Lc-10ad Im Rev0oc

228-10743
SOLVENT DELIVERY MODULE LC-1OAD FOR SHIMADZU HIGH PERFORMANCE LIQUID CHROMATOGRAPH
INSTRUCTION MANUAL
SHIMADZU CORPORATION
A N A LYT IC A L INSTRUM E N S DlVlS ION T
KYOTO, J A P A N
CONTENTS
Caution
General 1.1 Outline ............................................................................................................ 1.2 Features .......................................................................................................... Details of Parts 2.1 Details of Parts ............................................................................................... Construction and Function 3.1 The Front ........................................................................................................ 3.2 The Rear ......................................................................................................... 3.3 The Right Side and Bottom ............................................................................ Installation 4.1 Conditions for Installation Location .............................................................. 4.2 Examples of System Configuration ............................................................... 4.3 Unscrewing Fixing Screws for Transportation .............................................. 4.4 Mounting of Multiple Modules ...................................................................... 4.5 Electrical Connections ................................................................................... 4.6 Tubing of the Module ..................................................................................... .. 4.7 Connecting the Degasifier .............................................................................. 4.8 Mounting the Mixer ....................................................................................... 4.9 4.10 4.11 4.12 Connections of the Injector. Column, and Detector ...................................... Installation of High Pressure Gradient Delivery System .............................. Installation of the Low Pressure Gradient Delivery System ......................... Installation of the Automatic Washing Kit .....................................................
1-2 1-3
2-2
3
.
3-2 3-4 3-5
4-2
4-3
4-6 4-7 4-8 4-9 4-12 4-17 4-21 4-24 4-27 4-30
Operation 5.1 Basic Operation .............................................................................................. 5.2 Operation of Constant Flow Solvent delivery ............................................... 5.3 Operation of Constant Pressure Solvent delivery .......................................... 5.4 Creation of Time Programs and Execution .................................................... 5.5 AUX . Functions ............................................................................................. 5.6 High Pressure Gradient Delivery Mode ........................................................ 5.7 Low Pressure Gradient Delivery Mode ......................................................... 5.8 Operation of Automatic Washing Kit ............................................................ 5.9 Operation of Manual Washing ....................................................................... 5.10 Replacement of Mobile Phase .......................................................................
5-2 5-7 5-10 5-11 5-17 5-26 5-28 5-29 5-30 5-31
. .
Performance: Checking 6.1 Operation Checking for Systems ................................................................... 6.2 Checking; Concentration for High Pressure Gradient Delivery ..................... 6.3 Checking Concentration for Low Pressure Gradient Delivery .....................
6-2 6-5 6-7
Control from External Equipment 7.1 Connection of the Input/Output Terminals for External Equipment ............. 7-2 7-4 7.2 Control from the SCL-1OA ............................................................................ Maintance 8.1 Replacement of Plunger Seal ......................................................................... 8.2 Replacement of Plunger and Diaphragm ....................................................... 8.3 Cleaning and Replacement of Check Valves ................................................. 8.4 Replacement of Line Filter ............................................................................ 8.5 Replacement of Fuse ...................................................................................... 8.6 Cleaning ......................................................................................................... Troubleshooting Symptoms and Countermeasures for Troubles .............................................. Error M~:ssages ...............................................................................................
8-2 8-4 8-6 8-7 8-8 8-9
9.1 9.2 10
9-2 9-4
Specification 10.1 LC-1OA:D Unit Specifications ....................................................................... 10.2 High Pre:ssure Gradient Specifications .......................................................... 10.3 Low Pressure Gradient Specifications ........................................................... Spare Parts and Optional Modules 11.1 Consumable Parts List ................................................................................... 11.2 Lists of Other Necessary Parts ....................................................................... 1 1.3 Optional Modules List ................................................................................... Reference Material 12.1 Precautions on Static Electricity .................................................................... 12.2 Mobile Phase Characteristics .........................................................................
10-2 10-3 10-4
11
11-2 11-3 11-4
12
12-2 12-6
High performance liquid chromatographs, which use large volumes of solvent in general, need good care in handling and proper selection of an installation site. Be sure to take care for the precautions that follow of course and for each of those appear in this document.
1.
Ventilation
Solvents used in high performance liquid chromatographs are often inflammable and toxic, therefore the room in which they are used must be well ventilated.
2.
Fire
Never use an open flame in the vicinity of a high performance liquid chromatograph. Do not install other equipment that may generate sparks in the same room. Install fire extinguisher in case of fire hazard.
3.
Static charge
As well, static charge is a hazard that may be the cause of inflammation. Appropriate measures should be taken. See "Section 12.1 Precautions on Static Electricity."
4.
Protective goggles Other facilities required
Wear protective goggles when handling solvents.
5.
Install a sink as close as possible to the module so that toxic solvents may have splashed in the eyes or skin may be immediately rinsed off.
6.
Power source
Each section of the module uses many types of voltage including commercial power source. As maintenance may in general be carried out with the main cover closed, do not open the cover. If you need to open the cover, be sure to contact our branch office.
7.
Other considerations
Avoid installing the instrument in direct sunlight. It is also recommended that installation be in a place where variations in ambient temperature are at a minimum.
;
G
E
Chapter 1
General
1.1
1.2
Outline ...............................................................................................................................
Features .............................................................................................................................
1-2
1-3
1-1
LC-1OAD
0w t Iine
7
The LC-1OAD is a solvent delivery module with a double plunger reciprocating pump, which has been developed for improving accuracy and sensitivity, for use in a high-performance liquid chromatograph. Other than a solvent delivery module, a high performance liquid chromatography system needs an automated or manual injector, column, injector holder, and detector that are all supplied as optional special accessories. Note that this instruction manual covers operations for LC-1OAD and relevant accessories alone. For usage of the special accessories, please refer to the independent instruction manuals for each module.
1-2
LC- 1OAD
Im
1.
Features
Compared with conventional models, magnitude of flow pulsation is significantly reduced, and pulsation cycle is shortenednoticeably.This has been made possible by reducing discharge capacity to a micro volume of lop1 per plunger stroke and by high speed driving of the plunger. These features allows detectors such as differential refractometers and electrochemical detectors that are sensitive to flow pulsation, to be used in a range of high sensitivity. In a semi-micro volume range as well, unprecedentedly accurate gradient delivery has become possible.
Solvent Delivery of Ultra LOW Flow Pulsation and High Accuracy Gradient Delivery
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2.
A Variety of Functions for Gradient Delivery
Two gradient delivery modes, low and high pressure modes, are available. The high pressure gradient delivery mode is highly accurate and allows a minimum time lag, while the low pressure gradient delivery mode can handle solvent delivery of up to four liquids at a low cost. In addition, control of these gradient delivery modes is carried out in two types of system setup. One is to use system controller SCL-IOA, and the other is to control gradient delivery from the LC- 1OAD, without using any system controller.
3.
A Measure for Buffer Solution
The automatic washing mechanism at the back of plunger seal cleanses plunger automatically. When using a buffer solution of high salt concentration as the mobile phase, the mechanism effectively allows a longer life for the plunger seal.
1-3
LC- 1OAD
Chapter 2
Details of Parts
Contents
2.1
Details of Parts ................................................................................................................
2-2
2- 1
LC-1OAD
Details of Parts
1
The LC- 1OAD is composed of the following parts.

1.
LC-1OA Main Body
2.
Standard Accessories
category
Parts
I
Suction filter Drain tube kit
Part Name
Powercord (100/115V) or Power cord (220/230/240V)
PartNo.
071 -608 14-01 07 1-608 14-02 228- 18740-91 228-28161-91 228-10742 228- 10743 228-15084-91
Qty
1
1 1
Accessories
Instruction manual
(Japanese version) or (English version)
1
1
Accessory pack (See the following page.)
2-2
LC-I OAD
13.
Details o Parts f
Accessory Pack
Spilap
Syringe
Remote cable
018-26002
0.2m
1
046-00038-01 228-28253-9 1
2-3
LC-1OAD
Chapter 3
Construction and Function

U
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Contents
3.1
The Front ..........................................................................................................................
3-2
3.2
The Rear ...........................................................................................................................
3-4
3.3
The Right Side and Bottom ..........................................................................................
3-5
3-1
Thie Front
7
1.
The front
P
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flow/press pressure p.rnax
p.min
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Oh 1
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Description
Operation panel Front cover Drain valve lever Front cover opening button
Setting is made through this panel. Covers the flow line. The lever open/closes the drain valve. Press this button to open the front cover.
3-2
LC- 1OAD
12.
TheFront
Inside the Front Cover
No.
Name of Part
Pump head holder Pump head Washing tube A Check valve IN Pump inlet Washing tube B Pump outlet Line filter Drain valve Drain tube connection Check valve OUT on the holder.
Description
Has a flow line that washes the plunger. The pump head is mounted The plunger reciprocates in the pump head to deliver liquid. The suction filter is connected to this inlet. The check valve at the inlet. The suction filter is connected to this inlet. The tube is connected to the washing flow line. Piping to the injector is connected to this outlet in general. Protects columns from clogging. Used to replace mobile phase and to bleed air in the flow line. The valve has a built-in sensor. Drains waste from the drain valve. The check valve at the outlet.
a
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0
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0
3-3
The Rear
7
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3
C
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s
No. Parts Name
External input/ciutput terminal block Grounding tern inal Power cord connector Fuse holder
Description
Used to make connection with external equipment. Use this terminal for grounding the module. Used to connect a power cord.
a
0 @
6)
@
S0L.V connectx
A fuse is put in the holder. Use to connect a solenoid valve. See "Section 4.1 1.1 Wiring with
FCV- 1OAL." Used to connect with SCL-IOA or an additional LC-IOAD. See "Section 4.10 Installation of the High Pressure Gradient Delivery System."
REMOTE connector
3-4
LC- 1OAD
EQ
The Right Side and Bottom
No.
Name of Part
Drain opening for liquid leakage Mixer mounting screws Cooling fan Fixing screws for transportation
Description
See instruction manual for the drain tube kit. Mount here a mixer or manual injector. Used to cool inside of the module. Fix components in the module. See "Section 4.3 Unscrewing Fixing Screws for Transportation."
a
0
@
3-5
LC- 1OAD
Chapter 4
Installation
contents
4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9
Conditions for Installation Location ............................................................................... Examples of System Configuration ................................................................................ Unscrewing Fixing Screws for Transportation .............................................................. Mounting of Multiple Modules ...................................................................................... Electrical Connections ...................................................................................................... Tubing of the Module ..................................................................................................... Connecting the Degasifier ............................................................................................... Mounting the Mixer ......................................................................................................... Connections of the Injector, Column, and Detector ....................................................
4-2
4-3
4-6 4-7 4-8 4-9 4-12 4-17 4-2 1 4-24 4-27 4-30
4.10 Installation of the High Pressure Gradient Delivery System ..................................... 4.1 1 Installation of the Low Pressure Gradient Delivery System ...................................... 4.12 Installation of the Automatic Washing Kit ...................................................................
4-1
LC-1OAD
rnE
1. 2.
Conditions for Installation Location

For correct and safe use of the module, care should be taken for the following, when installing the module.
Environmental Conditions To assure long service life and good performance of the module, avoid installing in a place where corrosive gases or dust are present. Precautions on Ventilation and Fire
0
Be sure to ventilate the room when inflammable or toxic solvents are used as mobile phases. Never use open flames in the room particularly when inflammable solvents are used.
3.
Electromagnetic IUoise
Avoid installing in a vicinity of such equipment that generates a strong magnetism. Use an additional noise filter if the power line has much noise. The module is designed to be used on a table or stand, which should preferably be a solid and flat, having a minimum depth of 60cm. See "Section 4.2 Examples of System Configuration" for typical configurations of systems and installation spaces. LC-IOAD is not designed in consideration of the safety regulation for medical equipments. Therefore LC-lOAD can not be used in the patient environment*. * Patient environment: The area within a distance of 2.5m from patients. For a longer service life, give proper considerations to conditions that follow, when selecting an installation location. (1) Room temperature should be in a range of 5 to 35C. Variation in temperatures in a day should be minimum.
(2) (3) (4)
4.
Installation Space Requirements
5.
Use in the patient environment
<<Cautions>>
Avoid any direct below from a heater or cooler. Avoid installing the module in direct sunlight. No vibration is allowed.
4-2
LC- 1OAD
m
1.
Examples of System Configuration

The following shows examples of system configuration for a high performance liquid chromatograph incorporating the LC- 10AD.
Simple System
An example of simple system configuration. It includes a degasifier, column oven, detector, etc. that make a minimum set of modules needed for stable analyses.
Detector (SPD-1OA)
Column oven (CTO-1OA) Manual injector (7125) Pump (LC-1OAD) Reservoir box Degasi f i e r (DGU-4 . A ) Chromatopac (C-RGA)
Approx. 540mm
2.
LOW Pressure Gradient Delivery System 1
An example of configuration of low pressure gradient delivery system for manual sample injection. The system is highly economical and allows handling solvent delivery of up to four liquids.
Detector (SPD-1OA) Reservoir box Column oven (CTO-1OA) Manual injector (7125)
Degasifier (DGU- 3A) Option box S L o w pressure gradient delivery module (FCV-1OAL)
atopac ( C-R 6A)
4-3
LC- 1OAD
3.
Low Pressure Gradient Delivery System 2
A low pressure gradient delivery system including an automatic injec-
tor controlled by the system controller SCL-1 OA. Centralized control of each module is available through the use of the system controller allowing great ease of operation. The system can also readily be used for automatic analyses.
System controller (SCL-1OA) Fleservoi r box Detector (SPD-1OA) Column oven (CTO-1OA)
Degasifier (DG U-1OA) Syringe module
module (FCV-1OAL) Pump (LC-1OAD)
1 -
Approx. 800mm-I
4.
High Pressure Gradient Delivery System -1
An example of configuration of high pressure gradient delivery system for manual sample injection. The LC-1OAD high pressure gradient delivery system allows highly accurate gradient analyses with a minimum time lag.
Detector (SPD-1OA) Column oven (CTO-1OA)
Reservoir box Manual injector (7125)
Dega:,if i e r ( D G U -4A)
Pump (LC-1OAD)
C - 2 6 0 d
LApprox. 540mm
I,601,
\ d u m p (LC-1OAD)
4-4
LC- I OAD
15.
Examples of System Configuration

High Pressure Gradient Delivery System 2
A high pressure gradient delivery system including an automatic injector controlled by the system controller SCL- 10A. In contrast with High Pressure Gradient Delivery System 1, functions such as automatic sample injection, cooling sample, and selecting mobile phases are available with this system allowing flexible use for wider analyzing purposes.
System controller (SCL-1OA) Reservoir

~
Detector ( S P D-IOA)
Reservoir b o x A u t o m a t i c injector ~
C o l u m n oven (CTO-1OA)
uux
7
L n r o m a r o p a c (C-R4A)
UII
II
Yl
'I
SamDle cooler Mixer ,
Resevoir selector valve
A p p r o x . 800mm P u m p (LC-1OAD)
4-5
LC-1OAD
Urrscrewing Fixing Screws for Transportation

1
The module uses fixing screws for transportation to protect the module from shocks generated during transportation. Be sure to unscrew the fixing screws before use.
(1)
Unscrew the two fixing screws for transportation shown in the following illustration using the accessory allen wrench.
Fixing screws for transportation
<<Caution>>
If you use the module without removing the fixing screws, noises will be generated as a result of pump vibrations transmitted to the whole body of the module.
4-6
LC-IOAD
Em
Mounting of Multiple Modules

The module may be stacked on another for use. Detector SPD-IOA, column oven CTO-10A, automatic injector SIL-10A, etc. may also be stacked on the module. When stacking the modules for use, it is possible to fix modules together as a means to prevent from falling down at an earthquake or the like. The modules should be fixed using the accessory mounting plate.
(1) (2)
Unscrew the screws that are used to fix module cases. Use the screws unscrewed to fix the mounting plate.
Mounting plate
Screws
4-7
LC-1OAD
mK
1.
Electrical Connections
Before plugging in, check the points that follows: Source Voltage and Capacity Parts number 228-25000-9 1,92 90- 130V - lOOVA 50/60Hz Parts number 228-25000-93 200-25OV - lOOVA 50/60Hz If the source voltage is unstable or the capacity is short, the module cannot provide good performance. Make also sure that the capacity of power outlet is sufficient for overall system.
0
--.
Make sure that the power switch on the module is turned OFF. Plug in the female end of the power cord to the power supply connector on the back of the module. Connect the male end to the power outlet.
7
Connection to the Power Outlet
(1)
4-8
LC- 1OAD
Tubing of the Module

-
1.
Preparation of Reservoir
Prepare a reservoir of capacity 500ml at the minimum. We recommended use of a thick walled heat resistant screw capped glass container of 550ml liquid capacity.
2.
Removing the Front Cover To set the flow line of the module, remove the front cover.
( 1)
(2)
Press the opening button to open the cover. The cover may be removed by pulling it while widening the hinge as shown in the illustration below.
Pump inlet (Bush for transportation)
3.
Connecting the Suction Filter
(1)
(2) (3)
(4)
(5)
Remove the bush mounted on the inlet on the module front. (Reserve the bush so as to use it to protect the module from mixing of any foreign matter when it is not used for long.) Remove bush 3D from the suction filter tube. Cut the tube to an appropriate length according to the distance from the reservoir and pump inlet. Put the filter in the reservoir as shown in the following illustration and set the lid having four holes and the cap. Reset bush 3D to the tube. Connect bush 3D of the suction filter to the pump inlet.
4-9
LC-1 OAD
-/big
of the Module
(6)
Fix the tube using the tubing cramp as shown in the illustration below.
Bush 3 0
&
Remove bush 3D. Suction filter
Suction filter
Tubing cramp
<<Cautions>>
0
0
The greatest care should be taken not to tighten the bush excessively. Avoid getting the filter dirty. For constantly stable analyses, the mobile phase in the reservoir shall be degasified. See "Section 4.7 Connecting the Degasifier." Remove the bush mounted on the drain tube connector. Mount the accessory drain tubing's bush 3D to the connector. Prepare a container for drainage and put in the other end of the drain tube.
4.
Connecting the Drain Tube (1)

(2)
(3)
4-10
LC- 1OAD
m / - r u t i s of the Module
(4)
Fix the tube using the tubing cramp as shown in the illustration below.
Screw the bu
\
\ \
Tubing cramp Put the waste container on the floor o r the like so that it i s placed at a lower level than the module is.
5.
Connection of the Drain Tube for Liquid Leakage
If a liquid leaks in the module, it accumulates on a pan at the bottom of the module. Connect the tube for liquid leakage to discharge the leaked liquid. Refer to the instruction manual of the drain tube kit for connecting the tube.
<<Caution>>
Install the drain tube before mounting the mixer or column holder.
F i t the tube.
&
for l i q u i d leakage
Waste container
4-11
LC-1OAD
Connecting the Degasifier

?
Degassing the mobile phase has two effects that follow and is needed for constantly stable analyses. (1) It prevents troubles caused by generation of bubbles. (2) It prevents unstable measurements due to variation in the quantity of dissolved gas. Major degassing methods include helium degassing and vacuum degassing using resin membrane. Choose from these according to your analyzing purposes. See "Section 11.3 Optional Modules List." For examples of typical method, each connection will be shown using the DGU-2A and DGU-3A. The former is for the helium degassing, and the latter, vacuum degassing using resin membrane.
1.
Connection of the DGU-2A Use helium gas of high purity (99.995% or higher) for degassing. (helium degassing) (1) For tubing, set a pressure reducer (optional) and carrier gas pipe between the helium gas cylinder and the DGU-2A.
"
He GAS IN
"
Helium gas inlet
Helium gas c:ylinder
(2)
For reservoir, prepare a thick walled heat resistant screw capped glass container. (A commonly used glass reagent container of capacity 500 or 1000ml).
<<Caution>>
Never use a container with a crack or flow for reservoir.
4-12
LC-1OAD
(FrCorlnect
ing the Degasifier

(3)
Assemble the reservoir cap as shown in the illustration.
To DGU-2A
To the
inlet
-0
Category
Part Name
Bottle cap Lid Teflon packing Teflon tubing Teflon tubing Filter section of the suction filter Helium gas bubbling filter Teflon tubing Outer lid of the reservoir Inner lid of the reservoir Packing for the inner lid
Description
c 3 0
@
0 8
a
0
3.0~2.0~230 3.0x2.0 Connected to the pump inlet. Used to filter the mobile phase. Helium gas bubbling filter 3 x 2 ~ 6 0 0 be connected to an "OUT' (A, B, C, D) port of the To DGU-2A. 3 x 2 ~ 6 0 To be connected to an "IN" (A, B, C, port of the DGU-2A. 0 D)
Parts @ and @ above a::e accessories for the LC-1OAD. Parts of other numbers are accessories for the DGU-2A.
4-13
LC- 1OAD
p n n e c t i n g the Degasifier
(4)
Put the mobile phase in the reservoir. Put also the filter component assembled in (3) in the container, then fiimly close the cap.
T O DGU-2A
To pump inlet
(5)
Remove stop joints set to DGU-2A ports with which you will make connection. Connect Teflon tubing led from the reservoir to an OUT (A, B, C, or D) and IN (A, B, C, and D) ports of the DGU-2A, as shown in the illustration that follows. Keep unused ports being covered with stop joints. Reserve the removed stopjoints, which will be needed to protect the degasifier from mixing of dust in flow line when it is not used for long.
Helium gas
4-14
LC- 1OAD
FCorlnecting the Degasifier

2.
Ventilation of Helium Gas
(1)
Prepare a glass container. Fill it with a solvent that is miscible with the mobile phase. Connect the one end of the accessory Teflon tubing to the VENT port of the DGU-2A. Put the other end in the container and cover the container neck with an aluminum foil. Place the container near a ventilating fan or window so as to release the gas from the DGU-2A outside the room.
(2)
(3)
5;g
I
Ventilating fan
Ventilation f r o m the D G U - 2A
Aluminum foil
1' 1 37
'
"
Solvent miscible w i t h the m o b i l e phase
3.
Tubing of the DGll-3A
(1)
Carry out tubing from the reservoir to the DGU-3A and from the DGU-3A to the LC-1OAD module, as shown in the illustration below. Before tubing, remove stop joints set to DGU-3A ports with which you will make connection. Keep unused ports being covered with stop joints. Reserve the removed stopjoints, which will be needed to protect the degasifier from mixing of dust in flow line when it is not used for long.
DGU- 3A
Connect these tubes

to the pump inlet.
\
11 '
k Use bushes 3 0 t h a t
are accessories f o r the DGU-3A Bushes 3D t h a t are accessories for the suction f i l t e r m a y a l s o be used.
Accessory Teflon t u b i n g included i n the DGU- 3A

U s e bushes 3D that are accessories
f o r the DGU- 3A
4-15
LC-1 OAD
4.
When Connecting the By connecting the FCV-1OAL to the module, low pressure gradient DGU-3A to the FC'V-1OAL: delivery is available. If you use the DGU-3Afor degassing the mobile
phase in such low pressure gradient delivery, follow the instructions below:
(1)
For binary or ternary gradient delivery For ternary gradient delivery, as shown in the illustration below, connect mobile phases flow lines via the degasifier to the A, B, and C ports of the FCV-10AL. Note that unused flow lines of the FCV-IOAL should be covered with stop joints.
(2)
Quaternary gradient delivery Use two modules of the DGU-3A and make connections as follows:
DGU- 3A
0 3
0 2
IN
OUT L C - 1O A D
---.
=To injector
oc
00 - - - A - - a
IN OUT DGU- 3A
F C V - 1O A L
Mobile vhase
<<Cautions>>
To replace solvent in the degasifier, be sure to suck the degasifier. Never conduct operations that give it a pressure. After using a buffer solution for mobile phase and if it is expected that the degasifier will not be used for long, wash inside the degasifier thoroughly by distilled or deionized water (in this case also, only suction by pump or the like is allowed). Then run methanol for replacement. Finally, fit stop joints on the IN and OUT ports for storing.
4-16
LC-1 OAD
m F u n t i n g the Mixer
For gradient delivery using the module, a special mixer (P/N 22828000-9 1, optional) that is excellent in mixing solvents is available. Follow instructions below for mounting the mixer and selecting mixer capac icy.
1.
Mounting Position
The mixer may be mounted on either of the following positions. (1) The right side face of the module (2) The left side, inside the CTO-1OA (3) The right side, inside the CTO-IOA Options from three types of mixer capacity that follow is available. Select the right mixer capacity according to your analyzing purposes. (1) 0.5ml (2) 1.7ml
2.
Mixer Capacity
0 .c
Q
(3)
2.6ml
U J C
Q c
3.
Selecting Mixer Capacity
Selection of mixer capacity is made by altering tubing. When it is shipped in a standard manner, it is set to 2.6ml. To change the setting, follow the instructions below: (1) Remove the mixwe cover.
Screw
Cover
Screw Screw
4-17
(2)
According to the desired capacity, change tubing as shown in the following illustration:
(A) Tubing for 0.5ml
(B) Tubing for 1.7ml
(C) Tubing for 2.6ml
To the injector inlet T o the injector inlet

T o the injector inlet
Remove tubing and fit caps for dust prevention.

U
4.
Mounting on the Module
(1)
Move the pre-mixer section and fasten it by screws as shown in the following illustration:
Pre-mixer
position when shipped
Move i t to the left
c3
Unscrew the screws Refasten the screws.
(2)
Unscrew the screws on the right side of the module, and use the screws to mount the mixer, as shown below:
\
-.
Y
Unscrew the screws
Refasten the screws
4-18
LC- 1OAD
-punting
the Mixer
(3)
Carry out tubing between the mixer and injector referring to "Section 4.10 Installation of the High Pressure Gradient Delivery System" or "Section 4.11 Installation of the Low Pressure Gradient Delivery System." Remount the mixer cover.
Screw
(4)
0 .-
I
The pre- mixer section appears outside the cover.
5.
Building the Mixer into CTO-1OA (mounting)
Mount the mixer on the inner side face of the CTO- 10A, using the accessory screws as shown in the illustration below. The mixer is typically mounted on the position indicated in (A). Note, however, that when mounting manual injector model 7125 with position sensor, on the CTO-IOA, the mixer should be mounted at the position shown in (B).
5 mm
1 0 1
4-19
LC-1OAD
(A)
Mounting on ,the left side
(B)
Mounting on the right side (In contrast with mounting it on the left side, the mixer is mounted up side down.)
Yew I1 i
+Pre- mixer
'
4-20
LC-1OAD
Connections of the Injector, Column, and Detector
Examples of connections of systems using this module will be described. The following examples of connections apply to the basic system shown in the illustration below. Connections should be made according to each system, referring to the examples. For the method of mount the manual injector model 7 125 and acolumn
on the column oven CTO-lOA, refer to the instruction manual for the column oven. If not using the column oven, an injector holder and column holder (optional) are available for mounting the manual injector model 7 125 and column.
1.
Connection of the Manual Injector
Taking the case of connection between the module and manual injector model 7 125, the connection will be described. Cut the accessory SUS pipe 1.6xO.3 to the length needed for piping from the pump outlet to the injector port 2. Mount male nuts and ferrules on both ends of the SUS pipe. Fit the male nut 1.6MN and ferrule 1.6F that are accessories for the module at the pump outlet end of the SUS pipe, also fit the male nut and ferrule that are accessory of the manual injector at the other end that is to be connected to the manual injector model 7125. Connect these ends of the SUS pipe to the pump outlet and injector.
<<Cautions>>
The discharging pipes are connected to port 5 and 6 of the manual injector model 7125. The other ends of the discharging pipes should match the injector height. For connections to No. 1 to 6 of the manual injector model 7 125, use male nuts and ferrules that are accessory of the model 7 125.
, -
The manual injector rear view Injector holder
4-2 1
2.
Connection between the Injector and Colunnn
The following is an example of a typical connection between the manual injector model 7 125 and column.
(1)
(2) (3) <<Cautions>>

0
Cut the accessory SUS pipe 1.6x0.3 to the length needed for piping from the injector to the column. Fit male nuts and ferrules at both ends of the SUS pipe. Connect these ends of SUS pipe to the injector and column. In order to allow a minimum dispersion of the sample, set the piping between the injector and column as short as possible. Cut the pipe in such a manner that the sectional face is perpendicular to the pipe axis. Ensure that the connection generates no dead volume.
C y l i n d r i c a l section Cut the pipe perpendicular t o the axis
Male nut 1.6MF
Ferrule 1.6F
r-----
CTO-1QA
-- ---
,
T o the detector
The m a n u a l injector rear view
I I
4-22
LC-1OAD
m p m e c t i o n s of the Injector, Column, and Detector

3.
Connections between Column and Detector
Taking the case of using the detector SPD- 10A, connection between column and detector will be described.
(1)
(2)
(3)
Cut the ETFE tube 1.6xO.3 that is an accessory of the SPD-1OA to the length needed to make connection from the column outlet to the cell inlet of the SPD-1OA. Fit male nuts PEEK at both ends of the ETFE tube. Connect both ends of the ETFE tube to the column outlet and cell inlet (with a blue mark) of the detector, as shown in the following illustration. See cautions for "Section 4.9.2 Connection between the Injector and Column."
0 .c
Q
Coupling Pipe f r o m the inlcst of SPD-
Column
c .
v)
I
Male nut PEEK ETFE tube (Fasten man ua I Iv.)
F r o m the manual injector
4-23
of the High Pressure

System
' 7
The high pressure gradient delivery systems using LC- lOAD are available in two types of configuration characterized by its control method. A high pressure binary or ternary gradient delivery system controlled from the system controller SCL- 10A. Ahigh pressure binary gradient delivery system without system controller. The installation for each type of these configurations will be described in the following paragraphs.
1.
Wiring for Control through (1) the SCL-1OA
Connect the REMOTE connector on the rear of the module and the REMOTE connector on the rear of the SCL- 10A using the optical cabke included in accessories for the module. The ADRS parameter of each LC-1OAD shall be set to the channel number to identify which channel is used for the connection with the SCL-IOA. (See "Section 5.5 AUX.FUNC Functions.")
rear view
/
,/ '
Connect the cable to either of channels f r o m 1 to 8.
4-24
LC-IOAD
-pillation
2. Wiring for Control by Two Modules of the LC-1OAD
of the High Pressure Gradient Delivery System
(1)
Connect two modules of LC-1OAD at the REMOTEconnectors on the rear panel, using the accessory optical wiring cable.
The LC-1OAD rear view
" ,
, ,
Optical cable __
(2)
Set 85 to the ADRS parameter of each LC-10AD. (See "Section 5.5 AUX.FUNC Functions.")
3.
Piping of the High Pressure Gradient Delivery System
As a piping example, piping of two modules of LC-lOAD, degasifier,
and mixer that construct a binary high pressure gradient system will be described.
LC- 1 O A D
M I xer
V' Mobile phases
L C - 1O A D
Carry out piping referring to the following connection method.

(1)
(2)
Prepare a reservoir. Because degassing mobile phases is needed for stable gradient delivery of good reproducibility, carry out piping up to the pump inlet referring to "Section 4.7 Connecting the Degasifier." Referring to "Section 4.8 Mounting the Mixer," mount the mixer.
4-25
LC-1OAD
~
-/tallation
of the High Pressure Gradient Delivery System
(3)
When mounting a mixer on the module, make connection of the LC-1OAD and mixer inlet as shown in the following illustration. First remove caps on inlets A and B at the pre-mixer section, and carry out piping from the outlets of each LC-1OAD to the mixer, using the accessory SUS pipe 1.6x0.3. For ternary gradient system, remove the stop joint on inlet C and carry out piping from the inlet C to the pump outlet of the third LC-1OAD.
LC-1OAD
I injector
Pre- mixer sect Inlet B
(4)
(5)
Connect the injector and the mixer outlet by the SUS pipe 1.6x0.3. Mount the cover referring to "Section 4.8 Mounting the Mixer."
4-26
LC- 1OAD
of the Low Pressure System

This module allows configuration of the low pressure gradient delivery systems that can handle up to four liquids, using the low pressure gradient module FCV-10AL. The installation of the system is described in the following paragraphs.
1.
Wiring to the FCV-1OAL
(1)
(2)
Using the cable included in the accessories for the FCV-lOAL, connect the FCV-IOAL and the S0L.V connector on the rear of the module. Fasten the fixing screws on the connector of the module with screw driver. The FCV- lOAL end of the cable has a flat cable connector. As such, fixing by screw is not necessary for the
FCV- 1OAL.
Screws
Cable
FCV-IOAL
rear view
<<Cautions>>
Before connecting the cable, make sure that the power switch of the module is turned off. In order to reduce dead volume in the flow line, allowing a minimum time lag for gradient delivery, install the FCV- 1OAL as closer to the LC-1OAD as possible.
4-27
LC-1OAD
2.
Tubing of the Lowf Pressure Gradient Delivery System
Carry out tubing referring to the following connecting method. Prepare reservoir containers. Because degassing of the mobile (1) phases is needed, carry out piping to the inlet joints of the FCV-lOAL, refemng to "Section 4.7 Connecting the Degasifier." The FCV-1OAL has four inlet ports (from A to D). If not every port is used, remove the tube corresponding to the unused flow line, from the inlets (from A to D) of the 5-way branching block. Then, be sure to fit the stop joints included in the accessories for the FCV-1OAL. (2) Cut the tube included in the accessories for the FCV-IOAL to an appropriate length, and use it to connect the outlet of the 5-way branching block and the pump inlet of the module.
0
<<Caution>>
If not every flow line is used, be sure to fit stop joints on inlets (from A to D) of the 5-way branch block, which correspond to the unused flow line. If any inlet is kept open without mounting stop joint, correct gradient delivery is not available.
Accessory tube
5-way branching block
Suction f i l t e r
4-28
LC-1OAD
p a l l a t i o n of the Low Pressure Gradient Deliverv Svstem - -
Mount the mixer referring to "Section 4.8 Mounting the Mixer." After mounting the mixer, connect the module and inlet of the mixer as shown in the illustration. First, remove SUS pipes A and B from the module. Remove the stop joint (SUS) from the inlet C of the mixer. Fit the stop joint on the connection opening for SUS pipe A of the module. Remove the line filter from the module, and with an allen wrench, firmly fix the drain stopper included in the accessories for the mixer. Connect the module to each connection port on the mixer as shown in the following table.
Check valve OUT B
Inlet C
For the pipes used for connection, cut the SUS pipe 1.6xO.5 included in the accessories for the mixer to an appropriate length. Connect the injector and the mixer outlet with the accessory SUS pipe 1.6x0.3. Mount the mixer cover referring to "Section 4.8 Mounting the Mixer."
S U S pipe A
'\
\ ,
Connection p o r t for line f i l t e r
sus pipe
'
SUS pipe B
Check valve OUT A -
Check valve
ou
sus
,
Inlet B
4-29
Installation of the Automatic Washing Kit

I
Fill distilled water four-fifths full into the conical flask included in the accessory for the automatic washing kit and set the kit to the flask. Connect the Tygon@tube 200mm long included in the accessories for the automatic washing kit, between the washing tube A on the left and washing tube B on the right, as shown in the illustration. Connect the Tygon@tube of the inlet of the automatic washing kit to the washing tube A on the right, and the Tygon@tube of the outlet of the automatic washing kit to the washing tube B on the left, respectively.
(/
Washing tube B on the left Automatic washing k i t

I
I
1, 3
A
Teflon tube Washing tube B on the r i g h t

h..
Outlet
\ ,
, '
&\d,
7 -
Washing tube A on the left
<<Caution>>
Connection of each tube must be carried out according to the illustration above. If you conducted a wrong connection, the service life of diaphragm in the module may become short. Do not pull roughly washing tube Aand B sticking out of the pump head and each tube set o the automatic washing kit. If pulled excessively, they may come off.
4-30
LC-1OAD
Chapter 5
Operation
5.1
5.2 5.3
5.4
5.5
Basic Operation ................................................................................................................ Operation of Constant Flow Solvent delivery ............................................................. Operation of Constant Pressure Solvent delivery ........................................................ Creation of Time Programs and Execution .................................................................
AUX. Functions ...............................................................................................................
5-2
5-7
5-10
5-11
5-17 5-26
5.6
High Pressure Gradient Delivery Mode .......................................................................
5.7
5.8
Low Pressure: Gradient Delivery Mode ........................................................................

Operation of Automatic Washing Kit ........................................................................... Operation of Manual Washing ....................................................................................... Replacement of Mobile Phase .......................................................................................
5-28
5-29
5-30
5-3 1
5.9
5.10
5-1
LC- 1OAD
-~
Basic Operation
7
To operate the module, use keys on the operation panel. The status of operation may be checked on the display at any time. When using the SCL-10A for control, see "Section 7.2 Control from the SCL-IOA."
1.
Turning the Power On
(1)
Press the power switch located at the lower left of the front panel to switch power on. The power is turned off by repressing the switch.
0 .c E
Power switch OFF state
Power switch ON state
Q)
(2)
When power is turned on, the memory is automatically checked. If no abnormality exists, version No. of the ROM will be displayed for a while and then the display will show as indicated in the following illustration, and the module is ready for operation. This is the initial state.
flow/press
pressure
p.max
p.min
\ \ I / /
Ilo.000
v /I
pump
0 10 0
&ow
0 1
I
\ \
cpress
prog run remote
<<Caution>>
If an error message is displayed after switching power on, see "Section 9.2 Error Messages" for measures.
5-2
LC- I OAD
m
2.
Operation
The display has the display screen and LED lamps, whose names and functions are as follows:
Description of the Display
No.
Indication or Name
flow/press
Function
Indicates a set flow rate (ml/min) when the module is in the constant flow delivery mode, and a set pressure value (kgf/cm*), in the constant pressure solvent delivery mode.
pressure p.max p.min Pump
A pressure value measured by the pressure sensor (kgf/cm)
Maximum pressure limit (kgf/cm) Minimum pressure limit (kgf/cm) Pump operation indicator lamp The lamp is lit when the pump is in operation. Programmed operation indicator lamp The lamp is lit when a program is running. REMOTE mode indicator lamp Flashes when controlled by the SCL-IOA. Constant flow solvent delivery mode lamp The lamp is lit when the module is in the constant flow solvent delivery mode. Constant pressure solvent delivery mode lamp The lamp is lit when the module is in the constant pressure solvent delivery
prog run remote c.tlow c.press
5-3
LC- 1OAD
~
Bs )ai c
3.
Operation
The module has 20 keys on the front panel which are used for operation and setting. Functions of each key are as follows.
Description of Keys
edit
(pump) Pumpkey 1
\ -
Key for start/stop of the pump. Press this key to start the pump. By pressing this key during operation the pump stops. Key for start/stop of purging. Press this key to start purging. By pressing this key or pump key during operation, purging stops or it stops automatically in 3 minutes.
[m) Purgekey
i
0,
(del) Delete key

ledlt) Edit key
Deletes one line in the program displayed during time programming. Shifts to the edit mode of time programming. Key for stadstop of a time program. Sets the display screen to the initial state. When it is pressed during entry of numerical values, entered values so far are cleared. If it is pressed when a error message is on the display, the screen is cleared and the alarm is canceled. (Some fatal errors can not be cleared.) Press this key when editing the time program to return to the previous parameter. When it is pressed during AUX.FUNC setting, the setting screen returns to the previous parameter.
If this key is pressed when setting the module for the basic operation, entry position for setting parameter moves. Press this key when editing a time program to move to the following parameter for entry. When it is pressed during AUX.FUNC setting, the setting screen moves to the following parameter.
hd Run kev
(CE) Clear key
[backj Back key
(G) Function key
[Enter] Enter key
Puts into effect the entry value for each setting parameter. Used to enter numeric values for each setting parameter.
@-19)
5 -4
LC- 1OAD
Numeric keys
I s i c Operation
4.
Setting Parameter List
Setting parameters, setting ranges, minimum values, initial values, and modes used for basic operation are as follows:
Setting step
0.001ml/min
1kgf/cm2
1kgf/cm' 1kgf/cm'
2
press pmax pmin
Setting parameter
Setting range
0-9.999ml/rnin
10-400kgf/cm2 10-440kgf/cm2
Note)
Initial value
Oml/min IOkgf/crn'
1OOkgf/cm2
Mode
Constant delivery
flow
solvent
Constant pressure solvent delivery
0-440kgf/cm2
Note)
Okgf/cm2
Set the module to the initial state (that appears when power is turned on). If the module is not in the initial state, press ICE)to set it to the initial state. Then a field will be flashing that prompts the user for entry.
flow/press
( / / / I
E
c
pressure
p.max
p.min
8
J
0 .E a
4-
I b:'b"o'
\ \ \
1 0 0
Enter a value with a numeric key then press to put the value into effect. When you want to set a different parameter, p r e s s 0 to move the flashing field.
flow/Dress Dressure
[ ] E
txrnax
\ \ I
//
D.min
0. 0 0 0
1 0 0
I \\
//
To cancel the value during setting, press
CCE]before pressing
(Enter).
a.
6.
Setting the Maximum Pressure Limit Value
To return the screen, after setting, to the initial state, press
To protect columns and other components in the flow line, set the maximum value for the limiter. If the pressure value exceeds the maximum pressure, the limiter will be activated to stop solvent delivery automatically. When the limiter is activated, an alarm beeps, also the message that follows will be displayed.
flow/press pressure p.max p.min
ERROR
P.MAX
1
5-5
LC- 1OAD
The setting procedures are as follows:
-/Basic
<<Setting Example>>
Operation
Example) To set p.max (maximum pressure value) to 150kgf/cm2: (1) Press (fu..) to set p.max to accept an entry (the entry field flashes).
flow/press pressure p.max
\ \ I
p.min
0. 0 0 0
(2)
PressQ,@,@,and[&].
flow/press
// I \ \
1 0 0
//
pressure
p.max
\ \ I
p.min
E
L
I
7.
lo.
0 0 0
1 5 0
//
// I \\
0 0 1 J
Setting the Minimum Pressure Limit Value
The following will be displayed, and the setting is complete. To prevent feeding air to the flow line when the mobile phase in a reservoir has been finished, or for safety measures in a case that liquid has leaked in the flow line, the minimum pressure for the limiter should be set. The limiter will be activated if the pressure is still lower than the minimum pressure even one minute after starting solvent delivery, and the solvent delivery stops automatically. When the limiter is activated, the alarm beeps and the following message will be displayed.
E R R O R P. M I N
<<Setting Example>>
The setting procedures are as follows: Example) To set p.min (minimum pressure) to 20kgf/cm2: (1) Press to set P.min to accept an entry (the entry field flashes).
flow/press pressure pmax p.min
\ \ I
0.
0 0 0
1 5 0
//
0 0
(2)
Press ,@ , and [Entel.) . The following will be displayed, and the setting is complete.
\ \ I
// I \ \
0.
<<Caution>>
0 0 0
1 5 0
2 0
//
Value 0 may be set for p.min but the limiter will not function.
5-6
LC-1 OAD
N m
1.
Operation of Constant Flow Solvent delivery

The following is an example of operation for constant flow solvent delivery. (1) Prepare a mobile phase and fill it into a reservoir, and set the suction filter into the reservoir.
An Operation Example of Constant Flow Solvent delivery
(2)
(3)
Make connections of flow line referring to "Section 4.9 Connections of the Injector, Column, and Detector." Turn the drain valve lever for 180" counterclockwise to open the drain valve. (Make sure that the drain tube is put into a waste container.)
1 8 0 "
0
(4) (5)
Press the power switch on. Check that the value indicating the pressure on the display is in a range from -3 to 3kgf/cm2. If not, carry out zero adjustment for the pressure sensor. (See "Section 5.5 AUX.FUNC Functions.") Check the maximum and minimum pressure limit values (See "Section 5.1 Basic Operation.") Check that the flow/press entry field is flashing, then press @ and (Enter). Confirm that the displayed value is updated to 2.000.
flow/press pressure p.rnax p.min
(6)
(7)
(2.
\ \ \ I / /
/ / / I
0 0 6
\ \ \
1 0 0
(8)
By pressing[=)
, the pump will operate.
5-7
LC- 1OAD
j p e r a t i o n of Constant Flow Solvent deliverv

Observe ten seconds the condition of liquid discharged from the drain tube. If the liquid is being discharged constantly, the module is operating normal.
Drain tube connection port Drain tube ,
i
Reservoir
Liquid flowing direction

\
I:
Suction filter
u
Waste container
<<Cautions>>
If liquid flows and stops synchronizing with pump sounds,

bubbles may be in the pump head. In this case, press(=) to bleed air from the pump head. If liquid does not flow, conduct the same operation or use the disposal syringe and syringe needle to suck the mobile phase as shown in the illustration below. Do not leave the drain valve open for longer time, or the mobile phase will be drained out by gravity.
Reservoir
Suck the mobile phase.
@g+ j
YT\\ u Tube cramps

1
Syringe needle Disposable syringe
5-8
LC-1OAD
-1
Operation of Constant Flow Solvent delivery

(10) Press(=) to stop the pump. ( 1 1) Set the desired flow rate. Example) When you want to set lml/min, press@and(=).
flowhress Dressure
D.rnax
pmin
(1.
\ \ I
0 0 6
I /
1 0 0
( 1 2) Turn the drain valve lever clockwise to close the drain valve. (1 3) Press(-) to operate the pump. (14) Check that the pressure at the pump outlet increases.
5-9
Operation
delivery
1.
of
Constant
Pressure Solvent
7
An Example of Operation of Constant Pressure Solvent delivery
The following is an example of the operation of constant pressure solvent delivery. (1) Carry out operation procedures from (1) to (10) of "Section 5.2 Operation of Constant Flow Solvent delivery." Shift the operation mode from the constant flow solvent delivery mode to the constant pressure solvent delivery mode. First, press till the following is displayed on the screen.
lf...I
flow/press
pressure
p.max
p.min
0.000
MODE
CHANGE]
(3)
Each time is pressed, solvent delivery modes shift. When the module is in the constant flow solvent delivery mode, the lamp will light, and in the constant pressure solvent delivery mode, c.press light. Now set the module so that the lamp is lit.
[Enter]
0 .c
Q)
E
(4)
op
Press @after shifting the mode, then the initial setting screen will return. Check that the flow/press entry field is in a ready state (flashing).
flow/press
\ \ I
pressure
mmax
txmin
// I \ \
10.
//
1 0 0
0 0
Set pressure with a numeric key. Example) When you want to set 20kgf/cm2, press and [Enter) .
0,, @
(20.
\ \ I
//
1 0 0
0 0 1
Turn the drain valve lever clockwise to close the drain valve. Press[@@) to operate the pump. Check that the pressure at the pump outlet increases and becomes constant at around 20kgf/cm2.
-\
5-10
LC-1OAD
rn
1.
Instruction
FLOW PRESS
Creation of Time Programs and Execution
The module permits control of parameters such as flow rate by a time program. The created time program is stored as a file.
Instruction List
The following is a list of instructions that are used for creating a time program.
Description Setting range
0-9.999ml/min
1 O-400kgf/cm2
Remarks
The miniinurn step is
Flow rate (effective only i n the constant flow
solvent delivery mode) Pressure (effective only in the constant pres-
0.001ml/min
The minimum step is 1kgf/cm'
I
sv
EVNT LOOP
sure solvent deliverv mode) Open/closes solenoid valve in the FCV- IOAL or FCV-I IAL(S) (optional). Event output ON/OFF Repeats a program from the first step.
I
I , 2. 3 , 4 0- 123 Note 1 ) 0, 1.2. 12 from 0 to 255 Value 0 repeats a program 256 times.
I
See Note 1. Select one among the four numeric values. The minimum step is 1.
El
E
0 .-
STOP GOT0 BCNC CCNC DCNC
Ends a propram.
Not applicable
Runs programs by linking riles.
0-9
8
The minimum step is 0.1 %. The minimum step is 0.1 c/o.
Q)
(UDto 10 tiles)
Concentration 0 1 liquid B (ellective only when SYS=7 or 1 Concentration of liquid C (cffcctivc only
0-100% Note 2)
0-IOOc/C Note 2)
I
1
when SYS=1) Concentration of liquid D (ell'cctivc only whenSYS=I)
0-100% Note 2)
The minimum step is 0.1 c/o.
Note 1.
If the FCV-10'4L has been selected by setting FCV TYPE, the setting range is 0, 1, 2, 3 , or 4.
Note 2.
If the FCV-1 lAL(S) has been selected, the setting range is from 0 to 123 that is a combination of 0. 1 , 2 , and 3. Setting should be made so that the sum of BCNC, CCNC, and DCNC may not exceed 100%. BCNC + CCNC + DCNC - 100 I The concentration of liquid A is determined by subtracting the sum of BCNC, CCNC, and DCNC from 100. ACNC = 100 - (BCNC + CCNC + DCNC)
5-11
2.
Description of the Display Screen
To create a time program, set the module to the edit mode, then proceed to programming. The procedures are as follows: Press @, then the following will be displayed. (1)
[ m q
flow/press pressure p.max pmin
@ Number of steps already programmed in the selected file Abbreviation of a word used
0Number of remaining steps

@ Abbreviation of a word left The above example shows that 10 steps of the time program is already set and that there are 3 10 remaining steps. then the following will be displayed. (2) Now press(=),
-.
0 .c
Q
L
@ Elapsed time (minute) from the start of program
0Instruction name 0Set value

(3)
Press(=) once again, then the following will be displayed.
flow/pren pressure pmax
pmin
5.00
FLOW 5.0
For further creation of the program, see "Section 3. Sequence of Creation of Time Programs."
5-12
LC- 1OAD
13.

Creation of Time Program
The sequence of creating a time program starting from the initial state is as follows.
flow/press pressure p.max p.rnin
. L
0. 0 0 0 0
4
1 0 0
/CEJ
Press
m.
0
flow/press
pressure
pmax
p.min
\
3 2 0
L E I
PressfEnter).
flow/press
pressure
pmax
p.rnin
\ \ \ I / / /
/ / / I
T I M E
\ \ \
FUNC
VALUE
Press (Enter).
flow/Dress
\ \ \ I / / /
Dressure
Dmax
D.min
/ / / I \ \ \
5.
0 0
FLOW
5.
0 0 0
Enter time value (with numeric keys), then press (Enter).

flow/press pressure
\ \ \ I / / /
/ / / I
pmax
p.min
20.
0 0
FLOW
\ \ \
1
p.max p.min
Each t i m e m is pressed, an instruction is displayed in turn. . When the desired instruction appears, press ( E the , then ) instruction is set.
\ j -
flow/press
pressure
20. 0 0
BCNC
VALUE
/ / / I \ \ \
\ \ \ I / / /
When you have selected any instruction except STOP, enter a set value for the instruction (with numeric keys), then press
(Enter).
flow/Dress Dressure D.max D.rnin
[ >/ / o/ I .
\ \ I
/ /
\ \ \
0 6
BCNC
30
1
5-13
LC-1OAD
next step
4.
An Example of Creating Time Program
An example of creating a time program will be described taking the case of varying flow rate. (The initial flow rate is lml/min.)
TIME 15.00 20.00 30.00
FUNC VALUE FLOW 2.000 FLOW 5 .000 STOP
rnl/min
t
.-
--.
I
I
I
I I
I 1
-A
15
20
30
min
Press @to
return to the initial screen.

\ \ I / /
/ [ I / ./ I 0 0 6
\ \ \
1 0 0
flow/press
pressure
p.max
p.min
3 2 0
LE
Press( Enter].
flow/Dress
\ \ \ I / / /
--.
Dressure D.max pmin
\ \ \
/ / / I
TIME
FUNC
VALUE
Enter the time (minute) for the initial step. Press
Q,@, and
[G) .
flowhress Dressure
\ \ \ I
Dmax
amin
15. 0 0
/ / / I \ \ \
FLOW
/ / /
1
pmax p.min
Select an instruction. When an instruction other than FLOW is displayed, press@ to display FLOW and press(=].
[Is.
flow/press
pressure
0 0
FLOW
V\ AI L /U g ] \ \ /
/ / / 1 \ \ \
5- 14
LC-1OAD
1-

Enter the flow rate. Press @ and
flowhress
\ \ \ I / / /
(GI.
p.max rxmin
pressure
/ / / I
15. 0 0
\ \ \
FLOW
2.
0 0 0
0, ,-(El, @
flow/press
\ \ \ I / / /
Similarly to from (4) (6) above, set the second step. Press to (Enter), and (Enter).
Q,
pressure
mmax
p.min
/ / / I
20. 0 0
\ \ \
FLOW
5.
0 0 0
Enter the step of STOP instruction. After entering a time value through the same procedure as (5),p r e s s m t o display STOP, then press
(Enter).
flow/press
\ \ \ I / / /
pressure
p.max
p.min
/ / / I \ \ \
30. 0 0
STOP
E
C
0 .-
Press @ to end the creation of the time program. A time program having three steps has been completed.
C I
[
return.
3 1 7
L E
By pressing @once
again, the initial screen shown in (1) will
5. Deleting a Step
Display the step you want to delete and press (dell . The following is an example of deleting the first step of the program created in "Section 4. An Example of Creating Time Program."
(1)
Similarly to creation of programs, display the program you want to delete.

flow/press
\ \ \ I
pressure
p.max
p.min
/ / / I
15. 0 0
\ \ \
/ / /
FLOW
2. 0 0 0
(2)
Press@.
\ \ \ I / /
(20.
/ / I I \ \ \
0 6
FLOW
5.
0 0 0 1
Now the first step of the program is deleted and the second step is displayed.
5-15
LC- 1OAD
6.
LOOP Instruction
Use of the LOOP instruction permits repeating a program for a number of times you set. TIME 0 15.00 0 20.00 30.00
FUNC FLOW FLOW LOOP
VALUE
2.000
5.000 3
The above setting will run steps @ and Q three times repeating a cycle of thirty minutes.
0
0 .c
E Q,
Any step except that has the GOTO instruction is disabled if it is set after the LOOP instruction. A number up to 255 may be set as VALUE for the LOOP instruction. Note, however, that setting 0 repeats LOOP 256 times. When setting multiple steps, it is not necessary to enter steps in time sequence. The module sorts the steps automatically. In the following cases, leave the program having no STOP instruction at the last step. 0To run the time program endlessly. 0 To link program files by the GOTO instruction.
fly
7.
Start/Stop
To start or stop a time program that has been completed, follow the procedures below. (1) Starting the Time Program Press lr..). The lamp lights up. The time program now starts. Stopping the Time Program To stop the time program, two types of procedures are available. One is to stop it forcibly while it is running, and the other is to stop by the means of STOP instruction set in the program. The case of a forced stop is described here. Press The prog run lamp is turned off. The time program now stops.
(2)
cr..).
5-16
LC- 1OAD
m1.
AUX. Functions
The module has an auxiliary function AUX.FUNC. Use of AUX.FUNC permits a variety of operations performed by this module. It also is possible to control the module from an external device.
AUX-FUNC List
Name
BCONC CCONC DCONC FILE NUM FILECOPY FILEDEL
The following table lists AUX.FUNC functions.

Function
Concentration of liquid B is set when selecting gradient delivery. Concentration of liquid C is set when selecting gradient delivery. Concentration of liquid D is set when selecting gradient delivery. A file number is selected. Copies a file. Deletes a tile. Solenoid valve in the optionally available FCV-IOAL or FCV-11AL is selected. Sets relay contact point output. Lets the EVENT 1 output work as a start signal for a time program. It also lets the EVENT 2 work as a stop signal for external equipment in occurrence of an error.
T Pe Y
1
Set value at plant

0
1 1
1
1
0
0
0 -
2
1
sv
EVENT EXT-S
0 .w
I
S-PROT
f 8
Reduces flow rate without stopping the pump when thc pressure exceeds the set value of p.max. Changes solvent delivery modes.
0
-
I
1
Monitors solvent delivery flow rate in the constant pressure solvent delivery
MoNFLoW
MON REV MON ID COND P-SET PULSE ZEROADJ
mode. Monitors elapsed time when running a time program. Monitors integrated number of uumu revolutions. Monitors pumps ID. Diagnose conditions of pumps solvent delivery, and displays the results. Used when replacing the plunger and plunger seal. Varies pulsation. Carries out zero adjustment for monitoring pressure. Key entry is disabled. Sets the man for uressure signals in the recorder outmt. Sets the type of selector valve connected to the S0L.V connector on the rear of
0
0
3
1
0 -
48
-
+%1 1
1
1
10
1
0 0
Enter a value according to the conditions of the system in use. the module. Selects whether control is made from the system controller or by the pump.
ADRS
Purge execution time. Sets the address of the device when making control from the system controller.
3.O
BCONC is displayed only when SYS=2 or 4. CCONC and DCONC are displayed only when SYS=4.
5-17
LC-1OAD
. . -
The type column in the list shows the type of operating method. Type 1 : Enter a value with a numeric key then press[=). Type 2 : Press the to execute the function. Type 3 : The current condition is displayed. 2.
iEnter)
Setting Procedures for AUX.FUNC BCONC, CCONC, DCONC (Concentration setting)
[ 0.
flow/press
pressure
p.rnax
p.rnin
// I \ \
0 0 0
BCONC
b\."d]
Concentration of each liquid is set when selecting gradient delivery mode. Enter concentration of each liquid with a numeric key, then press ( . (Unit: %'.> E )
--,
FILE NUM (File number setting)
The module permits creation of up to 10 time programs that can be stored in the memory. Each program file may be selected through the parameter.
\ I >
10. o o o
f
F I L E
COPY
/ I
'ij
Enter the desired file number with the numeric keys, then press
/Enterj.
FILE COPY (Selecting where the file is copied to)
flow/press
pressure
p.max
p.min
\ I / / I \
10. 0 0 0
F I L E
NUM
The contents of a program of the currently selected file is copied to a file of selected number. Enter the file number with the numeric keys, and press
[GI.
FILE DEL (Deleting a file)
flow/Dress
Dressure
p.max
p.min
0.
0 0 0
F I L E
DEL
J
7
The all contents of the time program of currently selected file is deleted. Press Enter 1 .
5- 18
LC-1OAD
- E X .
Functions
flow/press pressure
sv
(Setting solenoid valve)
p.max
p.min
\ I /
Io.
0 0 0
sv
The mobile phase to be delivered is selected, when using the optionally available FCV-lOAL or FCV-1lAL as a selector valve of mobile phase. Enter the value corresponding to the selected mobile phase with a numeric key, then press [G).
Solenoid valve type
FCV- 1OAL
Set value
1
Selected mobile phase

Liquid A Liquid B Liquid C Liquid D
2
3
4
Solenoid valve type

FCV-1lAL
Set value
0
Selected mobile phase

All channels are set to the A side. Channel 1 is set to the B side. Channel 2 is set to the B side. Channel 3 is set to the B side.
Example: By setting SV 123, channels 1,2, and 3 are all set to the B side.
<<Caution>>
Before setting SV, enter a value for FCV TYPE to select the solenoid valve unit used.
EVENT (Setting EVENT output terminals)
flow/Dress
Dressure
D.rnax
D.rnin
\ I
0.
0 0 0
EVENT
/ I \
- 0 -J
/)
ON (close) and OFF (open) of the EVENT outputs (relay contact points) on the rear of the module are set. Enter the set value with the numeric keys then press [Enter).
Set value
0
EVENT 1 output
Relay 1 OFF Relay 1 ON
Relay 1 OFF
EVENT 2 output
Relay 2 OFF Relay 2 OFF
Relay 2 ON
1
2
12
Relay 1 ON
Relay 2 ON
5-19
1-
AUX. Functions
EXT-S (Function setting for the EVENT output terminals)
-\
flow/press
pressure
p.max
p.min
\ I /
0.
0 0 0
EXT-
Sets control mode for the control of external equipment through the EVENT output (relays 1 and 2). Enter the set value with a numeric key, then press[=].
I
I
Set value
0
1
I
I
time Droeram.
Function
Relay contact points are controlled by the EVENT set value. Relay contact point 1 (EVENT 1) is used as a start signal for a
I
I
Relay contact point 2 (EVENT 2) is used as an error output
I
.-. . 0 c
2
C
simal. Both functions 1 and 2 may be used.
<<Caution>>
6
S-PROT (Setting the system protection)
flow/press Dressure mmax nmin
Q)
The use of the EXT-S function disables effects of the EVENT parameter relevant to the corresponding EVENT terminal.
[O.
0 0 0
S- PROT
bl
S-PROT controls solvent delivery in such a manner that when P.MAX is in effect, flow rate is reduced by one seconds without stopping the pump, until the flow rate becomes under the P.MAX value. Enter the set value with a numeric key, then press [Enter].
7
Set value
0
1
Function
Cancels the system protection. Sets the svstem Drotection.
To release the P.MAX error, press=. Then the alarm will stop, and the value that was set before the error occurrence is reset.
MODE CHANGE (Selecting a solvent delivery mode)
flowhress
Dressure
mmax
mmin
[O. 0 0 0
MODE CHANGE)
Selects the constant flow solvent delivery mode or constant pressure solvent delivery mode. Press (G) to select a desired solvent delivery mode.
5-20
LC-1OAD
mmX. Functions
MON FLOW (Displaying flow rate at the constant pressure solvent delivery mode)
1
\ I /
[ O .
0 0 0
MON
FLOW
0 1
Displays an approximate flow rate in the constant pressure solvent delivery mode. Enter the set value with a numeric key, then press
[ ) E .
Set value 0
1
Function
Cancels the flow rate displaying function. Sets the flow rate displaying function.
MON TIME (Monitoring the elapsed time of program)
10. 0 0 0
flow/press
pressure
p.max
p.min
\ I
MON
T I M E /-I0\
/>
0 .4-
The elapsed time from the start of program is displayed when running a time program. Enter the set value with a numeric key, then press[=).
Set value 0
.
Function
Cancels monitoring the elapsed time of program. Sets monitoring the elapsed time of program.
MON REV (Monitoring the integrated number of pump revolution)
flow/press
pressure
p.max
p.min
\ I /
0.
0 0 0
MON
REV
/ I \
The integrated number of pump revolution is monitored. It counts up to 16,777,215, then returns to 0. Enter the set value with a numeric key, then press(=).
Set value
0
1
Function
Cancels monitoring the integrated number of pump revolution.
Sets monitoring the integrated number of pump revnlirtinn
Monitoring the integrated number of pump revolution serves as an indicator for seal replacement. It is recommended to replace seal every 3 million times for operation at 100kg/cm2using water.
5-2! 1
MON ID
(ID indication for remote control)
\ I I
(0.
0 0 0
MON
I D
For connection with the SCL-lOA, pump connection address A, B, or C on the SCL-IOA is indicated on the initial screen. Enter the set value with a numeric key, then press[Enter) .
Function
0
1
Cancels the ID indication.

Sets the ID indication.
flow/press
pressure
p.max
p.min
--..
0. 0 0 0
PUMP
If the SCL- IOA is not connected, the following will be displayed.

flow/press pressure pmax pmin
( 0 . 0 0 0
NOT
L I N K E D ]
COND (Condition indication)
flow/press
pressure
p.max
D.min
10. 0 0 0
COND
NORMAL]
Indicates current conditions of the module. When it is normal, "NORMAL" is displayed. The discharging pressure of the pump on the right is low, the following is displayed.
. ,
0. 0 0 0
COND
XR
1
p.min
The discharging pressure of the pump on the left is low, the following is displayed.
flow/press pressure p.max
0.
0 0 0
COND
X L
If the pressure has increased 10% or more from five minutes ago. the following will be displayed.
0. 0 0 0
INC
5-22
LC-1OAD
mmX. Functions
If the pressure has decreased 10%or more from five minutes ago, the following will be displayed.
flow/press pressure
p.max
p.min
[
<<Cautions>>
0. 0 0 0
DEC
Indications INC and DEC are also displayed in the normal state such as pump start or stop. If XL appears, the cause may probably be one of the following. 0 Air remains in the pump head on the left. 0 The seal in the pump head on the left leaks. @ Check valve IN of the pump head on the left and the check valve OUT of the pump head on the right are not operating normally. If XR appears, the cause may probably be the same as above except that the left is replaced with the right and the right is replaced with the left.
flow/press pressure
p.max
E
C
0 .c
P-SET (Plunger set)
p.min
\ I /
0.
0 0 0
P- SET
/ I \
E K
Moves the plunger. Enter the set value with a numeric key, then press(Enter).
Function
Lets the plunger on the left withdraw. In this state, the seal on the left may be pulled out. Lets the plunger on the right withdraw. In this state, the seal on the right may be pulled out. Stops the plunger at an intermediate position.
PULSE (Fine adjustment of

pulsation compensation)
flow/press
pressure
p.max
p.min
0. 0 0 0
PULSE
4 8
Enter the set value with the numeric keys, then press(Enter) . Vary this value and select a value that generates the minimum pulsation. The following shows values for typical mobile phases. The initial value is 48.
~~
Mobile ph&e
Water Methanol Hexane
Typical value
As a standard, a smaller value is set to a liquid of greater compressibility.
5-23
1-
AUX. Functions
ZERO ADJ (Zero adjustment for pressure indication)
1 -.
0. 0 0 0
ZERO
ADJ
Output of the pressure sensor is set to zero. Press (Enter). Then zero adjustment is carried out. Before using this function, open the drain valve and set the conditions so that no pressure is applied.
CLOSE KEY (Disabling key entry)
flow/press
pressure
p.max
p.min
0. 0 0 0
CLOSE
K E Y
Disables key entry. Press[=]. The module is set to the state that disables key entry. To cancel this effect, press @and @concurrently.
0 .-. c
C
-.
RANGE (Changing the recorder range)
flow/press
pressure
p.max
\ \ I
p.min
//
0. 0 0 0
RANGE
// I \\
1 0
Sets the full scale for the output of the pressure recorder. Enter the set value with the numeric keys, then press[Enter ). Full scale = (Set value) x 50kgf/cm2FS Example) When set value = 1, the full scale is 50kg/cm2FS. When set value = 10, the full scale is 500kg/cm2FS.
SYS
(Setting the system parameter)
flow/press
f
pressure
pmax
pmin
\ I /)
---.
10. 0 0 0
\
SYS
/ I \
. , 4 1
Sets a system parameter. Enter the set value with a numeric key then, press[=).
Set value
1
Function
Set this value when using one unit of the module or when control is made externally. Set this value when using the module as a control pump in a two-module high pressure gradient delivery system. Set this value for a low pressure gradient delivery system.
2 4
Values other than the above shall not be set.
5-24
LC-1 OAD
1-
AUX. Functions
FCV.TYPE (Selection of solenoid valve unit)
flow/press
pressure
p.max
p.min
0.OOOFCV
TYPE
Type of the optional flow line selector valve that is connected to the S0L.V connector on the rear of the module is selected. Enter the set value with a numeric key, then press[Enter) .
I
LOCAL (Setting the local mode)
Set value
0 1
Solenoid valve unit

FCV- 1 OAL FCV- 1 1 AL
flow/press
pressure
p.max
p.min
\ I /
(0.
0 0 0
LOCAL
07
. I
Whether to control the pump from the system controller SCL-IOA or to operate the pump independently is set. Enter the set value with a numeric key then press
c ,
I%).
Function
0
1
Control is made from the SCL-IOA. The module is operated independently (local mode).
P TIME
flow/press
pressure
pmax
p.min
(Purge timer)
rl.000 P T I M E R
Set purge time in the range of 0.0 9.9(min).
3.0
'I
ADRS (Setting the remote address)
flow/press
pressure
p.max
p.min
\ I /
0. 0 0 0
ADRS
/ I \
The address used when using the module connecting with the system controller SCL- 10A is set. Enter the address number with the numeric keys, then press[Enter) .
I
I
Address
1-16
85
Function
TheseareuortnumbersusedwhencontrolledfromtheSCL-1OA. For a high pressure gradient delivery system without SCL-IOA.
I
I
Values other than the above shall not be set.
High Pressure Gradient Delivery Mode

There are two types of high pressure binary gradient system using LC-1OAD. One is with the system controller SCL-1OA and another is without system controller. The latter will be described here. For the operation through the system controller, see "System Controller Instruction Manual." For ternary high pressure gradient, the system controller is necessary. 1.
Preliminary Setting
(1)
(2)
Enter 2 for system parameter SYS of the LC- OAD that controls the other (called pump A). Enter 1 for system parameter SYS of the LC-1OAD that is controlled by the other (called pump B). For the procedures for setting the system parameter, see "Section 5.5 AUX. Functions." From now on operation is carried out through pump A alone. Enter 85 for parameter ADRS and enter 0 for parameter LOCAL of both pumps. Enter flow rate of the mobile phase (sum of flow rates of pumps A and B) for the set value of the flow rate. Referring to "Section 5.5 AUX. Functions," enter the value of concentration of liquid B (Unit: %) at parameter BCONC. The concentration of liquid of pump A (ACONC) is as follows. ACONC(%) = loo(%) - BCONC(%) For the BCONC parameter, setting range is from 0 to loo%, and the minimum step is 0.1%. By pressing (pump) on pump A, pumps A and B starts simultaneously.
--.
(3)
2.
Setting Initial Conditions
(1)
(2)
(3)
3.
High Pressure Gradient Delivery Program
By setting concentration of liquid B at certain times in a time program, it is possible to vary concentration of liquids A and B linearly on the time basis. The concentration of liquid of pump A (ACNC) is as follows. ACNC(%) = loo(%) - BCNC(%) For the BCNC instruction, setting range is from 0 to loo%, and the minimum step is 0.1%.
Do not use the time programs of pump B. Parameter LOCAL is effective only the module is controlled from SCL- 10A.
<<Caution>>
0
5-26
LC-1OAD
h (
4.
Pressure Gradient Delivery Mode

An Example o Program f Setting
Call the program setting screen. Enter time. (3) P r e s s m until BCNC is displayed on the setting screen. (4) Enter concentration. The following is an example of setting for varying the concentration through a time program. (See Section 5.4 Creation of Time Programs and Execution.) Initial value for BCNC: 0.0
(1) (2)
TIME 20.00 30.00 30.10 40.00
FUNC BCNC BCNC BCNC STOP
VALUE 100.0 100.0 0.0
5-27
LC-1OAD
-
rn
1.
Low Pressure Gradient Delivery Mode

The module itself allows setting of low pressure gradient delivery, also it is possible to carry out the setting from the system controller SCL-1OA. The following is a description of setting (A, B, C, and D) of the former. Refer to the instruction manual of SCL-10A for the later.
Preliminary Setting
(1) (2)
(3)
Enter 4 at the system parameter SYS of AUX.FUNC. Enter flow rate of the mobile phase (sum of flow rates of four liquids A, B, C, and D) for the set value of the flow rate. Set the flow rate to 9ml/min here. Next, concentration parameter is set. As the initial operation is set here, setting is made to set each flow rate to be equal to fill all flow lines with liquids. Set each BCONC, CCONC, and DCONC to 25%. (See "Section 5.5 AUX. Functions.") Concentration of liquid A (ACONC) is as follows. ACONC(%) = loo(%) - BCONC(%) - CCONC(%) DCONC(%) For parameters BCONC, CCONC, and DCONC, the setting range is from 0 to loo%, and the minimum step is 0.1%.
-\
2.
Initial Operation
(1)
Open the drain valve. (2) Press (pump) to start the pump. (3) Draw the mobile phase from the pump outlet to fill the flow line with the mobile phase. (4) Make sure that no bubbles are in the flow line. ( 5 ) Replace the content in the flow line with the mobile phase for about 6 minutes. ( 6 ) Close the drain valve and press [pump) to stop the pump. (1) Set the flow rate and concentration to the prescribed values, then press to start solvent delivery.
3.
Low Pressure Gradient Operation

Low Pressure Gradient Delivery Program
(z)
4.
By setting concentration of liquids B, C, and D at certain times in a time program, it is possible to vary concentration of liquids A, B, C, and D linearly on the time basis. The concentration of liquid A (ACNC) is as follows. ACNC(%) = loo(%) - BCNC(%) - CCNC(%) DCNC(%) For BCNC, CCNC, and DCNC instructions, the setting range is from 0 to loo%, and the minimum step is 0.1%.
5-28
LC-1 OAD
,--
mL
Operation of the Automatic Washing Kit
Use of a buffer solution as the mobile phase will produce crystalline substances upon dehydration or evaporation of the solution, which damage the plunger and plunger seal and shorten their service life. When using a buffer solution, accordingly, it is needed to wash the seal backside and plunger surface with distilled water. 1.
Preparation
(1)
(2)
(3)
Set the automatic washing kit to the module referring to "Section 4.12 Installation of the Automatic Washing Kit." From the conical flask, pull out the Teflon tube of the automatic washing kit outlet. Suck the washing solution using a disposable syringe to fill the washing flow line with the washing solution. Install the Teflon tube of the automatic washing kit outlet as it was before.
E
C
1
Suck the solution
Automatic\ washing k i t outlet
/l a f-
0 .-
CI
op
L i q u i d 1flowing direction
2.
Operation
(1)
Operate the pump at a flow rate of approx. 3ml/min to feed the solution. Then check that the solution is coming out of the end of the Teflon tube at the automatic washing kit outlet. Replace the washing solution with fresh distilled water everyday. If the amount of washing solution increases during feeding, the cause is leakage of solution at the plunger seal. In this case, dismount the washing kit and check which plunger seal is leaking at the left or right, then replace the plunger seal according to "Section 8.1 Replacement of Plunger Seal." If the amount of washing solution decreases during feeding, the cause is leakage of solution at the diaphragm. Check if the washing solution is leaking from the bottom of the head holder, then replace the diaphragm according to "8.2 Replacement of Diaphragm."
<<Cautions>>
5-29
m
1.
Operation of Manual Washing
-\
It is possible to wash the plunger and plunger seal manually without using the optional automatic washing kit.
Connections
(1)
(2)
Cut the Teflon and tygon tubes that are included in the accessories of the module to an appropriate length. Connect washing tube B on the left and washing tube B on the right as shown in the illustration below. Similarly, use a piece of the Teflon tube to connect washing tube A on the left to the disposal syringe included in the accessories of the module. Connect another piece of the Teflon tube to washing tube A on the right. Put the end into a beaker.
A on the left
Container such as beaker direction Disposable syringe
2.
Operation
Pull out the disposal syringe from the Teflon tube. Suck a washing solution into the disposal syringe and reconnect it to the Teflon tube. Feed the washing solution to the washing flow line. It is possible to conduct the manual washing irrespectively to whether the pump is in or out of operation. Recommended interval for manual washing are as follows. Phosphoric acid buffer solution (low concentration): Two or three times/day Boric acid buffer solution (low concentration): More than five times/day For ammonium sulfate (high concentration) use the automatic washing kit. Use of a buffer solution as mobile phase will produce crystalline substances upon dehydration or evaporation of the solution, which damage the plunger and plunger seal and shorten their service life. When using a buffer solution, accordingly, it is needed to wash the flow line.
--
ccCaution>>
5-30
LC- 1OAD
mz
1.
Replacement of Mobile Phase

Amobile phase may or not be miscible with another, or some are buffer solutions, so replacement of a mobile phase shall be conducted correctly following the description that follows. If you also replace a column. remove the column first.
Replacement of Mobile Phase with Another Miscible Mobile Phase
( 1)
Fill a new mobile phase approx. lOOml into a container of about 200ml capacity. Take out the suction filter from the reservoir and put it into the container ( l ) , then stir the solution well by slightly vibrating the filter. Put the suction filter into the reservoir filled with new mobile phase, open the drain valve, and press (K) to wash out completely, for approx. 3 minutes, the previous mobile phase which was in the flow line.
0 .Open the d r a i n valve. ( T u r the d r a i n valve lever ncounterclockwlse.) E
(2)
(3)
c ,
Waste container
5-3 1
LC- 1OAD
1-
Replacement of Mobile Phase

(4) Stop the purge by pressing
1
-\
key, then displace connection at the outlet of the manual injector and put it into the waste
[e)
container. Set the module to flow rate of 2-3 mllmin, press (pump) key to start the pump then close the drain valve. Thus the mobile phase in the manual injector may be replaced.
Close the d r a i n valve ' P u m p outlet ( T u r n the d r a i n valve lever clockwise.)-i,
R ese Iv o i r f i l l e d w i t h new m o b i l e phase
\ ' *
&!J
The inside of the
P u m p inlet
Waste container
1 1 ' I'"/
'i
(5)
Remount connection at the outlet of the manual injector, then replace the mobile phase in component in the flow line that follows the manual injector. Flow rate may be changed so as to reduce the column pressure to below the P.MAX value.
2.
Replacement Of Immiscible (1) Mobile Phase

(2)
(3)
Prepare an intermediate washing solution (such as isopropyl alcohol) that is miscible with both old and new mobile phase. Replace the old mobile phase with the intermediate washing solution. See procedures (1) to ( 5 ) of "Section 1. Replacement of Miscible Mobile Phase." Replace the intermediate washing solution with the new mobile phase. See procedures (1) to ( 5 ) of "Section 1. Replacement of Miscible Mobile Phase."
-\
5-32
LC-1OAD
K4 replacement of Mobile Phase

3.
Replacement of Mobile Phase of Buffer Solution
Use of a buffer solution as the mobile phase will produce crystalline substances upon dehydration or evaporation of the solution. Accordingly, replace the buffer solution as follows: Note that if organic solvent such as isopropyl alcohol is fed, crystalline substances may become irremovable, so care should be taken. (1) (2) Prepare distilled or deionized water. Flow 200ml or more of the solution prepared in (1). See procedures (1) to ( 5 ) of "Section 1. Replacement of Miscible Mobile Phase." Then replace the old with a new mobile phase. See procedures (1) to ( 5 ) of "Section 1 . Replacement of Miscible Mobile Phase."
<<Caution>>
(3)
4.
About Use of Buffer Solution(use o f washing flow line)
Use of a buffer solution as the mobile phase will produce crystalline substances upon dehydration or evaporation of the solution, which damage the plunger and plunger seal and shorten their service life. For use of a buffer solution, it is effective to wash the back side of plunger seal and plunger surface by feeding water to extend their service life. For washing method, see "Section 5.8 Operation of Automatic Washing Kit" or "Section 5.9 Operation of Manual Washing."
E
0 .c
C
f 8
<<Caution>>
If you are not going to use the module after feeding a buffer solution, replace the contents in the flow line with distilled or deionized water.
5-33
Chapter 6
Performance Checking
rn
Contents
6.1
6.2
6.3
Operation Checking for Systems ................................................................................... Checking Concentration for High Pressure Gradient Delivery.................................. Checking Concentration for Low Pressure Gradient Delivery ..................................
6-2
6-5
6-7
6- 1
Operation Checking for Systems

-\
Operation checking for a simple system as shown in the following illustration is described here.
f I
Reservoir box Degasifier( DGU- 4A) -
Detector ( S PD-1OA)
jReservoir
C o l u m n oven (CTO-1OA)
- R6A)
1 4 .
I IF
L 3 7 0
->
Chrornatopac
A p p r o x . 540rn
D G U - 4 A LC-1 O A D
C T 0-1 0 A
S P D- 1 0 A
r - - - T - -- - 1
!
1
I- 1
Manual i nj ecto r
column Electric connect i o n
1.
Preparation
Prepare reservoirs as many as required. Prepare a mobile phase. Connect the input cable for the Chromatopac to the relay terminal block attached to the Chromatopac, then make connection from the AUX port of the SPD-1OA to the relay terminal block using the signal cable included in the accessories for the SPD- 1OA.
(1) (2)
2.
Connection
-'
3.
Operation (example)
(3) (4)
Switch power on for the overall system. Purge the flow line (from the suction filter, degasifier to the pump drain). Use a syringe and suck the mobile phase approx. 40ml. Close the drain valve and operate the module at lml/min. Check that the pressure is stable and liquid is flowing from the outlet of the SPD-10A. Set the temperature of the CTO- 10A to 4OOC. With the SPD-IOA, set the wave length to 254nm, response to 4, and AUX FWG to 3. (The AUX output range becomes 2AUW.) At the Chromatopac, set ATTEN to 4.
16-2
LC- 1OAD
At the Chromatopac, press , to set the pen position at the center.
1( , 10/ , 5
and
-\
m i e r a t i o n Checking for Systems

(9)
At the Chromatopac, press PLOT and ENTER to carry out plotting.
(10) Wait until the baseline becomes stable.

E x a m p l e of good cases
0
x
Stable
Examples of bad cases
Having hairs Increases w i t h t i m e passage.
Decreases w i t h t i m e passage.
Unstable
(1 1) At the Chromatopac, set ATTEN to 8. (The Chromatopacs full scale becomes equivalent to 0.5AU.)
(12) At the Chromatopac, press ZERO ,
- ,
, and
E
.z x
0
Q)
IENTER].
(13) At the Chromatopac, press plotter.
1-
and
m] the to stop
6
of the Chromatopac.
(14) Inject sample into the flow line. (15) At the same t h e , press
v l
8 E
C CR
6-3
4.
An Example of Result of Analysis (analysis example)
The following is an example of analysis under the conditions that follows: Mobile phase : H20/Acetonitrile = 15/85 Shim-pac CLC-ODS 6.0mm@x 15cm Column 1ml/min Flow rate Wavelength 254nm, response 4 @Naphthalane lOmg 7 Samples in IOOml 0Biphenyl 5mg methanol. @ Acenaphthene 30mg Iniection @ Anthracene lmg @ Pyren 10mg
CI
(Analysis example)
START 1
0) C
0
Q,
z
0
Q,
2.597 3.322
f n
F8.463
CHROMRTOPRC SRMPLE N O REPORT N O
PKNO
6.882
C-R6R
0 51 5
T I ME
RRER
MK
FILE METHOD
0
41
ION0
CONE
NRME
Naphthalene Biphenyl Acenaphthene Anthracene Pyren
1 2 3 4 5
4.857 5 I44 6 358 6,882 8 463

I
214319 593455 241558 751233 599924
su
U U
8 , 947 1 24 ,7 171 10, 8683 3 1 , 2885 24 9865

I
--------TOTRL
-----------100
2488987
6-4
LC-1OAD
Concentration for High Pressure Gradient Delivery

1.
Conditions
Using liquid A B Flow rate Load pressure Measurement wavelength
: 0.3% acetone water solution
: Distilled water
: lml/min : 10-30kgf/cm2
: 2S4nm
2.
Specification
At liquid A mixing ratios 10, SO, and 90%, concentration error +1% maximum
(1) (2)
3.
Precautions for Measurement
Be sure to degas the mobile phase. Open the drain valves and wash the flow lines for S minutes, setting the flow rate to 9ml/min and BCONC parameter to 50%. ( 3 ) Then set the flow rate to 3ml/min. Close the drain valves and wash the flow line for 20 minutes. (4) Last, set the flow rate to lml/min and the BCONC parameter to loo%, and check that the baseline has become stable, then start measurement. Initial parameter setting Flow rate :lml/min BCONC : 100
4.
Measurement Example
E
w x
C
Q)
6
Q)
100%
Time program TIME 0.10 10.00 FUNC BCNC BCNC BCNC BCNC BCNC BCNC BCNC BCNC BCNC VALUE 90.0 90.0
&
!iz
0 C
10.10 20.00 20.10 30.00 30.10 40.00 i i 40.10
50.0 50.0
10.0 10.0 0.0 0.0 100.0
.-
6-5
Checking Concentration for High Pressure Gradient Delivery

-\
Calculation
= 10% actual concentration
A100
AS0 = 50% actual concentration A100 A90 = 90% actual concentration Aioo It is possible to read values of A10, A50, and A 100 directly from the recorder chart, however, this method yields measurement errors. Accordingly, it is recommended to run the following BASIC program on the Chromatopac, to check the LEVEL value. BASIC 10 20 30
PROGRAM PRINT LEVEL WAIT 60 GOT0 10
6-6
LC- 1OAD
Checking Concentration for Low Pressure

Gradient Delivery
1.
Conditions
Using liquid A Liquids B, C, and D Flow rate Load pressure Measurement wavelength
: 0.3%acetone water solution
: Distilled water : 2ml/min : 10-30kgf/cm2 : 254nm
2.
Specification
At liquid A mixing ratios 10, 50, 90% concentration error +1% maximum Be sure to degas the mobile phase. Open the drain valve and wash the flow line for 5 minutes setting the flow rate to 9ml/min and each BCONC, CCONC, and DCONC parameter to 25%. In this case, be sure to connect the unused inlets with the reservoir and conduct replacement with either solution used. Then set the flow rate to 3ml/min. Close the drain valve and wash the flow line for 20 minutes. Last, set the flow rate to 2ml/min and the BCONC parameter to loo%, CCONC and DCONC parameters to 0% and check that the base line has become stable, then start measurement. Low pressure gradient delivery using liquids A and B
3.
Precaution for Measurement
4.
Measurement Example
100%
1
I:
0
Initial parameter setting Flow rate: 2ml/min B.CONC : 100.0 C.CONC : 0.0 D.CONC : 0.0
6-7
LC-1OAD
~
Time program TIME 0.10 10.00 10.10 20.00 20.10 30.00 30.10 40.00 40.10 FUNC VALUE 90.0 BCNC 90.0 BCNC 50.0 BCNC 50.0 BCNC 10.0 BCNC 10.0 BCNC 0.0 BCNC 0.0 BCNC BCNC 100.0
Calculation
'0
Aioo A100
Aioo
A90
= 10% actual concentration
= 50% actual concentration = 90% actual concentration
It is possible to read values of A10, A50, and A 100 directly from the recorder chart, however, this method yields measurement errors. Accram on cordingly, it is recommended to run the following BASIC pro5 the integrator. to check the LEVEL value. BASIC 10 20 30 PROGRAM PRINT LEVEL WAIT 60 GOT0 10
6-8
LC- 1OAD
Chapter 7
Control from the External Equipment
Contents
7.1
Connections of the Input/Output Terminals for External Equipment ....................... Control from the SCL-IOA ............................................................................................
7-2
7-4
7.2
7-1
LC-1OAD
Connections of the InputlOutput Terminals for

External Equipment
1.
The InpuVOutput Terminals for External Equipment

EXTERNAL OUTPUT
I
m
I
I
I
EVENT2
EXTERNAL INPUT
----
EVENT1
1 ON
r-- 1 7-r 1
I
PRESSURE
OFF
START
STOP
COM
RECORDER
Signal name
EVENT 1
Description
Relay contact point output. The contact points make and break according to EVENT parameter values set in a program or AUX.FUNC setting.
Remarks
The rated values of the relay contact points are 30VDC and
0.1A
EVENT2
Relay contact point output. The contact points make and break according to EVENT parameter values set in a program or AUX.FUNC setting.
ON(PUMP) OFF(PUMP) START
The pump in the module operates activated by the external contact mint signal. The uumu in the module stous bv the external contact uoint simal. The time program for the module starts activated by the external contact point signal. If the signal comes again when the time program is running the time program starts again.
Control is made possible by short-circuiting these signal terminals and "COM" terminal at contact points in external equipment. The short-circuiting times (tc) shall be as follows:
STOP COM. RECORDER
The time program for the module stops by the external contact point signal. Common terminals for ON,, OFF,, START,, and STOP signals. Outputs pressure values of feeding to the recorder. The output scale may be set in ten steps within an output range of from (O-50kgf/cmz) to (0-500kgf/cm2). See "Section 5.5 AUX. Functions."
0.5 sec < tc < 10 sec
Full scale voltage = 1mV
7-2
LC-1 OAD
1
2.
Connections of the Inputloutput Terminals for External Equipment
Use accessory remote cable for single wiring. For more wiring prepare cables as follows.
Wiring
(1)
(2)
Strip the sheath of the connecting cable for approx. lOmm in length at the end. If the core wire is solid, just insert it into the hole of a terminal while pressing the button above the hole using a small screwdriver or the like. If it is stranded, twist the end well, then insert it into the hole while pressing the button above the hole using a small screwdriver or the like. To disconnect the cable, also press the button and pull the cable.
EXTERNAL OUTPUT
EXTERNAL INPUT
I
PRESSURE
I
EVENT1 EVENT2 ON
OFF
START
STOP
COM
RECORDER
Core wire
Button
Approx. 1Omm
<<Caution>>
To protect the cable from breaking of wire, we recommend to use stranded cables, if possible. Cables having a core wire of diameter within the range shown below may be used. Solid wire: @0.4-1.0(AWG 26-18) Stranded wire: 0.3mm2to 0.75mm2(AWG 22-20)
Element wire diameter: $0.18 at the minimum
7-3
Control from the SCL-1OA

For the basic operation of the system controller SCL-IOA, see "System Controller SCL- IOA Instruction Manual."
1.
Switching Power on and the CONFIG Screen
When the SCLpower switch is turned on, power is supplied and a few seconds later the CONFIG screen will be displayed. If solvent delivery modules and the SCL is correctly connected, ( e D ] is shown on the right of module names ,
(PUMP.B), [ F E E ) .
( m )
(For a configuration of three pumps connected to the SCL.) In this screen, connection of modules is defined to control the solvent delivery modules from the SCL. If this definition is not carried out for a module, checking link is not performed for the module during analyses even if it is connected to the SCL. Carry out this definition only one time when power is turned on for the first time from installation.The SCL stores the information in itself, so the definition is not needed unless you change the system configuration.
SYSTEM C O N F I G U R A T I O N L I N K E D
PUUP. A
PUMP. B
PUMP. C DET. A DET. A.
L INKED
L I N K E D
L I N K E D
L I N K E D L I N K E D L I N K E D L I N K E D L I N K E D MENU
LOCAL
I N J
FRC OVEN
P .3
W Q
L O C A L
SUBC
. . .
p r e s s
P
S
t u s READY
5
X
w E
c
Define connection of solvent delivery modules following the procedures below. (1) Display "a" in the following illustration at the function display. 0 If "b" is displayed at the function display, press (fun3 once.
a
PUW
(2)
With the function keys, select the solvent delivery modules

conncctcd to the SCL. The selected module names will be
highlighted on the screen. The highlighted modules on the screen are defined as connected.
<<Caution>>
If a module is marked with ,control from the SCL is not accepted in spite of its highlighted name. Set and update its local mode to 0, according to "Section 5.5 AUX. Functions."
1-
7-4
LC-1OAD
12.
Control from the SCL-IOA

The Main Menu Screen
From the CONFIG screen, press screen.
[l the main menu E display to
It is possible to return to the main menu screen whenever you press [ from any other screen in operation. E ]
MENU A N A L Y S I S F I L E PARAMETERS T I M E PUMP D E T F R A C T I O N AUTO COLLECTOR PROGRAM CONTROL CONTROL
:o
: 1
:2
: 3
: 4
INJECTOR/ANAL
S E P U E N C E : S : 6
M O N I T O R S Y S T E M
: 7
9 9 9 9 . 9
/ o
READY
tu.
3.
Setting the Initial Parameters
(1)
P r e s s a o r move the flashing position to 0 using the arrow keys
on the main menu screen, then press The parameter control screen for analysis files will be displayed. In addition to parameters for the solvent delivery modules, parameters for any module may be displayed and updated on the analysis file parameter control screen.
~~~~ ~ ~ ~~~ ~~ ~ ~~ ~
[GI.
-------P U M P (
A N A L Y T I C A L F I L E 0
I S O . FLOW FLOW FLOW P R E S P R E S P R E S MAX M I N
)
PARAMETERS -
Q .3
E
(P
-___
ml/rnin m l / m i n rnl/mi:
k g / c m kg/crn'
-- -- -- -D
WAVE RANGE WAVE2 WAVE RANGE WAVE2
Contact point
A. 6. C. A. 6. C. P . P .
0.000 0.000 0. 0 0 0
0
0
E 3 8 1 . 6 0
T . A- - - - - 0 nm 2 5 0 0 A U F S 0 nm
_______DET.
0
100 0
ka/crn' kg/cm' k E/crn'
6- - - - - nm 1 9 5 2. 5 6 0 0 A U F S 2 0 0 nrn
w
c
CT
Detector
E
X
4 u
6 5
K V .
D \I
RV. C
"
A. FLOW
t i m e 9 9 9 9 . 9
-. n
0
0
a m
im
/ o
READY
The
m] in the diagram shows parameters for the column
solvent delivery modules.
The solvent delivery mode in use is indicated inside the parentheses.
Operation
(1)
Press (funcjto display the functions that follow at the function line.
7-S
LC-1OAD
1-

-\
(2)
P .3
! i
Select a solvent delivery mode for the solvent delivery modules using the corresponding function key. ): Flow rates for up to three solvent delivery modules may be controlled independently. [B.GE]( (f2)): Conducts binary high pressure gradient delivery using two solvent delivery modules (A, B). Flow rate for solvent delivery module C is controlled independently. Conducts ternary high pressure gradient delivery using three solvent delivery modules. [LP.GEI( If4)): Four-liquid low pressure gradient delivery is carried out using solvent delivery module A. Flow rate for modules B and C is controlled independently. Depending on the solvent delivery mode set, the number and contents of the parameters displayed on the screen will vary. anda) (3) Move the cursor with the arrow keys @ to the parameter you want to change. Enter a new value and press [Enter J. 0 If the 1 lamp is lit, set parameters are sent to each module at once. 0 If function display field is switched to the help information by pressing the setting range and minimum step for the parameter at which the cursor is will be displayed. Example:
(m
m( a):
*\
,B,m,
0,
W Q
E
U
Q)
Parameters displayed on the screen are as follows (for the solvent delivery module only):
Parameter
Description
T.FLOW
B.PRES C.PRES B.CONC C.CONC
~~
Sum of flow rates (ml/min) at gradient delivery

Pressure of pump B (kg/cm2) Pressure of pump C (kglcm2)
Concentration of liquid B (%)
Concentration of liquid C (%) Concentration of liquid D (%) Gradient curve for liauid B Gradient curve for liquid C Gradient curve for liquid D Maximum pressure limit (kgf/cm') Minimum pressure limit (kgf/cm*)
' 7
D.CONC B.CURV C.CURV D.CURV P.MAX P.MIN
7-6
LC-1OAD
14.

Time Program
When the setting of the initial parameters from the parameter control screen is complete, press [menu)to return to the main menu screen and PROGRAM I. select From the time program screen, the time program described in "Section 5.4 Creation of Time Program and Execution" may be set through the SCL. In addition, programs set in this time program setting screen include parameters for other modules such as detector.
T I M E F I L E
PROGRAM 0 (8. G E ) T I M E
Program entry lines
X I
01
F U N C B. CONC WAVE S T O P
300
V A L U E
S T E P S
L E F T
30. 0 0
I 1 5 0 . 6 5 2 16000. 0
A l 3 5 0
I 1 0 0
Si
9 1
( D E T . A D 6 I 8 8. C U C. I 9 C. C U D . C O N C I 1 O D . C U
F U N C T I O N FOR 5 0 A . F L O W I 6 1 B. FLOW1 2 C. F L O W 1 7 4 T. F L O W 1
E T . R V I R V I R V I
O T H E R ) A. P R E S B. P R E S 1 3 C . P R E S 1 I
1 2
Instructions table.
9999.9
/ o
R E A D Y
I Operation
(1)
[GI,
(2)
If a time program has no contents, the cursor is at the ITIMEJ field in step No. 0. First, using the numeric keys, enter the desired time for the instruction you want to execute. After entering values, press then the cursor moves to the field. Press (func)to select the function display that follows:
1 (3)
Use key TABLEtl or TABLE-+I ( to move the highlighted box that follows FUNCTION FOR to select the module name that needs instructions.
F U N C T I O N FOR
(lf41) I
w)
(PUMP
D E T . A
D E T . 6
O T H E R )
(4)
If you select another module name, the instructions table below
changes to show another instructions table that corresponds to the selected module. The following is the instructions table for PUMP .
0 1 2 4
F L B. F L C. F L T. F L
A.
O O O O
W W W W
1 1 1 1
5
6 7
B. C O N C I
8 C. C O N C I 9 D. C O N C I I O
I 1 1 B. C U R V I 1 2 C. C U R V I 1 3 D . C U R V l
A . P R E S B. P R E S C. P R E S
7-'7
LC- 1OAD
1-
-\
For what appears instructions table by selecting other modules, refer to the System Controller Instruction Manual.
(5)
If you enter a number shown in the instructions table using the will show the number. By pressing numeric keys, the @field (Enter), the number disappears and the corresponding instruction will appear. The instructions table is displayed for ease of reference for instruction numbers. If an instruction has a number that is not displayed on the screen, it is possible to enter. (6) If the entered instruction needs parameter value to be set, the cursor will move to the field. Enter an appropriate value and press[=). If you select the help information by pressing the setting range and minimum step of the parameter needed for the entered instruction will be displayed. If the instruction needs no entry of value for parameter, the cursor will move to the field of the next step. Repeat the procedures (2) through (6) above and complete the (7) time program.
1-
[GI,
* 7
1-
The time you enter at the field must be equal to or later than that in the previous step. If you enter a wrong value, the alarm beeps when you press ( ) , and the entered time will be cleared. %
(8)
The following operation may be carried out using the function keys from the time program screen. the function field switches and displays By pressing each function.
m,
2 w-
piFq([T))
2
C
The time program on the screen is output to the printer of the Chromatopac. All the contents of time program corresponding to the file number on the screen will be deleted.
I . \ '
Icopvj([ 3 f) )
The time program corresponding to the file number on the screen will be copied to file of another number. Moves the cursor in the module name field of the instructions table to
the left.
ITABLEt/ (pi))
Moves the cursor in the module name field of the instructions table to the right.
I
1
I I
I
7
.\-
Any key entry is disabled except -](cancels
the key lock).
7-8
LC- 1OAD
15.

Pump Control Screen
Conditions of gradient control in a time program for the solvent delivery modules or changes in flow rate control are displayed graphically on the pump control screen, so that it is possible to view and check time programs during entry. To display the pump control screen, select IPUMP CONTROL from the main menu screen.
Screen mode
PUMP F I L E CONTROL O V E R L A Y
So I ven t
delivery mode Solvent delivery parameter
Change of solvent delivery parameters\

C. F L O W A . P R E S 6. P R E S C. P R E S STOP
TIMEV A L U E
- T i m e entry
1
0 . 0 1
t i m e
0 TIME
- f 9 9 e 9 . 9s r0 n p (l m il nn j 9 n i l /
0
field
9 9 9 9 . 9
f r c
s t a t u s READY
Parameter value entry field.
The horizontal axis of this graph indicates elapsed time of the time program. For the full scale for the horizontal axis, an appropriate time for putting an end and later than the time of STOP instruction is automatically chosen (if a STOP instruction is not included, the time of the last step). The vertical axis indicates pump flow rates, concentration, or pressures. For flow rates and pressures, the maximum flow rate and pressure of each solvent delivery module are shown. In the case of concentration, the maximum value is 100%. The solvent delivery mode field at the right shows currently selected mode as highlighted. Below it, in addition, the parameter names (instruction) for the solvent delivery modules in that mode are shown.
Operation
Presslfuncj to switch the function display as follows:
I
(2)
0
I
Select the desired solvent delivery mode with the function key. The selected solvent delivery mode is highlighted in the solvent delivery field at the upper right on the screen. Below it, parameter names corresponding to the mode are shown. the By pressing function key (PARAMI( @), highlighted box moves down one line in the parameter name field. Move it to the desired parameter name for setting. Below the W E I f i e l d , the cursor flashes.
(3)
7-5)
LC-1OAD
1-

Enter the desired time with the numeric keys and press IEnter). The entered time is displayed, and the cursor moves to the position below the (VALUEJfield. It is the same as in the time program. Enter a parameter value with the numeric keys and press
v l
The entered value is displayed and the cursor will move back to the h%dfield. It is the same as the parameter value in the VALUE \field of the time program. If you set the solvent delivery mode to the high pressure gradient delivery and selected in (3) for parameter name, proceed from ( 5 ) to (8). Procedures from (3) through ( 5 )are equal to the entry of 1 step in time programming. Changes in flow rate (pressure) of the solvent delivery module or concentration, which is caused by the entry of a new step are displayed graphically on the screen. Complete the time program, repeating the entry procedures from step (3). By entering a parameter value for with the numeric
v)
' 7
w]
keys, the cursor moves further down one step and flashes. Enter now the value for curve that starts from the current time. It is the parameter value for the I e l i n s t r u c t i o n in time programming. If the value for the curve is 0 (linear), just press(=]. For the value and shape of the curve, refer to the System Controller Instruction Manual. When the entry is complete, the screen returns to (3).
,, -
10
<<Notes on Entry>>
The times entered at the m f i e l d from the pump control screen may not be in order. The entered one step is added to the time program in the order of time.
7-10
LC-1OAD
1-
Control from the SCL-lOA

If you change solvent delivery mode on the pump control screen, the solvent delivery mode on the parameter control screen will also be changed. If a parameter of other solvent delivery mode is entered while programming, it will be disregarded in the actual analysis. It is impossible to correct a wrong entry from this screen. In such a case, press to return to the main menu and from the TIME PROGRAM screen, correct the wrong entry with the editing function.
I,,,,(
Switching the Screen Mode
The graphics display has two screen modes that follows:
/OVERLAY] :
p q:
v l
All parameters listed at the right of the screen are displayed graphically on the screen at once. Only the parameter selected with the key alone is displayed graphically.
Each time function key -( ] (f11)is pressed, the screen mode switches. The selected screen mode is highlighted at the right of the top line on the screen. The following operation is available using the function keys from the pump control screen.
Flow rates for up to three solvent delivery modules may be controlled independently.
p qB Z ( )
Conducts high pressure binary gradient delivery using two solvent delivery modules (A, B). Flow rate for solvent delivery module C is controlled independently. delivery modules.
Conducts high j ( ) ternary gradient delivery using three solvent l @ pressure
[rn](pq)
pAFiWJp5-J)
Low pressure gradient delivery is carried out using solvent delivery module A. Flow rate for modules B and C is controlled independently. Selects parameter name.
IG.MODE\(rn)
Switches the screen display mode. Any key entry is disabled except
j i ( W )
1-
(cancels the key lock).
LC- 1OAD
Chapter 8
Maintenance
Contents
8.1 8.2 8.3 8.4 8.5 8.6 Replacement of Plunger Seal ......................................................................................... Replacement of Plunger and Diaphragm ...................................................................... Cleaning and Replacement of Check Valves............................................................... Replacement of Line Filter ............................................................................................ Replacement of Fuse ....................................................................................................... Cleaning ............................................................................................................................ 8-2 8-4 8-6
8-7
8-8 8-9
8-'I
LC- 1OAD
Replacement of Plunger Seal

As a rule, the plunger seal shall be replaced approx. every 1000 hours of solvent delivery. (Water delivery at 1ml/min at 100kgf/cm.) See MON.REV in "Section 5.5 About AUX.FUNC Function." When the plunger seal has been worn, the pressure becomes unstable, or liquid leaks and effuse from the clearance between the head and head holder or from the washing solution outlet. For replacement of the plunger seal follow the procedures below: As an example, the seal on the right, is replaced. (1) Enter 2 for the P.SET parameter. (For the seal on the left, enter 2.) For the setting method of the P.SET parameter, see "Section 5.5 About AUX.FUNC Functions." (2) The jpump/ lamp will lights up. Wait until the lamp is turned off. Then the plunger on the left is at its maximum position of withdrawal. (3) Dismount the suction filter and remove SUS pipe A and the Teflon tube at the top and bottom of the pump head, respectively.
To disconnect SUS pipe A, loosen the male-nut connected to the check valve OUT. Bent the pipe a little upward and open the
loop of the pipe as illustrated in the picture. When dismounting the suction filter, lower the reservoir to a position lower than the inlet, or empty the mobile phase.
Bent
\
D r a i n valbe
(@ 0 @&Pump
head
Check valve I N
7\-Teflon@tube
(4)
Loosen the setscrew a thc center of the pump head clamping t
plate for a half turn using the accessory Allen wrench.
8-2
LC-1OAD
1-
Replacement of Plunger Seal

(5)
Unscrew the two screws at the left and right of the pump head clamping plate, which is fixed by the screws, and pull the pump head cramping plate away. Then remove the pump head.
Spacers
Mounting screw
I
Set screw
Pump head clamping plate Mounting screw
(6)
(7)
Remove the pump head seal using the accessory seal remover. Insert one end of the remover having a rim into the seal and pull the seal away. Fit a new seal to the other end of the remover and insert the seal into the pump head in a right angle.
To set a seal, f i t it to
this end, then insert i t into the pump head. Seal remover
To remove a seal, use this end t o pull it away
4L
I
a 0
lu
C
Having a r i m .
Pump head
(8) (9)
(10)
Remount the pump head at the original position. Mount the clamping plate and the spacers on the pump head, then tighten the two screws at the right and left.
Firmly tighten the setscrew at the center of the pump head
clamping plate.
<<Caution>>
Be sure not to remount the pump head upside down. Be sure to tighten the setscrew at the center of the pump head clamping plate after tightening the two screws at the right and left.
8-3
LC- 1OAD
Replacement of Plunger and Diaphragm

When liquid leakage continues if the plunger seal has been replaced, or when plunger seal's service life is extremely short, the plunger surface may have flaws. These flaws may have been caused by foreign matters mixed in the pump head or crystalline substances of buffer solutions. In that case, the plunger needs to be replaced. When the automatic washing kit is fitted, in addition, if liquid leaks from the washing line or the washing solution does not flow, the diaphragm needs to be replaced.
ccCaution>>
To identify liquid leakage from the washing line. check if the washing solution is leaking from the back of the head holder or the washing solution in the washing kit decreases. To replace the plunger or diaphragm, follow the procedures below. As an example, the plunger or diaphragm on the right is replaced. (1) Enter 2 for the PSET parameter. (For the plunger or diaphragm on the left, enter 1.) For the setting method of the P.SET parameter, see "Section 5.5 About AUX.FUNC Functions." (2) The Ipump/ lamp will lights up. Wait until the lamp is turned off. Then the plunger on the left is at its maximum position of withdrawal. ( 3 ) Dismount the suction filter and remove SUS pipe A and the Teflon tube at the top and bottom of the pump head, respectively* When dismounting the suction filter, lower the reservoir to a position lower than the inlet, or empty the mobile phase.
(4)
-7
Dismount the pump head referring to "Section 8.1 Replacement of Plunger Seal." Unscrew the mounting screws at the left and right of the head holder alternately with the accessory Allen wrench. If the head holder does not come off smoothly, put the removed two screws into the M4 threaded halls on the head holder and push the body with these screws. Two type of Allen wrenches are attached in the accessory.
Use A type Allen wrench to loosen and
-\
(5)
tighten the screws of head holder.
8-4
LC-1OAD
1-
Replacement of Plunger and Diaphragm

(6)
Enter 3 for the P.SET parameter. The Ipump/ lamp will lights up. Wait until the lamp is turned off. Use the accessory box driver to remove the plunger and diaphragm as turning counterclockwise the metal component set at the base of the plunger.
(7)
<<Caution>>
Be sure to set a handle to the box driver before a work.
Handle
(8)
Mount a new diaphragm and plunger. Firmly fix the plunger with the box driver.
<<Caution>>
When fixing the plunger, make sure that the diaphragm is not offset.
(9)
Enter 2 for the P.SET parameter. The /pump/ lamp will lights up. Wait until the lamp is turned off.
0 C
QI
(I I
(10) Remount the head holder, as fastening the screws firmly. ( 1 1) Remount the pump head. (12) Mount the clamping plate and the spacers on the pump head, then firmly tighten the two screws at the right and left.
.-
( 1 3) Firmly tighten the setscrew at the center of the pump head clamping plate.
<<Caution>>
Be sure to tighten the setscrew at the center of the pump head clamping plate after tightening the two screws at the right and left.
(14)
Connect the pipe and tube at the top and bottom of the pump
head, then connect the suction filter.
8-5 LC-1OAD
Cleaning and Replacement of Check Valves

1
A defective check valve may result in no reproducibility of retention time or unstable pressure in solvent delivery. Procedures for cleaning or replacement of check valves are as follows:
1.
Cleaning the Check Valves
Replace the mobile phase with isopropyl alcohol. Connect a dummy column (0.1 x 2m pipe) in place of the column, then feed the solution at 2ml/min for one hour at the minimum.
(1)
2.
Replacing the Check Valves
Dismount the suction filter and remove the SUS pipe and Teflon tube at the top and bottom of the pump head, respectively.
<<Caution>>
When dismounting the suction filter, lower the reservoir to a position lower than the inlet, or empty the mobile phase. Remove the check valves with the accessory wrench. Install new check valves. Care should be taken not to tighten excessively. Reset the flow line. Release the solution from the drain valve and check if it flows continuously.
' I
Do not disassemble a check valve. If it is disassembled, we

cannot guarantee the performance of the check valve. If a check valve is turned upside down, components in the check valve may come out, so be careful.
Remove it.
Qv
v,f&-
--\
Check valve OUT
Check valve I N
8-6
LC-IOAD
Replacement of Line Filter

If a back pressure exists with the tubing at the pump outlet disconnected, a possible cause is a clogged line filter. To replace the line filter follow the procedures below: Disconnect the tubing at the pump outlet.
Turn the line filter and remove with the accessory wrench. Wipe the dirt in the connecting hole of the line filter. Install a new line filter, then feed several milliliter of a mobile phase. Reset the tubing at the outlet.
D r a i n v a l v e lever
8-7
Replacement of Fuse
1
When the fuse is blown, replace it as follows. Be sure to use the specified one.
( 1)
(2)
Remove the power cord from the power cord connector. With a slotted screwdriver, catch the cover on the fuse holder and slide it out.
Fuse holder cover
(3)
After replacing the fuse, push the fuse holder back in until it clicks.
Fuses
Fuse holder cover
8-8
LC-1 OAD
Cleaning
If the cover or the panel of the unit is stained wipe out dint or dust with soft cloth or a piece of paper.
If necessory, use a synthetic detergent.
8-9
LC-1OAD
Chapter 9 Troubleshooting
I'
Contents
9.1 9.2
Symptoms and Countermeasures for Troubles ............................................................. Error Messages .................................................................................................................
9-2 9-4
9- 1
LC-1OAD
Symptoms and Countermeasures for Troubles

7
Pump operation troubles result from various causes all of which cannot be covered in this manual. This section describes the troubleshooting measures on the basis of the symptoms. For the countermeasures, detailed infoimation is given in each relevant section.
Symptom
~~ ~ ~
Cause
1. Bubbles in the pump head.
Remedy
I . Flush liquid through the drain to purge bubbles.
2. Suck u p bubbles through tlic drain tubing with
ii
Solvent dcl ivery is unstable. Fluctuation in

Ilow rate is large.
syringe.
2 . Old solvent rciiiains in the pump

chamber.
I . Increase llow rate and llusli solvent through tlic drain to

wash off the old mobile phase completely.
I . Increase the Ilo\v rate to wash off tlic old solvent through
3. Bubbles i n tlic pipe of suction lilter.
the drai 11tubing .
2. Shake tlie suction filter to purge bubbles.
3. I f the suction filter is clogginp, c m y out ultrasonic

clcaning. If tlie ultrasonic cleaning is not effective, replace
the suction film.
4. Degas the iiiobilc phase. 4. Malfunction of the check valves.
1. Clean or reulace the check valves.
S. Leak from the plunger se;iI.

6. Leak in tlie Ilow line.
1 . Replace the plunger seal.
2. Replace the plunger.

I . Retighten the joints.
2. Replacemelit of defective parts. 7. Clogged tlow line.

The pump
operates. but solvent is not 2. Air enters 1'1-om [lie joint betwccn the suction filter and inlet pipe.
1. Malfunction ol'tlie check valves 1. Bubbllcs in tlic pump clianibcr.
1. Clean or rcplacc the line filter.
2. Check the flow line. 1. Flush liquid through tlie drain to purge bubblcs.
2. Suck up bubbles through the drain tubing with a syrinze.

I . Fimily connect tlie joint.
1. Clcun or replace the check valves.
dc 1i v ercd .
Measured llow
rate is lower than
2. Clogged suction lilter

I
1. Cleiun or replace [lie suction filter.
the set flow rate.
9-2
LC- 1OAD
m i
Symptom
Prcssurc indicat i o n s o f two
Symptoms and Countermeasures for Troubles
Cause
1. The pressure giiugc docs no(
Remedy 1. Carry out zero adjustment.

I . Clean or rcplacc the line filtcr.
indicate zero properly.
pulllps arc not

itlc 11Iiccr I when
2. The line liltcr l'or either pump i s
clogged.
perlonning
gr;rdicnt delivery.
( Dill'crcncc
3. One Ilow line is cloggcd 111 ;I point before [low I incs or two pumps
becomes contlucnt.
I . Rcplucc the clogged tubing.
cclu;il
to or
under ~ l i d c i i ior 5% ~
is consiclcred to
he normal.)
Solvent i s not
tlclivcrcd.
1. The power switch i s
iiot
turned ON.
I . Turn the power switch ON.
2. Pump switch is not turned ON. The pump key LED i s 1101 lit.
3. Flow rate indic:itioii rcmuins
at
I . Prcss tlic pump key.

2. Control pumping from the SCL-IOA.
1. Set llow rate.
(Pump i h not opcratin_c.)
0.
3. An error message is tlisplaycd.
1
1
2. Set flow rate from the SCL-IOA.

I . Press@).
Prcssurc does not
(P.MAX. P.MIN. ctc.) 1 . Tlic drain \'aIvc is onen.

2. Leakage in flow line
I . Cltvged line l'ilicr
Rcmove thc cause of the error.

I . Close the drain valve.
1. Rctighleii joints.
rise.
Prcshurc rises cx-
2. Replaccment of defective parts.

ccssivcly. I , Clean line filter. 2. Renliice linc filter.
I . Itlcntil'y the clopped component and replace it.
1. Rcplacc the tubing with another having an appropriate
2. Clogged Ilo\v line

3. The inside diamctcr ol'tubing is
excessivclv small.
insidc diameter.
9-3
Error Messages
This module has multiple self-diagnostic testing functions, which beep an alarm and then show an error message if they catch any abnormalities. Except for cases in which error (1) or (2) occurs, pressing (CE) will stop the alarm beep and return the display to the initial screen.
1.
ROM Error
ROM F A I L U R E
This error message will be displayed when there are any abnormalities in the ROM. If this error message is displayed, pressing ICE) will not release the system from the error. Turn off the power source for the module, and contact our office or agent.
2.
' Y
RAM Error
This error message: will be displayed when there are any abnormalities in the RAM. If this error message is displayed, pressing @ will not release the system from the error. Turn off the power source for the module, and contact our office or agent.
NOT PROTECTED
1
-, -,
.4-
This error message will be displayed when the contents of the RAM have been lost or destroyed due to power source abnormalities. By pressing @ , the module may become operable. However, if this error message is displayed every time the power switch is turned on, the problem may be caused by dead or low power backup batteries. Contact our office or agent for information on exchanging the backup batteries.
4.
Overstepping Error
This error message is displayed when the setting for the number of steps in the time program, 320 steps, has been exceeded. If this error message is displayed, the time program can not be prepared any further. Continue entering program data after deleting unnecessary files.
9-4
LC- 1OAD
15.
Error Messages
Maximum Pressure Error
E R R O R P- MAX
This error message will be displayed when the maximum value set for the pump output pressure, p.max, has been exceeded by the actual output pressure. When this error message appears, the limiter will function and automatically stop the solvent delivery. (However, when an S.PROT value has been set, the flow will continue at 1/2 of the original volume.) When this error message is displayed, check the flow line for clogging, and if there is no problem, set the P.MAX value to an appropriate value.
6.
Minimum Pressure Error
ERROR P- MIN
This error message will be displayed when the minimum value set for the pump output pressure, p.min, has exceeded the actual output pressure. When this error message appears, the limiter will function and automatically stop the solvent delivery. In this case, check the flow line for leakage, and if there is no problem, set the p.min value to an appropriate value. This error trapping will not function in the first one minute after the start of the solvent delivery.
7.
Home Position Error
[ E R R O R
HOME P O S
This error message is displayed when the home position of the motor can not be detected. It will also be displayed when the motor does not function of when it is slipping. In this case, turn off the power and then turn it on again, then press to start operations again. If this operation causes the error message to appear again, turn off the power for the module, and contact the our office or agent.
(e)
8.
Purge Error
OPEN
DRAIN
VALUE
This error message is displayed if the actual output pressure of the pump exceeds 5kgf/cm2 during purge operations started with the (G) Because the @key will release the system from the error, key. start the purge operation again after opening the drain valve. If the error message is displayed even with the drain valve open, perform the zero adjustment of the pressure sensor (see Section ZERO ADJ in "5.5 AUX.FUNC").
9-5
LC-1OAD
Chapter 10 Specification
Contents
10.1
10.2
LC-IOAD Unit Specifications ........................................................................................ High Pressure Gradient Specifications ..........................................................................

Low Pressure Gradient Specifications ...........................................................................
10-2 10-3
10.3
10-4
10-1
LC- 1OAD
~ _ _
LC-1OAD Unit Specifications

\
1.
Pump
Microvolume double plunger pump (Approx. 1Opl/stroke)
2.
Modes of solvent delivery Constant flow or constant pressure solvent delivery 1) Constant flow delivery Range of flow rate: 0.001-5ml/min ( 10-400kgf/cm2) 5.001-9.999ml/min (10-200kgf/cm2) Accuracy of flow rate Within &2% or f2pl/min whichever is higher setting: (0.01 -5ml/min, 10-400kgf/cm2, with water and room temperature at
20C) except for periods of low pressure gradient delivery. .9 Precision of flow rate Within M 3 6(O.l-5ml/min, 10-400kgf/cm2 with water and room temperature at 20C)
2) Constant pressure feeding Pressure setting range: Pressure setting accuracy:
10-400kgf/cm2 (at 1kgf/cm2 intervals) Less than 10% or lOkgf/cm', whichever is larger
3 Pressure limit: .
4.
Highbow pressure Internal capacity of approx. 2 0 0 ~ 1
Damper: Materials in contact with solvent : Suction filter:
5.
6.
SUS3 16, ruby, sapphire, Teflon' tempered with graphite, Hastelloy C PEEK, Kalrez', KelF ' ,
l o p mesh
7. Line filter:
2p mesh, capacity approx. 2OOyl

Flow rate, pressure, event, LOOP (repeated programs), a total of 10 files and 320 steps
a.
9.
Time program: Pressure indication accuracy: flow line:
f2% or 5kgf/cm2, whichever is larger

Automatic cleaning is possible with the connection of the optionally available automatic washing kit. 260W x 140H x 420D; however protruding components are not included. llkg
10. Plunger seal cleaning
11. Size:
12. Weight :
13. Operating temperature
s-3soc
(Power requirements vary depending upon the P/N.) P/N 228-25000-91,92 AC 90-1 30V 1 00VA
range:
14. Power requirements:
P/N 228-25000-93
AC 200-25OV lOOVA
10-2
LC-1OAD
m
1.
High Pressure Gradient Specifications
SCL-1OA Control - High Pressure Gradient Specifications

1) Number of mixed
2 or 3
solvents:
2) Gradient profile:
step, linear, and exponential functions possible at multiple levels a total of 20 files and 400 steps
3) Number of program steps:

4) Program time:
0.01-9999.9 min &loo% (0.1% stepiping)
5) Mixing ratio setting range:

6) Mixing ratio setting accuracy:
+1% (O-lOO%, 0.:l-3ml/min, 10-400kgf/cm2, with a water and acetone mix)
2.
LC-1OAD Control High Pressure Gradient Specifications

1) Number of mixed
2
solvents:
2) Gradient profile:
step and linear possible at multiple levels a total of 10 files anid 320 steps

4) Program time:
at the longest, 999.99 min. (0.01 min. stepping) &loo% (0.1% stepping)

6) Mixing ratio setting accuracy:
f l % (0-100%, 0.1-3ml/min,
10-400kgf/cm2, with a water and
acetone mix)
10-3
LC-1OAD
Low Pressure Gradient Specifications

/\
1.
SCL-1OA Control Low Pressure Gradient Specifications Number of mixed solvents: Gradient profile : Number of program steps: Program time: Mixing ratio setting range: Usable flow rate range:
up to 4
step, linear, and exponential functions possible at multiple levels a total of 20 files and 400 steps
0.01-9999.9 min
O-lOO%(O. 1% stepping)
0.1-9.99mVmin
2.
LC-1OAD Control Low Pressure Gradient Specifications 1) Number of mixed solvents: 2) Gradient profile:
up to 4
step and linear possible at multiple levels a total of 10 files and 320 steps

0 .cp 0 .'c
Y
4) Program time:
at the longest, 999.99 min. (0.01 min. stepping)
v)
8 .

6) Usable flow rate range:
0--100% (0.1% stepping)
0.1-9.999ml/min
10-4
LC-1OAD
Chapter I1
Space Parts and Optional Modules
Contents
I I .I Consumable Parts List .................................................................................................... Optional Modules List ....................................................................................................
11-2
I 1.1 List of Other Necessary Parts .......................................................................................

11.3
11-3 11-4
11-1
LC-1OAD
Consumable Parts List

\
Parts Name
-7 Parts Number
228- 18745 228-1 2642-93 228-12564 228-1 1647-93
Remarks
I 2
Seal Filter F6 assembly Packing Suction filter
These two parts need to be replaced together.
Filter main assembly only (already cleaned)
11-2
LC-1OAD
mm'
1.
List of Other Necessary Parts
Mechanical Parts
~~
Parts name
I
Parts number
228-1 8523-9 1 228-18522-91 228- 18522-92 228-18611 228-24464 228-28288-92 228- 18707 228-18866-91 228- 1 8740-9 1 228-18555 670-10321 228- 1 8648 228-18495-01 228-18748-91 228-2431 1-01 228-24473 228-24472 021 -0 IS60
Remarks
Plunger Check valve IN Check valve OUT Drain packing Pump head Photo interrupter Head holder Cleaning tube A Assembly Suction filter (assembly type) Bush 3D FEP tube 2x3 Inlet block
2
3 4
6
7
8
9
Cleaning tube B is the same. For the suction filter
10
11
12 13
14
15
For the suction filter For the pump inlet

The tube between the inlet block and the check valve IN
ETFE tube 1.6x0.8

Drain tube Diaphragm ( V, &) Pump head clamping plate Spacer Mounting screws
16 17
I8
2.
Electrical Parts
Parts Name
Fuse 2A Fuse I A Power source SLM 50224 Switch Print board PB- 1 (no ROM)
Parts Number
072-01652-19 072-01652-16 074-80368-01 064-54753-01 228-23685-91 228-24783-9 1 074-73306 228-23674 228-23024-9 1
Sheet keys
Remarks
for 1OOV-12OV input for 22OV-24OV input
Power source switch
ROM Assy
Batteries Panel switch 4431 PCB FIP Assv
Printed circuit board for the kevboard
11-3
LC-1 OAD
Optional Modules List

\
The following is a list of the optional modules that are connected directly to this module. For details on the available optional modules or for information on those not listed here, contact our office or agency.
Optional Module Identification
DGU-IA DGU-2A
PartsNumber
228- 17641-91
Description
A helium degasifier for one liquid system.
i
228-21996-91 DGU-3A 228-24200-91 228-24201-91 DGU-IOA FCV- 1OAL 228-24845-91 228-24861-91 228-24813-91 228-248 13-92
A helium degasifier for four liquid system. Up to four reservoirs may be degassed. An on-line degasifier for three liquid system. It permits continuous degassing by An on-line degasifier for two liquid system. It permits continuous degassing by pressure reduction through a resin membrane for up to 2 flow lines.
A full automatic helium degasifier for four liquid system. Controlled by the SCL- IOA
pressure reduction through a resin membrane for UD to 3 flow lines.
through option box L.
' 7
A solenoid valve module for low pressure gradients. Controlled by LC-I OAD or by
the SCL-IOA through option box L.
A solenoid valve module for switching reservoirs (for 3 flow lines).
Three unitsof three way solenoid valves are built in, permitting switching reservoirs with three pumps connected. Controlled by the LC-IOAD or by the SLC-IOA through option box L.
A solenoid valve module for switching reservoirs (for 1 flow lines).
One unit of three way solenoid valve is built in, permitting switching two reservoirs. Controlled by the LC-IOAD or by the SCL-10A through option box L. FCV- 13AL A valve unit for switching reservoir. Having 6 setting positions, this rotary valve unit permits switching 6 reservoirs. Controlled by the SCL-IOA through option box L.
11-4
LC- 1OAD
1bptional Module Identification

Option Box L
Optional Modules List

~~
Parts Number 228-25025-91

(1 00120V)
Description
This unit has 3 functions.
1. For control of the FCV-IOAL, FCV-IlAL, FCV-IlAL(S), FCV-l2AH, FCV-
228-25025-92 (200-26oV)
13AL, FCV-l4AH, syringe unit, and DGU-IOA units. However, setting is made through the SCL- 1O unit. A 2. The following units can be contained: FCV-IOAL, FCV-1 IAL, FCV-IlAL(S), FCV-l3AL, DGU-IA, DGU-2A, syringe unit, and DGU-IOA. 3. Supplies AC power for other modules included in a system. 100-12OV x 8, or 2W-26OV x 6.
Reservoir Box Mixer Automatic Washing Kit Manual Injector Model 71 25 Position Sensing Switch Manual Injector Model 8125 for semi-micron liquid chromatography Piping Parts Kit for semi-micro liquid chromatography Injector Mounting Plate Column Holder Air Trap
228-25038-9 1
228-28000-91 228-18803-91
Up to 2 of the following units can be contained FCV-IOAL, FCV-I IAL, FCV1 lAL(S), DGU-2A, etc. This unit can be placed under the LC-IOAD. This box provides housing space for the reservoirs, and permits installation of the manual injector. A static mixer for the high and low gradient delivery. This kit is for continuous automatic washing with washing solution of the rear of the plunger of the LC-IOAD. 'It is very effective when using a buffer solution containing salt of high concentration.
A manual injector for general analyses. The standard sample loop is 2 0 ~ 1 .
When connected to the manual injector Model 7125, a signal synchronizing with sample injection is sent to the system controller and Chromatopac.
228-21 999-91 670- 12098-15 228-23200-91
A manual injector for semi-micro liquid chromatography. The standard sample loop is 5pl. The unit has a built-in position sensing switch.
228-23198-91
This unit consists of a SUS pipe with an inside diameter of 0.2mm and joints for the manual injector.
228-25468-9 1 228-15418-93 228-23675-9 1
This unit is used as a momunting device when mounting the manual injector on the right side of the LC-IOAD. This unit is used when atl.aching a column on the right side of the LC-IOAD. This is attached to the tube for the suction filter and used to let the air out of the flow line.
11-5
LC- 1OAD
Chapter 12
Reference Material
Cantents
12.1 13.2 Precautions on Static Electricity .................................................................................... Mobile Phase Characteristics.......................................................................................... 12-2 12-6
12-1
LC-1OAD
Precautions on Static Electricity

7
Liquid chromatography using combustible organic solvents as mobile phase requires constant exercise against fire, explosion, etc. Particularly, among various possible accidents, those caused by static electricity are difficult to anticipate, and tend to occur only with unexpected conditions which often make countermeasures insufficient. At a site where preparative liquid chromatography is practiced, a large amount of combustible substances may be used. Therefore, once an accident happens, it could lead to tremendous damage. The mechanism of accident by static electrical discharge and preventive measures are described below. Exercise due care in safety measures in handling of equipment.
-\
1.
Mechanism of Static Electrical Discharge Accident (Example)
Accidents caused by static electricity take place through the following processes.
When liquid is fed at high speed through a small-diameter tube like the pipe of a liquid chromatograph, static electrical charge occurs by mass flow charge displacement as shown in Fig. 1 .
Flowing l i q u i d
Solid
Fig. 1 Occurrence of static electricity by friction between solid and liquid
12-2
LC- 1OAD
m i
Charging and storage of static electricity Energy release-by discharge
When the charged liquid is collected in an insulated vessel, its static charge gradually increases to a few kilo volts. If some other conductive object is brought near the vessel, electricity is discharged at a certain distance from the vessel releasing heat energy. This heat energy ignites any nearby combustible gas of appropriate concentration.
If a i r is d r y
substances
i s f l o w i n g a t a h i g h speed h a small- diametertube. ge i s easily accumulated i f les are included i n the d.

nsulated vessel l i k e polyethylene) Spark discharge Combustible gas i s stored i n the head space of the vessel.
Spark discharge rnbustible o r g a n i c solvent i s arged t o a great extent.
- -v =
F l o o r covered w i t h rubber, etc.. provides unwanted insulation.
, ---
Fig. 2 Conditions for Accidents
12-3
LC-1OAD
1
2.
1 -
Preventive Measures against Accidents
The principal preventive measure is on prevention of "charging and storage of static electricity" among those items shown in "Occurrence mechanism of static electrical discharge accidents." Although the preventive measures are shown below, it is important to exercise two or more measures simultaneously. :: Particularly when alarge quantity of combustible solvent is held : in a large vessel, be sure to observe the preventive measures 1, 2. and 3.
.. .
Preventive measure 1.
Use metallic (conductive) waste liquid vessel which is well grounded. This releases the charge of the waste liquid and vessel to ground. The following items are available. (1) Grounding cord with clip P/N 228-2 1353-9 1 (2) Metallic 18 litter can P/N 038-00044 (3) Metallic 4 litter can P/N 038-00043-01 -. Be sure to ground the vessel properly. Disconnecting of ground>:: . ing cord or poor grounding defeat the purpose of using a metallic vessel. % There are some metallic cans which have no conductivity due to an oxidized coating or lacquer on their surface. Be sure to check that vessels are grounded by a tester before application. % When a liquid with almost no conductivity (of 10-"s/m or less) is discharged into the vessel, it is necessary to mix it with another liquid with some conductivity. (The other liquid can be placed in the vessel in advance.) Minimize the clearance of both inlet and outlet of vessel to prevent an ignition source from entering the vessel. (1) Vessel provided with three holes for 3 caps (for 18 litter and 4 litter cans) P/N 228-21354-91
Connect c l i p t o m e t a l l i c p a r t
I /
M i n i m i z e clearance by attaching a cap.
t o the grounding, etc., of the device t o g r o u n d the m e t a l l i c vessel.
M e t a l l i c 18 l i t t e r can ( A plated can I S recommended.)
Static electricity of the l i q u i d is released via vessel.
Fig. 3 Anti-Static Electricity Measures for Vessel

12-4
LC- 1OAD
, \ - _
1-

Do not approach the vessel with charged objects including the human body. Charging prevention measures for human body Prevention of charging of shoes and clothes a) b) Grounding of human body c) Make working floor conductive Suitable products to be used for those measures a), b), and c) are available on the market. % When persons who use no charge prevention measures approach dangerous sections, they have to be grounded beforehand. (For example, they should contact grounded metal by hand.)
Use pipes with inner diameter of 2mm or more for waste liquid line
for large flow rates. +% Inclusion of bubbles in the tube may increase the amount of charging by ten times. Check that there is no inclusion of air via tube joints.
When it is impossible to make the vessel conductive, exercise caution in the following points. a) Set the vessel so that the pipe outlet will be placed below the liquid level in the vessel. Or, dip a grounded metal (ex. pipe connected to the main body of device) in the liquid. % This method is not effective for liquid with small conductivity (lO-'Os/m or less). Use a vessel of the smallest possible capacity to minimize the damage by fire if it should occur. Prevent the room from being dry. Humidity of 65% or more has charge prevention effects.
, -
b) c)
K
12-5
LC- 1OAD
Mobile Phase Characteristics

-\
(3) (2) Source

1.
Cutoff
uv
(4)
R.1.25'
Boiling Point Viscosity (5) ("c) (cP,25"c) p'
(6) e : -.25 -.25 -.25
(7) Water Solubility (8) %" inmt Dielectric Solvent Constantea 1.88 1.86 1.9
(9)
PI+
0.25 e const.
(a function in proportion to strength)
FC-78 (*) (LC characteristic) 210 rn 1.261 FC-75 (Fluorescent solvent) 2 10 (opaque 1.276 FC-43 210.or under) 1.291 Isooctane (*)(2,2,4tri methylpentane) n-Heptane (*) n-Hexane (*) n-Pentane (**) Cyclohexane Cyclopentane (*) 1 Chlorobutane (*) Carbon disulfide 2Chloropropane (**) Carbon tetrachloride n-Butyl ether Tricthylamine Bromoethane (*) i-Propyl ether (*) Toluene p-Xylene Chlorobenzene Bromobenzene Iodobenzene Phenyl ether Phenetole Ethyl ether (**) Benzene Tricresyl phosphate Ethyl iodide n-Octanol Fluorobenzene Benzylether Methylene chloride (**) Anisole
50 102 174
0.4 0.8 2.6
< -2 < -2 <-2
p' and Dielect.
2. 3. 4. 5. 6.
7.
8. 9. 10. 1 1. 12. 13. 14. 15. 16. 17. 18. 19. 20. 2I . 22. 23. 24. 25. 26. 27. 28. 29. 30. 31.
LC LC LC LC LC LC LC LC LC LC
197 195 190 195 200 200 220 380 230 265 220
LC
220 285 290
1.389 1.385 1.372 1.355 1.423 1.404 1.400 1.624 1.375 1.457 1.397 1.398 1.421 1.365 1.494 1.493 1.521 1.557 1.580 1.505 1.350 1.498 1.510 1.427 1.46 1.538 1.421 1.514 1.405 1.442 1.385 1.397 1.385 1.405 1.385 1.370 1.384 1.443 1.532 1.376 1.450
99 98 69 36 81 49 78 46 36 77 142 89 38 68
110
138 132 156 258 170 35 80 72 195 85 288 40 154 130 83 82 118 97 66 48 77 82 61 202 80 156
0.47 0.40 0.30 0.22 0.90 0.42 0.42 0.34 0.30 0.90 0.64 0.36 0.38 0.38 0.55 0.60 0.75 1.04 3.3 1.14 0.24 0.60 0.57 7.3 0.55 4.5 0.4 1 0.9 3.5 0.78 3.6 2.6 1.9 0.46 0.35 0.43 1.9 0.53 1.64 0.38
2.0
0.1 0.2 0.1 0.0 -0.2 -0.2

1.0
LC LC
218 280
0.3 1.2 1.6 2.1 1.9 2.0 2.4 2.4 2.5 2.7 2.7 2.8 3.4 3.3 2.8 2.7 2.2 3.4 3.1 4.1 3.1 3.8 3.7 3.5 4.1 3.9 4.0 4.0 4.2 4.4 3.9 4.1 4.8 4.7 4.7
0.01 0.01 0.01 0.00 0.04 0.05 0.26 0.15 0.29 0.18 0.25 0.54 0.35 0.28 0.29 0.26 0.30 0.32 0.35
0.01 1 0.010 0.010
0.0 10
0.0 12 0.014
0.005 0.008 0.19
0.62 0.046
1.94 1.92 1.88 1.84 2.02 1.97 7.4 2.64 9.82 2.24 2.8 2.4 9.4 3.9 2.4 2.3 5.6 5.4 3.7 4.2 4.3 2.3 7.8 10.3 5.4 8.9 4.3 14.7 10.4 12.5 17.5 20.3 7.6 5.3 6.0 20.3 4.8 17.4 18.3 18.3
0.1 0.5 0.5
0.5
0.5 0.6 2.8 1.7 3.7 2.3 2.4 2.4 4.3 3.2 2.9 3.0 4.1 4.1 3.7 4.9 4.0 3.6 4.2 5.8 4.6 5.6 4.6 1.3 6.3 8.3
--
0.38 0.32
1.3 0.058
r-1
205
0.5
3.9
LC
233
0.42 0.61 0.44 0.7 0.7 0.82 0.57 0.58 0.82 0.40 0.51
0.17 9.2 0.16 miscible 20.1 miscible miscible miscible 8.8 miscible 0.072 23.4
LC
228 210 240 212 256 205 245 329
.Q
L
36. n-Propanol
c Q,
3 a l
0
r Q,
37. 38. 39. 40. 4 1. 42. 43.
Tetrahydrofuran (*) Propylamine (*) Ethylacetate (*) i-Propanol Chloroform (*) Acetophenone Methylethyl ketone (*) 4 . Cyclohexanone 4
LC LC LC LC LC LC LC
5.8 5.6 8.7 9.1 9.1
-.
12-6
LC-IOAD
I
(I) Solvent
45. 46. 47. 48. 49. 50. 51. 52. 53.
54.
Mobile Phase Characteristics

(7) Water Solubility (8) %" inB': Dielectric Solvent Constant e 34.8 25.2 2.2 23.0 9.0 12.4
(3) *7<.5cP,>45 **7<.5cP,<45' (2) Source
uv
Cutoff
(4) R.I. 2s* 1.550 1.536 1.420 1.449 1.625 1SO7 1.390 1.356 1.538 1.400
Boiling Point Viscosity ( 5 ) ("c) (cP,25"c) p' 21 1 191 101 175 237 115 114 56 205 125 1.8 1.2 1.2 3.4 0.88 0.64 0.30 5.5 1.60 4.4 4.8 4.8 6.0 5.0 5.3 5.2 5.1 5.7 6.1 5.5 6.6 6.1 4.3 6.8 6.3 6.0 5.8 6.5 6.4 7.2 6.7 7.4 5.1 6.0 7.4 6.0 6.9 9.6 10.2
(9)
(6) e'.
P'+
0.25 e 13.2 10.9 10.7 7.4
55. 56.
57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 12. 73. 74.
Ni trobenzene Benzonitrile Dioxane Tetramethyl urea Quinoline Pyridine Nitroethane Acetone (*) Benzyl alcohol Tetramethyl guanidine Methox yethanol Tris (cyanoethoxy) propane Propylene carbonate Ethanol Ox ydipropionitrile Aniline Acetic acid Acetonitrile (*) N, N-dimethylacetamide Dimethylformamide Dimethylsulfoxide N-methyl-2-pyrolidone Hexamethyl phosphoric acid triamide Methanol (*) Nitromethane m-Cresol N-methylformamide Ethylene glycol Formamide Water
LC LC
215 265
miscible 0.56 miscible 0.9 miscible
LC
380 330
0.71 0.6
13.1 miscible 0.56

19.9
8.8
LC GC LC LC GC
210
210
1.359 1.584 1.370 1.341 1.436 1.428 1.477 1.468 1.457 1.326 1.380 1.540 1.447 1.431 1.447 1.333
78 184 118 82 166 153 189 202 233 65

101
1.08 3.77 1.1 0.34 0.78 0.80 2.00 1.67 3 0.54 0.61 14 1.65 16.5 3.3 0.89
miscible
24.6 6.9 6.2 37.5 37.8 36.7 4.7 32 30 32.7

11.8 182 37.7 111
8.1
LC LC LC LC LC
190
miscible miscible 0.88
268 268 268 285
0.62
miscible
0.65 miscible 2.1 miscible miscible miscible
LC
205 380
LC
202 182 182 210 100
10.0
80
12-'7
Solvents marked with an asterisk * are preferred for LC mobile phase because their boiling points (> 45C) permit easiness in use, and their viscosity 0 . 5 ~ is low. ~) Solvents marked with two asterisks ** have very low boiling points and viscosity. Symbol LC in the Source column indicates that the mobile phase is available from the following companies specially for liquid chromatography. Burdick & Jackson, Baker Chemical, Mallinkrodt Chemical, Fischer Scientifie, Waters Associate, Manufacturing Chemicals, Inc. (Note: The following companies also commercially supply such mobile phases. Wako Pure Chemical Industries, Ltd., Nakarai Chemical, and Kanto Chemical Co., Ltd.) Symbol GC in the Source column indicates that these mobile phases are used as a stationary phase for gas chromatography and are available from companies that sell GC columns and stationary phases. (These mobile phases are used as a stationary phase in liquid-liquid LC using a physically stationary phase.) The "UV Cutoff' column indicates that mobile phases are opaque at wavelengths shorter than the indicated wave length. The "R.I. 25" column indicates refractive index (") at 25C. The "p"' column indicates polarity parameter of mobile phase. The "ea" column indicates strength parameter of mobile phase for liquid-solid absorption using alumina. The "Water Solubility w% in 20C Solvent" indicates water solubility (w%) at 20C in the mobile phase used as liquid-solid absorption. The "Dielectric Constant e" column indicates dielectric constant. "P' + 0.25 e" is a function that consists of p' in proportion to the strength of mobile phase and the dielectric constant in ion pair chromatography. Source: A. Krstulovic, P.R. Brown: Reversed-Phase High-Performance Liquid Chromatography ( 1 982) Wiley Interscience: Translated by Makino et. al., Reversed-Phase High-Performance Liquid Chromatography (1985)
-'-.
,. -
" 7
12-8
LC- 1OAD

Lc-10ad Im Rev0oc

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228-10743

3-2 3-4 3-5

6-2 6-5 6-7

8-2 8-4 8-6 8-7 8-8 8-9

10-2 10-3 10-4

11-2 11-3 11-4

Protective goggles Other facilities required

Wear protective goggles when handling solvents.

A Variety of Functions for Gradient Delivery

A Measure for Buffer Solution

The LC- 1OAD is composed of the following parts.

LC-1OA Main Body

(Japanese version) or (English version)

Accessory pack (See the following page.)

Construction and Function

The Front ..........................................................................................................................

The Rear ...........................................................................................................................

The Right Side and Bottom ..........................................................................................

The Right Side and Bottom

Conditions for Installation Location

Installation Space Requirements

Use in the patient environment

Examples of System Configuration

LOW Pressure Gradient Delivery System 1

atopac ( C-R 6A)

Low Pressure Gradient Delivery System 2

A low pressure gradient delivery system including an automatic injec-

Degasifier (DG U-1OA) Syringe module

module (FCV-1OAL) Pump (LC-1OAD)

High Pressure Gradient Delivery System -1

Detector (SPD-1OA) Column oven (CTO-1OA)

Reservoir box Manual injector (7125)

Examples of System Configuration

System controller (SCL-1OA) Reservoir

SamDle cooler Mixer ,

Resevoir selector valve

Urrscrewing Fixing Screws for Transportation

Fixing screws for transportation

Mounting of Multiple Modules

Connection to the Power Outlet

Tubing of the Module

Pump inlet (Bush for transportation)

Connecting the Suction Filter

Remove bush 3D. Suction filter

Connecting the Drain Tube (1)

Connection of the Drain Tube for Liquid Leakage

Connecting the Degasifier

Helium gas inlet

Helium gas c:ylinder

Never use a container with a crack or flow for reservoir.

ing the Degasifier

FCorlnecting the Degasifier

Ventilation of Helium Gas

Solvent miscible w i t h the m o b i l e phase

Tubing of the DGll-3A

Connect these tubes

Accessory Teflon t u b i n g included i n the DGU- 3A

Selecting Mixer Capacity

(A) Tubing for 0.5ml

(B) Tubing for 1.7ml

(C) Tubing for 2.6ml

To the injector inlet T o the injector inlet

Remove tubing and fit caps for dust prevention.