (4) Sr Ta Tb Te (H) Te Ti Tl V W Y Yb Zn Zr
Wave length (nm) 217.0 283.3 247.6 495.1 265.9 780.0 346.0 349.9 217.6 217.6 391.2 196.0 196.0 251.6 429.7 286.3 224.6 286.3 224.6 286.3 460.7 271.5 432.6 214.3 214.3 364.3 276.8 318.4 255.1 410.2 398.8 213.9 360.1
L233 (mA) 12 10 10 14 14 14 20 20 13 13 10 23 23 15 14 10 10 10 10 10 8 18 10 14 14 12 6 10 24 14 10 8 18
L2433 (mA) 8/300 8/300 10/300 10/300
Slit (nm) 0.5 1.0 0.5 0.5 0.5 0.2 0.2
Flame Type Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Ar-H2 N2O-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2
Flow (l/min) 2.0 2.0 1.8 7.0 1.8 1.8 7.0 1.8 2.0 2.0 7.0 2.0 [3.7] 7.7 7.0 2.0 3.0 3.0 6.8 6.8 1.8 7.0 7.0 2.0 1.8 7.8 1.8 7.5 7.7 7.5 7.5 2.0 7.5
Burner. H (mm) 7 7 7 11 7 7 11 7 <HVG-1> 7 11 <HVG-1> 15 11 11 <HVG-1> 9 9 11 11 7 11 11 <HVG-1> 7 11 7 11 11 11 11 7 11
20/600 15/500 15/500 15/300 15/300 10/500 15/600 20/500 20/500 20/500 20/500 20/500 6/500
0.2 0.5 0.5 0.2 1.0 1.0 0.5 0.2 1.0 0.5 1.0 0.5 1.0 0.5 0.2 0.2
7
Appendix
7-2
15/400 15/400 10/600 10/600 10/600 5/200 10/300
0.2 0.2 0.5 0.5 0.5 0.2 0.5 0.5 0.5 0.2
AA-6800/6650
7.1 Measurement Conditions Table for Flame Atomic Absorption Analysis
NOTES 1. These measurement parameters are handled in the program as standard analysis parameters, but the optimum measurement parameters may vary depending on the properties of the sample. 2. When hydrogen gas is used as the fuel gas, the actual flow rate of the hydrogen is larger than the displayed fuel gas flow rate. The fuel gas flow rate in the brackets for the As or Se in this table is the displayed value. Use this value in the brackets as the parameter for fuel gas flow rate. The actual flow rate can be calculated as below. Actual hydrogen gas flow rate Displayed fuel gas flow rate3.5 3. <HVG-1> repersents the special accessory Hydride Vapor Generator. 4. Ar-H2 flame for As and Se is used for normal measurement, not for hydrogen vapor generating method.
7
Appendix
7-3 AA-6800/6650
7.2
Analysis Line Wavelength Table for Flame Emission Analysis
Element Ag Al As Au B Ba Be Bi Ca Cd Ce Co Cr Cs
Wavelength (nm) 328.1 396.2 193.7 267.6 518.0 455.4 234.9 306.8 422.7 326.1 494.0 345.4 425.4 455.5 324.8 404.6 400.8 459.4 372.0 417.2 622.0 265.1
Element Hf Hg In Ho Ir K La Li Lu Mg Mn Mo Na Nb Nd Ni Os Pb Pd Pr Pt Rb
Wavelength (nm) 531.2 253.7 451.1 410.4 550.0 766.5 442.0 670.8 451.9 285.2 403.3 390.3 589.0 405.9 492.5 352.5 442.1 405.8 363.5 495.1 265.9 794.8
Element Re Rh Ru Sc Si Sm Sn Sr Ta Tb Te Ti Th Tl U V W Y Yb Zn Zr
Wavelength (nm) 346.1 343.5 372.8 402.4 251.6 476.0 317.5 460.7 474.0 534.0 486.6 334.9 492.0 377.6 544.8 437.9 430.2 597.2 398.8 636.2 360.1
7
Appendix
7-4
Cu Dy Er Eu Fe Ga Gd Ge Band spectrum
AA-6800/6650
7.3
Graphite Tube Type Selection in Furnace Method
In furnace method, it is effective to select a graphite tube according to the element and sample. There are three graphite tube types widely used at present; high density graphite tube (hereinafter referred to as high density tube), pyrolytic coating graphite tube (hereinafter, pyro-coated tube) and platform type graphite tube (hereinafter, platform tube). The high density tube is made of ordinary graphite and most widely used. Since the graphite has a porous characteristic, the injected sample solution permeates into the graphite wall in some degree. On the other hand, the pyro-coated tube has a metalic luster on its surface, because it is made by forming a pyrolitic layer on the surface of high density tube by the CVD method. Since the density of the surface is higher than that of high density tube, the sample permeation into the wall is less. The platform tube refers to a graphite tube in which a plate with a basin for containing the sample (platform) is mounted. The Shimadzu platform tube has a platform made of 100% pyrolitic carbon. In this chapter, how to select these graphite tubes is described.
Pyro-coated Platform High density
7
Appendix
Pyro-coated
Pyro-coated : High-density (Cu : 6ppb) : (Cu : 60ppb)
Pyro-coated : Platform (Cu : 6ppb) : (Cu : 6ppb)
Figure 7-1 Comparison of Peak Profiles(Left: between the pyro-coated tube and high density tube, Right: between the platform tube and pyro-coated tube) 7.3.1 When Using a High Density Graphite Tube
The high density tube is used for measurements of various elements, and is often used especially for an element whose atomization temperature is low. For example, Cd, Pb, Na, K, Zn and Mg are such elements. It is also used to lower the measurement sensitivity in the case of a high concentration sample. For example, in the case of Al, Fe and Cu, althougth a level of 1 ppb can be measured when the pyro-coated tube is used, the measurement sensitivity can be lowered to a level of 100 ppb by using the high density tube. Figure 7.2 shows an example of calibration curves for Cu measurements using the high density tube and pyro-coated tube. The measurement points are 20, 40 and 60 ppb in the case of high density tube and 2, 4 and 6 ppb in the case of pyro-coated tube, although the simillar absorbances are shown.
7-5 AA-6800/6650
7.3 Graphite Tube Type Selection in Furnace Method
7.3.2 When Using a Pyrolitic Coating Graphite Tube

Generally, the pyro-coated graphite tube is effective for elements which are easily combined with carbon or the major component of graphite tube (carbide is easily formed). Ni, Ca, Ti, Si, V and Mo are the typical elements. In the high density tube, a sample easily permeates into the graphite, resulting in a larger contact area between the element and carbon. In the pyro-coated tube, however, a smaller contact area can suppress the carbide formation, and as the result, a higher sensitivity is obtained. When the peak profiles are compared, a sharp peak is observed in the case of pyro-coated tube, while a broad peak is observed in the case of high density tube. Figure 7.1 shows the example in Cu. In the case of pyro-coated tube, however, the result is easily affected by an acid concentration in sample and a sample spreading in the tube varies widely. As the result, the reproducibility is tend to be inferior to that of the high density tube. The effect of acid concentration on sensitivity is shown in Figure 7.3. The sensitivity varies more drastically as the acid concentration changes, when compared with those of platform tube or high density tube.
7.3.3 When Using the Platform Type Tube

As a feature of the platform tube, the sample solution is injected onto the platform and heated as shown in Figure 7.4. In the furnace method, the graphite tube is heated firstly from the wall, therefore, in normal
7
Appendix
7-6
tube, the sample is heated and atomized as the wall is heated. In platform tube, however, the sample is atomized after the temperature of entire tube reaches the atomization temperature (see Figure 7.5). In the measurment with platform tube, the atomization peak becomes more broad inspite that the platform material is pyrolitic graphite (see Figure 7.1). Also, it is more effective to set the temperature a little higher, comared with normal pyro-coated tube. With this difference of heating sequence, however, using the platform tube can minimize the influence of the sample liquid nature. This is because a recombination of atoms after atomization does not easily occur in the platform tube, while it easily occurs with a low temperature of tube center in the case of wall heating. As shown in Figure 7.3, the sensitivity change is small when the acid concentration changes largely. Also, when a background signal is generated, a timing of atomization signal can be shifted from it. Therefore, this is effective for samples with complicated matrix, such as biological sample, waste water and sea water. This feature of platform tube often makes the latter part of peak profile not get down to baseline level within the atomization stage. Set the time of atomization stage a little bit longer in such case.
AA-6800/6650
Sensitivity comparison among graphite tubes
Absorbance
Pyro-coated Platform High density
Cu Concentration/ ppb
Figure 7.2 Sensitivity Comparison among Graphite Tube Types
Graphite tube types and acid concetration High density Pyro-coated Platform
7
Appendix
Absorbance
HNO3 Concentration/ %
Figure 7.3 Effect of Nitric Acid Concentration on Pb Sensitivity among Graphite Tube Types (Pb: 5 ppb, 10L injection)
7-7 AA-6800/6650
Figure 7.4 Platform Type Graphite Tube
7
Appendix
Platform type graphite tube Pyro-coated(or high density) graphite tube
Figure 7.5 Temperature Distribution Image in Atomization Stage (Low temperature is indicated in dark color.)
7-8 AA-6800/6650
7.4
Error Messages
NOTES Before contacting your Shimadzu service representative, record the following items. Content of error message Status in which the error message is displayed (indication screen, performed operation, measurement file, "wizaa.ini" file in windows folder, etc.) Instrument information displayed at the upper in the initialization screen (model names of AA/ASC/GFA, ROM version and serial No.) AA software version No. ([Help]-[About WizAArd] menu)
Error Message
Cause/Details
Remedial Measure Select [None] for the Element field to clear the overlapped lamp in "Lamp Position Setup" dialog box. When using plural lamps of the same element and type simultaneously, register each of the lamps in [Instrument][Lamp History].
Number
x,x,x,...This lamp ID is already in use. Please select another ID.
A A ACK has not been Communication protocol with ASC Verify the ASC power supply and the cable connection accepted from ASC. between ASC and AA main unit, then connect the ASC in was not completed. (:A) [Instrument]-[Option Connect] menu. ACK has not been Communication protocol with GFA Verify the GFA power supply and the cable connection accepted from GFA. was not completed. (:A) between GFA and AA main unit, then connect the GFA in [Instrument]-[Option Connect] menu. After leak check is Residual gas combustion was tried Residual gas combustion cannot be done during execution of finished, ignite flame while executing the gas leak check. gas leak check. After finishing the gas leak check, ignite a again. flame and execute the residual gas combustion. Analytical Line is not Line Search has failed. (1) Verify that the lamp is correctly mounted to the socket and found. The following causes are considerable. the lamp turret position. (1) The lamp is not properly mounted (2) Perform the wavelength correction in [Instrument]to the lamp turret. [Maintenance]-[Wavelength Adjustment]. (2) The wavelength shift has occurred in the monochromator. Another error No. was The ROM program of the AA main unit has a problem. issued from GFA. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative. Another error occurred The ROM program of the AA main unit has a problem. while recovering ASC Record the instrument information displayed on the initial error. screen and the status in which this error occurs. Then contact your Shimadzu service representative. ASC arm motor slipped. Verify that the ASC arm movement is not impeded. Switch on the ASC again and connect the ASC in [Instrument]-[Option Connect] menu. ASC arm rotation position (1) The origin detector didn't detect the (1), (2) Switch on the ASC main unit again. origin correctly. cannot be initialized. If the error occurs again, record the status in which this error (2) The arm rotation drive motor message appears and contact your Shimadzu service doesn't operate. representative. ASC arm vertical position (1) The origin detector didn't detect the (1), (2) Switch on the ASC main unit again. cannot be initialized. origin correctly. If the error occurs again, record the status in which this error (2) The vertical arm drive motor message appears and contact your Shimadzu service doesn't operate. representative.
7
Appendix
7-9
AA-6800/6650
7.4 Error Messages
Error Message ASC cannot be detected.
Cause/Details Connection with ASC was interrupted.
ASC Error occurred during action. Press Cancel to close this dialog box. Resolve the ASC problem then retry. ASC I/F port is used for Communication with ASC is unstable. another device. ASC is disconnected, or ASC is set not to be used in sequence parameter settings. The ASC is not connected or the setup for using ASC is not made, although [ASC Sample Pos. for EMISSION Line Search] for Emission mode is selected in the Optics Parameters page to execute the Line Search/Beam Balance in Emission mode. ASC Syringe 1 cannot be (1) The origin detector didn't detect the initialized. origin correctly. (2) The syringe drive motor doesn't operate. ASC table cannot be (1) The origin detector didn't detect the initialized. origin correctly. (2) The turntable drive motor doesn't operate. ASC table motor slipped. -
Remedial Measure Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. Remove the cause of error and switch on the ASC power again. Then connect the ASC in [Instrument]-[Option Connect] menu and try this operation again.
Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. Switch on the ASC and use [Instrument]-[Option Connect] menu to connect the ASC. To make a setting to use the ASC, select [Using ASC] check box in the Sequence page.
7
Appendix
7-10
ASC Timedout.
Atomizer cannot be moved from the program with this instrument. Automatic burner/furnace change system does not exist.
(1), (2) Switch on the ASC main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. (1), (2) Switch on the ASC main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. Verify that rotation of the ASC table is not impeded. Switch on the ASC again and connect the ASC in [Instrument]-[Option Connect] menu. The ASC doesn't response on the way Verify the ASC power supply and the cable connection of the communication. between ASC and AA main unit, then connect the ASC in The communication cable with ASC [Instrument]-[Option Connect] menu. has a problem. The AA software tried to send the Verify that the [Instrument Type] (the main unit) is properly set automatic atomizer setup command to in [Instrument]-[Configuration]. the instrument but the atomizer position setup of the instrument type is manual. The AA software has sent a command Verify that [Instrument Type](Main Unit) is properly selected of atomizer automatic change, although from [Instrument]-[Configuration]. the instrument is the manual type of atomizer change. (1) Increase the hollow cathode lamp current (Low) (pay attention to the max. current). When the lamp mode is BGC-D2, narrow the slit width. (2) Set [Wavelength] correctly in Optics Parameters page. If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp.
B B Background signal is too Beam Balance failed because the light large to execute Beam intensity of BG measurement is too Balance. greater than the light intensity of hollow cathode lamp. The following causes are considerable. (1) The light intensity of the hollow cathode lamp becomes too smaller than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp.
AA-6800/6650
7.4 Error Messages
Error Message Background signal is too small to execute Beam Balance.
BG signal is too large.
BG signal is too small.
Cause/Details Beam Balance failed because the light intensity of hollow cathode lamp is too greater than the light intensity of BG measurement. The following causes are considerable. (1) The light intensity of hollow cathode lamp becomes too greater than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes greater because of the exhaustion of hollow cathode lamp. [When the lamp mode is BGC-D2] (4) The light intensity of BG measurement becomes smaller because of the exhaustion of D2 lamp. (5) The optical axis of D2 lamp is shifted. Beam Balance failed because the light intensity of BG measurement is too greater than the light intensity of hollow cathode lamp. The following causes are considerable. (1) The light intensity of the hollow cathode lamp becomes too smaller than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp. Beam Balance failed because the light intensity of hollow cathode lamp is too greater than the light intensity of BG measurement. The following causes are considerable. (1) The light intensity of hollow cathode lamp becomes too greater than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes greater because of the exhaustion of hollow cathode lamp. [When the lamp mode is BGC-D2] (4) The light intensity of BG measurement becomes smaller because of the exhaustion of D2 lamp. (5) The optical axis of D2 lamp is shifted.
Remedial Measure (1) Decrease the hollow cathode lamp current (Low). When the lamp mode is BGC-D2, widen the slit width (pay attention to the neighboring line). (2) Set [Wavelength] correctly in Optics Parameters page. Narrow the slit width so as not to catch the neighboring line. If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp. (4) Change the D2 lamp. (5) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].
(1) Increase the hollow cathode lamp current (Low) (pay attention to the max. current). When the lamp mode is BGC-D2, narrow the slit width. (2) Set [Wavelength] correctly in Optics Parameters page. If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp.
7
Appendix
(1) Decrease the hollow cathode lamp current (Low). When the lamp mode is BGC-D2, widen the slit width (pay attention to the neighboring line). (2) Set [Wavelength] correctly in Optics Parameters page. Narrow the slit width so as not to catch the neighboring line. If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp. (4) Change the D2 lamp. (5) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].
7-11 AA-6800/6650
7.4 Error Messages
Error Message Cause/Details Blank cannot be inserted Inserting a blank measurement row between the repeat measurement rows here. was tried. Buffer Overflow. Amount of the acquired data is larger than the communication buffer of AA software.
Remedial Measure Execute the blank measurement after the repeat measurements are finished. Switch on the PC power and the instrument power again. If the error occurs again, check the following items. Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. Don't start up other application software simultaneously.
7
Appendix
7-12
C C Calibration Curve cannot The calibration curve order doesn't When the Zero Intercept is not selected, set the calibration be created. match with the number of standard curve order below the number of standard samples. When the Zero Intercept is selected, set the calibration curve samples. order below the number of standard samples or the same. Calibration Curve does not Standard samples (STD or MSA) have Set up STD, in the case of calibration curve method, and MSA, exist! not been measured. in the case of standard addition method or simple standard addition method, on the MRT work sheet and measure them. Calibration Curve is not The calibration curve order doesn't When the Zero Intercept is not selected, set the calibration valid ! match with the number of standard curve order below the number of standard samples. samples. When the Zero Intercept is selected, set the calibration curve order below the number of standard samples or the same. Cannot load file. Change the current setting of [Measurement Type] to other type Measurement Type in "Edit Preparation Parameters" dialog box then read out the (Calibration/SMSA) is target file. different. Cannot load file. Mixing Change the current setting of [Mixing ON] check box to the ON/OFF status is different. opposite one in "Edit Preparation Parameters" dialog box then read out the target file. Can't find drive X: The setup disk of AA software is Try to recover the setup disk using the scan disk of Windows. broken (at the time of installation). Can't heat furnace during Heating was tried before the GFA Wait until the GFA transformer is cooled sufficiently, and then the GFA transformer transformer had been cooled try the operation again. cooling period. Please wait sufficiently. for transformer to cool then retry the operation. Can't set temperature Sending the command to change the Set the furnace program after the heating is finished. program when the GFA furnace program was tried during heats furnace. heating. Communication Timeout. The communication between AA Switch on the PC power and the instrument power again. If the software and AA main unit has a error occurs again, check the following items. problem. Switch on the power of the AA-6800/6650 main unit and wait until a peep sounds three times. Then set the Connect to ON. Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. Fix all the communication cables (AA-PC, AA-ASC, AAGFA-EX7) with screws to avoid an insufficient contact and ground level mismatch of communication port. Communication was The communication between AA Switch on the PC power and the instrument power again. If the aborted from the software and AA main unit has a error occurs again, check the following items. spectrophotometer side. problem. Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. Fix all the communication cables (AA-PC, AA-ASC, AAGFA-EX7) with screws to avoid an insufficient contact and ground level mismatch of communication port. Current measurement The lamp of current measurement Select [Lamp ON] check box in the Optics Parameters page to schedule cannot be element cannot be selected as warm-up light on the lamp of current measurement element. selected. lamp.
AA-6800/6650
7.4 Error Messages
Error Message D D D2 lamp energy is too low
Cause/Details
Remedial Measure (1) Change the D2 lamp. (2) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position]. (1) Change the D2 lamp. (2) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].
(1) The light intensity becomes smaller as the result of D2 lamp exhaustion. (2) The optical axis of D2 lamp is shifted. D2 lamp energy is too low Beam balance failed. The following causes are considerable. (1) The light intensity becomes smaller as the result of D2 lamp exhaustion. (2) The optical axis of D2 lamp is shifted. Drain tank water level is A flashback may be caused by an too low. ignition without sufficient water in drain tank. Therefore, be sure to fill the drain tank with water before igniting a flame.
Fill water via the breather at the top of drain tank little by little until the water overflows from the drain tank to waste container.
E E Emission vial position has Although the ASC is to be used to not been set in the execute Line Search/Beam Balance in following measurement. Emission mode in the setting, [ASC Sample Pos. for EMISSION Line Search] in Optics Parameters page is set to "NONE". Error: Pressure Too Low! (1) In the case of water pressure The water pressure supplied for the GFA-6500 is too low. The water pressure supplied for GFA-EX7 is too low or too high. (2) In the case of Ar gas pressure The Ar gas pressure supplied for GFA is too low.
Set the position of sample to be sprayed at the time of Line Search/Beam Balance in [ASC Sample Pos. for EMISSION Line Search]. Entry for [ASC Sample Pos. for EMISSION Line Search] is available when the [Lamp Mode] is set to "EMISSION" and [Lamp Current (Low)] to "0".
(1) In the case of water pressure Set the water pressure within the range of specification. In the case of GFA-6500, an error message is not indicated when the water pressure is too high. Since too high water pressure may cause water leak, be careful about it. In the case of GFA-EX7, note that the message "ERROR: Pressure is too low!" is also displayed even if the water pressure is too high. Be careful about it. (2) In the case of Ar gas pressure Open the stopcock of Ar gas and adjust the pressure regulator so that the supply pressure satisfies the specification. Error: Pressure Too Low The water pressure supplied for GFA- Set the water pressure within the range of specification. or Too High! EX7 is too low or too high. Expired Lamp is selected. The lamp selected in "Lamp Position Although the "Used Time" is one of the signs to change the Reestablish the setting ? Setup" dialog box has a relation "(Life lamp, a lamp used for longer than the life time can be used if Time) < (Used Time). Line Search/Beam Balance is performed successfully and if the noise level required for the analysis is satisfied. Select [Instrument]-[Configuration] menu and clear the check box of [Show lamp used time over operating life message] not to display this message.
7
Appendix
F F Failed to Schedule.
New When the number of Element Schedules on the MRT work sheet exceeds 20, the excess schedules cannot be read out on the MRT. Failed to detect burner (1) The origin detector couldn't detect moving motor (fore/back) the origin correctly. origin. (2) The burner forward/back movement motor doesn't operate properly. Failed to detect burner (1) The origin detector couldn't detect moving motor (up/down) the origin correctly. origin. (2) The burner up/down movement motor doesn't operate properly.
Add
Delete unnecessary Element Schedules in "Element Selection" page. Also, clear the check box of unnecessary element in [Element Selection] list when reading out parameters in the Template page of "Load Parameters" dialog box. (1), (2) Switch on the AA main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. (1), (2) Switch on the AA main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative.
7-13 AA-6800/6650
7.4 Error Messages
Error Message Cause/Details Failed to detect lamp turret (1) The origin detector couldn't detect motor origin. the origin correctly. (2) The lamp turret motor doesn't operate properly. Failed to detect slit motor (1) The origin detector didn't detect the origin. origin correctly. (2) The slit drive motor doesn't operate. Failed to detect (1) The origin detector couldn't detect wavelength motor origin. the origin correctly. (2) The wavelength drive motor doesn't operate properly. Failed to execute Gas Leak Gas leak check couldn't be started. Check command.
7
Appendix
7-14
Failed to extinguish the EXTINGUISH button of the instrument flame. was not pressed while executing the remaining gas combustion. Failed to load Cookbook The "cookbook.ref" file in the folder in which the AA software is installed cannot be read in. The version of "cookbook.ref" doesn't match the execution file, or the file is broken. Failed to load document. Measurement file or template file cannot be read out in Wizard Selection dialog box.
Remedial Measure (1), (2) Switch on the AA main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. (1), (2) Switch on the AA main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. (1), (2) Switch on the AA main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. Switch on the AA main unit again. If the error occurs again, stop using the instrument and record the error messages and status before and after this error. Then contact your Shimadzu service representative. Press the EXTINGUISH button following the instruction displayed while executing the residual gas combustion. Delete the "cookbook.ref" file and install it again.
Failed to open the serial The PC serial port cannot be used. port.
Failed to send parameters to the instrument. Wait until the instrument becomes READY then retry it. Failed to send the furnace The GFA instrument type selected in Set the correct [GFA] in [Instrument]-[Configuration] menu program for GFA cleaning. the AA software is wrong. then start up the AA software again.
Check the following points. The file tried to load actually exists. The file name contains no period except the period just before the extension (for example, a file named "Cu.Ag.aa" cannot read out ). Check the following points. [COM port] in [Instrument]-[Configuration] is properly set. Other application software (communication software, FAX software, etc.) is not used. The resource of the communication port doesn't compete with other device. Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again.
Failed to send the temperature coefficient. Failed to send the temperature stabilization time. Failed to set Flame Monitor Safety Device to OFF. Failed to turn OFF the gas pressure monitor.
The GFA instrument type selected in Set the correct [GFA] in [Instrument]-[Configuration] menu the AA software is wrong. then start up the AA software again. The GFA instrument type selected in Set the correct [GFA] in [Instrument]-[Configuration] menu the AA software is wrong. then start up the AA software again. Flame monitor couldn't be set OFF while executing the residual gas combustion. The gas pressure monitor couldn't be set OFF while executing the residual gas combustion. Stop using the instrument, switch on the power again and connect it with the PC again. If the item "Flame Monitor ON" becomes NG, contact your Shimadzu service representative. Stop using the instrument. Then switch on the power again and reconnect it with the PC. If NG is displayed for the item "Gas Pressure Monitor ON" on the initialization screen, contact your Shimadzu service representative.
AA-6800/6650
7.4 Error Messages
Error Message Cause/Details Failed to turn ON the gas The gas pressure monitor couldn't be set ON when the residual gas pressure monitor. combustion was finished or cancelled. Flame has extinguished. been (1) The flame monitor detected that the flame is extinguished although the EXTINGUISH button is not pressed. (2) When using Ar-H2 flame, the flame monitor was activated because the flame is colorless. Flame Monitor Safety Flame monitor couldn't be set ON Device was not set. while executing the residual gas combustion. Fuel gas leak detected. As the result of gas leak check, a gas leak from the tubing inside the gas controller was detected. Fuel gas pressure is too (1) The supply pressure of fuel gas low. (C2H2 or H2) or support gas (Air or N2O) has decreased. (2) The PURGE button on the gas controller panel of AA main unit was pressed. (3) Automatic flame extinction was executed at the end time of automatic measurement using the ASC. (4) The flame monitor safety device was activated. (5) There was a momentary AC power outage.
Remedial Measure Stop using the instrument. Then switch on the power again and reconnect it with the PC. If NG is displayed for the item "Gas Pressure Monitor ON" on the initialization screen, contact your Shimadzu service representative. (1) Verify that nothing obstructs the flame monitor. (2) When using Ar-H2 flame, clear [Flame Monitor ON] check box in [Instrument]-[Gas controller Status] to invalidate the flame monitor. When performing a measurement in this status, always stay near the instrument and check the flame doesn't go out. Stop using the instrument, switch on the power again and connect it with the PC again. If the item "Flame Monitor ON" becomes NG, contact your Shimadzu service representative. Stop using the instrument and contact your Shimadzu service representative.
(1) Open the stopcock and check the supply pressure of fuel/support gas by the meter of pressure regulator. If the required pressure is not satisfied, change the fuel/support gas cylinder, check/adjust the air compressor operation or perform other appropriate treatment. (2) ,(3) This doesn't mean an abnormal status. Close the message and continue the operation. (4) Eliminate the cause with which the flame was extinguished. If the supply pressure of fuel/support gas is not lowered and if an ignition is possible, there is no problem. (5) Start up the instrument again. If the supply pressure of fuel/support gas is not lowered and if an ignition is possible, there is no problem. If the error occurs again, record the status in which this error is displayed and contact the Shimadzu service representative. Furnace is not sufficiently Heating was tried before the graphite Wait until the graphite tube is cooled sufficiently, and then try the cooled. Check that cooling furnace is cooled sufficiently. The operation again. water is supplied properly. temperature of cooling water is high or the Verify that the cooling water temperature and pressure are flow of cooling water is not sufficient. within the specifications of the instrument and that the cooling tubes are not pressed or bent. Furnace program does not Original furnace program for the Return to Furnace Program page and set up a furnace program. exist. optimum furnace program search has not been set up.
7
Appendix
G G Gas leak was found.
(1)[When the error message is displayed within 10 minutes after the gas leak check is started] As the result of gas leak check, a gas leak from the tubing in the gas control unit was detected. (2)[When the error message is displayed after 10 minutes or more from the starting of gas leak check] This doesn't mean any abnormal status. In case of gas leak, an error occurs immediately after the starting of check. Gas pressure was too low to execute gas leak check. Please check that the fuel gas supply pressure and execute the gas leak check.
(1) Stop using the instrument and contact your Shimadzu service representative. (2) Close this message and continue the operation.
Check the gauge of the pressure regulator and verify that the supply pressure satisfies the specification. If the required pressure is not detected, perform appropriate measures such as replacement of fuel gas cylinder.
7-15 AA-6800/6650
7.4 Error Messages
Error Message GFA-6500: Furnace is not sufficiently cooled. GFA-EX7: Furnace is not sufficiently cooled or cooling water is too cool. Check that the cooling water temperature are within the specifications of the instrument and it is supplied properly. GFA cannot be detected.
Cause/Details Heating was tried before the graphite furnace is cooled sufficiently. The temperature of cooling water is high or the flow of cooling water is not sufficient. In the case of GFA-EX7, the lower limit of cooling water temperature is also checked. Therefore, the error also occurs when the cooling water is too cool. Connection with GFA was interrupted.
Remedial Measure Wait until the graphite tube is cooled sufficiently, and then try the operation again. Verify that the cooling tubes are not pressed or bent. Verify that the cooling water temperature and pressure are within the specifications of the instrument.
GFA gas pressure is too low. GFA heating is OFF. 1.Turn on the power switch(HEAT) of GFA. 2.Make sure that a graphite tube is set and the graphite furnace is fastened. GFA I/F port is used for other device.
If this error occurs again after executing the measures following the message, the contact between the graphite cap or holder and the graphite tube may be improper. Communication with GFA is unstable.
Verify the GFA power supply and the cable connection between GFA and AA main unit, then connect the GFA in [Instrument]-[Option Connect] menu. Open the Ar gas stopcock and verify that the supply pressure satisfies the specification. Open the graphite furnace and rotate the graphite tube forward and back while pressing the end of the graphite tube to the graphite cap or holder. Through this procedure, the contact with the graphite tube will be recovered.
7
Appendix
7-16
GFA is NOT initialized. Please perform option connect. If you see this message during option connect, check GFA instrument type in [ I n s t r u m e n t ] [Configuration]. GFA returns invalid Temperature Coefficient! (Value of Invalid Temperature Coefficient)GFA serial interface cannot be opened.
GFA Temperature Calibration Error.
GFA timed out.
GFA water pressure is too low.
GFA water pressure is too low or too high.
Verify the GFA power supply and the cable connection between GFA and AA main unit, then connect the GFA in [Instrument]-[Option Connect] menu. Although the initialization command of (1) Verify the GFA power supply and the cable connections GFA-EX7 had not been sent, other between GFA and AA main unit, then connect the GFA in command was sent. [Instrument]-[Option Connect] menu. (1) The power supply of GFA has once (2) Set the correct [GFA] in [Instrument]-[Configuration] failed then recovered. menu then start up the AA software again. (2) The initialization command was not sent because the GFA instrument type selected in the AA software was wrong. The temperature calibration couldn't be Switch on the GFA again. If the error occurs again, record the performed correctly. number indicated in this message and the status in which this error message appears. Then contact your Shimadzu service representative. The ROM program of the AA main unit has a problem. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative. The graphite tube may have been worn Change the graphite tube for a good one. out. If the error occurs again, contact your Shimadzu service Or the optical temperature sensor has a representative. problem. The GFA doesn't response on the way Verify the GFA power supply and the cable connection of the communication. between GFA and AA main unit, then connect the GFA in The communication cable with GFA [Instrument]-[Option Connect] menu. has a problem. [GFA-6500] Set the water pressure within the range of specification and use The water pressure of GFA is too low. it. [GFA-EX7] In the case of GFA-6500, an error message is not indicated The water pressure of GFA is too low when the water pressure is too high. Since too high water or too high. pressure may cause water leak, be careful about it. In the case of GFA-EX7, note that the message "ERROR: Pressure is too low !" is also displayed even if the water pressure is too high. Be careful about it. The water pressure of GFA-EX7 is too Set the water pressure within the range of specification and use low or too high. it.
AA-6800/6650
7.4 Error Messages
Error Message H H
Cause/Details
Remedial Measure (1) Verify that the atomizer or any other thing doesn't obstruct the optical axis. Verify that the lamp is correctly mounted to the socket and the lamp turret position. Rotate the hollow cathode lamp and adjust the optical axis. (2) Increase the hollow cathode lamp current (Low) (pay attention to the max. current). Widen the slit width (pay attention to neighboring lines). (3) Set [Wavelength] correctly in Optics Parameters page. (4) Change the hollow cathode lamp.
HC Lamp Energy is Sufficient light intensity of hollow cathode lamp could not be obtained insufficient. during the wavelength adjustment. The following causes are considerable. (1) The optical axis has a problem. (2) The light intensity of the hollow cathode lamp becomes too small as the result of change in the Optics Parameters, etc. (3) The Line Search failed to catch the correct analytical line. (4) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp. HC lamp energy is too The light intensity of the hollow low. cathode lamp (or emission intensity in the case of flame emission analysis) is small and the Line Search/Beam Balance failed. The following causes are considerable. [In the case of atomic absorption analysis] (1) The hollow cathode lamp is not set in the lamp turret correctly. (2) The optical path is obstructed. (3) The light intensity of the hollow cathode lamp becomes too smaller as the result of change in the Optics Parameters, etc. (4) The Line Search failed to catch the correct analytical line. (5) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp. [In the case of flame emission analysis] (6) The emission intensity of the standard sample of the highest concentration is too small.
(1) Verify that the socket to which the lamp is mounted and the lamp turret position are correctly set. Rotate the hollow cathode lamp to adjust the optical axis (2) Verify that there is no obstacle on the light path. If the burner head or furnace intercepts the light, adjust the origin position. (3) Increase the lamp current (Low) or widen the slit width in the Optics Parameters page. (4) Set [Wavelength] correctly in Optics Parameters page. If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (5) Change the hollow cathode lamp. (6) Use a proper flame type. Adjust the burner height so that the maximum signal may be obtained. Use a standard sample of higher concentration.
7
Appendix
I I Iinvalid Temperature Coefficient is saved in INI file! -(Value of Iinvalid Temperature Coefficient)-
Starting up the AA software detected that the temperature calibration coefficient (key: TempCoef) saved in "wizaa.ini" file in "windows" folder is out of the proper range. Incorrect interface handshake with ASC.
In the case of GFA-EX7, after connecting it with the instrument, mount the graphite tube to be used for measurement following <Change GFA Tube> in Furnace Program page then click <Temp.Calib> to execute the temperature calibration. The ROM program of the AA main unit has a problem. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative. The ROM program of the AA main unit has a problem. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative.
Incorrect interface handshake with GFA.
7-17 AA-6800/6650
7.4 Error Messages
Error Message Instrument failed to execute the command. Please restart the instrument and software and retry Leak Check. Instrument is not ready!
Cause/Details Remedial Measure Gas leak check start command was not Switch on the PC power and instrument power again. If the error occurs again, contact your Shimadzu service executed properly. representative.
(1) A command was tried to send when the communication between the instrument and PC is OFF. (2) While the instrument is executing the command, the next command was tried to send. Instrument is still busy. The operation that cannot be executed during BUSY status of instrument was tried. Invalid ASC Command. A command that is not supported by the ASC was sent from the AA software. Invalid ASC Parameter. Parameters that are not supported by the ASC were sent from the AA software. Invalid error No. has been sent from ASC.
(1) Set the communication with the instrument to ON from [Instrument]-[Connect] menu. (2) Close this message box and wait until the command currently executed in the instrument is finished. Perform the target operation again after "READY" is displayed at the right lower of the status bar. Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again. Verify that the AA software supports the your ASC.
Verify that the AA software supports the your ASC.
7
Appendix
7-18
The ROM program of the AA main unit has a problem. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative. Invalid error No. was sent The ROM program of the AA main unit has a problem. from GFA. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative. Invalid GFA Command A command that is not supported by Verify that the [GFA] is correctly selected in the [Instrument]the GFA was sent from the AA [Configuration]. software. Invalid GFA Parameters Parameters that are not supported by Verify that the [GFA] is correctly selected in the [Instrument]the GFA were sent from the AA [Configuration]. software.
J, K J,K L L Lamp energy is too low to Beam Balance failed because the light execute Beam Balance. intensity of hollow cathode lamp is too small. The following causes are considerable. (1) The light intensity of the hollow cathode lamp becomes too small as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp. Lamp History data file (1) "lamphist.ref" file doesn't exist in (lamphist.ref) cannot be the folder in which the AA software is found. installed. (2) Execution file (wizaa.exe) was copied in the folder other than the installation folder and was executed.
(1) Increase the hollow cathode lamp current (Low) (pay attention to the max. current). Widen the slit width (pay attention to neighboring lines). (2) Set [Wavelength] correctly in Optics Parameters page. If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp.
(1) Check whether the name "lamphist.ref" was changed or not and whether it has been moved to other folder or not. If so, set it back to original condition. If "lamphist.ref" file doesn't exist in the install folder, the AA software creates a new file. (2) Be sure to execute "wizaa.exe" from the install folder.
AA-6800/6650
7.4 Error Messages
Error Message Lamp ID is not valid. Register the proper lamp in Lamp History dialog box, then set the lamp turret position.
Cause/Details In "Lamp Position Setup" dialog box, select a lamp to be used from the lamps registered in "Lamp History" dialog box. Therefore, register the lamp in "Lamp History" dialog box when using a lamp that is not registered. Lamp Socket # is not [Socket #] in the Optics Parameters selected in this schedule. page of the element for warm-up is set "NONE".
Remedial Measure Select [Instrument]-[Lamp History] menu and register the lamp to be used.
Lamp Socket # is wrong. [Socket #] of the element for warm-up This schedule cannot be in the Optics Parameters page is set selected for warmup lamp. "NONE".
Lamp socket# is not specified! Please set socket# for the following elements.
Lamp Used Time exceeded In "Lamp History" dialog box, the lamp the Life Time to be used has a relation "(Life Time) < (Used Time).
Set up the Socket # in the Optics Parameters page of the element for warm-up. When the Socket # you wish to set is not displayed in the list, set up the lamp mounted to the Socket # in <Lamp Pos. Setup>. (If the Lamp ID of the lamp you wish to set is not displayed in the "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History]). Set up the Socket # in the Optics Parameters page. When the Socket # you wish to set is not displayed in the list, set up the lamp mounted to the Socket # in <Lamp Pos. Setup>. (If the Lamp ID of the lamp you wish to set is not displayed in the "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].) In the Optics Parameters page of the element named in the message, set the socket number. If the aimed socket number is not displayed on the list, set the lamp mounted to the aimed socket number in <Lamp Pos. Setup>. (Furthermore, if the lamp of aimed element and type is not displayed on the list in "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].) Although the "Used Time" is one of the sign to change the lamp, a lamp used for longer than the life time can be used if Line Search/Beam Balance is performed successfully and if the noise level required for the analysis is satisfied. Select [Instrument]-[Configuration] menu and clear the checkbox of [Show lamp used time over operating life message] not to display this message.
7
Appendix
M M Memory Lock Failure
Mixing is OFF and Injection volume is more than 100uL. Are you sure? Momentary electric shutdown occurred in the gas controller. Forcibly support gas type is changed to Air and flame monitor is set to ON.
The memory reserved for Switch on the PC power and the instrument power again. If the communication by AA software error occurs again, check the following items. Set all of the PC BIOS setup and the electric power saving couldn't be locked. function of control panel to OFF. Don't start up other application software simultaneously. If the injection volume is too large, the Select an appropriate injection volume after checking that the sample overflows from the graphite sample doesn't overflow from the graphite tube. tube. Momentary power failure of the AC Switch on the AA main unit again. power supply was detected. If the error occurs again, record the status in which this error occurs. Then contact your Shimadzu service representative.
N N No lamps which can be [Socket #] in the Optics Parameters Set up the Socket # in the Optics Parameters page. When the used for this measurement page is set "NONE". Socket # you wish to set is not displayed in the list, set up the are set. Set a lamp which is lamp mounted to the Socket # in <Lamp Pos. Setup>. (If the suitable for measurement Lamp ID of the lamp you wish to set is not displayed in the element and lamp mode. "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].) No. of Mixing Cycles is The setting of Mixing ON is not Set up [Mixing ON] in "ASC Parameters" page again. Invalid. properly saved in the measurement parameters.
7-19 AA-6800/6650
7.4 Error Messages
Error Message O O
Cause/Details
Remedial Measure (1) "lamphist.ref" can be renewed from the AA software firstly started up but cannot be renewed from the AA software secondly started up. Therefore, use the AA software firstly started up to perform measurement. There is no problem to use the AA software secondly started up to edit parameters. (2) Turn the read-only attribute of "lamphist.ref" file in AA software folder OFF. (1) "lampplace.ref" can be renewed from the AA software firstly started up but cannot be renewed from the AA software secondly started up. Therefore, use the AA software firstly started up to perform measurement. There is no problem to use the AA software secondly started up to edit parameters. (2) Turn the read-only attribute of "lampplace.ref" file in AA software folder OFF.
Other program is using "lamphist.ref" file is a data file for lamp lamphist.ref file. Lamp history. The following causes are data will not be saved. considerable when this message is displayed. (1) The second AA software has been started up. (2) The file attribute of "lamphist.ref" is read-only. Other program is using "lampplace.ref" file is a data file for lampplace. ref file. Lamp lamp position setup. The following data will not be saved. causes are considerable when this message is displayed. (1) The second AA software has been started up. (2)The file attribute of "lampplace.ref" is read-only.
P P Periodic Blank Preparation Parameters is Invalid.

Please connect ASC. (1) Although the auto-sampler is necessary for the operation, the ASC is not connected. (2) Although the ASC is used in the measurement conditions, the ASC is not connected.
7
Appendix
7-20 AA-6800/6650
Please connect GFA serial The GFA power is set OFF or the interface. communication cable between GFA and AA main unit is disconnected. Please connect GFA. The GFA is not connected although the GFA is necessary for the operation or measurement. Please connect the ASC The ASC power is set OFF or the serial interface. communication cable between ASC and AA main unit is disconnected. Please select the Flame Type. Please set the socket # combinig even/odd in turn. Flame type is not selected properly in Atomizer/Gas Flow Rate Setup page. The lamps cannot be lit on simultaneously when their socket # combination is even/even or odd/odd. Therefore, when measuring many elements, it is recommended to set up the even/odd of the socket # in turn to perform efficient warm-up. Please set the total time of Furnace Program less than 300 (sec). Please set the total time Since the data sampling is started before the sampling stage before executing the sampling stage in more than 3 (sec). the furnace program, a stage of 3 seconds or longer is always necessary prior to the sampling stage.
If an invalid value that is not usually entered has been entered in the Blank Samples table of the "Edit Preparation Parameters" dialog box, enter a correct value. (1) Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. (2) When the ASC is necessary for the measurement, connect the ASC in the procedure as above. When the ASC is not necessary, clear the [Using ASC] check box in the [Parameters]-[Edit Parameters]-[Sequence]. Verify the GFA power supply and the cable connection between GFA and AA main unit, then connect the GFA in [Instrument]-[Option Connect] menu. Fix the communication cable between GFA-EX7 and AA main unit with the screws. Verify the GFA power supply and the cable connection between GFA and AA main unit, then connect the GFA in [Instrument]-[Option Connect] menu. Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. Fix the communication cable between ASC and AA with the screws. Select a correct flame type in Atomizer/Gas Flow Rate Setup page. Change the order of measurements in the "Element Selection" page so that the socket number combination may be even/odd in turn. When you wish not to change the order of measurements or when changing the measurement order cannot make the even/odd combination, change the lamp mounting position by <Lamp Pos. Setup> in Optics Parameters page. Change the furnace program so that the total time of the furnace program may be within 300 seconds. [When the sampling stage is in the first row] Insert a stage of 3 seconds or longer before the sampling stage. [When the sampling stage is in the second row or after] Change the program so that the total time of the stages before the sampling stage may be 3 seconds or longer.
7.4 Error Messages
Error Message Cause/Details Please specify the lamp Line Search/Beam Balance couldn't be executed because [Socket #] in the socket#. Optics Parameters page is set "NONE".
Remedial Measure Set up the Socket # in Optics Parameters page of the current measurement element. When the Socket # you wish to set is not displayed in the list, set up the lamp mounted to the Socket # in <Lamp Pos. Setup>. (If the Lamp ID of the lamp you wish to set is not displayed in the "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].)
Q, R Q,R S S Sample Preparation Parameters is Invalid.

Schedule does not exist! If an invalid value that is not usually entered has been entered, enter a correct value in the Unknown Samples table in the "Edit Preparation Parameters" dialog box. In the measurement using the ASC, Select the measurement element and set up the measurement Element schedule has not been procedure in [Action] fields on the MRT work sheet. selected, or the measurement procedure has not been set up although the element schedule exists. The ROM program of the AA main unit has a problem. Record the instrument information displayed on the initialization screen and the status in which this error occurs. Then contact your Shimadzu service representative. The PC serial port has a problem. Switch on the PC power and the instrument power again. If the error occurs again, check the following items. Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. Fix all the communication cables (AA-PC, AA-ASC, AAGFA-EX7) with screws to avoid an insufficient contact and ground level mismatch of communication port. To avoid overrun of PC serial port, lower the receive buffer of FIFO on the control panel. The tried operation cannot be executed After changing the measurement mode of the instrument to unless the flame measurement mode is flame, execute the target operation. Perform the following set in the instrument. operation to change the measurement mode of the instrument to flame. [When the flame measurement exists on the MRT] Select the flame measurement from the measurement element tool bar. [When the flame measurement doesn't exist on the MRT] Select [Parameters]-[Element Selection Wizard] and add a flame measurement by <Select Elements> in the "Element Selection" page. Then select the measurement from the [Meas. Element] drop-down list as current measurement element and click on <Finish>. The tried operation cannot be executed After changing the measurement mode of the instrument to unless the furnace measurement mode furnace, execute the target operation. Perform the following is set in the instrument. operation to change the measurement mode of the instrument to furnace. [When the furnace measurement exists on the MRT] Select the furnace measurement from the measurement element tool bar. [When the furnace measurement doesn't exist on the MRT] Select [Parameters]-[Element Selection Wizard] and add a furnace measurement by <Select Elements> in the "Element Selection" page. Then select the measurement from the [Meas. Element] drop-down list as current measurement element and click on <Finish>.
Serial interface cannot be opened.
Serial Port Error.
7
Appendix
Set the flame measurement as a current measurement.
Set the furnace measurement as a current measurement.
7-21 AA-6800/6650
7.4 Error Messages
Error Message Since odd/even of the socket # was the same as that of measurement lamp, the warmup lamp was lit off and the setting was cleared. Spectrophotometer has not been turned ON or cable is disconnected.
Cause/Details The measurement element is edited when the warm-up lamp is lit on, and as the result, the warm-up lamp socket # and the measurement element lamp socket # become the same odd/even number. -
Remedial Measure Close the message and set up the warm-up lamp again in Optics Parameters page of the current measurement element.
Standard Preparation Parameters is Invalid. Support gas pressure is too (1) The supply pressure of support gas low. (Air or N2O) has decreased. (2) The support gas pressure was lowered from the gas controller panel on the right side of the AA main unit. Switch the Flame Type to When the support gas is N2O, AIR-C2H2 before the executing the residual gas combustion remaining gas combustion. may cause a flashback.
7
Appendix
7-22
Switch on the PC power and the instrument power again. If the error occurs again, check the following items. Verify that the communication cables between AA main unit and PC are connected properly and fixed with screws. Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. If an invalid value that is not usually entered has been entered in the STD Samples table of the "Edit Preparation Parameters" dialog box, enter a correct value. (1) Open the stopcock and check the supply pressure of support gas by the meter of the pressure regulator. If the required pressure is not satisfied, change the support gas cylinder, check/adjust the air compressor operation or perform other appropriate treatment. (2) Set the proper pressure. Set [Flame Type] to [AIR-C2H2] in Atomizer/Gas Flow Rate Setup page and switch [BURNER SELECT] (burner selection key switch) of the AA main unit to [AIR-C2H2] side. Then execute the residual gas combustion.
T T Termination has not been Communication protocol with ASC Verify the ASC power supply and the cable connection accepted from ASC. was not completed. (:T) between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. Termination has not been Communication protocol with GFA Verify the GFA power supply and the cable connection accepted from GFA. was not completed. (:T) between GFA and AA main unit, then connect the GFA in [Instrument]-[Option Connect] menu. The following lamps exist The data mismatching between the Click on <Yes> and delete the data from the lamp position in the Lamp Position Setup lamp history and the lamp position setup. Register the necessary lamps in [Instrument]-[Lamp Dialog Box, but do not setup was detected at the time of History]. Next, make a setting of the lamp mounted to each exist in the Lamp History starting up the AA software. socket in [Instrument]-[Lamp Position Setup]. Dialog Box. Please update the Lamp History Dialog Box or delete lamps from the Lamp Position Setup Dialog Box. Socket #x,x,x, The GFA instrument type The GFA instrument type selected in Set the correct [GFA] in [Instrument]-[Configuration] menu is not selected correctly. the AA software is wrong. then start up the AA software again. Please select proper GFA instrument type and restart this software. The instrument fail to The gas flow rate setup command has When an error occurs to the fuel gas flow rate setup in adjust the gas flow rate to failed. Atomizer/Gas Flow Rate Setup page, stop using the instrument the optimal position. and contact your Shimadzu service representative. The instrument fail to The burner movement command has Remove the obstacles that disturb the burner movement then move the burner to the failed. switch on the instrument power again. optimal position. The selected area cannot In [Instrument]-[Lamp Position Setup] menu, select [NONE] be cleared as the for [Element] field of the lamp ID you wish to clear, and click information is stored in the on <OK>. Then clear the target lamp in "Lamp History" dialog Lamp Position Setup box. Dialog Box.
AA-6800/6650
7.4 Error Messages
Error Message The selected area cannot be deleted as the information is stored in the Lamp Position Setup Dialog Box. The selected area contains the D2 lamp. D2 lamp row cannot be deleted. This file cannot be loaded because instrument type is different.***Flow Rate X isn't suitable for this instrument. This file cannot be loaded because instrument type is different.***Slit Width X isn't suitable for this instrument. This file is not to be loaded. Software doesn't support this file. This operation cannot be executed during action or measurement. This operation cannot be executed while the hollow cathode lamp is lit ON. Please retry it after you turn off the lamp. Time out occured during the GFA transformer is cooling down. Timer cannot be created. After closing other applications, try it again. Too many schedules. Failed to add all schedules.
Cause/Details -
Remedial Measure In [Instrument]-[Lamp Position Setup] menu, select [NONE] for [Element] field of the lamp ID you wish to delete, and click on <OK>. Then delete the target lamp in "Lamp History" dialog box.
Deleting the first row for D2 lamp in The first row for D2 lamp is fixed and cannot be deleted. "Lamp History" table was tried. Measurement file (*.aa) measured in different model (AA main unit) may not be read out because of parameter mismatch. Measurement file (*.aa) measured in different model (AA main unit) may not be read out because of parameter mismatch. The extension of file is wrong. Use the software that corresponds with the same (or compatible) model to read out the file. When reading out only the parameters, use the template file (*.taa). The parameters are read out after converted to match with the model. Use the software that corresponds with the same (or compatible) model to read out the file. When reading out only the parameters, use the template file (*.taa). The parameters are read out after converted to match with the model. Load a file that has the extension indicated in [Files of type] in "Open" dialog box. Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again. Turn off the lamp in Optics Parameters page of the current measurement element. Use [Lamp ON] check box in the case of measurement lamp and <Warmup Lamp> button in the case of warm-up lamp. Then, execute the aimed operation. Switch on the GFA and PC again. If the error occurs again, record the status in which this error occurs. Then contact your Shimadzu service representative. Start up the PC again. Also, don't start other applications.
The operation tried cannot be executed when the instrument is BUSY status or while the measurement is executed. -
7
Appendix
The GFA is in waiting status for cooling transformer and cannot recover. The number of timers currently used exceeds the limit of the Windows system. When executing [File]-[Additional Load], the excess schedules cannot be read out on the MRT work sheet if the number of Element Schedules on the MRT work sheet exceeds 20.
When the Element schedule you wish to add is located in the latter part of the original file of adding, start up another AA software and load the original file for adding and move the order of target Element schedule. Or take out only the element schedule and save it as different file name to create an original file for adding. Load a file that has the extension indicated in [Files of type] in "Open" dialog box. Switch on the PC power and the instrument power again. If the error occurs again, record the number indicated in the error message and the status in which the errors occurred. Then contact your Shimadzu service representative. It is possible to input the values as "(Life Time) < (Used Time)". If the values are not wrong, continue the input.
U U Unexpected file format.
The extension of file is wrong.
Unknown Status Code: An error that is not defined in the AA /(Error Code) software inside has occurred.
Usage time has exceed When registering the lamp in "Lamp lamp life time. History" dialog box, the input values has a relation "(Life Time) < (Used Time)".
7-23 AA-6800/6650
7.4 Error Messages
Error Message V V Valid Injection position is not set. Use <Move Upward>/<Move Downward> button to move the nozzle to proper position.
Cause/Details
Remedial Measure
The injection position is set higher than Set the injection position properly then <Move near to Tube> the destination nozzle position in "ASC can be used. Furnace Nozzle Position Adjustment" dialog box, and as the result, <Move Near to Tube> cannot be executed.
W W Wizard cannot be executed during measurement or when the instrument is BUSY. X, Y, X,Y,Z Z
Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again.
7
Appendix
7-24 AA-6800/6650

AA-6800-6650 IM VerFocr

Transféré par

Informations du document

Titre original

Copyright

Formats disponibles

Partager ce document

Partager ou intégrer le document

Options de partage

Avez-vous trouvé ce document utile ?

Ce contenu est-il inapproprié ?

Droits d'auteur :

Formats disponibles

AA-6800-6650 IM VerFocr

Transféré par

Droits d'auteur :

Formats disponibles

206-94425F

Precautions for Safe Operation

Precautions on the Installation Site and Handling

High temperature burner

Standard analytical conditions

Internal repair and maintenance

Gas supply hoses

Precautions on Handling High Pressure Gas

Installation of gas cylinder

After use of gas

Precautions on Handling Hollow Cathode Lamp

Precautions on Handling Deuterium(D2) Lamp

Supply Period of Replacement Parts

Warning Marking on the Equipment

WARNING RISK OF EXPLOSION Do not use oxygen gas.

Power switch Power cable

Power Switch and Power Cable of Atomic Absorption Spectrophotometer

Figure 7 Power Switch and Power Cable of GFA-6500

Inspection Procedure in Case of Flashback

Burner head Gas tube

Burner head fixing port O-rings

Ceramic ball Retaining plate Fixing screw

Chamber fixing screw

Mixer O-ring Drain tube

Figure 8 Burner Unit

Liquid level sensor Drain tank

Figure 9 Drain Tank

Assembling the AA-6800/6650 2-18

Assembling GFA-6500 2-26

2.5.4.1 2.5.4.2 2.6 2.7

Mounting a Hollow Cathode Lamp2-32 Installing the ACF-6800 2-33

Deuterium Lamp3-3 Burner Module 3-4 AA-6800 3-4 AA-6650 3-5

3.1.4.1 3.1.4.2 3.1.5 3.1.6 3.1.7 3.1.8 3.2.1 3.2.2 3.2.3

3.2 GFA-6500 Configuration 3-12

Software Basic Operation (Furnace Method) 4-20

Saving the Template4-38

4.3 Measurement Procedures 4-39

4.3.1 4.3.2 4.4 4.4.1 4.4.2 4.4.3 4.5 4.6

Saving/Printing/Deleting the Data 4-43

Operating the MRT work sheet 4-56

Copy and Paste 4-65

Igniting and Extinguishing the Flame 4-67

Standard Addition Method and Simple Standard Addition Method 4-74

Conditions and Operation for Flame Emission Analysis 4-79

4.10.1 Optics ParametersPage 4-79

5.3 [Edit] 5-14

5.5.1 Element SelectionPage 5-18

5.5.9 Furnace ProgramPage (for furnace method) 5-46

[Edit Parameters] 5-54

5.8 [Instrument] 5-69

5.8.6.1 5.8.6.2 5.8.6.3 5.8.6.4 5.8.6.6 5.8.6.7

5.8.6.5 [Burner Origin Position Adjustment](AA-6650) 5-82

[Maintenance only for service engineer] 5-85

Furnace Position Adjustment 6-3

6.2.2.1 6.2.2.2 6.2.3 6.3 6.4

Cleaning the Chamber 6-7

Replacing Graphite Tube (GFA-6500) 6-11

6.11.1 6.11.2 6.12 6.12.1 6.12.2 6.12.3 6.12.4 6.12.5

Special Accessories 6-23

6.12.6 6.12.7 6.12.8

Error Messages 7-9

AA-6650F6650G Common Specifications

Baseline Correction Sensitivity Correction Table Data Processing Functions