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WinFLOW Software V4.

2
Operators Manual

Flow Solution 3100 System

Flow Solution IV System

151 Graham Road P.O. Box 9010 College Station, Texas 77842-9010
Telephone (979) 690-1711 FAX (979) 690-0440 www.oico.com oimail@oico.com

Notice
The information contained in this document may be revised without notice.
OI Analytical shall not be liable for errors contained herein or for incidental or
consequential damages in connection with the furnishing, performance, or use of this
material.
No part of this document may be reproduced, photocopied, or translated to another
language without the prior written consent of OI Analytical.
Rev. 2.3 July 2007

Adobe and Acrobat Reader are registered trademarks of Adobe Systems, Inc.
Windows is a registered trademark of Microsoft Corporation.
CNSolution, Flow Solution, and WinFLOW are trademarks or registered trademarks of OI Analytical.

OI Analytical Part Number A001965


Printed in the U.S.A.
Publication 134800707
Copyright 20052007 OI Analytical

ii

Limited Warranty
OI Analytical warrants each OI Analytical manufactured product against defects in
materials and workmanship under normal use and service for a period of one year.
Equipment installed by OI Analytical is warranted from the installation date; all other
equipment is warranted from the ship date. If purchaser schedules or delays installation
more than 90 days after delivery, then the warranty period starts on the 91st day from
date of shipment. This warranty extends only to the original purchaser. OI Analytical
will, at its option, repair or replace equipment that proves to be defective during the
warranty period, provided the equipment is returned to OI Analytical at the expense of
the purchaser.
Consumables, expendables, and parts are warranted for 30 days and are not covered
under extended warranties or service contracts.
OI Analytical warrants for a period of one year from the date of delivery: (i) the
Software, when installed and used with an OI Analytical recommended hardware
configuration, will perform in substantial conformance with the documentation
supplied with the Software; and (ii) the physical media on which the Software is
furnished will be free from defects in materials and workmanship under normal use.
This warranty shall not apply to defects originating from, but not limited to, the
following:

Improper maintenance or operation by the purchaser;

Purchaser supplied accessories or consumables;

Modification or misuse by the purchaser;

Operation outside the products environmental and electrical specifications;

Software, interfacing, parts, or supplies not supplied by OI Analytical;

A computer not meeting the minimum specifications recommended by OI


Analytical;

Improper or inadequate site preparation;

Purchaser induced contamination or leaks.

THE FOREGOING WARRANTY IS IN LIEU OF ALL OTHER WARRANTIES,


EXPRESSED OR IMPLIED, INCLUDING BUT NOT LIMITED TO ANY
WARRANTY OF MERCHANTABILITY, FITNESS, OR ADEQUACY FOR ANY
PARTICULAR PURPOSE OR USE. OI ANALYTICAL SHALL NOT BE LIABLE
FOR ANY SPECIAL, INCIDENTAL, OR CONSEQUENTIAL DAMAGES,
WHETHER IN CONTRACT, TORT, OR OTHERWISE.
Any service requests or questions should be directed to the OI Analytical Customer
Support Center at (800) 336-1911 or (979) 690-1711.

iii

Safety Information
For operator safety, pay special attention to the WARNING and CAUTION statements
throughout the manual.

A WARNING indicates a condition or possible situation that could result in


physical injury to the operator.
A CAUTION indicates a condition or possible situation that could damage or
destroy the product or the operators work.

Warnings and precautions in this manual or on the instrument must be followed during
operation, service, and repair of the instrument. Failure to follow these warnings and
precautions violates the safety design standards and intended use of the instrument.
OI Analytical is not liable for the operators failure to comply with warnings and
precautions.

iv

Table of Contents
Notice .............................................................................................................................. ii
Limited Warranty ........................................................................................................ iii
Safety Information ....................................................................................................... iv

Chapter 1: Introduction ........................................................ 1


Features .......................................................................................................................... 1
Computer Requirements .............................................................................................. 2
Security Settings for Windows XP Operating Systems...........................................2

Chapter 2: Installation .......................................................... 4


Installing WinFLOW .................................................................................................... 4
Security Settings for Windows XP Operating Systems ........................................... 5

Chapter 3: Configuration ..................................................... 7


Configuring WinFLOW ............................................................................................... 7
Configuring the RA Sampler ....................................................................................... 9
Vial Depths..............................................................................................................10
Dilutor Setup ...........................................................................................................12
Wash and Diluent ....................................................................................................13
Rack Placement .......................................................................................................14
Rack Editor..............................................................................................................15
Configuring the 3360 Sampler ................................................................................... 18
Vial Depths..............................................................................................................19
Dilutor Setup ...........................................................................................................20
Wash and Diluent ....................................................................................................21
Rack Placement .......................................................................................................21
Peck Probe during Rinse .........................................................................................22
Configuring the 3090 Sampler ................................................................................... 22
Vial Depths..............................................................................................................23
Wash and Diluent ....................................................................................................24
Rack Placement .......................................................................................................25
Peck Probe during Rinse .........................................................................................25

Chapter 4: Introduction to WinFLOW ............................... 26


Starting WinFLOW .................................................................................................... 26
Select View Dialog Box ..........................................................................................26
Tools Menu................................................................................................................... 27
Preferences ..............................................................................................................28
Configuration...........................................................................................................28
Events Scheduler .....................................................................................................29
Instrument Control...................................................................................................30
Pump Timer .............................................................................................................30
Window Menu ............................................................................................................. 30
About Menu ................................................................................................................. 31

Shortcut Keys .............................................................................................................. 31


Icon Ribbon.................................................................................................................. 31
System Security ........................................................................................................... 33
WinFLOW Quick Start .............................................................................................. 34

Chapter 5: Method Editor................................................... 36


General Description .................................................................................................... 36
Method Editor Icon Ribbon..................................................................................... 37
Opening a Method ...................................................................................................37
Creating a Method ...................................................................................................38
Saving a Method......................................................................................................38
Flow Control Settings Screen ..................................................................................... 38
Instrument................................................................................................................39
Sampling Mode .......................................................................................................39
CCV/Drift Fail.........................................................................................................41
Vial Types ...............................................................................................................41
Off-scale (HI) Samples............................................................................................41
Insert Baselines........................................................................................................42
Pump Control...........................................................................................................42
Detector/Channel Settings Screen ............................................................................. 43
Channels ..................................................................................................................43
Name .......................................................................................................................43
Methodology ...........................................................................................................44
CAS Number ...........................................................................................................44
Detector Settings .....................................................................................................44
Channel Subtractions...............................................................................................45
Signal Filter and Marking Settings Screen............................................................... 46
Smoothing ...............................................................................................................47
Baseline Marking.....................................................................................................48
Inverted Chemistry ..................................................................................................48
Peak Marking...........................................................................................................48
Calibration/Quantitation Settings Screen................................................................. 50
Calibration ...............................................................................................................51
Quantitation .............................................................................................................51
Flagging...................................................................................................................52
Overlimit Samples ...................................................................................................52
Timed Events Editor Screen....................................................................................... 52
B (Basis of Timing) .................................................................................................53
Time.........................................................................................................................53
Device......................................................................................................................53
# (Selector) ..............................................................................................................54
State .........................................................................................................................54
Calibrants Table Editor Screen ................................................................................. 55
Calibrants.................................................................................................................55
Independent Calibration Verification ......................................................................56
Continuing Calibration Verification........................................................................56
Spike........................................................................................................................56
Stock Calibrants.......................................................................................................57
Drift Correction .......................................................................................................57
Verifying Method Settings .......................................................................................... 57

vi

Chapter 6: Sample Table.................................................... 58


Cup Number ............................................................................................................59
Sample Names .........................................................................................................60
Sample Type............................................................................................................60
Replicate ..................................................................................................................61
Dilution and Weight Factors ...................................................................................61
Vial Type .................................................................................................................61
Comments................................................................................................................61
Sample Table Menu Options ...................................................................................... 62
File Menu ................................................................................................................62
Edit Menu ................................................................................................................62
Tools and Window Menus.......................................................................................63
Creating a Sample Table............................................................................................. 63
Synchronization Peak (SYNC)................................................................................63
Carryover Correction (CO)......................................................................................63
Calibrants.................................................................................................................63
Calibrants To Be Diluted.........................................................................................63
Unknowns To Be Diluted ........................................................................................64
Stock Solutions........................................................................................................64
Incremental Sensitivity Drift Correction .................................................................65
Total Sensitivity Drift Correction............................................................................65
Independent Calibration Verification ......................................................................65
Continuing Calibration Verification........................................................................65
Spiked Samples .......................................................................................................66
Blanks and Baseline Samples ..................................................................................66
Autodilution ................................................................................................................. 67
Import and Export Functions .................................................................................... 68
Exporting a Table ....................................................................................................68
Importing a Table ....................................................................................................68

Chapter 7: Data Collection................................................. 69


Initiating Data Collection ........................................................................................... 69
Monitoring the Baseline.............................................................................................. 72
Starting a Sample Analysis......................................................................................... 73
Peak Plot Screen ......................................................................................................73
Calibration Plot Screen............................................................................................73
Calibration Results Screen ......................................................................................74
Peak Table Results Screen.......................................................................................75
Adding Samples to a Sample Table.........................................................................75
Modifying a Sample Table During a Run ................................................................. 76
Stopping a Run ............................................................................................................ 76
Operator-Stopped Run.............................................................................................76
WinFLOW-Stopped Run.........................................................................................76

vii

Chapter 8: Results and Analysis....................................... 77


Loading a Data File..................................................................................................... 77
Data Processing Tools ................................................................................................. 78
Data Analysis Screen...............................................................................................78
Grid On/Off Icon .....................................................................................................78
Peak Editor Icon ......................................................................................................78
Recalculate Icon ......................................................................................................78
Delete/Reprocess Peaks Icon...................................................................................79
Menu Options ..........................................................................................................80
Peak Plot Screen .......................................................................................................... 82
Magnifying the Peak Plot ........................................................................................82
Using the Cursor For Peak Identification ................................................................83
Changing a Peak State (Add, Delete, Toggle Baseline Point).................................83
Calibration Plot Screen............................................................................................... 84
Magnifying the Calibration Plot ..............................................................................84
Using the Cursor for Calibration Point Identification .............................................84
Removing Outlier Calibration Points ......................................................................84
Peak Results Table Screen .......................................................................................... 85
Peak Results Table Fields........................................................................................85
Calibration Results Table Screen............................................................................... 87
Calibrant ID .............................................................................................................87
Calibration Coefficients...........................................................................................87
Correlation Coefficient............................................................................................87
Carryover.................................................................................................................87
Drift Correction .......................................................................................................87
Reports ......................................................................................................................... 88
Exporting a Report ..................................................................................................... 89

Chapter 9: Troubleshooting............................................... 90
Instrument Errors ....................................................................................................... 90
WinFLOW Errors....................................................................................................... 91
Reporting Errors ......................................................................................................92

viii

Chapter 1 Introduction
The WinFLOW software is a Windows-based program designed to offer a high
level of automation when used with any of the OI Analytical Flow Solution systems,
as well as many other automated chemistry analyzers.

Features

Automatic startup and shutdown enhances system productivity.*


Pause option permits run and sample table modification anytime during a run.
Sensitivity drift correction eliminates the need to fully recalibrate after ICV/CCV
failure.
Operator-defined dilution factors add operator flexibility in autodilution mode.*
Sample dilution before the run reduces analysis time.
Automatic working calibration standard preparation from stock solutions reduces
operator workload.*
Manual injection mode permits system operation without an autosampler.
Peak editing improves peak height and area marking.
Post-run peak height, area, and digital signal processing algorithms enhance
analyte detectability.
Mean and RSD values add important QA/QC data to reports.
Options provide customized reporting capabilities.
Complete French, German, and Spanish language support provides enhanced
usability.
*This feature requires specific hardware for full system functionality.

The WinFLOW software package includes the following:

CD-ROM containing the following:


WinFLOW Software
Hardware Operators Manual (one of the following):
WinFLOW Software Operators Manual
Flow Solution IV Operators Manual
Flow Solution IV Operators Manual
Flow Solution 3000 Operators Manual
Flow Solution 3100 Operators Manual
CNSolution FS 3100 Operators Manual
Adobe Acrobat Reader

WinFLOW software serial number (labeled on the outside of the CD-ROM case)

WinFLOW Software Operators Manual: Chapter 1


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Introduction

Computer Requirements
The following table contains minimum and recommended computer requirements for
successfully installing and using the WinFLOW software.
Table 1.1. Computer requirements

Parameter

Minimum

Recommended

Type

IBM compatible

IBM compatible

Processor speed

1 GHz

3 GHz

Memory

512 MB

1 GB or greater

Free disk space

500 MB

1 GB or greater

Operating system

Windows 2000 or XP
Pro

Windows XP Pro

Graphics

SVGA

XGA

COM port

One available RS-232 or


USB-to-RS-232 converter

One available RS-232

NOTE: Using WinFLOW software requires a working knowledge of the Windows


2000 or Windows XP Pro operating system.
NOTE: Flow Solution III and Flow Solution IV systems larger than three channels
or Flow Solution 3000 systems larger than two channels require the
recommended computer requirements.
NOTE: Power management features (excluding the monitor) can cause shutdowns
and errors during analysis.

Security Settings
for Windows XP
Operating
Systems

When using the WinFLOW software with a Windows XP Pro operating system, set
permissions to Everyone for full control of all WinFLOW software features. The
default setting for the Windows XP Pro operating system is NO users. Therefore,
change permissions to Everyone after installing WinFLOW software on the
computer.
1. Enable Full Control to Everyone by right-clicking Start at the screens lower left
corner.
2. Click Explore.
3. Find the Folder named Flow_4.

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Introduction

NOTE: WinFLOW normally installs in this folder. If the software installed in a


different location, go to that folder.
4. Right-click the Flow_4 folder and select Properties.
5. Under the Security tab, click the Add button.
6. In the Select Users, Computers, or Groups dialog box, type the word Everyone
under the Enter the object names to select section and click OK (see Figure 1.1).

Figure 1.1. Permissions dialog box

7. Click the checkbox under Allow next to Full Control to enable full control.
8. Click Apply and OK to exit the screen.

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Rev. 2.3

Chapter 2 Installation
This chapter presents step-by-step procedures for properly installing WinFLOW.

Installing WinFLOW
The WinFLOW CD contains WinFLOW software, the WinFLOW software manual,
and all instrument operation manuals. Install WinFLOW using the following
instructions:
1. From the Windows environment, insert the WinFLOW CD into the available CDROM drive. The WinFLOW Setup Disc screen appears (Figure 2.1).

Figure 2.1. WinFLOW Setup Disc screen

If the WinFLOW Setup Disc screen does not automatically appear after inserting
the CD:

Click the Windows Start button.

Select Run.

Type x:\setup, where x represents the letter assigned to the CD-ROM drive.

Click OK to display the WinFLOW Setup Disc screen.

2. Select the appropriate language and click Install to begin the installation process.
Follow the instructions on the screen.
NOTE: Do not use more than eight characters or spaces in the directory names.

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Installation

3. After WinFLOW installs, click OK. The Configure WinFLOW dialog box appears
(Figure 2.2). Proceed to Chapter 3, Configuration on page 7 for details on
configuring WinFLOW.

Figure 2.2. Configure WinFLOW dialog box

Security Settings for Windows XP Operating Systems


When using WinFLOW with a Windows XP operating system, set permissions to
Everyone for full control of all of WinFLOW software features. The default setting for
a Windows XP operating system is NO users. Therefore, change permissions to
Everyone after installing WinFLOW on the computer.
1. Enable Full Control to Everyone by right-clicking Start at the screens lower left
corner.
2. Click Explore.

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Installation

3. Find the Folder named Flow_4.


NOTE: WinFLOW normally installs in this folder. If the software installed in a
different location, go to that folder.
4. Right-click the Flow_4 folder and select Properties.
5. Click the Security tab and add the group Everyone if not already created
(Figure 2.3).

Figure 2.3. Permissions dialog box

6. Click the checkbox under Allow next to Full Control to allow everyone full control
permissions.
7. Click Apply and OK to exit the screen.

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Rev. 2.3

Chapter 3 Configuration
After installing WinFLOW, configure communications to the analyzer and autosampler.

Configuring WinFLOW
1. Access the Configuration Editor by selecting FLOW config 4.2 from the Start
menu. Click Programs, WinFLOW, and then the FLOW config icon (or go to
Tools Configuration in WinFLOW). The Configure WinFLOW dialog box appears
(see Figure 3.1).

Figure 3.1. Configure WinFLOW dialog box

2. Under Configure Software, select the appropriate language for WinFLOW to


display for its titles, buttons, labels, etc. The language options are English, French,
Dutch, and Spanish.

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Configuration

3. Click the Edit Facility Information button to enter a facility name and department
to display on hard-copy reports.
4. Select the Create Debug Files checkbox to generate text files that assist OI
Analytical support personnel with troubleshooting software and performance
problems.
5. Select the communication port (Com Port), Sampler Control, and the analyzer
type (Platform) to use. Only available communication ports appear as choices.
6. Select the appropriate Sampler Control.
a. Select Standalone if using an autosampler not listed or if no autosampler is
used. If using an autosampler not listed, the autosamplers timing cycle must
match WinFLOW. The autosampler and data collection must initiate at the
same time.
b. Select RA to use vials and vial racks provided with the RA Sampler. The RA
Sampler supports any combination of three trays: 21, 24, 40, 60, or 90
positions; the RA sampler also supports the Autodilutor.
c. Select 3360 to use vials and vial racks provided with the Model 3360 Sampler.
The Model 3360 supports any combination of four 60-position and 90-position
racks; the Model 3360 also supports the Autodilutor.
d. Select 3090 to use vials and vial racks provided with the Model 3090 Sampler;
the Model 3090 supports either one 60-position or one 90-position rack.
e. Click the Configure Sampler button to set the sampler to utilize up to four
different types of sample cups, configure any dilutor in use, specify the desired
rack options, and define alternate locations for wash and diluent fluids.
7. Check the Auto 502 check box, if appropriate:
If using a Flow Solution IV or IV system, check the Auto 502 checkbox to control
the Precision Pump through the Instrument Control dialog box or the Auto Events
Scheduler (see Chapter 4, Tools Menu on page 27).
If using an Flow Solution 3100 system, select the Auto 502 checkbox to control the
Precision Pump.
The CNSolution FS 3100 uses the Model 3090 Autosampler. Flow Solution 3100
systems use either the Model 3090 or Model 3360 Autosampler. Flow Solution III
and IV systems use any of the samplers, including the RA, Model 3090, and Model
3360. Run upgraded systems without one of the listed autosamplers in the standalone sampler control mode, provided the autosampler being used is capable of independent operation.
NOTE: Configuring WinFLOW every time the software opens is not necessary.
Change WinFLOW configuration settings only if altering the instrument
configuration.
WinFLOW Software Operators Manual: Chapter 3
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Configuration

8. After selecting the checkbox to control the Precision Pump, use the Pump Turns
pulldown menu to select the pump direction (when viewed from the front of the
pump). Left indicates the negative pump direction (the pump pushes the liquids
clockwise), while Right indicates the positive direction (counter-clockwise).
Most Flow Solution IV customers will select Right. Most Flow Solution 3100 customers will select Left.

Configuring the RA Sampler


1. Select the RA sampler in the Configure WinFLOW dialog box.
2. Click Configure Sampler. The RA Configuration dialog box appears as shown in
Figure 3.2.

Figure 3.2. RA Configuration dialog box

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Configuration

Vial Depths

Using a Traveling Wash Reservoir (TWR)


Adjust the depth that the sample probe travels into a sample cup.
1. Click Vial Depths in the RA Configuration dialog box. The Vial Depths dialog box
appears (see Figure 3.3).

Figure 3.3. Vial Depths dialog box

2. Enter the appropriate vial depths (in millimeters) in the corresponding boxes. The
maximum probe depth in the sample vial is approximately 95 mm.
Using a Static Wash Reservoir (No TWR)
Adjust the depth that the sample probe travels into a sample cup.
Due to variations of individual sampler setups, no exact default depths are available,
although starting depths are provided in Table 3.1 on page 11. Instead, the process is
completed by trial and error where the optimal probe positions are determined for each
vial.
Any of the Vial Type numbers can be assigned to any of the vials available (2 mL,
4 mL, 8 mL, and 12 mL). Follow the steps below to configure the vial depths for each
Vial Type.

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Configuration

1. Click Vial Depths in the RA Configuration dialog box. The Vial Depths dialog box
appears (see Figure 3.3).

Figure 3.4. Vial Depths dialog box

2. Enter the appropriate vial depths (in millimeters) in the corresponding boxes. If
using a static wash reservoir (no TWR), the range depends on the setup probe
position in the autosampler arm and the wash reservoir type being used; the range is
generally larger than 95 mm.
To get the maximum probe depth into the vial, set the probe at its uppermost position and adjust the needle so that the tip of the needle barely clears the lip of the
wash reservoir. Lock the needle into position with a set screw.
Needle
Just clear the
reservoir

Wash
Reservoir

Figure 3.5. Probe needle in relation to the wash reservoir


Table 3.1. Vial Depth starting values

Vial Size
(mL)

Rack Size

Approximate
Starting Value (mm)

90-position

65

60-position with shelf

75

90-position

100

12

60-position

100

a. Determine which vial size will be used the most (from 2 mL, 4 mL, 8 mL, and
12 mL). This value normally designates Vial Type 1.
b. Verify Vial Type 1 is set as the Default Vial Type in the Method Editor (see
Chapter 5, Flow Control Settings Screen on page 38).
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Configuration

c. Open the WinFLOW software and create a Sample Table with a cup position
adjacent to the position that contains a vial of Vial Type 1.
d. Send the sampler to the position chosen in step 1 by starting a run. Check the
depth of the probe tip to determine whether to raise, lower, or leave the tip.
NOTE: For 8-mL and 12-mL tubes: If the probe goes over the vial, but doesn't go
down, the depth is set deeper than the sampler can go. Decrease the depth
until the probe will lower. This value is the maximum depth for any vial; the
maximum possible depth is 100mm.
e. If the depth needs adjustment, close WinFLOW and open Configure Winflow.
Make the appropriate depth changes and click OK.
f.

Open Winflow and repeat steps d through e until the optimal depth is reached.

g. Repeat steps a through f for each Vial Type.


NOTE: If only using one vial type, only set the depth for the default Vial Type.
NOTE: Vial types other than the default must be designated with their type number in
the Vial column of the Sample Table for each non-default vial position.

Dilutor Setup

If using the Autodilutor with the RA Sampler, click Dilutor Setup in the RA
Configuration dialog box. The Dilutor Setup dialog box appears (see Figure 3.6).

Figure 3.6. Dilutor Setup dialog box

By selecting Use Dilutor, Syringe Size and Syringe Speed settings become available
for input.
Use the pull-down menu to select the syringe size. The default syringe size is 2,500 L.
The available syringe sizes include the following: 1,000 L, 2,500 L, 5,000 L, and
10,000 L.

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Configuration

Syringe size and the application determine proper syringe speed. The speed ranges from
25 for larger syringes to 50 for smaller syringes. The default speed values for each
syringe size are shown in Table 3.2.
Table 3.2. Recommended Values for Syringe Sizes

Syringe Size
(L)

Recommended
Speed

Recommended Cup
Size

1,000

50

2-mL

90-position

2,500

35

4-mL

60-position with shelf

5,000

25

8-mL

90-position

10,000

22

12-mL

60-position

Wash and Diluent

Rack Size for


Recommended Cup

OI Analytical offers two RA Sampler probe arm configurations. Specify which type to
use by clicking Wash and Diluent in the RA Configuration dialog box. The Wash and
Diluent dialog box appears (Figure 3.7).

Figure 3.7. Wash and Diluent dialog box

1. Choose a Wash Source:

TWR (traveling wash reservoir)

Reservoir (fixed reservoir)

Cup Number (any specified cup location)

Most applications recommend using the TWR as the wash source. This configuration allows a two-stage rinsing process.
Use the fixed reservoir as the recommended alternative to the TWR. Using a specified cup or vial location as the wash source is possible, but not recommended due to
volume limitations.

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Configuration

2. Choose a Diluent Source:

Reservoir

Cup Number

3. Click OK to close the Wash and Diluent dialog box.

Rack Placement

Setup the racks being used with the RA Sampler by clicking Rack Placement in the
RA Configuration dialog box. The Rack Placement dialog box appears (Figure 3.8).

Figure 3.8. Rack Placement dialog box

The RA Samplers default configuration uses three sample racks and one standards
rack. Use up to six sample racks:

The preprogrammed sample rack sizes are 21, 24, 40, 60, 90, Incubtr2, and
Incubtr3.

The default sample rack size is 90.

The available standard rack sizes are 10 and 20.

The default standards rack size is 20.

Click OK to close the Rack Placement dialog box.

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Configuration

Rack Editor

The Rack Editor configures the RA Sampler to use virtually any size or type of rack.
Program the rack size and type by clicking Custom Rack Editor from the RA
Configuration dialog box. The Rack Editor dialog box appears (Figure 3.9).

Figure 3.9. Rack Editor dialog box

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Configuration

To use racks other than those provided with the RA Sampler, measure the rack and vial
slot dimensions and the distance between each vial slot. Enter these measurements into
the corresponding locations in the Rack Editor. When saved, custom racks display as an
option in the Rack Placement screen. Create both sample and standard racks using the
following steps.
1. Click Add New Type. Type the custom rack name and click OK.
2. Select Add Cups. The Add Cups dialog box appears (see Figure 3.10).

Figure 3.10. Add Cups dialog box

3.

Enter the following information in the corresponding fields:

First Cup #:

Number between 1 and 99

Cup Wid (mm):

Cup width in millimeters

Number of Cups:

Number of rows (left to right) and number of


columns (back to front)

First Cup Position (mm):

Distance in millimeters from the standard


trays upper left corner (closest to the sampler
body) to the middle of the first cup

Inter-Cup Spacing (mm):

Distance from the cup-to-cup center in


millimeters

4. Click OK. Click Close to exit the Rack Editor dialog box.

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Configuration

5. Click Rack Placement in the RA Sampler Configuration dialog box to access the
Rack Placement dialog box (Figure 3.7).

Figure 3.11. Rack Placement dialog box

4. Select the custom rack name just created for the appropriate rack placement. After
selecting a custom rack, the Align Rack dialog box appears as shown in Figure
3.12 (if the dialog box does not appear, click the Align button beside the custom
rack).

Figure 3.12. Align Rack dialog box

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Configuration

6. Click OK to accept the default settings or enter new values to adjust the offset. The
RA Sampler rack is now ready and displays the custom rack as shown in Figure
3.13 (if the custom rack screen does not appear, click OK to close the Rack
Placement dialog box and the Custom Rack Editor button).

Figure 3.13. Rack Editor dialog box displays a custom RA Sampler rack ready for use

Configuring the 3360 Sampler


1. Select 3360 in the Configure WinFLOW dialog box.
2. Click Configure Sampler. The 3090/3360 Configuration dialog box appears
(Figure 3.14).

Figure 3.14. 3090/3360 Configuration dialog box

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Configuration

Vial Depths

Adjust the depth that the sample probe travels into a sample cup.
1. Click Vial Depths. The Vial Depths dialog box appears (Figure 3.15).

Figure 3.15. Vial Depths dialog box

Enter the desired vial depths (in millimeters) in the corresponding boxes. The depths
correspond to the depth of the needle when used with the following cups:
Table 3.3. Vial Depths

Cup Type

Default Depth
(mm)

Cup Dimensions
(mm)

Cup Capacity
(mL)

150

13 x 100

93

12 x 25

113

12 x 30

150

16 x 100

12

Other settings may be used if other types of cups are used in the sampler. This
information is utilized in the sample table, to allow the operator to include multiple cup
types in a single run.

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Configuration

Dilutor Setup

If using the Autodilutor with the 3360 Sampler, click Dilutor Setup in the 3090/3360
Configuration dialog box. The Dilutor Setup dialog box appears (Figure 3.16).

Figure 3.16. Dilutor Setup dialog box

By selecting Use Dilutor, Syringe Size and Syringe Speed settings become available
for input.
Use the pull-down menu to select the syringe size. The default syringe size is 2,500 L.
Syringe size and the application determine proper syringe speed. Table 3.4 shows the
recommended speeds for each syringe size, as well as the cup size that is typically
utilized for each syringe size.
Table 3.4. Recommended Values for Syringe Sizes

Syringe Size
(L)

Recommended
Speed

2,500

23

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Recommended Cup
Size and Type
4-mL type 3
8-mL type 1
12 mL type 4

Rack Size for


Recommended Cup
60-position with shelf or
90-position

20

Configuration

Wash and Diluent

To provide an alternate source of wash or diluent solution, click the Wash and Diluent
button. The Wash and Diluent dialog box appears (Figure 3.17).

Figure 3.17. Wash and Diluent dialog box

1. Choose Reservoir to draw wash/diluent from the rinse station.


2. Click Cup Number and supply a cup number and cup type if an alternate solution
is needed.
Using a specified cup or vial location as the wash source is possible, but not recommended due to volume limitations.

Rack Placement

Setup the racks being used with the 3360 Sampler by clicking Rack Placement in the
3090/3360 Configuration dialog box. The Rack Placement dialog box appears (Figure
3.18).

Figure 3.18. Rack Placement dialog box

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Configuration

The 3360 Sampler uses four sample racks and one standards rack.

Peck Probe during


Rinse

The preprogrammed sample rack sizes are 60 and 90.


The default sample rack size is 90.
The available standard rack sizes are 10 and 12.
The default standards rack size is 10.

Check this checkbox to rinse the sampler probe by pecking. Pecking is where the probe
is plunged into and out of the rinse position three times between samples. This rinse
method is typically used with SFA.
Leave this box unchecked in order to rinse the probe by simply lowering it into the rinse
position. This rinse method is typically used with FIA.

Configuring the 3090 Sampler


1. Select 3090 in the Configure WinFLOW dialog box.
2. Click Configure Sampler. The 3090/3360 Configuration dialog box appears
(Figure 3.19).

Figure 3.19. 3090/3360 Configuration dialog box

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Configuration

Vial Depths

Adjust the depth that the sample probe travels into a sample cup.
1. Click Vial Depths in the 3090/3360 Configuration dialog box. The Vial Depths
dialog box appears (Figure 3.20).

Figure 3.20. Vial Depths dialog box

2. Enter the appropriate vial depths (in millimeters) in the corresponding boxes. The
vial depths correspond to the depth of the needle when used with the following
cups:
Table 3.5. Vial Depths

Cup Type

Default Depth
(mm)

Cup Dimensions
(mm)

Cup Capacity
(mL)

150

13 x 100

93

12 x 25

113

12 x 30

150

16 x 100

12

Other settings may be used if other types of cups are used in the sampler. This
information is utilized in the sample table to allow the operator to include multiple cup
types in a single run.
3. Click OK to close the Vial Depths dialog box.

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Configuration

Wash and Diluent

To provide an alternate source of wash or diluent solution, click the Wash and Diluent
button. The Wash and Diluent dialog box appears (Figure 3.21).

Figure 3.21. Wash and Diluent dialog box

1. Select a Wash Source:


a. Choose Reservoir to draw wash from the rinse station.
b. Click Cup Number and supply a cup number and cup type if an alternate
solution is needed.
Using a specified cup or vial location as the wash source is possible, but not
recommended due to volume limitations.
2. Choose a Diluent Source.
a. Choose Reservoir to draw diluent from the rinse station.
b. Click Cup Number and supply a cup number and cup type if an alternate
solution is needed.

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Configuration

Rack Placement

Setup the racks being used with the 3090 Sampler by clicking Rack Placement in the
3090/3360 Configuration dialog box. The Rack Placement dialog box appears (Figure
3.22).

Figure 3.22. Rack Placement dialog box

The 3090 uses a single sample rack and one standards rack.

Peck Probe during


Rinse

The supported sample rack sizes are 60 and 90.


The default sample rack size is 90.
The only supported standard rack sizes is a 10-position rack.

Check this checkbox to rinse the sampler probe by pecking. Pecking is where the probe
is plunged into and out of the rinse position three times between samples. This rinse
method is typically used with SFA.
Leave this box unchecked in order to rinse the probe by simply lowering it into the rinse
position. This rinse method is typically used with FIA.

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Chapter 4 Introduction to
WinFLOW
Starting WinFLOW
1. Double-click the WinFLOW icon or select WinFLOW from the Start menu.
2. Enter the serial number included in the WinFLOW documentation.
NOTE: WinFLOW only requests the serial number the first time the software starts.
3. If password protection is enabled for program startup, enter the user name and
password, and click OK. For more information on password protection see
System Security in this chapter.
NOTE: All instrument modules must be properly powered on and initialized for
online operation.

Select View Dialog


Box

WinFLOW displays the Select View dialog box on startup (Figure 4.1).

Figure 4.1. Select View dialog box

The Select View dialog box allows easy, single-click access to WinFLOWs four
primary options. It also provides an icon to exit WinFLOW. Table 4.1 outlines
WinFLOWs four main options.

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When the Select View dialog box appears, the main menu bar displays File, Tools, and
Window menus, which can also be accessed from any WinFLOW screen. The File
menu also provides an Exit option.
Table 4.1. WinFLOW main options

Main Option

Select View
Icon

Shortcut
Key

Small Icon

Function

Collect Data

F2

Initiates data collection following


sample table and method selection.

Sample Table

F3

Opens a table displaying sample


cup number, name, type, replicate,
dilution, and weight factors.

Method Editor

F4

Sets data collection parameters and


calibrant and QC information.

Data Analysis

F5

Accesses results from any


previously saved run. Contains
peak plot, peak table, calibration
plot, and calibration data tables.

Exit

F6

N/A

Exits WinFLOW.

Tools Menu
The Tools menu provides access to screens that establish WinFLOW preferences,
configure instruments, and set pump speeds, valve states, and heater temperatures.
Figure 4.2. Tools Menu

Preferences accesses the Preferences dialog box.


Configuration accesses the Configuration dialog box.
Auto Event Scheduler accesses the Event Scheduler dialog box.
Instrument Control accesses the Instrument Control dialog box.
Pump Timer displays the number of hours the pumps are used.

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Introduction to WinFLOW

Preferences

Set global WinFLOW preferences such as default views and languages using the
Preferences dialog box (Figure 4.3).

Figure 4.3. Preferences dialog box

Security

Sets WinFLOW to request a password on startup. For more


information see System Security on page 33 in this
chapter.

Save Views

Sets WinFLOW to display any screen on startup that


remained open when WinFLOW closed.

NOTE: Save Views does not bring up results and analysis files left open when
exiting.

Configuration

Verify Close

Sets WinFLOW to automatically prompt to verify the


operators intention to exit the program.

Re-enable Helpers

Implements various warning screens that can be disabled


as operators gain experience with WinFLOW.

Language

Select from English, French, German, or Spanish. Contact


your local OI Analytical distributor for more information
about other available languages.

The Configuration dialog box (Figure 4.4) provides information about the instrument
platform, such as the autosampler installed with the system, the firmware version, and
the number of communicating detectors (channels), valves, and pumps.
The Configuration dialog box allows the operator to determine if the analyzer, as well
as each installed component, communicates with the computer. Selecting Configure
when the analyzer or a component loses communication to re-establish a link between it
and the computer.

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Figure 4.4. Configuration dialog box

Events Scheduler

The Events Scheduler dialog box (Figure 4.5) sets what action(s) the pump(s) take(s)
when any of the specified events occur, such as the end of an analysis.

Figure 4.5. Events Scheduler dialog box

Add

Selects the event, time, and action.

Edit

Edits any previously chosen event.

Remove

Removes any previously chosen event.

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Instrument Control

Manually set pump speeds, valve states, and heater temperatures from the Instrument
Control dialog box (Figure 4.6).
NOTE: The heater temperature settings do not control the Power Base cartridge
heaters.

Figure 4.6. Instrument Control dialog box

Pump Timer

The Pump Timer dialog box (Figure 4.6) indicates the number of hours the pump(s)
run. Use this feature to determine when consumables, such as pump tubes and
membranes, need replacing. Reset the pump timer at any time.

Figure 4.7. Pump Timer dialog box

Window Menu
The Window menu contains options for displaying open windows within WinFLOW.
The Window menu lists all open windows. Access any open window from the Window
menu by selecting the name or entering the number associated with the window.
Figure 4.8. Window menu

Cascade overlaps open windows.


Tile places open windows side by side.
Arrange Icons places minimized WinFLOW screens along the bottom the Select View
dialog box.

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Introduction to WinFLOW

About Menu
The About menu contains information about software and firmware versions, as well as
provides technical support access numbers.

Shortcut Keys
WinFLOW contains several keyboard shortcuts. These function keys provide an
additional method for locating and enabling various software activities. Table 4.2
describes the available function keys.
These function keys duplicate the Select View icons, which are also available from the
icon ribbon or the pulldown menu. Therefore, WinFLOW provides multiple avenues for
accessing the most frequently used software features.
Table 4.2. Shortcut keys

Function Key

Description

F2

Opens the Data Collection dialog box.

F3

Opens the Sample Table dialog box.

F4

Opens the Method Editor dialog box.

F5

Opens the Data Analysis dialog box.

F12

Exits WinFLOW.

Icon Ribbon
The following list details the various icons and their purposes.
Opens the Data Collection screen.
Opens the Sample Table screen.
Opens the Method Editor screen.
Opens the Data Analysis screen.
Initiates data display.

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Resets to the baseline views beginning, which deletes all data collected.
Fast forward icon, which initiates data collection.
Pauses data collection.
Stops data collection.
Zeros the baseline signal on the peak plot.
Removes or restores the grid lines in the peak plot and calibration plot.
Peak plot update lock freezes the baseline update used during data
collection.
Activates the peak editor cross.
Deletes or reprocesses peaks.
Recalculates results.

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System Security
System security reduces unauthorized WinFLOW software access or use. It provides
simple, password-protected access to WinFLOW and some of its features. Accessing
the Security screen always requires a password.
If the system password is lost, contact OI Analytical Customer Support at
(800) 336-1911 or (979) 690-1711.
1. Select Preferences from the Tools menu to access the Preferences dialog box
(Figure 4.3). Select the Security checkbox. The password dialog box appears
(Figure 4.9).

Figure 4.9. Password dialog box.

2. Enter the user name and password. Click OK to return to the Preferences dialog
box.
NOTE: Use the default user name and password when first activating the Security
option. The default user name is system and the default password is
manager. Neither entry is case-sensitive.

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Introduction to WinFLOW

3. Click Set Privileges to edit, delete, or add a new user name and password. The
Security dialog box appears (Figure 4.10).

Figure 4.10. Security dialog box

4. Select Edit, Delete, or Add, and follow the instructions presented to edit, delete, or
add a user name and password.

WinFLOW Quick Start


NOTE: The following instructions assume all modules and hydraulic connections are
installed.
1. Turn on all Flow Solution modules and the computer.
2. Start the WinFLOW software.
3. Verify all tubing connections are made. Initiate pump(s) rotation by pressing the
pumps Run button.
4. Click the Method Editor icon. Verify the method is configured for the analysis to
be performed. Save any changes to the appropriate file.
5. Click the Sample Table icon. Alter an existing table or create a new sample table.
Save any changes to the appropriate file.
6. Click the Data Collect icon. Select a method and sample table.
7. Enter an operator name, operator ID, and filename for the run results.
8. Click the Play icon and monitor the baseline. Once the baseline stabilizes with
startup solution, switch to reagents and again monitor the baseline until it stabilizes
(typically 1530 minutes).

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9. While the baseline stabilizes, load the autosampler trays according to the sample
table.
10. Click the Fast Forward icon when the baseline stabilizes.
11. Monitor the run until the SYNC peak elutes and is successfully marked. Allow the
run to continue.
If the operator completes the run or the run completes automatically, the data saves
automatically to the result file defined in step 7.
NOTE: Select the Stop icon to stop the run. Save results once the completed run
displays.
12. Review the results.

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Chapter 5 Method Editor


The WinFLOW Method Editor controls how WinFLOW collects and interprets data.

General Description
Open the Method Editor using one of the following ways:

Click the Method Editor icon from the Select View dialog box,

Click the Method Editor icon on the main icon ribbon, or

Press [F4].

Depending on the installed hardware, the Method Editor includes screens that modify
all method parameters necessary for running an analysis. Use the following six screens
with flow analysis hardware:

Flow Control Settings

Detector/Channel Settings

Signal Filter and Marking Settings

Calibration/Quantitation Settings

Timed Events Editor

Calibrants Table

This chapter discusses each of these screens and their associated menus. After setting
parameters properly, these screens do not require modifying during future analyses for
specific analytes.
Locate each screens title at the top of the window. The window bar also contains the
open methods name. Access each screen using one of the following ways:

Click the screens icon in the Method Editor icon ribbon,

Click the Method Editor icon ribbons advance or reverse arrow until the desired
screen appears, or

Go to the Method Editors Page menu, which lists each of the screens separately
along with their associated quick key functions.

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Method Editor

Method Editor Icon


Ribbon
Advances to the next screen.

Accesses the Flow Control Settings screen.

Accesses the Detector/Channel Settings screen.

Accesses the Signal Filter/Marking Settings screen.

Accesses the Calibration/Quantitation Settings screen.

Accesses the Timed Events Editor screen.

Accesses the Calibrants Table screen.

Returns to the previous screen.

Opening a Method

A method automatically opens when accessing the Method Editor. Open a previously
saved method or an installed method using the following steps:
1. Go to the File menu and select Open.
2. Select the method to open, then click OK.
NOTE: If the methods platform is not the same as the current platform, a dialog box
appears warning that other method options need updating to match the
platform selected. If selecting Yes, WinFLOW adapts some method
parameters to allow WinFLOW to work on the current platform.

CAUTION:
Always use Save As when
altering an existing
method so the original
does not become
overwritten.

3. After the method loads, modify it if necessary. See Creating a Method on page 38
in this chapter.

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Method Editor

Creating a Method

The fastest way to create a method consists of altering an existing method and then
using Save As to save the new method under a new filename. WinFLOW installs with
the following six preset methods: single and dual methods for the Flow Solution 3000
(FS 3000) and the Flow Solution IV (FS IV), and a three-channel method for the FS IV.
Use these methods as templates for creating new methods. Most parameters in the
preset methods do not need changing when creating a new method for a given
chemistry.

Saving a Method

When altering a method and the changes have not been previously saved, the Save As
dialog box automatically appears when another method opens.
NOTE: Saving a modified method as its original name overwrites the original settings
in that method. Save As modifies a method under a different name to maintain
the original settings.

Flow Control Settings Screen


Select an instrument, activate channels, enable the baseline verification function, set the
sampling mode, set the default vial type (when using the Model 3090, Model 3360, or
RA Sampler), and define pump speeds from the Flow Control Settings screen
(Figure 5.1). Access the Flow Control Settings screen by clicking its icon from the
Method Editor icon ribbon, by going to the Page menu and selecting Flow Control, or
by pressing [Shift]+[F1].

Figure 5.1. Flow Control Settings screen

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Method Editor

Instrument

Specify one of three instrument platform groups:

FS III/IV/3100

FS 3000

Microbes-Coli

If the platform changes, a warning message displays stating that parameters need
updating to reflect the new platform.
NOTE: Changing the instrument selected does not automatically change the hardware
configuration. Although methods for any platform can be created at any time,
a method cannot be used unless WinFLOW is configured to function with the
current hardware (see Chapter 3, Configuration).

Sampling Mode

Set Sampling Mode to one of two options:


Uninterrupted

Allows operation with an integrated autosampler. All samples in


a sample table analyze in a single, uninterrupted run.

Single Sample

Allows flow injection analysis (FIA) operation with or without


an autosampler, or continuous flow analysis operation with an
autosampler. Each sample loads and injects when the operator
chooses.

Interval

Currently unavailable.

Use Single Sample mode by performing the following steps:


1. Select Single Sample as the Sampling Mode in the Flow Control Settings screen.
2. Proceed with data collection as described in Chapter 7, Data Collection on
page 69.
At the point of data collection, the Single Sample Mode dialog box appears
(Figure 5.2).

Figure 5.2. Single Sample Mode dialog box

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Method Editor

3. For FIA operation without an autosampler, manually place the sample needle into
the sample or standard solution and click Sample. The sample or standard aspirates
into the sample loop for the time specified in the timed events table (Figure 5.8)
(see Timed Events Editor Screen on page 52 in this chapter). When the loop
valve rotates to the inject position, place the sample needle into the wash source.
For FIA or segmented flow analysis (SFA)-continuous flow operation with an
autosampler, click Sample when the next sample standard is ready. The
autosampler automatically places the sample needle into the sample or standard vial
and extracts the sample or standard for the time specified in the timed events table
(Figure 5.8). The sample needle then returns to the wash source.
Figure 5.2 displays after each samples cycle time completes until all the samples in
the sample table are processed.

The operator can also use a blank table each time a sample or standard aspirates.
1. Select Generate Blank Table in the Run Setup dialog box, which appears when
data collection initiates (Figure 5.3).

Figure 5.3. Selecting the single sample blank table option

2. When the Single Sample Mode dialog box appears (Figure 5.2), click Edit. A blank
table appears.
3. Fill in the next sample or standard and close the window. WinFLOW prompts to
save the table. Saving the table automatically begins the analysis.

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Method Editor

CCV/Drift Fail

Automatic recalibration options require deciding on a system action following a failed


continuing calibration verification (CCV). For more information on CCVs, see
Continuing Calibration Verification on page 56 in this chapter.
Flag Only

Places an F in the results tables flag column.

Pause Run

Flags the calibrant and aborts the analysis.

Recalibrate

Flags the calibrant and reruns the calibration section. Sampling


resumes at the cup after the last successful CCV.

Vial Types

Set Vial Types when using the Model 3090, Model 3360, or RA Samplers. WinFLOW
can use four operator-defined vial types within each analysis. Define each vial types
depth in the WinFLOW Configuration dialog box (see Chapter 3, Configuration on
page 7). Set the default vial type to represent the majority of the operator-defined vial
types used.

Off-scale (HI)
Samples

Set autodilution options when using the Model 3360 or RA Samplers with the
Autodilutor. Enable autodilution by selecting Enable Autodilution. Once autodilution
enables, the following options become available:
Dilution Factors

The Model 511 Autodilutor contains hardware-fixed


dilution factors.
The Autodilutor allows selecting a continuously variable
set of dilution factors. Enter up to five dilution factors,
each separated by commas. The Autodilutor uses the first
entered dilution factor for any sample that goes over the
highest calibration standard concentration. The autodilutor
uses subsequent operator-defined dilution factors if the
diluted sample concentration is still too high. Although the
autodilutor has a 1:24,000-step resolution, dilution factors
greater than 200 should not be used.

CCV Frequency

Chooses the frequency of running CCVs with the diluted


samples (e.g., run a CCV every 10 samples). Designate the
CCV in the sample table after the dilution cups (see
Figure 6.1 on page 58 and Table 6.2 on page 60).

Number of
Followers

Selects the number of followers to be run. A follower is the


sample(s) after an over-limit (HI) sample. The
recommended setting is two followers.

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Method Editor

Insert Baselines

Insert wash baseline (WBL) points at regular intervals. A WBL point forces the
baseline through that point. When using the RA, Model 3090, and Model 3360
samplers in a segmented system, the WBL sample is taken from the wash reservoir
instead of a sample cup. For a FIA system, the sample probe stays in the wash, but the
valve does not inject, and carrier solution determines the baseline. Enable baseline
verification by selecting Enable under Insert Baselines, then set the desired First
position, Interval, and Duration.
When enabled, the baseline verification operates on all the activated channels. Baseline
verification points, which are designated WBL, do not appear in the sample table, but
they do appear in the sequence table preview.

Pump Control

Start Position

Provides the sample table location where the first baseline


verification point occurs. Check the sequence table preview in the
Data Collection screen to verify correct placement.

Interval

Sets the number of samples between baseline verifications (250).

Duration

Sets the number of baseline verifications to run consecutively (1


5).

Control pump speed when operating the Precision Pump with the FS 3100, FS 3000,
and CNSolution analyzers. Set these values in 1% increments.
Run Speed

Sets the desired pump speed during normal operation.

Slow Speed

Sets the desired pump speed used when the Pump Slow command
activates either manually or automatically. For manual operation,
see Chapter 4, Instrument Control on page 30. For automatic
operation, see Chapter 4, Events Scheduler on page 29.

Automated Precision Pump Control Options


Refer to the method for the operating speed of the pump for the individual application.
Operate the Precision Pump at 40% speed in a counterclockwise direction
(40 setting) for most applications. Typically use a 10% slow speed (10 setting).
Automated FS 3000 and CNSolution 3000 Pump Control Options
The FS 3000 and CNSolution 3000 pump typically operates at 100% full speed in a
clockwise direction with the pump speed switch in the low position. A common slow
speed setting is 50%, which means the pump turns at full speed 50% of the time and
turns off 50% of the time. For a 30-second cycle time and a 50% slow speed setting, the
pump operates for 15 seconds and then stops for 15 seconds.

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Method Editor

Detector/Channel Settings Screen


The Detector/Channel Settings screen (Figure 5.4) sets parameters for each detector
channel individually. Update information for a particular channel by selecting the
channels line in the Channels list box. The information on the screen pertains only to
the highlighted channel. Only available channels appear in the Detector/Channel
Settings screen. Access the Detector/Channel Settings screen by clicking its icon from
the Method Editor icon ribbon, by going to the Page menu and selecting Detector/
Channel, or by pressing [Shift]+[F2].

Figure 5.4. Detector/Channel Settings screen

Channels

The Channels listbox displays all the available channels. The number of available
channels depends on the number of installed detectors. A channel presents as available
following successful communication with a detector.
Activate a channel by double-clicking the channel name. A number sign (#) sign
appears to the left of the activated channel name (Figure 5.4). Deactivate a channel by
double-clicking the channel name again. Method parameters only apply to active
channels. Therefore, channels must be activated before moving to other Method Editor
screens.
NOTE: If opening a method that designates an unavailable channel, an X appears
on the channel names left. Re-establish contact with the channel by going to
the Main menu and selecting Setup and Configure. If unsuccessful, the
systems exits and restarts WinFLOW.

Name

Designate a name to describe the chemistry being run. WinFLOW uses the channel
designation (e.g., Channel 1) as the default name.

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Method Editor

Methodology

Designate a methodology that describe the specific chemistry being run.

CAS Number

Enter the Chemical Abstract Service (CAS) number for the standard used in the
selected channel, if applicable.

Detector Settings
Mode

Sets the detector mode as Photometric, Amperometric, ISE


(ion-selective electrode), Fluorometric, or Matrix (seawater
matrix). Select Photometric for the Expanded Range (ER)
detector. Select Amperometric for the Amperometric detector
and for the analog-to-digital (A/D) converter. Use ISE for all ionselective probes such as pH or fluoride. Use Fluorometric with
the fluorometric plug-in detector.

Acquisition Rate

Determines the data collection rate in Hz (or points per second).


Options include 1, 2, 3, 5, or 10 Hz. The 1-Hz default value
usually suffices. When running very low analyte levels,
increasing the acquisition rate can result in a sensitivity increase.
When operating multiple channels, set the acquisition rate to 1
Hz so the computer does not overload with data.

Cell Potential

Set the cell potential in amperometric mode using the detectors


10-turn precision potentiometer. Setting cell potential via
software is a future option.

A-D Gain

Sets the analog-to-digital gain for the sample and reference.


Options include 1, 2, 4, 8, 16, 32, 64, 128, or Auto. Set Sample to
Auto for all photometric detectors. The photometric detector
automatically sets the optimum gain based on the amount of light
reaching the photodiode. Set the amperometric detector to a fixed
gain of 1.
Set Reference to Auto for all photometric detectors. The
photometric detector automatically sets the optimum gain based
on the amount of light reaching the photodiode. The
amperometric detector does not have a reference gain.

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Method Editor

Channel
Subtractions

Subtract peak concentration, peak height, or area in one channel from peak
concentration, peak height, or area in another channel. For example, nitrate-plus-nitrite
analysis typically occurs on one channel and nitrite-only analysis on another. Use the
Channel Subtractions function for automatically calculating nitrate concentration by
subtracting nitrite concentration from nitrate-plus-nitrite concentration. Enable Channel
Subtractions on only one of the two channels because peak concentrations in one
channel subtract from peak concentrations in another channel. For example, channel 1
peak concentrations (nitrite) subtract from channel 2 concentrations (nitrate-plusnitrite). Therefore, enable Channel Subtractions on channel 1 and not channel 2.
Subtracted data (nitrate) appears with other data in the peak results table.
NOTE: When using Channel Subtractions, OI Analytical recommends using
concentrations rather than peak height or area.
Subtracted From
Channel

Selects the channel from which the current channel subtracts.


In the nitrate-plus-nitrite example, the Subtract From Channel
is the nitrate-plus-nitrite channel (channel 2).

Subtraction Name

Designates the subtracted datas name. For example, if nitrite


peak concentrations subtract from nitrate-plus-nitrite peak
concentrations, name the subtracted data Nitrate.

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Method Editor

Signal Filter and Marking Settings Screen


Set smoothing, baseline marking, and peak marking options for each channel
individually from the Signal Filter and Marking Settings screen (Figure 5.5).
Access the Signal Filter and Marking Settings screen by clicking its icon from the
Method Editor icon ribbon, by going to the Page menu and selecting Signal Filter/
Peak Marking, or by pressing [Shift]+[F3].

Figure 5.5. Signal Filter and Marking Settings screen

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Method Editor

Smoothing

Select one of three software-based signal processing algorithms to reduce noise,


improve precision, and ease integrating difficult peaks (small size relative to noise).
Choose None, Moving Average, Olympic, or Savitzky-Golay. Select one of these
algorithms in advance. If selecting None, access these algorithms after the run
completes and apply them in the results file.
Moving Average

Selects a simple algorithm for filtering where the average of an


input set is used to generate one output value. This algorithm
tends to reduce peak height maxima due to the lower values on
either side of the peak. Peak area measurements remain largely
unaffected. Use a maximum of nine data points and one
iteration for best results with this algorithm.

Olympic

Selects a variation of the moving average algorithm. It


eliminates high and low values and averages the remaining
values. This algorithm very effectively screens out spikes (high
frequency noise). Like moving average, the olympic algorithm
tends to reduce peak height. Peak area measurements remain
largely unaffected. Use seven data points (11 maximum) and
one iteration for best results with this algorithm when acquiring
data at 1 Hz.

Savitzky-Golay

Selects an algorithm that multiplies each point by a weighting


factor and then averages the points in a data set. The factors,
derived from second- and third-degree polynomials, weight the
center of the data point set and progressively lessen the
weighting to the points further out. Unlike the other algorithms,
this setting minimizes peak height maxima distortions. Peak
area measurements also remain unaffected. Use several data
points and multiple iterations for best results with this
algorithm when acquiring data at 1 Hz.

Points

Defines the number of input data points processed to generate


each output data point. Options include 3, 5, 7, 9, 11, 13, and
15. The data acquisition rate is a very important parameter in
determining the optimum number of points for a given peak
width. The default setting uses five data points, which is
adequate for most applications. Use a higher value when
processing extremely wide peaks.

Iterations

Sets the repetition number that the algorithm treats the output
of one operation (filtering algorithm) as the input for the next
operation. It increases the degree of filtering (smoothing) while
keeping the filter width (points) optimized for the peak width.

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Method Editor

Baseline Marking

Inverted
Chemistry

Baseline Marking consists of the following three parameters:


Lead Time

Sets the time in seconds before the SYNC peak, which is used
as the initial baseline point. WinFLOW determines the
baseline lead after marking the SYNC peak by counting
backward from the SYNC peak marker. Be sure to set the
baseline lead time longer than half the SYNC peaks width so
WinFLOW does not mark the baseline on the rising slope of
the SYNC peak itself. As a general rule, set the baseline lead
time to 15 seconds more than the peak width. The default
setting is 60 seconds.

Lag Time

Sets the time in seconds of the last peak used for final baseline
determination after elution. This parameter does not require
modifying. The default setting is 120 seconds.

Mark BL Samples
as Peaks

Allows baseline samples to be marked as peaks so high


background blanks can be used as the baseline value.

Select Inverted Chemistry when the chemistry being run measures a decrease in
response instead of an increase. Select this option only if the analytical method for the
chemistry used states that it is an inverse chemistry.
NOTE: This feature can only be used with certain detector types.

Peak Marking
Sync Ignore Time

Sets the time in seconds that no peaks are marked whether or


not they satisfy the peak recognition parameters. This ensures
WinFLOW does not mistakenly recognize a spurious peak or
noise spike in the baseline before the SYNC peak appears. For
this reason, set the Ignore Time in seconds for less time than
the SYNC peak takes to reach the detector (see Chapter 6,
Synchronization Peak (SYNC) on page 63). Set it to
approximately 30 seconds less than the samples actual dwell
time (residence time) from autosampler to detector. The
default value is 30 seconds.

Peak Measurement

Sets the peak measurement mode. Choose Peak Height or


Peak Area. Peak height is the most commonly used method
for quantitating flow analyses.

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Method Editor

Peak Recognition

Allows the operator to control how WinFLOW finds peaks.


Set the Rise and Fall using a requirement of x seconds with a
vertical difference of y response in micro-absorbance units
(AU) or picoAmperes (pA).
The peak recognition parameters find peaks based on shape.
WinFLOW attempts to find all peaks except baseline types
using these peak finding parameters. Once WinFLOW marks
the SYNC peak, it forecasts the data trace location where it
looks for the next peak using the cycle duration time (see
Timed Events Editor Screen on page 52 in this chapter).
WinFLOW locates the actual peak in the forecasted region
using the peak marking parameters. If no peak meeting the
peak marking parameters is found, WinFLOW marks the peak
using less stringent parameters. WinFLOW marks baseline
and blank type peaks using only the cycle duration time.
When running a noisy, high range chemistry, optimize peak
recognition by increasing the number of points used in the rise
and fall. When running low level chemistries, optimize peak
recognition by decreasing the number of points used in the rise
and fall and decreasing the slope values. Table 5.1 shows the
default values, which are usually appropriate for the majority
of analysis conditions.

Table 5.1. Recommended peak recognition parameters

Low
Range
Settings

Default
Settings

High
Range
Settings

Rise threshold (seconds)

Rise slope (val/point)

50

200

500

Fall threshold (seconds)

Fall slope (val/point)

50

200

500

Parameter

Peak Window

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Defines the peak area integration times in seconds specified


by the Start and End times. Proper peak quantitation depends
on the accurate window designation within the overall peak
zone. The default values are 30.0 and 30.0, resulting in a 60second wide window. When setting start and end markers, be
aware that 0.00 is the peak middle. Therefore, set the start
marker to be a negative number and the end marker to be a
positive number.

49

Method Editor

Calibration/Quantitation Settings Screen


Set calibration and quantitation options (Figure 5.7) individually for each data
collection channel.
Access the Calibration/Quantitation Settings screen by clicking its icon from the
Method Editor icon ribbon, by going to the Page menu and selecting Calibration and
Quantitation Settings, or by pressing [Shift]+[F4].

Figure 5.6. Calibration/Quantitation Settings screen

NOTE: Set calibration and quantitation settings for each channel individually. View
each channels settings by selecting the channel in the Channel listbox.

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Method Editor

Calibration
Fitting Method

Sets the calibration curve fit to First Order (linear), Second


Order, Third Order, or Weighted Linear. The default setting is
first order. Use second- and third-order curve fits when operating
over an expanded concentration range. The weighted linear fitting
method applies an additional statistical analysis to calibration
data, enhancing low level results when operating over an
expanded range with a linear chemistry. This technique gives
greater statistical weight to low concentration measurements
compared to its linear model. The analytical method for each
chemistry cartridge typically designates the calibration curve
fitting technique.

Logarithmic

Select this setting if the calibration concentrations are in a


logarithmic progression. This option is rarely used.

Include Origin

Sets the origin as an additional point when WinFLOW performs


the curve fit regression. This does not force the regression to zero,
but includes the point (0,0) in the calculations. For best results,
analyze a blank sample as the zero concentration calibrant rather
than including the origin.

Exclude Outliers

Automatically removes replicate data points that are outliers and


does not use them in the curve fit. The final report identifies the
excluded outliers.

NOTE: If using weighted linear fitting for three repetitions, WinFLOW removes the
entire point if one of the repetitions is an outlier.

Quantitation

This function allows sample measurement reporting in different units than the calibrant
units.
Calibrant Units

Sets the units for the calibrants being used. This becomes the
text label that displays in the report unless a conversion is
used.

Final Units

Sets the sample final units if using a conversion factor to


report measurements in units different than the calibrant
units. For instance, final units may be used to convert from
the calibrants ppm units to M final units. All results report
in the final units.

Conversion Factor

Specifies a multiplier needed to convert units. WinFLOW


multiplies the conversion factor by the concentrations for all
values in the results table.

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Method Editor

Flagging

Overlimit Samples

This feature displays flags next to samples that exceed operator-defined low and high
values. The flags appear under the Flags column on the report by peak (available from
the View menu). Set low and high detection limits for the flags based on reported
sample concentrations. WinFLOW automatically displays the lowest and highest
calibrant concentrations as entered in the calibrants table (see Calibrants Table Editor
Screen on page 55 in this chapter).
Low Detection
Limits

Sets the sample concentrations below which a LO flag appears on


the report by peak. Set the Low limit to 10% below the lower
quantitation limit for a given analyte.

High Detection
Limits

Sets the sample concentrations above which a HI flag appears on


the report by peak. Set the High limit to 10% above the upper
quantitation limit for a given analyte.

This feature sets actions to be taken when analyzing sample(s) with concentrations over
an operator-defined limit.
Action

Sets WinFLOW to automatically Notify User or Assert Alarm


when a samples concentration measures above a defined limit.

Trigger Level

Sets the operator-defined concentration limit for overlimit


samples.

Timed Events Editor Screen


The Timed Events Editor screen (Figure 5.8) lists time-based events that control various
devices and their associated actions during operation.
Access the Timed Events Editor screen by clicking its icon from the Method Editor icon
ribbon, by going to the Page menu and selecting Timed Events Editor, or by pressing
[Shift]+[F5].

Figure 5.7. Timed Events Editor screen

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Method Editor

B (Basis of
Timing)

The B field determines the timing basis for the timed events entered. Make a selection
by right-clicking the particular cell in the B column. Choose from the following three
choices:
Run-Based (R)

Choose for items that occur one time during the run and are
timed using run-based timing. The timing is set in
hours:minutes:seconds (hh:mm:ss).

Injection-Based (I)

Choose for events used for each sample injection. Timing is


set in xx.xxx seconds or in hh:mm:ss for long events (greater
than two minutes).

Shutdown (S)

Choose for events occurring at the end of a run. Shutdown


events begin after WinFLOW marks the baseline lag point.
Timing is set in hh:mm:ss.

Time

The Time field specifies a time for an event to occur. Select a cell in the Time column
and enter the time in the appropriate format based on the basis of timing.

Device

The Device field sets the device such as pumps, valves, and autosamplers, as well as
software functions, on which the timing event occurs. Select a device by right-clicking
the particular cell in the Device column, and then selecting the desired device in the
Device menu.
Pump

Sets FS 3000 pump control during a timed event. Generally, the


pump turns On at time 0. Use run-based (R) timing for the
pump. To set the pump to automatically turn Off when the
analysis completes, add a second shutdown-based (S) line in the
timed events table that turns the pump Off.

Valve

Switches the injection valve between Load and Inject during the
run, which is an injection-based event. Use this setting for FIA
only. The valve loads at time 0 and injects when enough time
passes (operator selectable) to allow the sample loop to fill
completely. The valve stays in the inject position from the time it
switched to the end of the cycle duration time. At the end of the
inject cycle, it returns to the load position to begin another cycle.

Heater

This setting is not used.

Sampler

Switches the autosampler between sample cups and the wash


reservoir throughout the run, which is an injection-based (I)
event. Set to Sample at time 0 then switch to Wash. This timing
depends on the method used. Refer to the method for specific
recommended values.

Autozero Time

Sets the autozero start time. Set for one minute less than the
cycle start time to start autozero when data collection initiates.
This is a run-based (R) event only.

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Method Editor

Cycle Start

Sets the time when data collection begins. The detectors and
display reset at this point. The cycle start time is always a runbased (R) event and can be a long setting to allow baseline
stabilization before the run.

Cycle Duration

Sets the timing for the analysis cycle and is always an injectionbased (I) event. The method specifies the time, which is
determined by the chemistry, carryover, and desired throughput.
The time includes sample time plus wash time.

Table 5.2 presents a matrix of timed events, their basis, devices, and applicable states.
Table 5.2. Timed events devices and states

B
(Basis of Timing)

Devices

State

Run-based (R)

Pump

On or Off

Valve

Load or Inject

Heater

Off

Sampler

Sample or Wash

Autozero

On

Cycle Start

On

Pump

On or Off

Valve

Load or Inject

Sampler

Sample or Wash

Cycle Duration

On

Pump

On or Off

Valve

Load or Inject

Sampler

Sample or Wash

Injection-based (I)

Shutdown (S)

# (Selector)

The Selector field selects the specific heater, valve, or pump to be controlled. Set 13
heaters, 16 pumps, or 16 valves, depending on the hardware configuration.

State

State defines the instrument device status. Table 5.2 shows the states associated with
each device. Right-click the cell to select the state.

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Method Editor

Calibrants Table Editor Screen


Use the Calibrants Table Editor screen (Figure 5.8) to identify calibrants (C),
independent calibration verification (ICV), continuing calibration verification (CCV),
and spikes (SPK) used with the sample table (see Chapter 6, Sample Table Menu
Options on page 62). The table lists the name, type (T), concentration, and percent
acceptable deviation (%) for each standard. The calibrants table presents one column
for each active channel in the method. Access the Calibrants Table screen by clicking its
icon from the Method Editor icon ribbon, by going to the Page menu and selecting
Calibrants Table Editor, or by pressing [Shift]+[F6].

Figure 5.8. Calibrants Table Editor screen

Calibrants

Calibrants (C) are standards with known concentrations used to create the calibration
curve. WinFLOW uses the calibration curve to determine sample concentrations.
Choose calibrants to bracket the expected sample concentration range. When taking
multiple aspirations of a single calibrant, WinFLOW uses each point when calculating
the curve. It does not average calibrant points. The curve fit chosen defines the
minimum number of calibrants. First-order curves require two calibrants, second-order
curves require three, and third-order curves require four. Weighted linear curves require
triplicate aspirations of a minimum of two calibrants.
Calibrant names cannot be more than 20 characters. They must exactly match the
calibrant name typed into the sample table since WinFLOW distinguishes between
calibrants only by name. If an undesignated calibrant appears in the sample table,
WinFLOW prompts the operator to fix the problem. Enter a name, type (C), and
concentration for each calibrant.

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Method Editor

Independent
Calibration
Verification

Independent calibration verifications (ICV) are standards with known concentration


usually prepared by an independent source such as the National Institute of Standards
and Technology (NIST). Use ICVs to check instrument performance and the validity of
prepared standards. Run an ICV immediately following the calibration curve. If an ICV
fails, the run automatically aborts. If analyzing more than one ICV replicate, the run
does not abort unless all the ICVs in the group fail. If running two separate ICVs, the
run aborts if either ICV fails. Always precede and follow ICVs by at least one blank and
a baseline sample (e.g., BLNK, RB, ICV, BLNK, RB).
Like calibrants, WinFLOW recognizes ICVs both by name and type. Enter a unique
name, type (ICV), concentration, and percent acceptable deviation (%) for each ICV.
ICV names cannot be longer than 20 characters. They must exactly match the name in
the sample table since WinFLOW distinguishes between ICVs only by their name. If an
undesignated ICV appears in the sample table, WinFLOW prompt the operator to fix
the problem.

Continuing
Calibration
Verification

Continuing calibration verifications (CCV) are samples of known concentration used to


verify the calibration curve remains valid over the course of a sample run. The CCV
determines if recalibration is necessary. Designate the action taken in response to a
CCV failure under CCV/Drift Fail options (see Flow Control Settings Screen on
page 38 in this chapter). If analyzing more than one CCV replicate, the group does not
fail unless all CCVs in the group fail.
Typically use one calibration standard as the CCV. Prepare CCVs from midrange
calibrants. Place CCVs at regular intervals throughout the series of unknowns, usually
every 10 samples. Always precede and follow CCVs with at least one blank and a
baseline sample (e.g., BLNK, RB, CCV, BLNK, RB).
Provide a unique name, type (CCV), concentration, and percent acceptable deviation
(%) for each CCV. CCV names cannot be longer than 20 characters. They must match
the CCV name in the sample table since WinFLOW distinguishes between CCVs only
by their name. If an undesignated CCV appears in the sample table, WinFLOW prompts
the operator to fix the problem.

Spike

Use a spiked sample (SPK) to determine the sample matrix effect on the sample results.
This function calculates the percent recovery of a known concentration addition made
to a sample. It compares the spiked sample value to the sample immediately before it in
the sample table. Enter the known added analyte concentration (e.g., 1 mg/L) in the
calibrants table. Spike names cannot be longer than 20 characters. They must match the
spike name in the sample table since WinFLOW distinguishes between spikes only by
their name. If an undesignated spike appears in the sample table, WinFLOW prompts
the operator to fix the problem. See Figure 5.8 and Figure 6.1.

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Method Editor

Stock Calibrants

When used with the Autodilutor, WinFLOW directs working calibration standard
preparation from predefined stock calibration solutions (STOK). After defining stocks,
add the working calibration standards to the calibrant table. Also list the stocks and
calibrants in the sample table. WinFLOW identifies instrument prepared working
calibrants in the sample table with C* notation, and the operator prepared standards
using normal C notation.

Drift Correction

When using one or more calibrants to perform sensitivity drift correction, a percent fail
value must be assigned to the calibrants chosen as drift peaks. Use name of the calibrant
in the Sample Table with a type of DRI or DRT (see Table 6.2 on page 60 for a
description of sample types and functions).
If the calculated concentration for the drift peak is within the range set in the calibrant
table, the software applies the drift correction. If the concentration is outside the range,
the drift peak will Fail (like a CCV) and perform the action set in the method for
CCV Fail. See Figure 5.8.

Verifying Method Settings


After entering all settings in the Method Editor, verify proper settings. From the File
menu, click Verify Method, Verify Timed Events, or Verify Calibrants to check each
setting. These functions identify basic conflicts in the methods, but may not identify all
errors.

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Chapter 6 Sample Table


Open the Sample Table screen (Figure 6.1) by doing one of the following:

From the Select View dialog box, click the Sample Table icon,
Click the Sample Table icon on the main icon ribbon, or
Press [F3].

Figure 6.1. Sample Table screen

Use the sample table to map sample and calibrant positions in the autosampler. It also
defines sample types and sample calculation parameters for each entry. Every sample
table row corresponds to a specific position on the autosampler.
The Model 3090 (90-place), Model 3360 (360-place), and RA (270-place) Samplers are
all true random-access autosamplers when used with WinFLOW. The autosampler
probe can be sent to any cup at any time throughout a run. Table 6.1 describes the
available sample table fields.

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Sample Table

Begin filling in the table by clicking on an empty cell in the Name column and entering
the sample name. WinFLOW automatically fills in default values if no operatorsupplied values are provided.
Table 6.1. Sample table fields

Item

Description

Use

Cup

Cup number

Corresponds to an autosampler cup.

Name

Sample name

Operator input with a 20-character limit. Names for calibrants, ICV,


CCV, and SPK samples must correspond exactly to those listed in the
calibrants table of the Method Editor.

Type

Sample type

SYNC, STOK, C*, C, DRI, DRT, ICV, CCV, BLMK, RB, U*, U, CO,
DIL, NULL, SPK (see Table 6.2)

Replicate count

Allows up to nine replicates from each sample cup. The default is one.

Dil

Dilution factor

Multiplies the final concentration by the factor input. The default is one.

Wt

Weight factor

Divides the final concentration by the factor input. The default is one.

Vial

Vial type

Inserts a vial type for a specific sample. Set the default in the Method
Editor. Four types are available (14). Use this field with the RA, Model
3090, and Model 3360 samplers.

Comment

Cup comment

Provides space to detail extra information about the sample. Notes kept
here do not appear in the final report.

Cup Number

The Cup Number corresponds to the position numbers on the autosampler.


For all autosamplers except the Model 3090, WinFLOW recognizes cup 0 as the wash
position (either TWR or fixed reservoir). Use this number with any type designation
(BLNK, U, CCV, etc.). For the Model 3090, WinFLOW recognizes cup 900 as the wash
position.
Choose from several wash and diluent source possibilities when using the Model 3090,
Model 3360, or RA Sampler.
NOTE: The RA Sampler cup numbering scheme differs from most other
autosamplers. The cup positions in the standards rack are numbered 110 or
120. Three-digit numbers define the sample racks. The first digit indicates
the rack number and the second two digits indicate the cup position within
that rack. For example, when using a 90-place tray, the first sample rack is
numbered 101190, the second sample rack 201290, and the third sample
rack 301390. Custom racks follow this numbering system as well.
NOTE: For the Model 3090, the cup positions for the standards rack are numbered
901909. The sample cups are numbered 101190.

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Sample Table

NOTE: For the Model 3360, the cup positions for the standards rack are numbered
901910. The sample cups are numbered 101190, 201290, 301390, and
401490.

Sample Names

Sample names are limited to 20 characters. Names of calibrants (STOK, C), check
calibrants (CCV, ICV, DRI, DRT), and spikes (SPK) must correspond to those given in
the methods calibration table. When proceeding with the analysis, if any of these
names do not correspond, a warning appears on the screen describing the faulty entries.
Correct this error before continuing to analyze samples.

Sample Type

The sample type determines how WinFLOW treats a sample in a run. WinFLOW
contains 15 sample types, described in Table 6.2.
Table 6.2. Sample types and functions

Code

Type

Function

BLNK

Blank

Allows a blank, which it treats as an unknown sample.

Calibrant

Correlates response to concentration as defined in the Method Editor.

C*

Calibrant (to be
prepared)

Instructs WinFLOW to prepare this calibrant. C* changes to C after the


calibrant is diluted.

CCV

Continuing
calibration
verification

Verifies continued calibration validity throughout the run and


determines if recalibration is necessary according to operator-defined
qualifications.

CO

Carryover

Corrects for carryover due to high concentration samples. It requires


one or more replicates, preferably following the SYNC peak.

DIL

Dilution

Placed at the end of the table to designate a cup as a dilution cup. Use
this type for autodilution of overlimit samples.

DRI

Sensitivity drift
correction
(incremental)

Reslopes the most recent full calibration to account for any measured
sensitivity drift. WinFLOW calculates the value in increments during
the run (i.e., it adjusts from last DRI to current DRI).

DRT

Sensitivity drift
correction (total)

Reslopes the most recent full calibration to account for any measured
sensitivity drift. WinFLOW calculates the value for the entire (total)
run.

ICV

Independent
calibration
verifications

Standards with known concentration usually prepared by an


independent source such as NIST. ICVs check instrument performance
and the validity of prepared standards.

SPK

Spiked Sample

Determines the sample matrix effect on the sample results. This


function calculates the percent recovery of a known concentration
addition made to a sample by comparing the spiked sample value to the
sample immediately before it in the sample table.

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Sample Table

Table 6.2. Sample types and functions

Code

Type

Function

STOK

Stock calibrant

Used as the stock calibrant solution when using automatic standard


preparation.

SYNC

Synchronization
Peak

As the sample tables first entry, the SYNC peak initiates the peak
recognition process. The SYNC peak height must be above the
minimum peak recognition parameters set for each channel in the
method.

Source Unknown

The sample for analysis.

U*

Unknown (to be
prepared)

Unknowns designated by U* dilute before the run starts. Use this


feature for samples known to be above the analysis calibration range.

Replicate

Replicate defines the number of times a specific sample cup aspirates or injects. Enter
replicate values between one and nine. Use another line in the sample table to draw
from the same cup more than nine times. Specify zero replicates to deliberately skip the
sample on that line, e.g., when running U* samples when only analyzing the dilution
and not the original. Also, STOK cups always force the replicate value to zero.
WinFLOW directs the dilution of that sample if enabling the dilution function and the
concentration of a sample is outside the range specified in the Method Editors
Calibration/Quantitation Settings screen (see Chapter 5, Calibration/Quantitation
Settings Screen on page 50). If analyzing replicates, the autodilutor performs only be
one dilution and then takes the replicates from the single dilution cup.

Dilution and
Weight Factors

If diluting samples manually before the run, enter the dilution or weight factors into the
sample table for automatically calculating the original sample concentration. If an
autodilution occurs during the run, the dilution factor automatically enters into the
results and analysis table. If a sample is out of range and is manually diluted during a
run, the operator must enter the dilution factor into the sample tables add-on screen.

Vial Type

Use the Vial Type column only with the RA, Model 3090, and Model 3360 samplers.
Set the default vial type in the Method Editors Flow Control Settings screen (Chapter
5, Flow Control Settings Screen on page 38). Therefore, only list the vial types
separately for types other than the default.

Comments

The Comments section provides the operator space to record notes about the sample.
This field appears in the results and analysis table if the operator selects comments
information in the reports option section (see Chapter 8, Reports on page 88).

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Sample Table

Sample Table Menu Options


The sample table performs much like a standard spreadsheet. Click to highlight a
particular cell and enter the desired information. WinFLOW designates cells as alpha,
numeric, or alphanumeric cells. If an entry is incorrect, an error message appears
pointing the operator to the wrong entry in the table.
The Sample Table menu bar contains the following four menus: File, Edit, Tools, and
Window.

File Menu
Figure 6.2. File menu

New creates a new table.


Open accesses an existing, previously saved table.
From Analysis accesses the sample table when an analysis runs.
Import transfers a table from another program. Tables import in text format.
Save updates to the current table.
Save As preserves the current table under a new name.
Export sends the current table to a text file for opening in another Windows program.
Verify checks the sample table for errors. It may not identify all errors.
Print Setup configures printer preferences.
Print sends the current table to a printer or file.
Exit closes the sample table.

Edit Menu

Figure 6.3. Edit menu

The Edit menu contains standard editing functions for working with text. Many of these
features allow the operator to copy the current sample table to spreadsheet or word
processing programs. The editing tools use the standard Windows clipboard in a similar
fashion as other Windows programs.
Cut removes highlighted text from its current location and places the text on the
clipboard.
Copy duplicates highlighted text and places it on the clipboard.
Paste places the clipboard contents into the desired location.
Clear deletes the highlighted text or values without storing anything on the clipboard.
Insert Rows introduces a row above the highlighted row.
Delete Rows removes the entire selected row from the table.
Go To selects a specific column and row for viewing.
Sort arranges the table in numeric or alphabetical order. Click a cell in the desired field
to be sorted, then select Sort.

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Tools and Window


Menus

See Chapter 4, Tools Menu on page 27 and Chapter 4, Window Menu on page 30.

Creating a Sample Table


Throughout this section, refer to Figure 6.1 on page 58 for an example of a typical
sample table.

Synchronization
Peak (SYNC)

The sample tables first entry is always the SYNC peak. The SYNC peak initiates the
peak recognition process. The SYNC peak height must be above the minimum peak
recognition parameters set for each channel in the method.

Carryover
Correction (CO)

The carryover correction feature calculates the percent carryover. This correction then
applies to all samples in a run. The carryover group must contain one or more blank
samples taken from the same cup. Perform carryover correction immediately following
the SYNC peak so the correction applies in real-time to the rest of the run. The percent
carryover displays in the Calibration Results Table screen.

Calibrants

Calibrants (C) are standards with known concentrations used to create the calibration
curve. WinFLOW uses the calibration curve to determine sample concentrations.
Choose calibrants to bracket the expected sample concentration range. When taking
multiple aspirations of a single calibrant, WinFLOW uses each point when calculating
the curve. It does not average calibrant points. The curve fit chosen defines the
minimum number of calibrants. First-order curves require two calibrants, second-order
curves require three, and third-order curves require four. Weighted linear curves require
triplicate aspirations of a minimum of two calibrants.
Calibrant names cannot be more than 20 characters. They must exactly match the
calibrant name in the sample table since WinFLOW distinguishes between calibrants
only by name. If an undesignated calibrant appears in the sample table, WinFLOW
prompts the operator to fix the problem. Enter a name, type (C), and concentration for
each calibrant.

Calibrants To Be
Diluted

Calibrants that need to be prepared via dilution are designated with a C* in the sample
table rather than a C. The system automatically determines how to dilute STOK and Ctype samples to achieve the requested concentration for each C* sample. The dilutions
are performed at the start of the run, prior to any sample processing. After each C* is
prepared, its sample type is changed by the WinFLOW software to C. Either all
calibrants or any of the individual calibrants may be prepared by dilution.
If the required volume of standard prepared by dilution is less than the syringe volume,
a single cup position can be designated as C*. The required quantity of replicates is
then entered in the appropriate column of the sample table.

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If the total volume of dilutor-prepared standard is greater than the syringe volume,
including any drift correction peaks or CCV peaks, the WinFLOW software allows for
multiple dilutions into a single cup position. When entering the sample table, repeat the
same cup number and sample name for several entries in a row, denoting each as type
C*. Enter the desired replicates to run as calibration points for only the first row of the
group of identical C* samples. Enter zero (0) for the replicates needed for the other
rows (refer to rows 5 through 14 in Figure 6.1).
For example, if approximately 8 mL of diluted standard is needed for processing as C,
CCV, DRI, or other samples (with a 2.5 mL syringe in use), the operator should create
4 total entries in the sample table for the single diluted standard. Each entry should use
the same cup number and be of type C*, resulting in 10 mL of diluted standard being
dispensed into the desired cup. Similarly, if approximately 7 mL of diluted standard is
needed (with a 2.5 mL syringe), then a total of three C* entries, each using the same
cup number and sample name, are required (see Table 6.3).
Table 6.3. Examples with the Standard 2.5-mL Syringe

Entries
for C*

Volume of
Prepared
Standard (mL)

7.5

10

Unknowns To Be
Diluted

Unknowns designated by U* dilute before the run starts. Use this feature for samples
known to be above the analysis calibration range. Enter the desired dilution factor in the
Dil column. Place an empty sample cup in the autosampler location defined by U*.
Place the source unknown with the U designation in the sample table and at the cup
location immediately prior to the U* location. Source unknowns must have a replicate
zero value entered to ensure these unknowns are not analyzed directly.

Stock Solutions

When used with the Autodilutor, WinFLOW directs working calibration standard
preparation from predefined stock calibration solutions (STOK). After defining stocks,
add the working calibration standards to the calibrant table. Also list the stocks and
calibrants in the sample table. WinFLOW identifies instrument prepared working
calibrants in the sample table with C* notation, and operator prepared standards using
normal C notation.

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Incremental
Sensitivity Drift
Correction

Use the incremental sensitivity drift correction (DRI) to adjust a calibration that
becomes invalid due to sensitivity drift. Designate a calibrant as a drift correction cup.
The drift correction applies to all peaks following the first drift cup to the next drift cup.
If the incremental drift is outside an operator specified range, WinFLOW takes the
same action as a failed CCV. Also use the DRI to perform a run without running a
calibration, using the DRI to adjust a previous calibration curve (see Chapter 8, Data
Processing Tools on page 78).

Total Sensitivity
Drift Correction

Use the total sensitivity drift correction (DRT) to adjust a calibration that becomes
invalid due to sensitivity drift. Designate a calibrant to act as a drift correction cup. The
drift correction applies to all peaks following the drift cup. If the total run drift is not
within the operator specified range, WinFLOW takes the same action as with a failed
CCV. Also use the DRT to perform a run without running a calibration, using the DRT
to update a previous calibration curve (see Chapter 8, Data Processing Tools on
page 78).

Independent
Calibration
Verification

Independent calibration verifications (ICV) are standards with known concentration


usually prepared by an independent source such as NIST. Use ICVs to check instrument
performance and the validity of prepared standards. Run an ICV immediately following
the calibration curve. If an ICV fails, the run automatically aborts. If analyzing more
than one ICV replicate, the run does not abort unless all the ICVs in the group fail. If
running two separate ICVs, the run aborts if either ICV fails. Always precede and
follow ICVs by at least one blank and a baseline sample (e.g., BLNK, RB, ICV, BLNK,
RB).
Like calibrants, WinFLOW recognizes ICVs both by name and type. Enter a unique
name, type (ICV), concentration, and percent acceptable deviation (%) for each ICV.
ICV names cannot be longer than 20 characters. They must exactly match the name in
the sample table since WinFLOW distinguishes between ICVs only by their name. If an
undesignated ICV appears in the sample table, WinFLOW prompts the operator to fix
the problem.

Continuing
Calibration
Verification

Continuing calibration verifications (CCV) are samples of known concentration used to


verify the calibration curve remains valid over the course of a sample run. The CCV
determines if recalibration is necessary. Designate the action taken in response to a
CCV failure under CCV/Drift Fail options (see Chapter 5, Flow Control Settings
Screen on page 38). If analyzing more than one CCV replicate, the group does not fail
unless all CCVs in the group fail.
Typically use one calibration standard as the CCV. Prepare CCVs from midrange
calibrants. Place CCVs at regular intervals throughout the series of unknowns, usually
every 10 samples. Always precede and follow CCVs with at least one blank and a
baseline sample (e.g., BLNK, RB, CCV, BLNK, RB).

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Provide a unique name, type (CCV), concentration, and percent acceptable deviation
(%) for each CCV. CCV names cannot be longer than 20 characters. They must match
the CCV name in the sample table since WinFLOW distinguishes between CCVs only
by their name. If an undesignated CCV appears in the sample table, WinFLOW
prompts the operator to fix the problem.

Spiked Samples

Use a spiked sample (SPK) to determine the sample matrix effect on the sample results.
This function calculates the percent recovery of a known concentration addition made
to a sample. It compares the spiked sample value to the sample immediately before it in
the sample table. Enter the known added analyte concentration (e.g., 1 mg/L) in the
calibrants table. Spike names cannot be longer than 20 characters. They must match the
spike name in the sample table since WinFLOW distinguishes between spikes only by
their name. If an undesignated spike appears in the sample table, WinFLOW prompts
the operator to fix the problem.

Blanks and
Baseline Samples

Blanks (BLNK) are samples drawn from the wash position defined in the autosampler
configuration. They minimize tailing of calibrants or unknowns into the CCVs or ICVs.
and are placed throughout the sample run preceding CCVs and ICVs.
Baseline samples (RB) are also drawn from the wash position defined in the
autosampler configuration. Baseline samples force the baseline through that point and
correct baseline drift. Typically place them before a series of unknowns and before the
calibration series. Set up baseline samples to run in duplicate to allow maximum
flexibility in adjusting the baseline.
WinFLOW treats baseline samples automatically added through the method settings the
same as other baseline samples and denotes them as WBL in the results report.

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Autodilution
The autodilution function requires using the RA and Model 3360 samplers or with the
Autodilutor. This feature dilutes and resamples over-range samples in a single run. Any
sample concentration that falls above the limits set in the Method Editors Calibration/
Quantitation Settings screen (see Chapter 5, Calibration/Quantitation Settings Screen
on page 50) becomes marked as high and is diluted. All over-range sample dilutions are
performed at the end of the regular run. Follow the instructions below to use the
autodilution feature properly.
1. Before opening WinFLOW, ensure the sampler and the autodilutor options are
selected in the WinFLOW Configuration dialog box (see Chapter 3, Configuration on page 7).
2. Open WinFLOW. Open the Method Editor (Chapter 5, Method Editor on
page 36).
3. Go to the Flow Control Settings screen and select Enable Autodilution (see
Chapter 5, Flow Control Settings Screen on page 38).
The Autodilutor uses the dilution sequence specified in the Dilution Factors in the
Method Editors Flow Control Settings screen.
4. Select the CCV groups frequency. Typically run a CCV group every 10 samples.
Enter the CCV group to be run in the sample table at the end of the DIL cups.
5. Select the number of followers to be run, most often set at two. A follower is
defined as the sample(s) after an over-range sample.
6. Go to the Calibrants Table Editor screen and define the stock and CCV. See
Figure 5.8 on page 55.
7. Go to Sample Table screen, and setup the sample table properly. See Figure 6.1 on
page 58.
8. After the sample tables last sample, enter several cups with the type DIL and
supply an identifier in the Name column.
9. At the end of the DIL cups, enter the CCV group used throughout the dilution
samples.

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Import and Export Functions


Exporting a Table

Export a sample table by going to the Sample Table screens File menu and selecting
Export. A dialog box appears requesting the name and location for the exported file.
All tables export as text files (*.txt). The sample table can then be opened in any
program that can read text files.

Importing a Table

Import a table from an external program by going to the Sample Table screens File
menu and selecting Import. A dialog box appears requesting the name and location of
the desired file. All tables must be in text file (*.txt) format to import. Importing is
much easier if first exporting an actual WinFLOW sample table to the program of
choice. Then use this table as a template for creating new tables for importing.

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Chapter 7 Data Collection


Initiating WinFLOW instrument control and data collection uses an easy four-step
process. After opening WinFLOW, click the Collect Data icon. WinFLOW prompts
the operator to do the following:
1.
2.
3.
4.

Enter the operator name and ID.


Select a sample table to use.
Select a method to use.
Enter a results file name.

Initiating Data Collection


1. Click the Collect Data icon. The Operator Name and ID dialog box appears.
2. Enter the operator name and ID, and click OK. The Run Setup dialog box appears
(Figure 7.1).

Figure 7.1. Run Setup dialog box

3. Select the sample table and method to use. Click OK.

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4. WinFLOW requests a file name under which to store the final results. Enter a
suitable results file name and click OK. The Data Collection screen appears. The
Data Collection screen displays the number of channels in use, as defined in the
method.
If using a single channel, the Data Collection screen automatically displays four
windows (see Figure 7.2).

Figure 7.2. Single-channel Data Collection screen

If using more than one channel, only the peak plot window of each channel displays
(see Figure 7.3). Access the Data Collection screen for each individual channel by
double-clicking a peak plot window. That channels four windows then display.
Also access the required channel from the View menu.

Figure 7.3. Two-channel Data Collection screen

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5. Go to the Pumps menu and select the appropriate pump(s) to start.


6. Initiate baseline data collection from the detector by clicking the Play icon.
Baseline monitoring begins.
The cycle start time set in the Timed Events Editor defines the length of this monitoring
period (see Chapter 5, Method Editor on page 36). This defined time period allows
the operator to monitor the baseline and verify system stability before beginning the
run. The status bar in the screens bottom left displays Baseline View during this
period.
A real-time signal begins displaying in the Peak Plot window. The Fast Forward, Stop,
and Zero icons become active on the Data Collection icon ribbon. The Peak Results
Table, Calibration Plot, and Calibration Results Table windows become active once the
sample run initiates.
NOTE: Obtain percent full scale and detector gain values for the reference and sample
by going to the Window menu and selecting Serial Communication. This
indicates if the lamp functions properly.

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Monitoring the Baseline


During the monitoring period, the signal produced by a startup solution displays and
should meet the criteria shown in Table 7.1.
Table 7.1. Baseline criteria for startup solution

Parameter

Photometric or
Seawater Matrix
Detector

Amperometric
Detector

Vertical noise

<100 AU

<1,000 pA

Drift

<200 AU/300 seconds

<1,000 pAU/300 seconds

Dynamic software scaling occurs in real time. The highest point on the screen at any
one time sets the scale. Therefore, when monitoring the baseline, note the scale on the
vertical axis when determining whether or not it is stable. Figure 7.4 shows an example
of a quiet photometric detector baseline.

Figure 7.4. Baseline signal display

1. Establish a stable baseline using startup solution and then switch to reagents.
If discontinuing baseline collection by selecting the Stop icon, the Rewind icon
becomes available. Selecting the Rewind icon clears the screen and resets WinFLOW to collect baseline data.
2. After establishing a stable baseline with reagents, correctly place all appropriate
standards, blanks, and samples in the autosampler. The system can now initiate a
sampling sequence.

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Starting a Sample Analysis


Initiate the sampling sequence by selecting the Fast Forward icon from the Select
View bar or from the Data Collect menu. The autosampler proceeds to the vials as
defined in the sample table specified for the run. Because the operator accesses realtime data as it collects, all four windows of the Data Collection screen become available
during the run. Each of the screens is described below. Many editing functions are
available in these windows during data collection. For a detailed description, refer to
Chapter 8, Results and Analysis on page 77.

Peak Plot Screen

Figure 7.5 shows the Peak Plot screen. WinFLOW displays the signal continuously
throughout the run. Based on the SYNC peak, WinFLOW marks each subsequent peak
maximum (apex) according to parameters defined in the method and by the sample
sequence defined in the sample table. It uses this peak marker to measure peak height
from the established baseline. For peak area, WinFLOW places a mark in front and
behind the apex according to parameters set in the Method Editor. The integration area
becomes shaded for easy recognition.

Figure 7.5. Peak Plot screen

Calibration Plot
Screen

The Calibration Plot screen displays the calibration curve produced by the calibrants
during the run (Figure 7.6). Calibration points considered undesirable can be removed
while data collects by double-clicking on any point with the Peak Editor cross or by
changing the calibrants sample type from C to U in the Peak Table Results screen
(Figure 7.8). Making these changes removes this data point from the standard curve
calculations. Reinsert the point by reversing the process.

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Figure 7.6. Calibration Plot screen

Calibration
Results Screen

This screen displays calibrants as entered in the method, corresponding peak heights or
areas, calibration curve equation, correlation coefficient, and carryover percentage
(Figure 7.7). An asterisk (*) next to the calibrant name identifies that calibrant as being
used in the calculated calibration curve.

Figure 7.7. Calibration Results screen

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Peak Table
Results Screen

This screen displays information such as peak heights, calculated concentrations,


informational flags, and any sample specific information previously entered into the
sample table used for that run (Figure 7.8). Changing the Type, Dil, or Wt produces
corresponding changes in calculated results both while the data collects and during
post-run analysis.

Figure 7.8. Peak Table Results screen

Adding Samples to
a Sample Table

Add samples to the end of an already initiated sample table using the following steps.
1. Click the Sample Table icon. The active sample table displays with all current
samples grayed-out indicating these samples cannot be edited (Figure 7.9). The rest
of the table remains available for adding samples.

Figure 7.9. Adding samples to a sample table

2. Enter the cup number, name, type, number of replicates, etc.


3. Close the sample table. A dialog box appears to confirm the changes. Click Yes.

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Modifying a Sample Table During a Run


Once data collection begins, pause the run to edit the current sample table in any way as
required. Pause the run by clicking the Pause icon.
The following then occurs:

Any single group of replicates currently being injected complete injecting and
marking.

WinFLOW waits for the sampling pass to end and marks baseline lag points (null
peaks). Usually two or three Ns display during this lag period. At the end of the lag
period, the sample table becomes available for editing. Samples already analyzed
appear grayed out and are not available for editing.

Edit the sample table by performing the following steps:


1. Click the Sample Table icon and perform any editing as required. All normal
sample table parameters become available.
2. After editing, close the sample table. Click Yes to save the changes and incorporate
them into the run once it restarts.
3. Restart the run by selecting the Play icon.

Stopping a Run
Sample runs stop in several ways. The run most commonly completes on its own. Other
software-controlled stops include ICV failure or a second failure of a CCV standard.
The operator can stop a run at any point by selecting the Stop icon from the Data
Collection screen.

Operator-Stopped
Run

WinFLOW verifies the command to manually stop a run using the Stop icon.
Data collection continues if selecting Cancel. If selecting OK, a Run Aborted dialog
box appears asking whether or not to save the data. If selecting Yes, WinFLOW saves
the data. If selecting No, the data remains on the screen until the operator takes further
action.

WinFLOWStopped Run

If the run completes or if it stops due to a failed CCV or ICV, WinFLOW automatically
saves the data under the operator-defined filename and then proceeds directly to the
Results and Analysis screen.
NOTE: In the case of a sudden power loss, WinFLOW automatically preserves all
data collected when possible. When WinFLOW restarts, the data file displays
and the operator can choose to save it.

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Chapter 8 Results and


Analysis
This chapter discusses data processing following a completed run. Since WinFLOW
contains online editing capabilities, most of the processes described in this chapter also
become available during data collection (see Chapter 7, Data Collection on page 69).
This chapter uses a single data file throughout as an example. Thoroughly exploring
one data file helps the operator develop a better understanding of WinFLOWs data
processing capabilities and to process acquired data more quickly, efficiently, and
accurately.

Loading a Data File


Load a saved data file to the Data Analysis screen by doing one of the following:

Select the Data Analysis icon from the icon ribbon,


Select Data Analysis from the Select View Bar, or
From the Data Analysis screen, go to the File menu and select Open.

The Open Results dialog box appears. Select the data file to open, and click OK.
A file loads from any active computer drive. During processing, a data file can open
from any drive, process, and save to any location.

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Data Processing Tools


Data Analysis
Screen

The Data Analysis screen for each channel splits into four windows: Peak Plot,
Calibration Plot, Peak Results Table, and Calibration Results Table (Figure 8.1).

Figure 8.1. Data Analysis screen

Access each of the Data Analysis screens four windows for post-run processing by
clicking the Maximize icon in the screens top right corner. Clicking the Minimize
icon returns the operator to the main windows.

Grid On/Off Icon

Selecting the Grid On/Off icon removes or restores the grid lines in the peak plot and
calibration plot. Removing the grid lines increases print speed.

Peak Editor Icon

Selecting the Peak Editor icon toggles the mouse cursor between the standard pointer
and the peak editor cross. With the peak editor cross active, move peak markers and
baseline points by dragging and dropping the markers.

Recalculate Icon

Selecting the Recalculate icon recomputes results according to changes made by the
operator (such as moving a peak marker or baseline point). The Recalculate icon
becomes available after any data editing that could result in a change in calculated
values. Once selected, WinFLOW applies the edited data to all four Data Analysis
screen windows. Results also recalculate automatically when exiting or entering
another window.

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Delete/Reprocess
Peaks Icon

Use this icon primarily to recalculate peaks to eliminate any mismarked peaks. For
example, if WinFLOW marks the SYNC peak in the wrong place, all subsequent peaks
become marked incorrectly. In this case, delete the incorrectly placed SYNC peak
mark, remark at the proper sync peaks apex, and recalculate.
1. A new cursor appears when selecting the Delete/Reprocess Peaks icon (Figure
8.2). Place the new cursor over a peak and release the left mouse button. The Delete
All Peaks Warning dialog box appears.

Figure 8.2. Delete/reprocess cursor

2. Click Yes to delete the selected peaks markers and all peaks that follow the
selected peak.
3. After deleting the peak markers, add a peak marker to the first available unmarked
peak using the Peak Editor icon. This peak now determines how the peaks to the
right recalculate. WinFLOW uses information previously saved in the Method
Editor, such as cycle time and peak finding parameters, as the reprocessing factors.
After marking the first peak in the series of deleted peaks, select the Recalculate icon
and the rest of the peaks become marked automatically. If making these changes after
collecting results, be sure to save any changes made. Post-run changes cannot be saved
under the same filename. Specify a new filename.

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Menu Options

The Data Analysis pull-down menus contain standard menu options as well as options
specific to the Data Analysis screen (see Chapter 4, Introduction to WinFLOW on
page 26 for a discussion of standard menu options). Many of the operations discussed
throughout this chapter are duplicated in mouse and menu options. Items not used in the
Data Analysis screen become grayed out.

File Menu
Figure 8.3. File menu

Open accesses a new results file.


Save updates the current results file.
Save As preserves the current results file under another file name.
Export sends the peak table or calibration table to a text (*.txt) file. This option is only
available when the Peak Table or Calibration Table screen is maximized.
Update Method refreshes the Method Editor file with changes made (e.g., changing
from a first-order to a second-order curve fit).
Print Setup configures printer preferences.
Print sends the current window to the printer or a file. Maximize one of the four
windows to print.
Exit closes the Data Analysis screen.

Data Collect Menu


Figure 8.4. Data Collect
menu

Run Setup initiates the data collection process.


Play initiates the baseline view.
Rewind erases data collected up to the moment Stop run was selected.
FastFwd initiates data collection.
Pause run pauses data collection. Continue the run by selecting FastFwd.
Stop run halts data collection.
Zero zeros the baseline signal on the peak plot.
Single Sample Mode toggles the sampling mode to uninterrupted sample mode during
data collection.

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Analysis Menu
Figure 8.5. Analysis menu

Smoothing selects one of three algorithms. See Chapter 5, Signal Filter and Marking
Settings Screen on page 46 for more information.
Detection edits detection levels.
Recalculate updates the results according to changes made by the operator.
Delete Peaks recalculates peaks to eliminate any mismarked peaks. See Delete/
Reprocess Peaks Icon on page 79 in this chapter.
Include Origin adds the 0,0 point to the calibration curve. This selection is standard for
single point calibration and optional for other calibration routines.
Calculation Mode chooses between measuring peaks by height or area. A check mark
indicates the current selection. See Recalculate Icon on page 78 in this chapter.
Fitting Model applies first, second, or third order, or weighted linear curve fitting to
the results. See Chapter 5, Calibration/Quantitation Settings Screen on page 50 for
more information.
Logarithmic converts the calibration curve using a logarithmic curve fit.

Calibration Menu
Figure 8.6. Calibration
menu

The Calibration menu allows calibration curves to be imported and exported. The
menu also displays a list of the calibration curves used in the run.
Load Calibrations imports a previously saved calibration curve into the current data
file.
Save Calibrations preserves the current calibration curve to a separate file for use with
another results file.
Use Loaded applies the loaded calibration curve to the current data file.

View Menu
Figure 8.7. View menu

The View menus lower portion displays each channel used to collect data for the
currently open file. The channels list by the name (if any) given by the operator in the
Detector/Channel Settings screen of the Method Editor (see Chapter 5, Method
Editor on page 36). Move directly to another channel without closing the windows
each time by selecting one of these channels.
Show Baseline views or hides the peak plot baseline.
Peak Labels on Printout displays the sample name and sample concentration above
each peak on the printout. These labels are only visible in the printout.
Format Analysis selects color schemes for the peak plot.
Format Calibration selects color schemes for the calibration plot.

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Reports displays results information from all channels used to collect data. Choose
from four available options: Peak, Sample, Sample (pass/fail), and Sample (summary).
See Reports on page 88 in this chapter for details and examples.
Preview displays sequence of the currently loaded sample table.
Scroll Lock freezes the baseline update used during data collection.
Grid displays or hides grid lines in the peak and calibration plots.

Peak Plot Screen


Magnifying the
Peak Plot

Magnify any portion of the peak plot by placing the cursor near the desired point to be
enlarged. Hold the right mouse button and drag to highlight the area (Figure 8.8).

Figure 8.8. Peak plot magnification

Release the right mouse button, and the highlighted area fills the entire Peak Plot
screen. Produce several magnification levels by sequentially repeating this process.
Click the right mouse button to display a menu (Figure 8.9) to reverse the zoom stepby-step or return immediately to the original full-scale plot.

Figure 8.9. Peak plot magnification menu

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Using the Cursor


For Peak
Identification

This ID/Information tool provides information about the peak plot or calibration plot
points. Place the cursor on a peak number, and press and hold the left mouse button
while the cursor appears as an arrow. The Peak Plot screen displays the peak number,
type, height, cup number, and concentration of the selected point (Figure 8.10).

Figure 8.10. Peak identification

1. To move a peak marker, select the Peak Editor icon.


2. Place the peak editor cross on the desired marker. Click and hold the left mouse
button, drag to the desired location, and release the left mouse button.

Changing a Peak
State (Add, Delete,
Toggle Baseline
Point)

1. Select the Peak Editor icon.


2. Place the peak editor cross on the desired peak and click the right mouse button.
The magnification and peak state options display (Figure 8.9).
3. Add or remove a peak by selecting Add Peak Mark or Delete Peak Mark.
Convert a blank or other peak mark into a baseline point (B) by right-clicking the
marker with the peak editor cross and selecting Toggle Baseline Point in the menu
that appears.
Change the marker back to its original state by selecting Toggle Baseline Point
again.

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Calibration Plot Screen


Magnifying the
Calibration Plot

Magnify any portion of the calibration plot by placing the cursor near the desired point
to be magnified. Hold the right mouse button and drag to highlight the area (Figure
8.11). Releasing the right mouse button and the highlighted area fills the entire
Calibration Plot screen. Produce several magnification levels by repeating this process.
Click the right mouse button to return the display to the previous magnification level.

Figure 8.11. Calibration plot magnification

Using the Cursor


for Calibration
Point Identification

This ID/Information tool provides information about the calibration plot points. Place
the cursor on a peak number and hold down the left mouse button. The identification
name, theoretical concentration, and height of the selected point display (Figure 8.12).

Figure 8.12. Calibration point identification

Removing Outlier
Calibration Points

Remove an undesired point by placing the peak editor cross on the point to be removed
and double-clicking the left mouse button. Return the point to the plot by repeating the
process. WinFLOW does not use the removed values in the calibration curve
calculations. Removed calibration points appear shaded gray.

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Peak Results Table Screen


The Peak Results Table screen (Figure 8.8) displays information, such as peak height,
for each resulting peak.

Figure 8.13. Peak Results Table screen

Peak Results Table


Fields
Peak

Displays the numeric identifier given in series to each peak marker.

Cup

Displays the sample source location in the sample tray.

Name

Displays the sample name.

Replicate (R)

Identifies the replicate number on each peak.

Type

Displays the sample type (see Table 6.2 on page 60).

Dilution (Dil)

Displays the sample dilution factor.

Weight (Wt)

Accounts for weight factors in soil and plant analysis.

Height

Displays the peak height measured from the baseline to the peak
marker.

Calc.

Displays the calculated value relating height to concentration based


on the calibration curve.

Flags

Displays any flags for each sample (see Table 8.1).

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Table 8.1. Peak results table flags

Flag

Name

BL

Baseline

HI

High

Marks peaks above method-specified limits.

LO

Low

Marks peaks that are below method-specified


limits.

UM

User modified

Failed

Marks all CCVs and ICVs that do not meet


percent deviation requirements.

Invalid

Marks all peaks before a failed CCV section.

PE

Preempted

Shows when CCV fails on one channel but not the


other.

FL

Follower

Used to specify peaks run again after an overscale


diluted sample.

Diluted

Marks overlimit peaks to show they were diluted


and analyzed later in the run.

XD

No DIL cup

Shows when more samples need dilution than


cups provided for dilution. The system dilutes as
many samples as there are cups, and flags the
others.

OL

Over limit

Indicates the sample result was over the highest


calibration value.

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Function
Used for all RB and WBL baseline samples (see
Chapter 6, Blanks and Baseline Samples on
page 66).

Marks all samples with peak markers moved by


the operator.

86

Results and Analysis

Calibration Results Table Screen


The Calibration Results Table screen (Figure 8.14) provides important information
about calibration process efficiency, such as the calibration coefficient (e.g., slope,
y-intercept) and correlation coefficient. Carryover calculations also display in this table.

Figure 8.14. Calibration Results Table screen

Calibrant ID

The first section of the calibration results table lists the calibrant names, theoretical
concentrations, and peak heights. A calibrant name marked with a * indicates its use in
the calibration curve (i.e., the data point was not removed by the operator). The
concentration values are editable. Therefore, if the operator mispoured cups or
mislabeled the concentration value before the run, these values can be corrected after
the run.

Calibration
Coefficients

The second section lists the calibration coefficients. The number of coefficients
depends on the curve fit. First order has two, second order has three, and third order has
four calibration coefficients.

Correlation
Coefficient

The correlation coefficient is a mathematical indicator of the correlation between two


data sets (peak height or peak area and calibrant concentrations). A perfect correlation
results in a correlation coefficient of 1.00. A correlation coefficient greater than 0.995
represents a correlation strong enough to consider a calibration curve valid according to
USEPA standards.

Carryover

The percent carryover is the number used to correct for interactions between peaks. If
WinFLOW did not implement carryover correction properly or did not use it at all, the
percent carryover displays n/a.

Drift Correction

If using drift correction, the drift cups and percent sensitivity drift display.

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Reports
WinFLOW data from all channels used to collect data display as a report. Choose from
four report display options: by peak, by sample, by sample (pass/fail), and by sample
(summary). Print or export these reports to other programs as needed. Access the
reports by going to the View menu and selecting Reports. Then select the desired
option.
by Peak

Contains the same information as the peak results table


with a time stamp for each analysis and mean and RSD
calculations for any sample or calibrant analyzed in
triplicate or greater (Figure 8.16). Sorted by time, no batch
correlation or status is provided. Other information may be
added by selecting Options from the View menu. The
Report Options dialog box displays (Figure 8.15).

by Sample

Sorts by actual sample and provides an ongoing status


during the run (Figure 8.18). It reports results in both
response value as well as pass/fail for each batch sampling
iteration.

by Sample (Pass/Fail)

This option is not used with this platform.

by Sample
(Summary)

Provides a summary format for batch mode analysis. Use


it for remote reporting where a concise report is desired. It
reports status and pass/fail only (Figure 8.18).

Figure 8.15. Report Options dialog box

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Figure 8.16. Report by peak

Figure 8.17. Report by sample

Figure 8.18. Report by sample (summary)

Exporting a Report
All reports export as text files that can be opened in any program that reads text (*.txt)
files. Export reports using the following steps.
1. Open the report for exporting.
2. From the File menu, select Export Report. The Export Sample Table To dialog
box appears.
3. Enter the name and location for the exported file.
4. Click OK.

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Chapter 9 Troubleshooting
Instrument Errors
The following lists errors that the Flow Solution or CNSolution can generate.
WinFLOW reports these errors the operator in a message box that identifies
instrument error encountered: and then lists the exact text received from the
instrument.
Code

Error

Cause and Solution

01

Syntax error

Unrecognized command or parameters invalid. Contact OI Analytical


Customer Support.

02

Out of memory

Command sent is not valid in this mode. The sample table may be too long,
or too many timed events listed.

03

Invalid mode

The label number specified in a GTL command does not exist.

04

Label not found

Contact OI Analytical Customer Support.

06

Invalid parameter

Requested a communications (baud) rate not supported. Contact OI


Analytical Customer Support.

42

Detector timeout or
overflow

Detector does not respond. Reset the instrument. Contact OI Analytical


Customer Support.

43

Invalid detector data

Detector sent incorrect data. Reset the instrument.

44

Bad detector
command

Detector reports that it received a bad command, indicating a possible octal


UART board problem. Reset the instrument.

45

Serial channel Rx
buffer full

Reset the instrument. An octal UART board problem may exist.

46

Serial channel Tx
buffer full

The buffer used for sending data to a device overflowed. Reset the
instrument.

71

PC RHR overrun

Instrument cannot keep up with serial communications from the PC. Check
serial cables and connections.

72

PC framing error

Communications error. Check serial cables and connections.

73

PC parity error

Communications error. Check serial cables and connections.

74

PC Rx buffer full

Contact OI Analytical Customer Support.

75

PC Tx buffer full

Contact OI Analytical Customer Support.

81

Exception

Stack frame error. Contact OI Analytical Customer Support.

82

Exception

Invalid command code generated. Contact OI Analytical Customer Support.

83

Exception

Analyzer mode set to invalid value. Contact OI Analytical Customer


Support.

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Troubleshooting

Code

Error

Cause and Solution

84

Exception

Impossible code passed to GET-PARAM-RANGE. Contact OI Analytical


Customer Support.

C2

Exception

Value received from detector in an invalid mode (not A or P). Contact OI


Analytical Customer Support.

C3

Exception

DUART input ready flag generated, but no delimiter found. Contact OI


Analytical Customer Support.

F1

Exception

PC input ready flag generated, but no delimiter found. Contact OI


Analytical Customer Support.
Even the most robust electronic device occasionally malfunctions due to environmental
problems such as a static charge, current or voltage spikes, brown-outs, moisture, or
physical shock (such as a hit or drop) to the system. In these cases, the error generated
may have little to do with what initially caused the problem and can be impossible to
trace. This error type generally occurs infrequently, and it cannot be reproduced. An
error occurring consistently or repeatedly usually indicates a hardware problem.

WinFLOW Errors
WinFLOW can generate a number of possible software-based errors while running.
They range from fatal (e.g., general protection fault), to inconvenient (e.g., problem
initializing autosampler), to helpful (e.g., must have three data points for second-order
curves). Maintain a log of reported errors and what was performed to fix them.
General Protection Fault (GPF): All Windows software occasionally experiences a
GPF. The Windows operating system actually causes many GPF. However, if a certain
area of the software or the performing certain activities causes GPFs consistently, this
usually indicates a problem with WinFLOW.
Assert: WinFLOW was programmed with what are known as asserts. These are put in
the software where certain conditions must be true (e.g., the analysis window has to
exist to draw the curve trace). These asserts assist in debugging the software. Asserts
are considered to be very similar to GPFs. However, they usually offer more
information about what went wrong and where in the program the problem occurred.

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Reporting Errors

The most important thing about tracking down an error is its reproducibility. If the
problem cannot be reproduced, chances are that the factory will not be able to find it.
When calling OI Analytical Customer Support, be prepared to answer the following:

Explain the error in as much detail as possible.

List the exact text from the error message.

What was the software doing when the error occurred?

What did you expect to happen instead of the error?

Can you cause it to happen again? If yes, how?

How many times did this exact error occur?

What software revision and firmware are used? (Find this in the About menu.)

How many channels are used?

What is your computer type and processor speed?

How many MB or RAM?

What operating system are you using (e.g., Windows 98, 2000, NT, XP)?

You may be asked to submit copies of the following files:

Sample table (*.tbl) on which the run is based

Method (*.mtd) on which the run is based

Result file (*.rst) that was generated or being used

WinFLOW.ini file

All files with this type of name: debugXX.txt

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