Lc-10ad Im Rev0oc

228-1 0743

SOLVENT DELIVERY MODULE

FOR SHIMADZU HIGH PERFORMANCE LIQUID

CHROMATOGRAPH

INSTRUCTION MANUAL

LC-1 OAD

SHIMADZU CORPORATION A N A LYT IC A L IN STRUM E NT S DlVlS ION

KYOTO, J A P A N

.

CONTENTS

Caution

1 General 1.1 Outline ............................................................................................................ 1-2 1.2 Features .......................................................................................................... 1-3

2 Details of Parts 2.1 Details of Parts ............................................................................................... 2-2

3 Construction and Function 3.1 The Front ........................................................................................................ 3-2 3.2 The Rear ......................................................................................................... 3-4 3.3 The Right Side and Bottom ............................................................................ 3-5

4 Installation 4.1 4.2 4.3 4.4 Mounting of Multiple Modules ...................................................................... 4.5 Electrical Connections ................................................................................... 4.6 Tubing of the Module ..................................................................................... 4.7 Connecting the Degasifier ..............................................................................

Conditions for Installation Location .............................................................. Examples of System Configuration ............................................................... Unscrewing Fixing Screws for Transportation ..............................................

. .

4.8 Mounting the Mixer ....................................................................................... Connections of the Injector. Column, and Detector ...................................... 4.9

4.10 Installation of High Pressure Gradient Delivery System .............................. 4.11 Installation of the Low Pressure Gradient Delivery System ......................... 4.12 Installation of the Automatic Washing Kit .....................................................

5 Operation 5.1 Basic Operation .............................................................................................. 5.2 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 5.9 5.10 Replacement of Mobile Phase .......................................................................

Operation of Constant Flow Solvent delivery ...............................................

Operation of Automatic Washing Kit ............................................................ Operation of Manual Washing .......................................................................

4-2 4-3 4-6 4-7 4-8 4-9 4-12 4-17 4-21 4-24 4-27 4-30

5-2 5-7 5-10 5-11 5-17 5-26 5-28 5-29 5-30 5-31

..

6 Performance: Checking 6.1 Operation Checking for Systems ................................................................... 6-2 6.2 Checking; Concentration for High Pressure Gradient Delivery ..................... 6-5 6.3 Checking Concentration for Low Pressure Gradient Delivery ..................... 6-7

7 Control from External Equipment 7.1 7-2 7.2 Control from the SCL-1OA ............................................................................ 7-4

Connection of the Input/Output Terminals for External Equipment .............

8 Maintance 8.1 Replacement of Plunger Seal ......................................................................... 8-2

8.3 Cleaning and Replacement of Check Valves ................................................. 8-6

8.5 Replacement of Fuse ...................................................................................... 8-8 8.6 Cleaning ......................................................................................................... 8-9

8.2 Replacement of Plunger and Diaphragm ....................................................... 8-4

8.4 Replacement of Line Filter ............................................................................ 8-7

9 Troubleshooting 9.1 Symptoms and Countermeasures for Troubles .............................................. 9-2 9.2 Error M~:ssages ............................................................................................... 9-4

10 Specification 10.1 LC-1OA:D Unit Specifications ....................................................................... 10-2 10.2 High Pre:ssure Gradient Specifications .......................................................... 10-3 10.3 Low Pressure Gradient Specifications ........................................................... 10-4

11 Spare Parts and Optional Modules 1 1.1 Consumable Parts List ................................................................................... 11-2 1 1.2 Lists of Other Necessary Parts ....................................................................... 11-3 1 1.3 Optional Modules List ................................................................................... 11-4

12 Reference Material 12.1 Precautions on Static Electricity .................................................................... 12-2 12.2 Mobile Phase Characteristics ......................................................................... 12-6

1. Ventilation

2. Fire

3. Static charge

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.

Solvents used in high performance liquid chromatographs are often

inflammable and toxic, therefore the room in which they are used must

be well ventilated.

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.

As well, static charge is a hazard that may be the cause of inflamma-

tion. Appropriate measures should be taken. See "Section 12.1 Precau-

tions on Static Electricity."

4. Protective goggles Wear protective goggles when handling solvents.

5. Other facilities required 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 recom-

mended that installation be in a place where variations in ambient temperature are at a minimum.

- ; G E

Chapter 1 General

1.1 Outline ............................................................................................................................... 1-2

1.2 Features ............................................................................................................................. 1-3

1-1

LC-1 OAD

L

b

0 w t I i ne 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- 1 OAD

Im 1. Solvent Delivery of Ultra

LOW Flow Pulsation and High Accuracy Gradient

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

Features

Delivery -

volume of lop1 per plunger stroke and by high speed driving of the plunger. These features allows detectors such as differential refrac- tometers 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.

E Q, E

8

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- 1 OAD, without using any system controller.

3. A Measure for Buffer 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.

Solution

1-3 LC- 1 OAD

Chapter 2 Details of Parts

Contents

2.1 Details of Parts ................................................................................................................ 2-2

2- 1 LC-1 OAD

Details of Parts 1

Parts

Accessories

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

Powercord (100/115V) or 071 -608 14-01 1

Power cord (220/230/240V) Suction filter 228- 18740-9 1 1

Drain tube kit 228-28161-91 1

07 1 -608 14-02

Instruction manual (Japanese version) or 228-10742 1

Accessory pack (See the following page.) 228-15084-91 1

(English version) 228- 10743

1. LC-1 OA Main Body

2. Standard Accessories

category I Part Name 1 PartNo. 1 Qty I

1

2-2 LC-I OAD

-1 Details of Parts

Spilap Syringe Remote cable

3. Accessory Pack

01 8-26002 0.2m 046-00038-01 1

228-28253-9 1 1

2-3 LC-1 OAD

Chapter 3 Construction and Function

Con tents

3.1 The Front .......................................................................................................................... 3-2

3.2 The Rear ........................................................................................................................... 3-4

3.3 The Right Side and Bottom .......................................................................................... 3-5

U E (P

3-1

Thie Front 7

Operation panel Front cover

Drain valve lever Front cover opening button

1. The front

Description

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.

P

a Oh 1

OFF0

I I

flow/press pressure p.rnax p.min r-3 L J I

\ I

7

3-2 LC- 1 OAD

-1 TheFront

No. Name of Part

0 Pump head holder

a Pump head Q Washing tube A

@ Check valve IN 0 Pump inlet @ Washing tube B

0 Pump outlet

@ Line filter Q Drain valve

0 Drain tube connection

0 Check valve OUT

2. Inside the Front Cover

Description

Has a flow line that washes the plunger. The pump head is mounted

on the holder. 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.

U C Q

3-3

C 0 0 C 3 l A U C (II

C 0 0

u) C

.- c

.- c 2 CI

s

T

The Rear 7

\ I

Q

No. Parts Name

0 External input/ciutput terminal block

a Grounding tern inal

0 Power cord connector

@ Fuse holder 6) S0L.V connectx

@ REMOTE connector

Description

Used to make connection with external equipment.

Use this terminal for grounding the module.

Used to connect a power cord.

A fuse is put in the holder. Use to connect a solenoid valve. See "Section 4.1 1.1 Wiring with

FCV- 1 OAL." Used to connect with SCL-IOA or an additional LC-IOAD. See "Section 4.10 Installation of the High Pressure Gradient Delivery

System." 1

3-4 LC- 1 OAD

EQ

7 1

The Right Side and Bottom

No.

0 a 0 @

Name of Part Description

Drain opening for liquid leakage

Mixer mounting screws

Cooling fan Fixing screws for transportation

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

3-5

Screws for Transportation."

LC- 1 OAD

Chapter 4 Installation

4.1

4.2

4.3

4.4

4.5

4.6

4.7

4.8

4.9

contents

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

4.10 Installation of the High Pressure Gradient Delivery System ..................................... 4-24

4.1 1 Installation of the Low Pressure Gradient Delivery System ...................................... 4-27

4.12 Installation of the Automatic Washing Kit ................................................................... 4-30

4-1

LC-1 OAD

Conditions for Installation Location r n E For correct and safe use of the module, care should be taken for the following, when installing the module.

1. Environmental Conditions

2. Precautions on Ventilation and Fire

3. Electromagnetic IUoise

4. Installation Space Requirements

5. Use in the patient environment

<<Cautions>>

To assure long service life and good performance of the module, avoid installing in a place where corrosive gases or dust are present.

0 Be sure to ventilate the room when inflammable or toxic solvents are used as mobile phases.

0 Never use open flames in the room particularly when inflammable solvents are used.

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 35°C. Variation

in temperatures in a day should be minimum. (2) Avoid any direct below from a heater or cooler. (3) Avoid installing the module in direct sunlight. (4) No vibration is allowed.

4-2 LC- 1 OAD

Examples of System Configuration m The following shows examples of system configuration for a high performance liquid chromatograph incorporating the LC- 10AD.

1. Simple System

Degasi

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.

Reservoir

f i e r (DGU-4

box

.A ) ~

Detector (SPD-1OA)

Column oven (CTO-1OA)

Manual injector (7125)

Pump (LC-1OAD)

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)


Manual injector (7125) Reservoir box

Degasifier (DGU-3A)

Option box S

delivery module (FCV-1OAL)

atopac ( C-R 6A)

Low pressure gradient 0

4-3 LC- 1 OAD

3. Low Pressure Gradient Delivery System 2

A low pressure gradient delivery system including an automatic injector 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)


Degasifier (DG U-1OA)

Syringe module

module (FCV-1OAL)

-1- Approx. 800mm-I Pump (LC-1OAD)

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)


Manual injector (7125) Reservoir box

Dega:,if i e r ( D G U -4A)

C - 2 6 0 d I, ,601- I 4 0 0 Pump (LC-1OAD)

\ d u m p (LC-1OAD) L Approx. 540mm

7

4-4 LC- I OAD

-1 Examples of System Configuration

5. 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 control ler (SCL-1OA) - Detector (SP D-IOA) Reservoir ~

-7 Reservoir box - Automat ic injector ~ -

Lnromaropac


SamDle cooler 1 UII uux L w I I Y l ' I M ixe r , !

Resevoir selector valve

Approx. 800mm Pump (LC-1OAD)

(C-R4A)

4-5 LC-1 OAD

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.

<<Caution>>

Fixing screws for transportation

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

Mounting of Multiple Modules Em 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 ) Unscrew the screws that are used to fix module cases. (2) Use the screws unscrewed to fix the mounting plate.

, Mounting plate

/ Screws

4-7 LC-1 OAD

Electrical Connections m K 1 --.

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.

1. Connection to the Power Outlet

(1) 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

7

4-8 LC- 1 OAD

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.

c

Connecting the Suction Filter

(1) 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.

(2) ( 3 )

(4)

( 5 )

4-9 LC-1 OAD

- /b ig of the Module 1

( 6 ) Fix the tube using the tubing cramp as shown in the illustration below.

Bush 3 0

<<Cautions>>

Suction filter

0

0

0

4. Connecting the Drain Tube (1)

(2) (3)

& Remove bush 3D.

Suction filter

7

7

Tubing cramp

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.

4-10 LC- 1 OAD

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 “\

\

-, ‘\

I

Tubing cramp

Put the waste container on the f loor o r the like so that it is 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.

for l iquid leakage

F i t the tube. & Waste container

4-1 1 LC-1 OAD

Connecting the Degasifier ?

Degassing the mobile phase has two effects that follow and is needed for constantly stable analyses. (1) (2)

It prevents troubles caused by generation of bubbles. 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. 7

1. Connection of the DGU-2A (helium degassing)

Use helium gas of high purity (99.995% or higher) for degassing. (1) For tubing, set a pressure reducer (optional) and carrier gas pipe

between the helium gas cylinder and the DGU-2A.

<<Caution>>

?

" He GAS IN " Helium gas inlet

(2) For reservoir, prepare a thick walled heat resistant screw capped glass container. (A commonly used glass reagent container of capacity 500 or 1000ml).

Helium gas c:ylinder

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

7

4-12 LC-1 OAD

(FrCorlnect ing the Degasifier

Part Name Description Category

0 c3

Bottle cap

Lid

Outer lid of the reservoir

Inner lid of the reservoir 0 Teflon packing Packing for the inner lid

@ Teflon tubing 3 .0~2 .0~230 -

0 Teflon tubing 3.0x2.0 Connected to the pump inlet. Filter section of the suction filter Helium gas bubbling filter

Used to filter the mobile phase. Helium gas bubbling filter 3x2~600 To be connected to an "OUT' (A, B, C, D) port of the

8 a 0 Teflon tubing

(3) Assemble the reservoir cap as shown in the illustration.

To DGU-2A

To the

-0 inlet

DGU-2A. 3x2~600 To be connected to an "IN" (A, B, C, D) port of the DGU-2A.

Parts @ and @ above a::e accessories for the LC-1OAD. Parts of other numbers are accessories for the DGU-2A.

4-13 LC- 1 OAD

7 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.

TO 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 stop joints, 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- 1 OAD

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)

Venti lat ion f r o m the D G U - I A l u m i n u m f o i l

5;g Vent i la t ing fan

-2A

' " ''1 Solvent miscible w i t h 1 3 7 the mobi le 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 stop joints, which will be needed to protect the degasifier from mixing of dust in flow line when it is not used for long.

D G U - 3 A

Connect these tubes to the pump inlet.

Accessory Tef lon tub ing included i n the DGU- 3A

Use bushes 3D that are accessories

k Use bushes 3 0 that are \ accessories fo r the DGU-3A

1'1 Bushes 3D that are accessories for the suction f i l ter m a y a lso be used. fo r the DGU- 3A

4-15 LC-1 OAD

4. When Connecting the By connecting the FCV-1OAL to the module, low pressure gradient delivery is available. If you use the DGU-3Afor degassing the mobile phase in such low pressure gradient delivery, follow the instructions below:

DGU-3A to the FC'V-1OAL:

(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:

D G U - 3 A

0 3 0

0 2 0 IN OUT

---. L C- 1 O A D

oc 0 =- To injector 00

-----a A

D G U - 3 A F C V - 1 O A L IN OUT

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 228- 28000-9 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) (2)

The right side face of the module The left side, inside the CTO-1OA

2. Mixer Capacity

(3)

Options from three types of mixer capacity that follow is available. Select the right mixer capacity according to your analyzing purposes.

The right side, inside the CTO-IOA

c 0 Q

Q UJ C

(1) 0.5ml (2) 1.7ml

.- c - - (3) 2.6ml c

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.

- 3. Selecting Mixer Capacity

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

/ T o the injector inlet /

Remove tubing and f i t caps for dust prevention.

To the injector inlet

U

To the injector inlet

7

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 I

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:

\

-.

Unscrew the screws Y

Refasten the screws

4-18

LC- 1 OAD

- - p u n t i n g 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."

(4) Remount the mixer cover.

Screw

E 0 .-

5. Building the Mixer into CTO-1OA (mounting)

I The pre- mixer section appears outside the cover.

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).

1 0 1 5 m m

4-19 LC-1 OAD

(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 1 1 ' + Pre-mixer

7

4-20 LC-1 OAD

I

,-

Connections of the Injector, Column, and Detector

I

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 Taking the case of connection between the module and manual injector model 7 125, the connection will be described. Manual Injector

<<Cautions>>

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.

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) 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.

(2) ( 3 )

<<Cautions>> 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.

0

Cut the pipe perpendicular Cyl indr ica l section t o the axis

Male nut 1.6MF Ferrule 1.6F

C T O - 1 Q A , r - - - - - -- ---

To the detector

I

I I

The manual injector rear view I

7

4-22 LC-1 OAD

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) 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

(2)

(3)

following illustration. See cautions for "Section 4.9.2 Connection between the Injector and Column."

E 0

Q

v) E

.- c Coupling Column

- - Pipe f rom the inlcst of SPD- Q c.

I

Male nut PEEK ETFE tube (Fasten man ua I I v.) From 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.

1. Wiring for Control through (1) the SCL-1OA

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.

Connect the REMOTE connector on the rear of the module and the REMOTE connector on the rear of the SCL- 10A using the

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.")

optical cabke included in accessories for the module. ?

rear view ,'/ /

,

Connect the cable to either of channels f rom 1 to 8.

4-24 LC-IOAD

- p i l l a t i o n of the High Pressure Gradient Delivery System

2. Wiring for Control by Two (1) Connect two modules of LC-1OAD at the REMOTEconnectors Modules of the LC-1OAD on the rear panel, using the accessory optical wiring cable.

Optical cable __

The LC-1OAD ", ,, rear view

(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 be described.

As a piping example, piping of two modules of LC-lOAD, degasifier, and mixer that construct a binary high pressure gradient system will

LC-1 O A D M I xer

L C - 1 O A D V' Mobile phases

Carry out piping referring to the following connection method.

(1) 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.

(2)

4-25 LC-1 OAD

~

-/tallation of the High Pressure Gradient Delivery System ] 7

(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.

A L C - 1 O A D

Pre- mixer sect

I in jector

Inlet B

(4) 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." ( 5 ) -

4-26 LC- 1 OAD

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-1 OAL (1) 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.

(2) 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- 1 OAL.

<<Cautions>>

Screws

FCV-IOAL rear view Cable

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- 1 OAL as closer to the LC-1OAD as possible.

4-27 LC-1 OAD

2. Tubing of the Lowf Pressure Gradient Delivery System

Carry out tubing referring to the following connecting method.

(1 ) Prepare reservoir containers. Because degassing of the mobile 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. 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.

(2)

<<Caution>> 0 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-1 OAD

, p a l l a t i o n of the Low Pressure Gradient Deliverv Svstem - - I

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."

SUS pipe A '\ Connection por t for sus pipe A

\\, 1 l ine f i l ter

Check valve

Check

OUT

valve

A -

ou

,

/

A

Inlet B

' SUS pipe B

sus

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.

<<Caution>>

(/ \

I Outlet \, ,' &\d, A h. . , . .

Washing 13, Teflon tube tube B on the left

Washing tube B on the r ight Automatic washing k i t

I

-7 Washing tube A on the left

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.

T

4-30 LC-1 OAD

Chapter 5 Operation

5.1

5.2

5.3

5.4

5.5

5.6

5.7

5.8

5.9

5.10

Basic Operation ................................................................................................................ 5-2

Operation of Constant Flow Solvent delivery ............................................................. 5-7

Operation of Constant Pressure Solvent delivery ........................................................ 5-10

Creation of Time Programs and Execution ................................................................. 5-1 1

AUX. Functions ............................................................................................................... 5-17

High Pressure Gradient Delivery Mode ....................................................................... 5-26

Low Pressure: Gradient Delivery Mode ........................................................................ 5-28

Operation of Automatic Washing Kit ........................................................................... 5-29

Operation of Manual Washing ....................................................................................... 5-30

Replacement of Mobile Phase ....................................................................................... 5-3 1

5-1 LC- 1 OAD

-~

C 0 .- c E 0 Q) P

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)

(2)

<<Caution>>

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.

Power switch OFF state Power switch ON state

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.

f flow/press pressure p.max p.min

\ \ I / /

I lo.000 0 100 01 v / I \ \ I pump prog run remote &ow cpress 0 0 0 1 0

-\

If an error message is displayed after switching power on, see "Section 9.2 Error Messages" for measures.

5-2 LC- I OAD

m ( i c Operation

Indication or Name

flow/press

pressure p.max

p.min

Pump

prog run

remote

c.tlow

c.press

2. Description of the Display The display has the display screen and LED lamps, whose names and

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. 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 l i t when the pump is in operation.

Programmed operation indicator lamp The lamp is l i t 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 l i t when the module is in the constant flow solvent delivery mode.

Constant pressure solvent delivery mode lamp

The lamp is l i t when the module is in the constant pressure solvent delivery

functions are as follows:

No.

0

8

5-3 LC- 1 OAD

~

i

)Basic Operation 7

3. Description of Keys The module has 20 keys on the front panel which are used for operation and setting. Functions of each key are as follows.

(pump) Pumpkey \ - 1

[m) Purgekey

0, 8 (del) Delete key

ledlt) Edit key

hd Run kev I

(CE) Clear key

[backj Back key

(G) Function key

edit

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. 1

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.

-.

[Enter] Enter key

@-19) Numeric keys

Puts into effect the entry value for each setting parameter.

Used to enter numeric values for each setting parameter.

5 -4 LC- 1 OAD

I s i c Operation

Setting parameter

press

pmax

pmin 2 4. Setting Parameter List Setting parameters, setting ranges, minimum values, initial values, and

modes used for basic operation are as follows:

Setting range Setting step Initial value Mode

0-9.999ml/rnin 0.001 ml/min Oml/min Constant flow solvent

1 0-400kgf/cm2 1 kgf/cm2 IOkgf/crn' Constant pressure solvent

1 0-440kgf/cm2 1 kgf/cm' 1 OOkgf/cm2

0-440kgf/cm2 1 kgf/cm' Okgf/cm2

delivery

delivery

Note)

Note)

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 pressure p.max p.min I I b:'b"o' 0 1 0 0 0 I

( / / / I \ \ \ J

Enter a value with a numeric key then press [E] 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 txrnax D.min \ \ I / /

/ / I \ \ 1 0 0 0 0 . 0 0 0 0 1

To cancel the value during setting, press CCE] before pressing (Enter). I

To return the screen, after setting, to the initial state, press a. 6. Setting the Maximum

Pressure Limit Value 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

E R R O R P . M A X 1

E c

0 .- 4- E a 8

The setting procedures are as follows:

5-5 LC- 1 OAD

- / B a s i c Operation

<<Setting Example>> 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 p.min \ \ I / /

/ / I \ \ 1 0 0 0 0 . 0 0 0 0 3

(2) PressQ,@,@,and[&].


l o . 0 0 0 0 \ \ I / / 1 5 0 0 0 1 I / / I \ \ J

7. 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 E

L

<<Setting Example>>

<<Caution>>

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 1 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 0 1 5 0 0 0

(2) Press 0 ,@ , and [Entel.) . The following will be displayed, and the setting is complete.


/ / I \ \ 1 5 0 2 0 0 . 0 0 0 0

Value 0 may be set for p.min but the limiter will not function.

5-6 LC-1 OAD

Operation of Constant Flow Solvent delivery Nm 1. An Operation Example of

Constant Flow Solvent delivery. delivery

The following is an example of operation for constant flow solvent

(1) Prepare a mobile phase and fill it into a reservoir, and set the suction filter into the reservoir.

(2) Make connections of flow line referring to "Section 4.9 Con- nections 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.)

(3)

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 Func- tions.") 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.

(6)

(7)

flow/press pressure p.rnax p.min

1 0 0 0 \ \ \ I / /

( 2 . 0 0 6 0 / / / I \ \ \ 1

(8) By pressing[=) , the pump will operate.

5-7 LC- 1 OAD

j p e r a t i o n of Constant Flow Solvent deliverv

<<Cautions>>

Observe ten seconds the condition of liquid discharged from the drain tube. If the liquid is being discharged constantly, the module is operating normal.

i Reservoir

L iquid f lowing \

direction

‘I:

Drain tube connection port Drain tube 1 , 9

Suction filter

u Waste container

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 YT\\ u Syringe needle

@g-j-+ Tube cramps

Disposable syringe e Suck the

mobile phase. -1

5-8 LC-1 OAD

-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 0 0 0 \ \ I I / ( 1 . 0 0 6 o

( 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

C 0 .- c E Q)

op

Operation of Constant Pressure Solvent delivery 7

1. An Example of Operation The following is an example of the operation of constant pressure of Constant Pressure solvent delivery.

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 lf...I till the following is displayed on the screen.


0 . 0 0 0 M O D E C H A N G E ]

(3) Each time [Enter] 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.

(4) 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 pressure mmax txmin \ \ I / /

/ / I \ \ 1 0 . 0 1 0 0 0 0

Set pressure with a numeric key. Example) When you want to set 20kgf/cm2, press 0, @ ,

and [ Enter) .


( 2 0 . 0 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-1 OAD

Creation of Time Programs and Execution rn

Instruction Description Setting range

FLOW Flow rate (effective only i n the constant flow 0-9.999ml/min

The module permits control of parameters such as flow rate by a time program. The created time program is stored as a file.

Remarks

The miniinurn step is

1. Instruction List

PRESS

The following is a list of instructions that are used for creating a time program.

solvent delivery mode) 0.001 ml/min Pressure (effective only in the constant pres- 1 O-400kgf/cm2 The minimum step is 1 kgf/cm'

sv

EVNT

LOOP

STOP

GOT0

Open/closes solenoid valve in the FCV- IOAL or FCV-I IAL(S) (optional). Event output ON/OFF 0, 1.2. 12 Select one among the four

I , 2. 3 ,4 0- 123 Note 1 )

See Note 1.

numeric values.

The minimum step is 1. Repeats a program from the first step. from 0 to 255

Value 0 repeats a program 256 times.

Ends a propram. Not applicable

Runs programs by linking riles. 0-9

(UD to 10 tiles)

I sure solvent deliverv mode) I I

BCNC

CCNC

Concentration 0 1 liquid B (ellective only 0-IOOc/C Note 2) The minimum step is 0.1 %.

when SYS=7 or 1

Concentration of liquid C (cffcctivc only 0-100% Note 2) The minimum step is 0.1 c/o.

when SYS=1) DCNC I Concentration of liquid D (ell'cctivc only 1 0-100% Note 2) 1 The minimum step is 0.1 c / o .

1 whenSYS=I)

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%.

The concentration of liquid A is determined by subtracting the sum of BCNC, CCNC, and DCNC from 100.

BCNC + CCNC + DCNC - I 100

ACNC = 100 - (BCNC + CCNC + DCNC)

El E

0

Q)

.- c E 8

5-11

C 0

Q .- c L

2. Description of the To create a time program, set the module to the edit mode, then proceed to programming. The procedures are as follows:

(1) Display Screen

Press @, then the following will be displayed.

flow/press pressure p.max pmin [ m q @ Number of steps already programmed in the selected file

0 Number 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. (2) Now press(=), then the following will be displayed.

Abbreviation of a word used


@ Elapsed time (minute) from the start of program 0 Instruction name 0 Set value Press(=) once again, then the following will be displayed. (3 )

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- 1 OAD

-1 Creation of Time Programs and Execution

3. 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

0 . 0 0 0 0 1 0 0 0

Press m. 4 /CEJ i

flow/press pressure pmax p.min f \ . 0 U 3 2 0 L E I

L PressfEnter).

flow/press pressure pmax p.rnin \ \ \ I / / /

/ / / I \ \ \ T I M E F U N C V A L U E

Press (Enter).

flow/Dress Dressure Dmax D.min \ \ \ I / / /

/ / / I \ \ \ 5 . 0 0 F L O W 5 . 0 0 0 -

Enter time value (with numeric keys), then press (Enter). flow/press pressure pmax p.min

\ \ \ I / / / 2 0 . 0 0 F L O W

/ / / I \ \ \ 1 Each t i m e m is pressed, an instruction is displayed in turn. . - \ j -

When the desired instruction appears, press (E) , then the instruction is set.


2 0 . 0 0 B C N C V A L U E \ \ \ 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

3 0 \ \ I / / [ > o . 0 6 B C N C

/ / / I \ \ \ 1 next step

LC-1 OAD 5-13

4. An Example of Creating 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 Program

TIME FUNC 15.00 FLOW 20.00 FLOW 30.00 STOP

rnl/min

t

.-

VALUE 2.000 5 .000

I I I

I I I I 1 I -A

15 20 30 min

Press @to return to the initial screen.


/ / / I \ \ \ 1 0 0 0 [ I . 0 0 6 0


r 0 U 3 2 0 L E

--.

Press( Enter].

flow/Dress Dressure D.max pmin

--. \ \ \ I / / /

/ / / I \ \ \ T I M E F U N C V A L U E

Enter the time (minute) for the initial step. Press Q, @, and [G) .

flowhress Dressure Dmax amin \ \ \ I / / /

1 5 . 0 0 F L O W / / / I \ \ \ 1

Select an instruction. When an instruction other than FLOW is displayed, press@ to display FLOW and press(=].

flow/press pressure pmax p.min [ I s . 0 0 F L O W V A L U g ] \ \ \ I / /

/ / / 1 \ \ \

5- 14 LC-1 OAD

-1 Creation of Time Programs and Execution

5. Deleting a Step

Enter the flow rate. Press @ and ( G I . flowhress pressure p.max rxmin

\ \ \ I / / /

/ / / I \ \ \ 1 5 . 0 0 F L O W 2 . 0 0 0

Similarly to from (4) to (6) above, set the second step. Press 0, @ , - ( E l , (Enter), Q, and (Enter).

flow/press pressure mmax p.min \ \ \ I / / /

/ / / I \ \ \ 2 0 . 0 0 F L O W 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 pressure p.max p.min \ \ \ I / / / 3 0 . 0 0 S T O P / / / I \ \ \ 1

Press @ to end the creation of the time program. A time program having three steps has been completed.


3 U 3 1 7 L E

By pressing @once again, the initial screen shown in (1 ) will return.

[

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.


1 5 . 0 0 F L O W 2 . 0 0 0 \ \ \ I / / /

/ / / I \ \ \

(2) Press@.


( 2 0 . 0 6 F L O W 5 . 0 0 0 1 \ \ \ I / /

/ / I I \ \ \

Now the first step of the program is deleted and the second step is displayed .

E C

0 .- CI

f 8

5-15 LC- 1 OAD

6. LOOP Instruction Use of the LOOP instruction permits repeating a program for a number of times you set.

TIME FUNC VALUE 0 15.00 FLOW 2.000 0 20.00 FLOW 5.000

30.00 LOOP 3

The above setting will run steps @ and Q three times repeating a cycle of thirty minutes.

t 0 .- c E 0 Q, Q

7. Start/Stop

0 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. 0 To run the time program endlessly. 0 To link program files by the GOTO instruction.

fly

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.

(2) 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 cr..). The prog run lamp is turned off. The time program now stops. 1

5-16 LC- 1 OAD

m- 1. AUX-FUNC List

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.

The following table lists AUX.FUNC functions.

TY Pe Name Function

1 BCONC

1 CCONC 1 DCONC 1 FILE NUM A file number is selected.

1 FILECOPY Copies a file. 2 FILEDEL Deletes a tile.

1 sv I EVENT Sets relay contact point output.

I EXT-S

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.

Solenoid valve in the optionally available FCV-IOAL or FCV-11 AL is selected.

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

I error.

Set value at plant

0 0 0

0 -

-

1

0 0

S-PROT Reduces flow rate without stopping the pump when thc pressure exceeds the set

Changes solvent delivery modes.

value of p.max.

I MoNFLoW

0

-

Monitors solvent delivery flow rate in the constant pressure solvent delivery

mode.

MON REV

Monitors elapsed time when running a time program. 0 0 Monitors integrated number of uumu revolutions.

1

3 1

1

2

MON ID Monitors pump’s ID. 0

P-SET Used when replacing the plunger and plunger seal. -

PULSE Varies pulsation. 48 ZEROADJ Carries out zero adjustment for monitoring pressure. -

COND Diagnose conditions of pump’s solvent delivery, and displays the results. -

Key entry is disabled.

Sets the man for uressure signals in the recorder outmt.

1 1 the module.

-

10 +%- 1 I ADRS 1 Sets the address of the device when making control from the system controller. 1 1

Enter a value according to the conditions of the system in use. Sets the type of selector valve connected to the S0L.V connector on the rear of

1 0

BCONC is displayed only when SYS=2 or 4. CCONC and DCONC are displayed only when SYS=4.

Selects whether control is made from the system controller or by the pump.

Purge execution time.

c 0 .- w

f 8

0

3 .O

5-17 LC-1 OAD

..--

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 iEnter) to execute the function. Type 3 : The current condition is displayed.

2. Setting Procedures for AUX.FUNC

BCONC, CCONC, DCONC flow/press pressure p.rnax p.rnin

(Concentration setting) [ 0 . 0 0 0 B C O N C b\."d] / / I \ \

Concentration of each liquid is set when selecting gradient delivery mode. Enter concentration of each liquid with a numeric key, then press --,

(E) . (Unit: %'.>

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.

flow/press pressure p.max p.min f \ I > 10. o o o F I L E C O P Y / I ' i j

Enter the desired file number with the numeric keys, then press /Enterj.

FILE COPY (Selecting where the file is copied to)

FILE DEL (Deleting a file)

flow/press pressure p.max p.min \ I /

1 0 . 0 0 0 F I L E N U M / I \ 1

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 [ G I .

flow/Dress Dressure p.max p.min

0 . 0 0 0 F I L E D E L J The all contents of the time program of currently selected file is deleted. Press Enter 1 .

7

5- 18 LC-1 OAD

- E X . Functions

Solenoid valve type Set value

FCV- 1 OAL 1

2

3 4

sv (Setting

Selected mobile phase

Liquid A

Liquid B Liquid C Liquid D

<<Caution>>

Solenoid valve type Set value

FCV-1lAL 0

1

2 3

solenoid valve)

Selected mobile phase

All channels are set to the A side.

Channel 1 is set to the B side.



EVENT (Setting EVENT output terminals)

Set value EVENT 1 output

0 Relay 1 OFF 1 Relay 1 ON 2 Relay 1 OFF

12 Relay 1 ON

flow/press pressure p.max p.min -

EVENT 2 output

Relay 2 OFF

Relay 2 OFF Relay 2 ON

Relay 2 ON

I o . 0 0 0 s v \ I /

1 1

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).

Example: By setting SV 123, channels 1,2, and 3 are all set to the B side.

Before setting SV, enter a value for FCV TYPE to select the solenoid valve unit used.

flow/Dress Dressure D.rnax D.rnin f \ I /)

- 0 - J / I \

0 . 0 0 0 E V E N T

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).

5-19

-1 AUX. Functions

EXT-S (Function setting for the flow/press pressure p.max p.min

\ I / 0 . 0 0 0 E X T - S 1 EVENT output terminals)

-\

C .- .c. 0 <<Caution>> 2 Q)

6

0 1

S-PROT (Setting the system protection)

Relay contact points are controlled by the EVENT set value.

Relay contact point 1 (EVENT 1) is used as a start signal for a

MODE CHANGE (Selecting a solvent delivery mode)

0 1

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[=].

Cancels the system protection.

Sets the svstem Drotection.

I Set value I Function I

I I time Droeram. I Relay contact point 2 (EVENT 2) is used as an error output

simal.

I 3 I Both functions 1 and 2 may be used.

The use of the EXT-S function disables effects of the EVENT parameter relevant to the corresponding EVENT terminal.

flow/press Dressure mmax nmin

[ O . 0 0 0 S- PROT ‘ b’l

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 I Function

To release the P.MAX error, press=. Then the alarm will stop, and the value that was set before the error occurrence is reset.

flowhress Dressure mmax mmin

[ O . 0 0 0 M O D E C H A N G E )

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-1 OAD

mmX. Functions 1

Set value

MON FLOW (Displaying flow rate at the constant pressure solvent delivery mode)

Function


0 1

\ I / [ O . 0 0 0 M O N F L O W 0 1

Cancels the flow rate displaying function.

Sets the flow rate displaying function.

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 Function

0 Cancels monitoring the elapsed time of program.

. 1 Sets monitoring the elapsed time of program.

MON TIME (Monitoring the elapsed time of program)

Set value

0 1

Function

Cancels monitoring the integrated number of pump revolution. Sets monitoring the integrated number of pump revnlirtinn

flow/press pressure p.max p.min r \ I /> 1 0 . 0 0 0 M O N T I M E / I \ - 0

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[=).

MON REV (Monitoring the integrated number of pump revolution)


0 . 0 0 0 M O N R E V 0 \ I /

/ 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(=).

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/cm2 using water.

C 0

m .- 4-

5-2! 1

0

1

MON ID (ID indication for remote control)

Cancels the ID indication.

Sets the ID indication.

COND (Condition indication)

flow/press pressure p.max p.min \ I I

( 0 . 0 0 0 M O N I D 0

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) .

I Function


0 . 0 0 0 P U M P A

If the SCL- IOA is not connected, the following will be displayed.

flow/press pressure pmax pmin

( 0 . 0 0 0 N O T L I N K E D ]

flow/press pressure p.max D.min

10. 0 0 0 C O N D N O R M A L ]

--..

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 C O N D X R 1 The discharging pressure of the pump on the left is low, the following is displayed.


1 0 . 0 0 0 C O N D X L

If the pressure has increased 10% or more from five minutes ago. the following will be displayed.


0 . 0 0 0 I N C 7 5-22

LC-1 OAD

mmX. Functions

If the pressure has decreased 10% or more from five minutes ago, the following will be displayed.


<<Cautions>>

P-SET (Plunger set)

[ 0 . 0 0 0 D E C 1 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.


/ I \ 0 0 . 0 0 0 P - S E T

Moves the plunger. Enter the set value with a numeric key, then press(Enter).

Function I 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 flow/press pressure p.max p.min

pulsation compensation) 0 . 0 0 0 P U L S E 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.

~~ I Mobile ph&e 1 Typical value I Water Methanol Hexane

As a standard, a smaller value is set to a liquid of greater compres-

E C

0 .- c E 0 K

sibility.

5-23

C 0

m .- c.

Set value

1

2

4

-1 AUX. Functions 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.

ZERO ADJ (Zero adjustment for pressure indication)


0 . 0 0 0 Z E R O A D J

CLOSE KEY (Disabling key entry)

RANGE (Changing the recorder range)

SYS (Setting the system parameter)

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.


0 . 0 0 0 C L O S E 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.


/ / I \ \ 0 . 0 0 0 R A N G E 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.

flow/press pressure p m a x pmin f \ I /) . ,

4 1 \ / I \ 1 0 . 0 0 0 S Y S

Sets a system parameter. Enter the set value with a numeric key then, press[=).

-.

---.

Values other than the above shall not be set.

5-24 LC-1 OAD

-1 AUX. Functions

0 1

FCV.TY PE (Selection of solenoid valve unit)

FCV- 1 OAL

FCV- 1 1 AL

LOCAL (Setting the local mode)

0 1

P TIME (Purge timer)

Control is made from the SCL-IOA.

The module is operated independently (local mode).

ADRS (Setting the remote address)


0 . O O O F C V T Y P E 0

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 Set value 1 Solenoid valve unit I


( 0 . 0 0 0 L O C A L 0 7

.I c, 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 I%).

I Function

flow/press pressure pmax p.min

rl.000 P T I M E R 3.0 'I Set purge time in the range of 0.0 - 9.9(min).


/ I \ 3 0 . 0 0 0 A D R S

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 Address I Function I I 1-16 1 Theseareuortnumbersusedwhencontrolledfrom theSCL-1OA. I

85 1 For a high pressure gradient delivery system without SCL-IOA.

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.

1. Preliminary Setting (1)

(2)

(3)

2. Setting Initial Conditions (1)

(2)

( 3 )

For the operation through the system controller, see "System Controller Instruction Manual." For ternary high pressure gradient, the system controller is necessary.

Enter 2 for system parameter SYS of the LC- the other (called pump A). Enter 1 for system parameter SYS of the controlled by the other (called pump B).

OAD that controls

LC-1OAD that is

For the procedures for setting the system parameter, see "Sec- tion 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.

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 simul- taneousl y.

ACONC(%) = loo(%) - BCONC(%)

-,

3. High Pressure Gradient 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.

Delivery Program

ACNC(%) = loo(%) - BCNC(%) For the BCNC instruction, setting range is from 0 to loo%, and the minimum step is 0.1 %.

<<Caution>> 0

Do not use the time programs of pump B. Parameter LOCAL is effective only the module is controlled from SCL- 10A.

5-26 LC-1 OAD

-(-h Pressure Gradient Delivery Mode

4. An Example of Program (1) Call the program setting screen. Setting (2) Enter time.

(3) (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.)

P r e s s m until BCNC is displayed on the setting screen.

Initial value for BCNC: 0.0

TIME FUNC VALUE 20.00 BCNC 100.0 30.00 BCNC 100.0 30.10 BCNC 0.0 40.00 STOP

5-27 LC-1 OAD

-

Low Pressure Gradient Delivery Mode rn 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.

1. Preliminary Setting (1) (2)

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

Concentration of liquid A (ACONC) is as follows.

(3)

DCONC to 25%. (See "Section 5.5 AUX. Functions.") -\

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) (3)

(4) ( 5 )

Press (pump) to start the pump. Draw the mobile phase from the pump outlet to fill the flow line with the mobile phase. Make sure that no bubbles are in the flow line. 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.

3. Low Pressure Gradient (1) Set the flow rate and concentration to the prescribed values, then press (z) to start solvent delivery. Operation

4. Low Pressure Gradient Delivery Program

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

m- ,--

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.

Operation of the Automatic Washing Kit L

1. Preparation (1) Set the automatic washing kit to the module referring to "Sec- tion 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.

(2)

(3)

/ \

Suck the solution

2. Operation

<<Cautions>>

(1)

1 Automatic\ /fl washing k i t outlet -a

-- Liquid 1 f lowing direction

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."

E C

0 .- CI

f op

5-29

1. Connections

Operation of Manual Washing m 7 -\ It is possible to wash the plunger and plunger seal manually without using the optional automatic washing kit.

2. Operation

ccCaution>>

(1) 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.

(2)

A on the left

Container such as beaker

direct ion Disposable syr inge

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.

5-30 LC- 1 OAD

Replacement of Mobile Phase m z 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.

1. Replacement of Mobile Phase with Another 200ml capacity. Miscible Mobile Phase

( 1) Fill a new mobile phase approx. lOOml into a container of about

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

(2)

(3) 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.

E 0

\ c, .- Open the d ra in valve. E (Turn the dra in valve 8 lever counterclockwlse.)

Waste container

5-3 1 LC- 1 OAD

C

-1 Replacement of Mobile Phase 1 -\ (4) Stop the purge by pressing [e) key, then displace connec-

tion at the outlet of the manual injector and put it into the waste 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 ra in valve ' Pump outlet (Turn the d ra in valve lever clockwise.)-i,

R ese I v o i r f i l led w i t h

&!J The inside of the m \*' Pump inlet Waste 1 1 ' 'i /"'I container u

new mobi le phase u

( 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)

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."

( 3 ) -\

5-32 LC-1 OAD

K4 replacement of Mobile Phase

3. Replacement of Mobile Use of a buffer solution as the mobile phase will produce crystalline substances upon dehydration or evaporation of the solution. Accord- ingly, replace the buffer solution as follows:

Phase of Buffer Solution

<<Caution>> 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."

E (3) Then replace the old with a new mobile phase. See procedures (1) to ( 5 ) of "Section 1 . Replacement of Miscible Mobile Phase ."

C 0 Use of a buffer solution as the mobile phase will produce crystalline

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 Wash- ing Kit" or "Section 5.9 Operation of Manual Washing."

.- 4. About Use of Buffer Solution(use of substances upon dehydration or evaporation of the solution, which c

f 8 washing flow line)

<<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 Operation Checking for Systems ................................................................................... 6-2

6.2 Checking Concentration for High Pressure Gradient Delivery .................................. 6-5

6.3 Checking Concentration for Low Pressure Gradient Delivery .................................. 6-7

6- 1

-\

Operation Checking for Systems

Operation checking for a simple system as shown in the following illustration is described here.

Detector (S PD-1OA) f I jReservoir Column oven (CTO-1OA)

1. Preparation

2. Connection

Reservoir box

Degasif ier( DGU- 4A) - 1. 4 I IF

L 3 7 0 -> Approx . 540rn

- R6A)

D G U - 4 A LC-1 O A D C T 0 - 1 0 A

r - - - T - -- - 1 ! 1

S P D- 1 0 A Chrornatopac

I - 1

Manual co lumn i n j ecto r Electric connect ion

3. Operation (example) (1) (2)

( 3 ) (4)

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- 1 OA.

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.

At the Chromatopac, press , 15( , 10/ , and -1 to set the pen position at the center. -\

6-2 LC- 1 OAD

m i e r a t i o n Checking for Systems

(9) At the Chromatopac, press I PLOT I and I ENTER I to carry out

(10) Wait until the baseline becomes stable.

plotting.

Example of good cases 0 Stable

Examples of bad cases x Having hai rs

Increases w i th t ime / passage. X

Decreases w i t h t ime passage.

X Unstable

E (1 1) At the Chromatopac, set ATTEN to 8. (The Chromatopac’s full scale becomes equivalent to 0.5AU.) - -

(12) At the Chromatopac, press I ZERO I , , , and

(13) At the Chromatopac, press -1 and m] to stop the .- z 6

(14) Inject sample into the flow line. 8 (15) At the same t h e , press vl of the Chromatopac.

E

x 0 Q)

IENTER].

plotter.

C CR

6-3

0) C z 0 Q, S 0 Q, 0 c Q

E f n

4. An Example of Result The following is an example of analysis under the conditions that of Analysis follows: (analysis example) Mobile phase :

Column Flow rate

Samples

(Analysis example)

H20/Acetonitrile = 15/85 Shim-pac CLC-ODS 6.0mm@ x 15cm 1 ml/min Wavelength 254nm, response 4 @Naphthalane lOmg 7

in IOOml methanol. CI Iniection

0 Biphenyl 5mg @ Acenaphthene 30mg @ Anthracene lmg @ Pyren 10mg

START 1

2.597 3.322

6.882

F8.463

C H R O M R T O P R C C-R6R SRMPLE N O 0 R E P O R T N O 5 1 5

P K N O T I ME R R E R M K I O N 0

1 4 . 8 5 7 2 1 4 3 1 9 2 5 I 4 4 5 9 3 4 5 5 s u 3 6 3 5 8 2 4 1 5 5 8 U 4 6 , 8 8 2 7 5 1 2 3 3 U 5 8 I 4 6 3 5 9 9 9 2 4

T O T R L 2 4 8 8 9 8 7 - - - - - - - - -

F I L E 0 M E T H O D 4 1

C O N E N R M E

8 , 9 4 7 1 2 4 , 7 1 7 1 1 0 , 8 6 8 3 Acenaphthene

3 1 , 2 8 8 5 Anthracene

2 4 I 9 8 6 5 Pyren

Naphthalene

Biphenyl

- - - - - - - - - - - - 1 0 0

6-4 LC-1 OAD

Concentration for High Pressure Gradient Delivery

1. Conditions

2. Specification

3. Precautions for Measurement

Using liquid A B : Distilled water

Flow rate : lml/min Load pressure : 1 0-30kgf/cm2 Measurement wavelength : 2S4nm

: 0.3% acetone water solution

At liquid A mixing ratios 10, SO, and 90%, concentration error +1% maximum

(1) (2)

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%. Then set the flow rate to 3ml/min. Close the drain valves and wash the flow line for 20 minutes.

( 3 )

E (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.

4. Measurement Example Initial parameter setting Flow rate : lml/min BCONC : 100

100%

ii

Time program

TIME FUNC 0.10 BCNC

10.00 BCNC 10.10 BCNC 20.00 BCNC 20.10 BCNC 30.00 BCNC 30.10 BCNC 40.00 BCNC 40.10 BCNC

VALUE 90.0 90.0 50.0 50.0 10.0 10.0 0.0 0.0

100.0

.-

6-5

w C x 0 Q)

- 6

i! 5

Q) 0 C

z &

[ Checking Concentration for High Pressure Gradient Delivery -\

Calculation

= 10% actual concentration A100

= 50% actual concentration AS0 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. Ac- cordingly, it is recommended to run the following BASIC program on the Chromatopac, to check the LEVEL value.

BASIC PROGRAM 10 PRINT LEVEL 20 WAIT 60 30 GOT0 10

6-6 LC- 1 OAD

Checking Concentration for Low Pressure Gradient Delivery

1. Conditions

2. Specification

3. Precaution for Measurement

Using liquid A : 0.3% acetone water solution Liquids B, C, and D : Distilled water Flow rate : 2ml/min Load pressure : 1 0-30kgf/cm2 Measurement wavelength : 254nm

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.

4. Measurement Example Low pressure gradient delivery using liquids A and B

I 100%

1 I 0

:I

Initial parameter setting Flow rate: 2ml/min B.CONC : 100.0 C.CONC : 0.0 D.CONC : 0.0

6-7 LC-1 OAD

~

Time program

TIME FUNC 0.10 BCNC

10.00 BCNC 10.10 BCNC 20.00 BCNC 20.10 BCNC 30.00 BCNC 30.10 BCNC 40.00 BCNC 40.10 BCNC

Calculation

VALUE 90.0 90.0 50.0 50.0 10.0 10.0 0.0 0.0

100.0

BASIC PROGRAM 10 PRINT LEVEL 20 WAIT 60 30 GOT0 10

''0 = 10% actual concentration Aioo

A100 = 50% actual concentration

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. Ac-

cram on cordingly, it is recommended to run the following BASIC pro5 the integrator. to check the LEVEL value.

6-8 LC- 1 OAD

Chapter 7 Control from the External Equipment

Contents

7.1 Connections of the Input/Output Terminals for External Equipment ....................... 7-2

7.2 Control from the SCL-IOA ............................................................................................ 7-4

7- 1

LC-1 OAD

Connections of the InputlOutput Terminals for External Equipment

1. The InpuVOutput Terminals for External Equipment

EXTERNAL OUTPUT - m I

EXTERNAL INPUT

I r-- 7-r ----

I EVENT1 EVENT2 ON OFF START STOP COM

I I I 1 I 1 1 I

PRESSURE

RECORDER

Signal name

EVENT 1

EVENT2

ON(PUMP)

OFF(PUMP)

START

STOP

COM. RECORDER

Description

Relay contact point output. The contact points make and break according to EVENT parameter values set in a program or AUX.FUNC setting. Relay contact point output. The contact points make and break according to EVENT parameter values set in a program or AUX.FUNC setting. 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.

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."

~

Remarks

The rated values of the relay contact points are 30VDC and

0.1A

Control is made possible by short-circuiting these signal terminals and "COM" terminal at contact points in external equip-

ment. The short-circuiting times (tc) shall be as follows: 0.5 sec < tc < 10 sec

Full scale voltage = 1 mV

7-2 LC-1 OAD

1 Connections of the Inputloutput Terminals for External Equipment

I I

2. Wiring

Use accessory remote cable for single wiring. For more wiring prepare cables as follows. (1) 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.

(2)

EXTERNAL OUTPUT EXTERNAL INPUT PRESSURE

EVENT1 EVENT2 ON OFF START STOP COM RECORDER

Core wire 1 Button 1 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: 0.3mm2 to 0.75mm2(AWG 22-20)

Element wire diameter: $0.18 at the minimum

7-3

c C

E P 3 U W Q

.-

- c 5 X w E E c

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 (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.

(PUMP.B), [ F E E ) .

--,

<<Caution>>

S Y S T E M C O N F I G U R A T I O N

P U U P . A L I N K E D

P U M P . B L I N K E D

P U M P . C L I N K E D

D E T . A L I N K E D

D E T . B L I N K E D L O C A L

A . I N J L I N K E D

F R C L I N K E D

O V E N L I N K E D L O C A L

S U B C L I N K E D

. . . p r e s s M E N U

P S t u s

/ o 0 R E A D Y

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.

7

a I P U W I b

(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.

If a module is marked with -1 , 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."

0

7-4 LC-1 OAD

-1 Control from the SCL-IOA

2. The Main Menu Screen From the CONFIG screen, press [El to display the main menu screen. It is possible to return to the main menu screen whenever you press [E] from any other screen in operation.

M E N U

A N A L Y S I S F I L E P A R A M E T E R S : o T I M E P R O G R A M : 1

P U M P C O N T R O L : 2

D E T C O N T R O L : 3

F R A C T I O N C O L L E C T O R : 4

A U T O I N J E C T O R / A N A L S E P U E N C E : S

M O N I T O R : 6

S Y S T E M : 7

t u . 9 9 9 9 . 9 0 / o 0 R E A D Y

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 [ G I . 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.

~~~~ ~ ~ ~~~ ~~ ~ ~~ ~

A N A L Y T I C A L P A R A M E T E R S F I L E 0

( I S O . ) A . F L O W 0 . 0 0 0 6 . F L O W 0 . 0 0 0 C . F L O W 0. 0 0 0 A . P R E S 0 6 . P R E S 0 C . P R E S 0 P . M A X 1 0 0 P . M I N 0 k E / c r n '

P U M P - - - - - - - - -

Contact point

D E T . A - - - - - - - _ _ _ - - - - - - - W A V E 3 8 0 n m

m l / r n i n R A N G E 1 . 2 5 0 0 A U F S m l / m i n W A V E 2 6 0 0 n m r n l / m i :

k g / c r n ' W A V E 1 9 5 n m k a / c r n ' R A N G E 2 . 5 6 0 0 A U F S k g / c m ' W A V E 2 2 0 0 nrn

k g / c m _ _ _ _ _ _ _ D E T . 6 - - - - - -

Operation

I 4 u L K V . 0

D \I " R V . C K 6 5 c

A . F L O W 0 - 9 i m t i m e n . a m

9 9 9 9 . 9 0 / o 0 R E A D Y

Detector 1 0 The m] column in the diagram shows parameters for the

solvent delivery modules.

The solvent delivery mode in use is indicated inside the paren- theses.

Press (funcj to display the functions that follow at the function line.

(1)

c C

Q 3 CT w (P

E .- - c E X w

7-S LC-1 OAD

c C

i! P 3 U W

.-

B.PRES

C.PRES

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

B.CONC C.CONC D.CONC B.CURV

~~

- Q

Q)

x

E U

C.CURV

D.CURV

P.MAX

P.MIN

W

Gradient curve for liquid C

Gradient curve for liquid D

Maximum pressure limit (kgf/cm') '7

Minimum pressure limit (kgf/cm*)

-\ -1 Control from the SCL-IOA

(2) Select a solvent delivery mode for the solvent delivery modules using the corresponding function key. (m ): Flow rates for up to three solvent delivery

modules may be controlled independently.

delivery using two solvent delivery modules (A, B). Flow rate for solvent delivery module C is controlled independently. m( a): 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

[B.GE] ( (f2) ): Conducts binary high pressure gradient

independently. Depending on the solvent delivery mode set, the number and contents of the parameters displayed on the screen will vary. Move the cursor with the arrow keys @ ,B ,m, a n d a ) to the parameter you want to change. Enter a new value and

*\

(3)

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 0, the setting range and minimum step for the parameter at which the cursor is will be displayed.

Example:

0 Parameters displayed on the screen are as follows (for the solvent delivery module only): -7

I Parameter 1 Description I

T.FLOW Sum of flow rates (ml/min) at gradient delivery

7-6 LC-1 OAD

-1 Control from the SCL-IOA

01 3 0 . 0 0 I 1 5 0 . 6 5 2 1 6 0 0 0 . 0

4. Time Program

B . C O N C I 1 0 0 W A V E A l 3 5 0 S T O P r

Program entry l ines

When the setting of the initial parameters from the parameter control screen is complete, press [menu)to return to the main menu screen and select PROGRAM I.

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 P R O G R A M F I L E 0 ( 8 . G E )

3 0 0 S T E P S L E F T X I T I M E I F U N C 1 V A L U E

S i 9 1

Instructions table.

F U N C T I O N F O R ( D E T . A D E T . B O T H E R ) 0 A . F L O W I 5 6 I 8 8. C U R V I 1 I A . P R E S 1 B . F L O W 1 6 C . I 9 C . C U R V I 1 2 B . P R E S 2 C . F L O W 1 7 D . C O N C I 1 O D . C U R V I 1 3 C . P R E S 4 T . F L O W 1 I I

9 9 9 9 . 9 0 / o 0 R E A D Y

I Operation (1) 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

Press (func) to select the function display that follows: [ G I , then the cursor moves to the field.

(2)

1 - I , - I -

(3) Use key I TABLEtl (lf41) or I TABLE-+I ( w) 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 F O R ( P U M P D E T . A D E T . 6 O T H E R ) I (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 1 PUMP I .

I 1 1 A . P R E S 1 B . F L O W 1 5 B . C O N C I 8 B . C U R V I 1 2 B . P R E S 2 C . F L O W 1 6 C . C O N C I 9 C . C U R V I 1 3 C . P R E S 4 T . F L O W 1 7 D . C O N C I I O D . C U R V l

0 A . F L O W 1 I

LC- 1 OAD 7-'7

-1 Control from the SCL-1OA I -\

E 2

w- - 2 c C s

piFq([T))

I.\'

Icopvj( [f3) )

ITABLEt/ (pi))

I I . \ -

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 numeric keys, the @field will show the number. By pressing

(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. If the entered instruction needs parameter value to be set, the cursor will move to the -1 field. Enter an appropriate value and press[=). If you select the help information by pressing [GI, 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 -1 field of the next step. Repeat the procedures (2) through (6) above and complete the time program.

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

(6)

*7

(7)

(%) , and the entered time will be cleared.

(8) The following operation may be carried out using the function keys from the time program screen. By pressing m, the function field switches and displays each function.

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.

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.

Moves the cursor in the module name field of the instructions table to the right.

I I 1 I

7

Any key entry is disabled except -](cancels the key lock).

7-8 LC- 1 OAD

-1 Control from the SCL-1OA

5. 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 1 from the main menu screen.

Screen mode

P U M P C O N T R O L O V E R L A Y / F I L E 0

Change of solvent delivery parameters\

0

0 t i m e n f i l e s r n p l / i n j f r c s t a t u s

T I M E 0 . 0 1 - 9 9 9 9 . 9 0 ( m l n 9 9 9 9 . 9 0 / o 0 R E A D Y

C . F L O W A . P R E S 6. P R E S C . P R E S S T O P

T I M E -

V A L U E 1

So I ven t 3 delivery mode

Solvent delivery parameter 1

- T i m e entry f ield

. Parameter value entry

field.

Operation

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.

Presslfuncj to switch the function display as follows:

I I (2)

0

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. By pressing function key (PARAMI( @), the 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 )

0

7 -5) LC-1 OAD

-1 Control from the SCL-IOA -7

<<Notes on Entry>>

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 vl in the time program.

Enter a parameter value with the numeric keys and press

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 I VALUE \field of the time program. If you set the solvent delivery mode to the high pressure gradient delivery and selected v) in (3) for parameter name, proceed from ( 5 ) to (8). '7

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 w] with the numeric 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).

0 10

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-1 OAD

-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 (,,,,I to return to the main menu and from the I TIME PROGRAM I screen, correct the wrong entry with the editing function.

Switching the Screen Mode The graphics display has two screen modes that follows: /OVERLAY] : All parameters listed at the right of the screen

are displayed graphically on the screen at once.

p q : Only the parameter selected with the vl 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.

Conducts high pressure binary gradient delivery using two solvent delivery modules (A, B). Flow rate for solvent delivery module C is controlled independently.

Conducts high pressure ternary gradient delivery using three solvent delivery modules.

Low pressure gradient delivery is carried out using solvent delivery module A. Flow rate for modules B and C is controlled independently.

pZq(B)

jl(@)

[ rn ] (pq) pAFiWJp5-J) Selects parameter name.

IG.MODE\(rn) Switches the screen display mode.

j i ( W ) Any key entry is disabled except -1 (cancels the key lock).

LC- 1 OAD

Chapter 8 Maintenance

Contents

8.1 Replacement of Plunger Seal ......................................................................................... 8-2

8.2 Replacement of Plunger and Diaphragm ...................................................................... 8-4

8.3 Cleaning and Replacement of Check Valves ............................................................... 8-6

8.4 Replacement of Line Filter ............................................................................................ 8-7

8.5 Replacement of Fuse ....................................................................................................... 8-8

8.6 Cleaning ............................................................................................................................ 8-9

8-'I LC- 1 OAD

Replacement of Plunger Seal

As a rule, the plunger seal shall be replaced approx. every 1000 hours of solvent delivery. (Water delivery at 1 ml/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." 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. Dismount the suction filter and remove SUS pipe A and the Teflon tube at the top and bottom of the pump head, respective-

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.

(2)

(3)

ly.

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 IN

7 \ - T e f l o n @ t u b e A

(4) Loosen the setscrew at thc center of the pump head clamping

plate for a half turn using the accessory Allen wrench.

8-2 LC-1 OAD

L

-1 Replacement of Plunger Seal

<<Caution>>

( 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 \ Pump head clamping plate Set screw Mounting screw

(6) 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.

(7 )

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 to pul l it away

a 0 C 4L Having a r im. lu I

Pump head

(8) (9)

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. (10)

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- 1 OAD

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." 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. Dismount the suction filter and remove SUS pipe A and the Teflon tube at the top and bottom of the pump head, respective-

-7

(2)

( 3 )

ly *

When dismounting the suction filter, lower the reservoir to a position lower than the inlet, or empty the mobile phase.

(4) Dismount the pump head referring to "Section 8.1 Replacement

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.

of Plunger Seal." -\

( 5 )

Two type of Allen wrenches are attached in the accessory. Use A type Allen wrench to loosen and

tighten the screws of head holder.

8-4 LC-1 OAD

-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.

<<Caution >>

<<Caution>>

Handle

(8) Mount a new diaphragm and plunger. Firmly fix the plunger with the box driver.

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.

(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.

QI 0 C (II

C c .- i

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-1 OAD

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 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.

Valves

2. Replacing the Check (1) Dismount the suction filter and remove the SUS pipe and Teflon tube at the top and bottom of the pump head, respectively. Valves

<<Caution>> When dismounting the suction filter, lower the reservoir to a position lower than the inlet, or empty the mobile phase. 'I

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.

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.

Qv Check valve OUT

Remove i t .

v,f&- Check valve I N

u

--\

8-6 LC-IOAD

Replacement of Line Filter

If a back pressure exists with the tubing at the pump outlet discon- nected, 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.

Drain 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-1 OAD

Chapter 9 Troubleshooting

I'

Contents

9.1 Symptoms and Countermeasures for Troubles ............................................................. 9-2

9.2 Error Messages ................................................................................................................. 9-4

9- 1

LC-1 OAD

Symptoms and Countermeasures for Troubles 7

Cause

1. Bubbles in the pump head.

2 . Old solvent rciiiains in the pump

chamber.

3. Bubbles i n tlic pipe of suction l i lter.

4. Malfunction of the check valves.

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.

Remedy

I . Flush liquid through the drain to purge bubbles.

2. Suck u p bubbles through tlic drain tubing with ii syringe.

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 the drai 11 tubing .

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.

1. Clean or reulace the check valves.

Symptom

S. Leak from the plunger se;iI.

6. Leak in tlie Ilow line.

7. Clogged tlow line.

1. Bubbllcs i n tlic pump clianibcr.

2. Air enters 1'1-om [lie joint betwccn the

suction filter and inlet pipe.

~~ ~ ~

Solvent dcl ivery is unstable.

Fluctuation in

Ilow rate is large.

1 . Replace the plunger seal.

2. Replace the plunger.

I . Retighten the joints.

2. Replacemelit of defective parts. 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.

The pump

operates. but solvent is not

dc 1 i v ercd .

1. Malfunction ol'tlie check valves

2. Clogged suction lilter

Measured llow

rate is lower than

the set flow rate.

1. Clcun or replace the check valves.

1. Cleiun or replace [lie suction filter.

I

9-2 LC- 1 OAD

mi Symptoms and Countermeasures for Troubles

1. The pressure giiugc docs no(

indicate zero properly.

2. The line liltcr l'or either pump i s

clogged.

3. One Ilow line is cloggcd 111 ;I point before [low I incs or two pumps becomes contlucnt.

Symptom

1. Carry out zero adjustment.

I . Clean or rcplacc the line filtcr.

I . Rcplucc the clogged tubing.

Prcssurc indica- t i o n s o f two

pulllps arc not

i tlc 11 I iccr I when

perlonning gr;rdicnt delivery. ( Dill'crcncc cclu;il

to or under ~ l i d c i i i ~ or 5% is consiclcred to

he normal.)

1. The power switch i s i iot turned ON. 2. Pump switch is not turned ON. The

pump key LED i s 1101 lit.

3. Flow rate indic:itioii rcmuins at 0.

Solvent i s not

tlclivcrcd.

(Pump i h not

opcratin_c. )

I . Turn the power switch ON. I . Prcss tlic pump key. 2. Control pumping from the SCL-IOA.

1. Set llow rate. 2. Set flow rate from the SCL-IOA.

Prcssurc does not

rise. 2. Leakage in flow line

I . Cltvged line l'ilicr Prcshurc rises cx-

ccssivcly.

1. Rctighleii joints.

2. Replaccment of defective parts.

I , Clean line filter. 2. Renliice linc filter.

Cause I Remedy

2. Clogged Ilo\v line 3. The inside diamctcr ol'tubing is

excessivclv small.

I . Itlcntil'y the clopped component and replace it. 1. Rcplacc the tubing with another having an appropriate

insidc diameter.

3. An error message is tlisplaycd. 1 I . Press@).

(P.MAX. P.MIN. ctc.)

1 . Tlic drain \'aIvc is onen. Rcmove thc cause of the error.

1 I . Close the drain valve.

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

2. RAM Error

R O M F A I L U R E J 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. 'Y

L 4- .- 0

4. Overstepping 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.

N O T P R O T E C T E D 1 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.

--,,

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- 1 OAD

-1 Error Messages

E R R O R P- M A X 5. Maximum Pressure Error 1 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

7. Home Position Error

8. Purge Error

E R R O R P - M I N

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 deli very.

[ E R R O R H O M E P O S 7

the solvent

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 (e) 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.

O P E N D R A I N V A L U E 1 This error message is displayed if the actual output pressure of the pump exceeds 5kgf/cm2 during purge operations started with the (G) key. Because the @key will release the system from the error, 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-1 OAD

Chapter 10 Specification

Contents

10.1

10.2

10.3

LC-IOAD Unit Specifications ........................................................................................ 10-2

High Pressure Gradient Specifications .......................................................................... 10-3

Low Pressure Gradient Specifications ........................................................................... 10-4

10-1 LC- 1 OAD

~ _ _

LC-1 OAD Unit Specifications \

1.

2.

3.

4.

5.

6.

7.

a.

9.

10.

11.

12.

13.

14.

Pump

Modes of solvent delivery 1) Constant flow delivery

Range of flow rate:

Accuracy of flow rate setting:

Precision of flow rate

2) Constant pressure feeding

Pressure setting range: Pressure setting accuracy:

Pressure limit:

Damper:

Materials in contact with solvent :

Suction filter:

Line filter:

Time program:

Pressure indication accuracy:

Plunger seal cleaning flow line:

Size:

Weight :

Operating temperature range:

Power requirements:

Microvolume double plunger pump (Approx. 1 Opl/stroke)

Constant flow or constant pressure solvent delivery

0.001-5ml/min ( 10-400kgf/cm2) 5.001 -9.999ml/min (1 0-200kgf/cm2) Within &2% or f2pl/min whichever is higher (0.0 1 -5ml/min, 1 0-400kgf/cm2, with water and room temperature at 20°C) except for periods of low pressure gradient delivery. Within M.396 (O.l-5ml/min, 10-400kgf/cm2 with water and room temperature at 20°C)

10-400kgf/cm2 (at 1 kgf/cm2 intervals)

Less than 10% or lOkgf/cm', whichever is larger

Highbow pressure

Internal capacity of approx. 200~1

SUS3 16, ruby, sapphire, Teflon' tempered with graphite, Hastelloy C', PEEK, Kalrez', KelF

lop mesh

2p mesh, capacity approx. 2OOyl

Flow rate, pressure, event, LOOP (repeated programs), a total of 10 files and 320 steps

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.

l lkg

s-3soc

(Power requirements vary depending upon the P/N.) P/N 228-25000-91,92 AC 90-1 30V 1 00VA P/N 228-25000-93 AC 200-25OV lOOVA

10-2

LC-1 OAD

m m m High Pressure Gradient Specifications

1. SCL-1 OA 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

3) Number of program a total of 20 files and 400 steps steps:

4) Program time: 0.01-9999.9 min

5) Mixing ratio setting &loo% (0.1% stepiping) range:

6) Mixing ratio setting +1% (O-lOO%, 0.:l-3ml/min, 10-400kgf/cm2, with a water and accuracy: 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

3) Number of program a total of 10 files anid 320 steps steps:

4) Program time: at the longest, 999.99 min. (0.01 min. stepping)

5) Mixing ratio setting &loo% (0.1% stepping) range:

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

10-3 LC-1 OAD

Low Pressure Gradient Specifications /\

1. SCL-1 OA 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 up to 4 solvents:

2) Gradient profile: step and linear possible at multiple levels

3) Number of program a total of 10 files and 320 steps steps:

c 4) Program time: at the longest, 999.99 min. (0.01 min. stepping) 0 .- Y - cp 0 'c 5) Mixing ratio setting 0--100% (0.1% stepping) .- 0

v) 8. range:

6) Usable flow rate 0.1-9.999ml/min range:

10-4 LC-1 OAD

Chapter I1 Space Parts and Optional Modules

Contents

I I . I I 1.1

11.3

Consumable Parts List .................................................................................................... 11-2

List of Other Necessary Parts ....................................................................................... 11-3

Optional Modules List .................................................................................................... 11-4

11-1 LC-1 OAD

Consumable Parts List \

I 2

3

Parts Name -7 Parts Number

Seal Filter F6 assembly Packing Suction filter

228- 18745 228-1 2642-93 228-12564 228-1 1647-93

Remarks

These two parts need to be replaced together. 1 Filter main assembly only (already cleaned)

11-2 LC-1 OAD

mm' List of Other Necessary Parts

Parts Number

072-01652-19

1. Mechanical Parts

Remarks

for 1OOV-12OV input

I

2 3 4 5 6 7 8 9

10

11

12 13

14 15

16 17 I8

Parts name

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 ETFE tube 1.6x0.8

Drain tube

Diaphragm ( V, &) Pump head clamping plate Spacer Mounting screws

2. Electrical Parts

Parts Name

Fuse 2A Fuse I A

Power source SLM 50224 Switch Print board PB- 1 (no ROM)

ROM Assy

Batteries Panel switch 4431 PCB FIP Assv

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

228-1 8555 670-10321

228- 1 8648 228-18495-01

228-18748-91 228-2431 1-01 228-24473 228-24472 021 -0 IS60

~~

Remarks

Cleaning tube B is the same.

For the suction filter For the suction filter

For the pump inlet The tube between the inlet block and the check valve IN

072-01652-16 074-80368-01 064-54753-0 1

228-23685-9 1

228-24783-9 1

074-73306 228-23674 228-23024-9 1

for 22OV-24OV input

Power source switch

Sheet keys Printed circuit board for the kevboard

11-3 LC-1 OAD

Optional Modules List \

228- 17641-91 228-21996-91

228-24200-91

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.

A helium degasifier for one liquid system. 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 pressure reduction through a resin membrane for UD to 3 flow lines.

Optional Module Identification

DGU-IA DGU-2A i DGU-3A

DGU-IOA

FCV- 1 OAL

FCV- 13AL

PartsNumber I Description

228-24201-91 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 through option box L.

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.

228-24845-91

228-24861-91

228-24813-91

228-248 13-92 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.

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.

'7

m

11-4 LC- 1 OAD

-1 Optional Modules List I]

bptional Module Identification

Option Box L

Parts Number

228-25025-91 (1 00- 120V) 228-25025-92 (200-26oV)

Reservoir Box 228-25038-9 1

Mixer 1 228-28000-91 Automatic Wash- ing Kit

228-18803-91

Manual Injector Model 71 25

228-21 999-91

Position Sensing Switch

670- 12098- 15

Manual Injector Model 8125 for semi-micron liquid chromatog-

raphy Piping Parts Kit for semi-micro liquid chromatography Injector Mount- ing Plate Column Holder

228-23200-91

228-23198-91

228-25468-9 1

228-15418-93 Air Trap 228-23675-9 1

~~

Description

This unit has 3 functions. 1. For control of the FCV-IOAL, FCV-IlAL, FCV-IlAL(S), FCV-l2AH, FCV- 13AL, FCV-l4AH, syringe unit, and DGU-IOA units. However, setting is made through the SCL- 1 OA unit. 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.

Up to 2 of the following units can be contained FCV-IOAL, FCV-I IAL, FCV- 1 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 20~1.

When connected to the manual injector Model 7125, a signal synchronizing with sample injection is sent to the system controller and Chromatopac. A manual injector for semi-micro liquid chromatography. The standard sample loop is 5pl. The unit has a built-in position sensing switch.

This unit consists of a SUS pipe with an inside diameter of 0.2mm and joints for the manual injector.

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- 1 OAD

Chapter 12 Reference Material

Cantents

12.1 Precautions on Static Electricity .................................................................................... 12-2

13.2 Mobile Phase Characteristics .......................................................................................... 12-6

12- 1 LC-1 OAD

Precautions on Static Electricity 7

1.

Liquid chromatography using combustible organic solvents as mobile phase requires constant exercise against fire, explosion, etc. Par- ticularly, 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 insuffi- cient. 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.

Accidents caused by static electricity take place through the following -\

Mechanism of Static Electrical Discharge processes. Accident (Example)

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 .

I Flowing l iqu id -

Solid

Fig. 1 Occurrence of static electricity by friction between solid and liquid

12-2 LC- 1 OAD

,---

mi Precautions on Static Electricity

Charging and storage of static electricity

Energy release-by discharge

substances

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

is f l ow ing a t a h igh speed h a small- diametertube. ge i s easi ly accumulated i f les are included i n the d.

nsulated vessel l ike polyethylene)

Combustible gas is stored i n the head space of the vessel.

Spark discharge

Spark discharge rnbustible organic solvent i s arged to a great extent.

-v-= - - Floor covered w i t h rubber, etc.. provides unwanted insulation.

Fig. 2 Conditions for Accidents

12-3 LC-1 OAD

1 Precautions on Static Electricity 1- 2. 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.)

%

%

Preventive measure 2. 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 meta l l ic pa r t I /

t o the grounding,

ground the meta l l ic vessel. Min imize clearance etc., of the device t o

by attaching a cap.

Meta l l ic 18 l i t ter can (A plated can IS recommended.)

Static electricity of the l i qu id is released via vessel.

Fig. 3 Anti-Static Electricity Measures for Vessel

,-\_

12-4

LC- 1 OAD

-1 Precautions on Static Electricity

Preventive measure 3. Do not approach the vessel with charged objects including the human body. Charging prevention measures for human body

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 ap-

proach dangerous sections, they have to be grounded beforehand. (For example, they should contact grounded metal by hand.)

Prevention of charging of shoes and clothes

Preventive measure 4. 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.

,-

Preventive measure 5. 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

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.

(lO-'Os/m or less).

b)

c)

LC- 1 OAD

L

K

12-5

Mobile Phase Characteristics -\

(7) Water

(3) Boiling Solubility (8) (9) (2) uv (4) Point Viscosity (5) (6) %" inmt Dielectric PI+

Source Cutoff R.1.25' ("c) (cP,25"c) p' e: Solvent Constantea 0.25 e

1. FC-78 (*) (LC characteristic) 210 rn 1.261 FC-75 (Fluorescent solvent) FC-43

2. Isooctane (*)(2,2,4-

3. n-Heptane (*) 4. n-Hexane (*) 5. n-Pentane (**) 6. Cyclohexane 7. Cyclopentane (*) 8. 1 Chlorobutane (*) 9. Carbon disulfide 10. 2Chloropropane (**) 1 1. Carbon tetrachloride 12. n-Butyl ether 13. Tricthylamine 14. Bromoethane (*) 15. i-Propyl ether (*) 16. Toluene 17. p-Xylene 18. Chlorobenzene 19. Bromobenzene 20. Iodobenzene 2 I . Phenyl ether 22. Phenetole 23. Ethyl ether (**) 24. Benzene 25. Tricresyl phosphate 26. Ethyl iodide 27. n-Octanol 28. Fluorobenzene 29. Benzylether 30. Methylene chloride (**) 31. Anisole

tri methylpentane)

- 36. n-Propanol .- Q 37. Tetrahydrofuran (*) c Q, 38. Propylamine (*)

39. Ethylacetate (*) 40. i-Propanol al

0 c 4 1. Chloroform (*)

42. Acetophenone 43. Methylethyl ketone (*) Q,

44. Cyclohexanone

L

3

r

12-6 LC-IOAD

LC LC LC LC LC LC LC LC LC LC

LC

LC LC

LC

LC

LC LC LC

LC LC LC

LC

2 10 (opaque 1.276 210.or under) 1.291

197 195 190 195 200 200 220 380 230 265 220

220 285 290

218 280

205

233

228

210 240 212

256 205 245

329

1.389 1.385 1.372 1.355 1.423 1.404 1.400 1.624 1.375 1.457 1.397 1.398 1.42 1 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 1.42 1 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

50 102 174

99 98 69 36 81 49 78 46 36 77

142 89 38 68

110 138 132 156

25 8 170 35 80

72 195 85

288 40

154 130 83 82

118 97 66 48 77 82 61

202 80

156

0.4 0.8 2.6

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

< -2 -.25 < -2 -.25 <-2 -.25

0.1 0.01 0.2 0.01 0.1 0.01 0.0 0.00

-0.2 0.04 -0.2 0.05 1.0 0.26 0.3 0.15 1.2 0.29 1.6 0.18 2.1 0.25 1.9 0.54 2.0 0.35 2.4 0.28 2.4 0.29 2.5 0.26 2.7 0.30 2.7 0.32 2.8 0.35 3.4 3.3 2.8 0.38 2.7 0.32

2.2 3.4 0.5 3.1 4.1 3.1 0.42 3.8 3.7 0.61 3.5 0.44 4.1 0.7 3.9 0.7 4.0 0.82 4.0 0.57 4.2 4.4 0.58 3.9 0.82 4.1 0.40 4.8 4.7 0.51 4.7

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

1.3 0.058

3.9

0.17

9.2 0.16 miscible 20.1 miscible miscible miscible 8.8 miscible 0.072

23.4

1.88 1.86 1.9

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

p' and Dielect. const.

(a function in proportion to strength)

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

r-1

4.2 5.8 4.6

5.6 4.6 1.3 6.3

8.3

5.8

5.6 8.7 9.1 9.1

-.

I Mobile Phase Characteristics

(7) Water

(3) Boiling Solubility (8) (9) ( I ) *7<.5cP,>45° (2) uv (4) Point Viscosity ( 5 ) (6) %" inB': Dielectric P'+

Solvent **7<.5cP,<45' Source Cutoff R.I. 2s* ("c) (cP,25"c) p' e'. Solvent Constant e 0.25 e

45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 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-dimethylaceta- mide

Dimethylformamide Dimethylsulfoxide N-methyl-2-pyrolidone Hexamethyl phosphoric

Methanol (*) Nitromethane m-Cresol N-methylformamide Ethylene glycol Formamide Water

acid triamide

LC LC

LC

LC

GC LC LC GC

LC LC

LC LC LC

LC

LC

215 265

380 330

210

210

190 268

268 268 285

205 380

1.550 1.536 1.420 1.449 1.625 1 SO7 1.390 1.356 1.538

1.400

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 1.43 1 1.447 1.333

21 1 191 101 175 237 115 114 56

205

125

78

184 118 82

166

153 189 202

233 65

101 202 182 182 210 100

1.8 1.2 1.2

3.4 0.88 0.64 0.30 5.5

1.60

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

4.4 4.8 4.8 6.0 0.56 5.0 5.3 5.2 5.1 0.71 5.7 6.1 0.6 5.5

0.56 6.6 6.1 4.3 6.8 6.3 6.0 5.8 6.5 0.88

miscible

miscible 0.9 miscible

miscible

miscible

miscible miscible

6.4 7.2 0.62 miscible 6.7

7.4 0.65 5.1 miscible 6.0 2.1 7.4 6.0 miscible 6.9 miscible 9.6 miscible

34.8 13.2 25.2 10.9 2.2

23.0 10.7 9.0 7.4

12.4

13.1 8.8

19.9

24.6

6.9 8.1 6.2

37.5 37.8

36.7 4.7

32

30 32.7

11.8 10.0 182 37.7

111 0.89 10.2 80

12-'7

Solvents marked with an asterisk * are preferred for LC mobile phase because their boiling points (> 45°C) permit easiness in use, and their viscosity 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 Chemi- cals, 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 25°C. 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 20°C Solvent" indicates water solubility (w%) at 20°C 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.

0 . 5 ~ ~ ) is low.

-'-.

,,.-

Source: A. Krstulovic, P.R. Brown: Reversed-Phase High-Per- formance Liquid Chromatography ( 1 982) Wiley Interscience: Translated by Makino et. al., Reversed-Phase High-Performance Liquid Chromatog- raphy (1985)

"7

12-8 LC- 1 OAD

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