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High Performance GPC System

HLC-8320GPC
Operators Manual

Revision G

Thank you very much for purchasing TOSOHs High


Performance GPC System HLC-8320GPC. For the correct use of
this instrument, be sure to read this operators manual thoroughly.

Tosoh Corporation
Bioscience Division
Safety Precautions

Introduction

Operators who use this instrument should read the safety precautions first and handle
the instrument correctly.
WARNING and CAUTION are defined below. For safe use, be sure to observe the
warnings and cautions.

Indicates a potentially hazardous situation which, if not avoided, could


result in death or serious injury.

Indicates a potentially hazardous situation which, if not avoided, could


result in minor or moderate injury.

At installation

Install the instrument in a place with ventilation facilities.


Inflammable or toxic liquid may be used with the high performance GPC system.
For safety, be sure to install the instrument in a place with ventilation facilities.
Ventilate continuously or periodically when using the instrument.
Do not use an open flame where the instrument is installed because it may cause a
fire or explosion by inflammation.

Connect the instrument to an appropriate power supply.


Be sure to connect the instrument to a power socket with a ground.
Using a power socket with no ground may result in a fire or electric shock.
If an extension cord is necessary, choose a cord that has a ground and a sufficient
current capacity.
Connect the instrument to a power supply of stable voltage with a capacity margin.
A power supply shortage or an overvoltage may cause a fire.
Solvents may damage the power cable. Route the power cable such that it will not
be exposed to a solvent.

II
Safety Precautions

Do not use insufficiently rated extension cords or power distribution


adapters.
This may result in a fire or electrical shocks.
Check that the power plug is free of dust and insert the power plug securely and
completely. Dust or loose objects may cause a fire or electric shock.

Install the instrument in an appropriate place.


Do not block the main power switch with other equipment or the wall. In the case of
an emergency, it may be difficult to turn off the power.

Take care not to bump the instrument.


This is a delicate instrument. Take care not to bump the instrument while carrying it.

On use

Do not touch the power plug or main power switch with wet hands.
Touching the power plug or main power switch with wet hands may result in electric
shock.

Do not start or stop the instrument by means of the power cable.


Starting or stopping the instrument by means of the power cable may result in a fire
or electric shock.
Be sure to use the main power switch on the right side of the instrument and the
POWER key on the front.

III
Safety Precautions

Do not place containers of liquid on the instrument.


Liquid dripping into the instrument may cause a short circuit or electric shock by low
insulation.

Use this instrument in accordance with the instruction in this manual.


Any other operation may result in a instrument failure, accident or inaccurate
measurement.

When using inflammable liquids, take care regarding the accumulation


of static electricity.
When inflammable liquid is used, static electricity may cause a fire or explosion. To
prevent such an accident, take care regarding the accumulation of static electricity.
(See 13.5, Countermeasures against Static Electricity.)

Take care with regard to liquid leakage.


Leakage of a solvent or washing liquid may cause a fire, electric shock, or
corrosion.
In the case of liquid leakage, stop the instrument, turn the power off, and unplug the
power cable.
When wiping liquid from the instrument, wear appropriate protective items (goggles,
gloves, mask, etc.).
After wiping liquid from the instrument, be sure to prevent leakage from tubing joints
and other such locations.
If the leakage does not stop, contact TOSOHS service center.
Before using the instrument, check with MSDS or another such organization
regarding what to do if a solvent gets on the skin.

While the instrument is running, keep the covers and doors closed.
You may be caught or pulled in by movable or heat generating sections or by
high-voltage electric circuits inside the instrument and suffer a burn or electric
shock.

In case of an abnormality (burning smell, etc.), stop the instrument, turn


the power off, unplug the power cable, and contact TOSOHs service
center.
Continued running in an abnormal state may result in a fire or electric shock.

IV
Safety Precautions

Be careful not to damage the power cable.


Pulling or bending may damage the power cable and cause a fire or electric shock.
When unplugging the power cable, be sure to hold the plug.

Remove tubings or columns when the pump pressure is low.


If tubings or columns are removed when the pump pressure is high, the solvent
may spew out. When removing tubings or columns, wait until the pump pressure
becomes 0 MPa.

Work inside of an oven when the internal temperature is low.


When the pump oven or column oven is opened, the power supply to the heater is
forcibly stopped. Since heat remains inside for some time after temperature control,
the user may be burned in physical contact with the inside of the oven. Before
working inside of the oven, confirm that the internal temperature is low.

Wear appropriate protective items for the liquid to be used.


When handling a solvent of strong acid of alkali or organic solvent, be sure to wear
appropriate protective items (goggles, gloves, mask, etc.).

Check miscibility, before solvent substitution.


For solvent substitution, check miscibility and reactivity in advance because
chemical reaction may cause heating, explosion, or a fire. (See 13.1, Solvent
Miscibility.)

When using a chlorine solvent, take care with respect to corrosion.


If a chlorine solvent is used for a long time, instrument corrosion will be accelerated.
Be sure to add a stabilizer to the solvent and substitute the solvent with ethanol or
other solvents if the solvent is not used for one week or longer.

V
Safety Precautions

Check the gas sensors with the liquid to be used.


The gas sensors of the pump oven and column oven react only with an organic
solvent. When using the instrument, confirm that the gas sensors react under the
specified conditions.

About the installation location of waste liquid containers


To secure the drainage of a solvent or washing liquid, place a waste liquid container
lower than the outlet of the drain tubing.

Note the characteristics of the solvent to be used.


Do not use a solvent having a boiling point that is equal to or lower than room
temperature +10C or the set temperature of the pump oven. If a solvent having a
low boiling point is used, the instrument may not be able to exhibit its full
performance.
Under some relationships between the solvent and wet components, a instrument
of standard specifications may not be able to achieve full performance. For solvents
not mentioned in 13.2, Solvent Characteristics, salt-added solvents, or mixed
solvents, the wet components must be replaced according to the solvent. Contact
TOSOHs service center.

Take care with respect to clogging by dust in a solvent or sample.


To maximize the features of semi-micro-columns, this instrument has a lower
diameter tubing between the column and detector. Note that the tubing is not
clogged by dust in a solvent or sample.

When using TSKgel SuperAW5000, SuperAW6000, or SuperAWM-H,


take great care.
When attaching one of the above columns to the instrument, do not connect the
column outlet to the detector, but supply liquid of double the column capacity before
connection.
If the instrument is left unused for one week with a column attached, do not connect
the column outlet to the detector but supply liquid of double the column capacity
before connection.
When replacing the solvent, disconnect the column outlet from the detector and
supply liquid of four times the column capacity before connection.

VI
Safety Precautions

When using a column switching valve, note the flow rate at switching.
When an optional column switching valve is equipped to use columns of different
sizes, valve switching without changing the flow rate may damage the column. Set
an appropriate flow rate for the column size in advance.

Do not place fingers or objects into moving or rotating sections in the


instrument.
Since some sections are driven by motors, fingers or objects may be caught or
pulled into the instrument, causing serious injury.

When the rack of the auto sampler is out, keep your hands away from
the cover.
If your hand is near the cover of the auto sampler when rack is out, your hand may
be struck by the cover, or be caught or pulled into the instrument, causing serious
injury.

Perform maintenance carefully according to the operators manual.


Maintenance performed without a sufficient understanding of protective items
(goggles, gloves, mask, etc.) may result in injury.
Read the operators manual well and perform maintenance with a sufficient
understanding of the instrument.
Maintain the instrument only as instructed in this manual.
For questions about maintenance, contact TOSOHs service center.

Dispose of wastes appropriately.


Dispose of waste, such as sample cups, columns, and liquids used for
measurement, appropriately and according to the waste type.
When handling waste, wear gloves and do not to touch the waste directly.
Dispose of waste appropriately and according to related legal environmental and
health regulations.

VII
Safety Precautions

Do not place heavy items on the instrument.


The top face of the instrument is not designed to withstand heavy loads. Placing
heavy items on the instrument may damage the instrument. If such items fall from
the instrument, you may be injured.

Use parts specified by TOSOH.


Use consumables or replacement parts listed in the parts list of this operators
manual. (See Chapter 11, Parts List.)

Keep this operators manual in a safe place.


Keep this operators manual in a safe place nearby for quick reference at any time.
If the person responsible for maintaining changes, transfer possession of the
manual to the new person.

Explanations of the label on the instrument


The instrument is sticked a warning label. Check the label contents and use the
instrument safely.

WARNING Do not disassemble or repair the equipment.


Fire,electric shock or serious injury may result.



Be sure there is no leak in tubing. Leak of organic
CAUTION
solvent may cause corrosion, fire, electric shock or
poisoning.



CAUTION Keep away from an open flame. Organic solvent may
catch fire and explode.

Label position: Front of the pump oven

VIII
Safety Precautions

Label position: Front of the Degas/Suction unit, Upper panel


Do not remove except for maintenance.
In case removing the panel, turn the main power OFF (O) and remove
the power cable.

Label position: Front of the pump oven


There is an UV lamp in the instrument. In case removing the cell, do not
look directly at the light.
This is valid only when an optional UV detector is equipped.

If a warning or caution label becomes illegible due to stains, damage, or peeling,


contact TOSOHs service center or sales representative for a replacement label.

For installation, repairs, moving and disposal, contact the


TOSOH service engineer.
Disassembly, repair, or alteration by the user may result in a fire or electric shock.
For installation, repairs, moving, and disposal, contact the TOSOH service
engineer who received training for maintenance.

Notes
No part of this document may be quoted or reproduced in any form without prior
permission from TOSOH.
This document is subject to revision without notice.

Tosoh Corporation
Bioscience Division

IX
About This Document

This operators manual describes how to use and operate this instrument
correctly. This document is based on the following rules:

Section title
For sections that exceed
one page, the font size of
the section title is small
on the second and later
pages.

Illustration
Illustrations are provided
to help the reader to
understand the text.

Symbols
The symbols described
below indicate situations
in which care is required
during operation.

Page
Page numbers are by chapter.

Failure to observe this precaution may result in death or serious


injury.

Failure to observe this precaution may result in an injury or


physical damage.

Concerning the incorrect use of the instrument.

Points indicate useful advice on using the instrument.

X
Contents

Chapter 1 Section Names and Functions


1.1 Front 1-2
1.2 Sides 1-3
1.3 Rear 1-5
1.4 Operation-Display 1-6
1.5 I/O Terminals and Communication Port 1-8
1.6 Inside 1-9

Chapter 2 Operation
2.1 Operation Outline 2-2
2.2 Opening or Closing the Oven Doors 2-5
2.3 Turning the Power ON or OFF 2-6
2.4 Setting the Operation-display 2-7
2.5 Viewing the Monitor Screen 2-9
2.6 Stop Valve 2-11
2.7 Purge Function 2-12
2.8 Pump Drain 2-13
2.9 Changing the Degasser Vacuum Pressure 2-14
2.10 Changing the Degasser Volume 2-15
2.11 Controlling the Pump Unit 2-17
2.12 Controlling the Temperature Control 2-20
2.13 Controlling the Auto Sampler 2-22
2.14 Controlling the Detector (RI) 2-28
2.15 Setting the Warm-up Conditions 2-30
2.16 Executing Warmup 2-32
2.17 Setting the Shutdown Conditions 2-33
2.18 Executing Shutdown 2-35
2.19 Setting the Sample Queue 2-36
2.20 Preparing Samples 2-38
2.21 Loading Sample Cups 2-39
2.22 Starting and Stopping Analysis 2-40
2.23 Weekly Timer 2-41
2.24 Setting the Clock 2-42

XI
Contents

2.25 Checking the Device Program Version 2-43


2.26 Checking Error Logs 2-44

Chapter 3 Analysis
3.1 Analysis Notes 3-2
3.2 Analysis Flow Chart 3-4

Chapter 4 Performance Check


4.1 Checking Pump Unit Performance 4-2
4.2 Checking Pump and Column Oven Performance 4-3
4.3 Checking Detector (RI) Performance 4-4
4.4 Checking Auto Sampler Performance 4-6
4.5 Comprehensive Inspection 4-7

Chapter 5 Maintenance and Inspection


5.1 Washing the Check Valves 5-2
5.2 Replacing the Check Valves 5-4
5.3 Replacing the Plunger Seal 5-5
5.4 Replacing the Plunger 5-8
5.5 Washing or Replacing the Inline Filter 5-10
5.6 Replacing the 6way Valve Rotor Seal and Stator 5-12
5.7 Replacing the 4way Valve Rotor Seal and Stator 5-15
5.8 Replacing the Sample Loop 5-18
5.9 Replacing the Detector (RI) Cell 5-19
5.10 Washing the Inside of the System 5-20

Chapter 6 Troubleshooting
6.1 Checking Errors 6-2
6.2 Error Messages 6-3
6.3 Before Seeking Repairs 6-13

XII
Contents

Chapter 7 Installation
7.1 Installation Environment 7-2
7.2 Installation Place 7-3
7.3 Installation Space 7-5

Chapter 8 Connection
8.1 Connecting the Power Cable 8-2
8.2 Removing the Auto Sampler Fixture 8-3
8.3 Connecting a PC 8-4
8.4 Tubing 8-5
8.5 Attaching the Washing Tubing to the Rear of the Pump 8-12
8.6 Installing the Cases 8-13
8.7 Connecting the I/O Terminals 8-14

Chapter 9 Specifications
9.1 Specifications 9-2

Chapter 10 Options
10.1 UV Absorption Detector (UV-8320) 10-2
10.2 External Detector 10-10
10.3 Column Switching Valve 10-11

Chapter 11 Parts List


11.1 Accessories 11-2
11.2 Consumables 11-6
11.3 Options 11-10

XIII
Contents

Chapter 12 Theory
12.1 Instrument Configuration 12-2
12.2 Pump Unit 12-3
12.3 Auto Sampler 12-4
12.4 Detector (RI) 12-5
12.5 Detector (UV) 12-7

Chapter 13 References
13.1 Solvent Miscibility 13-2
13.2 Solvent Characteristics 13-3
13.3 Quick Reference for Boiling Point 13-8
13.4 Waste Liquid Treatment 13-9
13.5 Countermeasures against Static Electricity 13-10

XIV

Chapter 1

Section Names and Functions


1.1 Front

Operation-display Column oven

Auto sampler

Degas/Suction unit

Pump oven

1-2
1.2 Sides

Left side

Sampler syringe unit


Sampler syringe
4way valve
Drain block

Wash suction port


(WASH)
Drain port Wash drain port
(DRAIN) (AS-DRAIN)
Pump plunger wash port Solvent suction port

(Capped with a rubber stopper) (SOLVENT)

Teflon tubing are connected to the above ports.

If the outlets of the drain tubing and wash drain tubing are fixed higher than
those on the left side of the instrument, the solvent will not be drained
smoothly but will overflow from the drain block or washing port. For smooth
drainage, cut the tubing to appropriate lengths before putting them into a
waste container so that the ends of the tubing will be low.

1-3
1.2 Sides

Right side

Main power switch

External tubing connection


Power inlet

I/O terminals
See 1.5, I/O Terminals and Communication Port.

1-4
1.3 Rear

Back-pressure release
tubing

UV detector cooling fan Cooling fan


(Optional)
RI detector liquid leak tubing
connection port

1-5
1.4 Operation-display

POWER key
(Power ON/OFF)

Temperature control lamp Numeric keypad

CO: Column oven (For numeric setting)

PO: Pump oven Temperature control indicator


RI : Detector (RI)
Display

Function keys
(For functions displayed in
the bottom line)
Control keys 1 Control keys 2
(For executing and indicating (For executing and indicating
warmup, analyze, and sample rack ejection, sampler
shutdown) wash, auto balance, sample
pump flow, reference pump flow,
and purge)

1-6
1.4 Operation-display

Control keys 1
Start/stop warmup
WARMUP
The key lamp remains lit during execution. To stop warmup, press
and hold the key for one second.

Start/stop analysis
ANALYZE
The key lamp remains lit during execution and flashes to indicate
reservation. If this key is pressed during warmup, analysis will start
after warmup. To cancel or stop analysis after finishing the sample
that has already been injected, press and hold the key for one
second. For forced termination, press and hold the key again in this
state for one second.

Start/stop shutdown
SHUTDOWN
The key lamp remains lit during execution and flashes to indicate
reservation. If this key is pressed during analysis, shutdown will start
after analysis is complete. To cancel or abort shutdown, press and
hold the key for one second.

Control keys 2
Eject/insert rack
This key is used to eject or insert a sample rack. If rack is inserted ,
the LED lamp lights.

Execute sampler wash


WASH
The key lamp remains lit during execution.

Execute detector auto-balancing


BALANCE

Start/stop sample pump flow


S.FLOW
The key lamp remains lit during liquid supply. To stop liquid supply,
press and hold the key for one second.

Start/stop reference pump flow


R.FLOW
The key lamp remains lit during liquid supply. To stop liquid supply,
press and hold the key for one second.

Start/stop purge
PURGE
The key lamp remains lit during execution. To specify the capacity
by numeric keypad, press and hold the key for one second. If the
key is held for one second during execution, purge stops.

1-7
1.5 I/O Terminals and Communication Port

RI terminal
This terminal outputs analog signals from the RI detector.
Output value: Integrator range/1V

UV terminal
This terminal outputs analog signals from the UV
detector (option).
Output value: Integrator range/1V

INJ terminal
This signal outputs a relay contact signal at sample
injection by the auto sampler.

ERROR terminal
Connect a contact output terminal of external
instrument to this terminal. This instrument execute
error processing after signal input.
See P6-4 Error No.0022

PC terminal
Connect a USB cable to this terminal to control this
instrument and acquire data by the PC control program
EcoSEC WorkStation.

1-8
1.6 Inside

Pump oven

Inline filters

Check valves
UV detector (optional) housing

Sample pump
Reference pump

1-9
1.6 Inside

Degas/Suction unit

Degasser Stop valve

Purge pump Drain valve

1-10
1.6 Inside

Column oven

Column switching valve (option) housing

Sample injection valve


Gas sensor

Sample column IN tubing Reference column IN tubing

R.COL
S.COL

Detector (RI) sample IN tubing Detector (RI) reference IN tubing


RI.R
RI.S

1-11
MEMO

1-12

Chapter 2

Operation
2.1 Operation Outline

This instrument is controlled from the operation-display or PC control program EcoSEC


WorkStation. This manual explains how to control the instrument from the operation-
display.
For control from a PC, refer to the user's guide of the EcoSEC WorkStation.

This manual explains how to control the instrument from the operation-display. If a
PC is connected to this instrument by a USB cable, disconnect the USB cable.

Screen transition diagram

The figure below shows the transition diagram when this instrument is controlled from
the operation-display.

( Page )

Monitor screen 1 Monitor screen 2


( Page )

Process Screen
( Seq. )

( Page )

Warmup screen 1 Warmup screen 2


(Warmup) ( Page )

Sample queue
( Ana. ) screen

( Page )

Shutdown screen 1 Shutdown screen 2


(S.Down) ( Page )

( Page )

Weekly timer Weekly timer Weekly timer


(Timer ) screen 1 ( Page ) screen 2 ( Page ) screen 3

Date and time


( Date ) setting screen

( ) is displayed in the bottom line. Press the function key below the displayed
message to go to the corresponding screen.

2-2
2.1 Operation Outline

( Page )

Monitor screen 1 Monitor screen 2


( Page )

Unit selection
(Param.) screen

( Unit ) ( Page )

Pump parameter Pump parameter Pump parameter Pump parameter


screen 1 ( Page ) screen 2 ( Page ) screnn 3 ( Page ) screen 4

Drain valve screen


(Drain )

Stop valve screen


(E.Stop)

( Unit ) ( Page )

Sampler parameter Sampler parameter Sampler parameter


screen 1 ( Page ) screen 2 ( Page ) screen 3

Tube volume
(TubeV.) measurement screen

Air sensor sensitivity


(AirS. ) adjustment screen

( Unit )

Oven parameter
screen

( Unit )

Column switching
valve screen

( Unit )

RI detector
parameter screen

( Unit ) ( Page )

UV detector UV detector
parameter screen 1 ( Page ) parameter screen 2

Lamp intensity
(Power ) check screen

Press (Unit) to go to the next parameter screen.


If the destination parameter screen does not exist, the display changes to the next
screen.

*1 In case that a column switching valve (option) is equipped, the display changes to a screen
according to the selected column.
Column 1: Pump parameter screen 1
Column 2: Pump parameter screen 2
*2 In case that column switching valve (option) is not equipped, the display changes to Pump
parameter screen 3.

2-3
2.1 Operation Outline

*3 This is valid only when a column switching valve (option) is equipped.


*4 In case that column switching valve (option) is not equipped, the display changes to the RI
detector parameter screen.
*5 This is valid only when a UV detector (option) is equipped.
*6 In case that UV detector (option) is not equipped, the display changes to a screen
according to the conditions of *1.

( Page )

Monitor screen 1 Monitor screen 2


( Page )

Option screen
(Option)
( Page )

Error log screen 1 Error log screen 2 Error log screen 3


(E.Log ) ( Page ) ( Page )

When a PC is connected for control by an EcoSEC WorkStation, only the above


screens are displayed.

2-4
2.2 Opening or Closing the Oven Doors

[Opening]
1 Lift the OPEN buttons (B) at the bottom right of the pump oven door and at the
bottom left of the column oven door.
2 The doors open.

[Closing]
1 Press CLOSE (A) securely at the center of each door to close the doors.

If the two doors are not locked securely, temperature control fails.

2-5
2.3 Turning the Power ON or OFF

Main power ON/OFF

This instrument has the main power switch on the right side. Turn the switch to ON ( | )
to start using the instrument.
If the instrument will not be used for a long time, set the main power switch to OFF ({).
This will completely stop the power supply to the instrument.

<Main power switch>

------ ON

------ OFF

When the main power switch is OFF ({), the instrument cannot be operated
from a PC.
Once the main power switch has been turned OFF ({), do not turn it ON ( | )
again within five seconds.

Power ON/OFF

Turn the power ON or OFF by the POWER key on the operation-display.

Even when the POWER key on the operation-display is OFF, power is


supplied to parts of the electric board.
At power OFF, this instrument saves the current settings. Do not turn the main
power OFF or disconnect the power cable during power OFF processing.

The Power ON/OFF can also be controlled from the PC control program EcoSEC
WorkStation.

2-6
2.4 Setting the Operation-display

By introducing actual screens, this section explains how to set the operation-display.

For operating procedures and detailed functions of this instrument, see the
corresponding sections.

[Monitor screen 1]

RI : 100.000 S.Pump : 1.000 10.00


UV : 100.000 254 R.Pump : 1.000 10.00
CO : 40.00 PO : 40.00
( Page ) ( Seq. ) (Param.)

( ) is displayed in the bottom line. Press the function key below the displayed
message to go to the corresponding function screen.


Ex. Press below (Param.) to go to the unit selection screen.

[Unit selection screen]

Select Unit : 3
1: Pump 2: AS 3: Oven
4: Column Change 5: RI 6: UV 7: VIS
( Back )

The cursor is _ on the screen. Type in a figure from the numeric keys and press the
ENT key for confirmation.

ENT
Ex. Press and to go to the oven parameter screen.

CLR
Press to return to the initial value or the value before editing.
Press BACK
to erase the numeral at the cursor, and the cursor returns to the
previous digit.

2-7
2.4 Setting the Operation-display

[Oven parameter screen]

Oven CO Temp.: 40(40.00) Gas: 300( 50)


PO Temp.: 40(40.00) Gas: 300( 50)

<CO Ctr><PO Ctr> ( Unit ) ( Back )

If there are plural input items to one screen , the cursor moves to the next input item
each time the ENT key is pressed.

< > is displayed in the bottom line. Press the function key below the displayed
message to execute the corresponding function screen.


Ex. Press below <CO Ctr> to start temperature control of the column oven.

2-8
2.5 Viewing the Monitor

The monitor screen consists of two pages. Press (Page) to change pages.

[Monitor screen 1]
UV output (option) Sample pump set flow rate
RI output UV wavelength (option) Sample pump pressure

RI : 100.000 S.Pump : 1.000 10.00


UV : 100.000 254 R.Pump : 1.000 10.00
CO : 40.00 PO: 40.00
( Page ) ( Seq. ) (Param.)

Pump oven temperature Reference pump pressure

Reference pump set flow rate


Column oven temperature

RI Output [mV] of the differential refractometer (RI) detector.


UV Output [mV] and set wavelength [nm] of the ultraviolet absorbance (UV)
detector.
This is displayed only when an optional UV detector is mounted.
S.Pump Set flow rate [mL/min] and pressure [MPa] of the sample pump.
R.Pump Set the flow rate [mL/min] and pressure [MPa] of the reference pump.
CO Column oven temperature [C].
PO Pump oven temperature [C].

2-9
2.5 Viewing the Monitor

[Monitor screen 2]

Current date and time


Time Record number Column switching valve position

Time : 111.1 2007/11/10 FRI 09: 09


Record : 1 ( 1) Column: 1
CupNo : 1( 1- 1) Repeat: 1 (1)
( Page ) ( Seq. ) (Param.) (Option)

Cup number Number of Repetition

Time The elapsed time [min] from sample injection.


The current date, day of the week, and time are displayed at right.
Record Record number (total number of records) of sample queue.
Column Current column switching valve position (1 or 2).
This is displayed only when an optional column switching valve is
equipped.
CupNo Cup number (first cup number - last cup number) of sample queue.
Repeat Number of repetitions (set count) of sample queue.

2-10
2.6 Stop Valve

The solvent supply to a instrument can be blocked by switching the stop valve.
For maintenance and inspection such as the replacement of a check valve, switch the stop
valve to the stop position.

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT to display Pump parameter screen 1.
3 Press (E.STOP) to display the stop valve screen.
4 Press <STOP> to change the valve to the stop position. The display changes to
"STOP."

[Stop valve screen]

Solvent Line : STOP

< Stop >< Open > ( Back )

2-11
2.7 Purge Function

The purge function primes a solvent by a dedicated syringe pump. This function is used to
replace a solvent or to degas from a pump.

1 Press PURGE . Purge starts, and the LED lamp lights.


After priming a specified volume, the function automatically stops.
2 To stop purge halfway, press and hold PURGE for one second.

If PURGE
is pressed and held for one second while purge is not running, the purge screen
is displayed. To change the purge volume, enter an arbitrary value at "Volume" on this
screen and press ENT
. The input range is from 1 to 150 mL.

[Purge screen]
Purge : STOP
Volume : 10

( Back )

The purge volume can also be changed as follows:

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT
to display Pump parameter screen 1.
3 Press (Page) twice to display Pump parameter screen 3.
4 Enter an arbitrary value at "Purge Volume" and press ENT .

[Pump parameter screen 3]


Pump Degass Level : 0 (Normal)
Purge Volume : 10

( Page ) ( Unit )( Back )

Purge cannot be executed during flow.

If purge is executed, a solvent of the set volume + 3 mL is supplied so that air


will not enter the channel at the end.
The reference volume is 100 mL for solvent replacement and 10 mL for
degassing before warmup.

2-12
2.8 Pump Drain

For switching to the drain channel, only the sample side or reference side pump can be
switched.

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT
to display Pump parameter screen 1.
3 Press (Drain) to display the drain valve screen.
4 Press <Sam.> to switch the valve to the sample pump drain channel. The display
changes to "Sam."
5 Press <Ref.> to switch the valve to the reference pump drain channel. The display
changes to "Ref."
6 Press <Close> to switch the valve to the analysis channel. The display changes to
"Close."

[Drain valve screen]


Drain Position : Close

<Sam.>< Ref. ><Close >( Back )

2-13
2.9 Changing the Degasser Vacuum Pressure

This instrument has a degasser. Degasser control automatically starts at flow or purge.

If fluorine or any other solvent of great permeability through the PTFE film is used in the
degasser, change the vacuum pressure to Low.

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press
and ENT
to display Pump parameter screen 1.
3 Press (Page) twice to display Pump parameter screen 3.
4 Type in 1 for "Degass Level" and press ENT to change the vacuum pressure to
Low.
5 To return the vacuum pressure to Normal, enter 0 for "DegassLevel" at Step 4 and
press ENT
. The vacuum pressure changes to Normal.

[Pump parameter screen 3]


Pump Degas Level : 0 (Normal)
Purge Volume : 10

( Page ) ( Unit )( Back )

2-14
2.10 Changing the Degasser Volume

The degasser volume on the solvent side is determined by two systems of 20 mL. Change
the degasser volume according to the flow rate. The reference capacity is 20 mL when the
total flow rate of the sample and reference pumps is less than 1.0 mL/min and is 40 mL
when it is 1.0 mL/min or more.

Before changing the degasser volume, turn the main power OFF. Since
some sections are driven by motors, fingers or objects may be caught or
pulled into the instrument, causing serious injury.

1 Turn the main power OFF.


2 Open the column oven door.
3 Take out the screws on the left side of the main unit, loosen the screws beside
the column oven and remove the cover from the suction unit.

2-15
2.10 Changing the Degasser Volume

4 When setting the degasser volume to 40 mL, make the following connections:

Wash suction tubing To sampler 4way valve

(WASH)

Solvent suction
tubing

To stop valve

5 When setting the degasser volume to 20 mL, make the following connections:

Wash suction tubing


To sampler 4way valve
(WASH)

Solvent suction
To stop valve
tubing

Replace to air from the unused series.


Purging with no solvent connection can replace air inside the system.

2-16
2.11 Controlling the Pump Unit

Flow start/stop

S.FLOW
1 To start the flow of the sample pump, press . The LED lamp lights ON
and S.Pump on Monitor screen 1 changes from STOP to Set flow rate.
R.FLOW
2 To start the flow of the reference pump, press . The LED lamp lights ON
and R.Pump on Monitor screen 1 changes from STOP to Set flow rate.
3 To stop the flow of the sample pump, press and hold S.FLOW for one second.
The LED lamp lights OFF and S.Pump on Monitor screen 1 changes from Flow
rate to STOP.
4 To stop the flow of the reference pump, press and hold R.FLOW for one second.
The LED lamp lights OFF and R.Pump on Monitor screen 1 changes from Flow
rate to STOP.

Pump setting change

Control the pump unit and change their settings as explained below.
First, display Pump parameter screen 1 by the following procedure:

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT to display Pump parameter screen 1.

The pump parameter screen consists of four screens. The screen changes each
time (Page) is pressed.

2-17
2.11 Controlling the Pump Unit

Pump parameter screen 1


The flow rates and the upper and lower pressure limits of the sample and reference
pumps can be set on this screen.

[Pump parameter screen 1]


Pump Column1
Sam. Flow: 1.000 P.Limit: 0.0 - 24.9
Ref. Flow: 1 (1.000) P.Limit: 0.1 - 25.0
( Page ) (Drain ) (E.Stop) ( Unit ) ( Back )

Sam. Flow When changing the flow rate of the sample pump, enter an arbitrary
numeric value at Sam.Flow and press ENT
.
The input range is from 0.010 to 2.000 mL.
Ref. Flow When changing the flow rate of the reference pump, set Ref.Flow in the
format of 1/X of the sample pump. Enter a numeric value from 1 to 4
and press ENT . The actual flow rate is displayed in ( ).
P.Limit When changing the upper or lower pressure limit, enter an arbitrary
numeric value at P.Limit and press ENT . The upper pressure limit is
the sample side, and the lower pressure limit is the reference side. The
input range of lower limit is from 0.0 to 24.9 MPa. The input range of
upper limit is 0.1 to 25.0 MPa. And the lower limit must be smaller than
the upper limit.

Pump parameter screen 2


When the column switching valve is switched to Column 2, the flow rates and the
upper and lower pressure limits of the sample and reference pumps can be set on this
screen. The input method is the same as for Pump parameter screen 1.

[Pump parameter screen 2]


Pump Column2
Sam. Flow: 1.000 P.Limit: 0.0 - 24.9
Ref. Flow: 1 (1.000) P.Limit: 0.1 - 25.0
( Page ) (Drain ) (E.Stop) ( Unit ) ( Back )

2-18
2.11 Controlling the Pump Unit

Column 2 is valid only when an optional column switching valve is mounted.

For the column switching method, see 10.3, Column Switching Valve.

Pump parameter screen 3


The vacuum pressure and the purge volume can be set on this screen.
For the input method, see 2.7, Purge Function or 2.9, Changing the Degasser
Vacuum Pressure.

[Pump parameter screen 3]


Pump Degas Level : 0 (Normal)
Purge Volume : 10

( Page ) ( Unit )( Back )

Pump parameter screen 4


The pump correction coefficient can be set on this screen.
Since the set and actual flow rates differ for some solvents, enter a correction
coefficient for accurate flow rate setting.

1 Measure the actual flow rate when flowing at the set flow rate.
2 Check the current setting at Control Flowrate.
3 Enter the measured flow rate at Measure Flowrate and press ENT .
4 Press (Calc.) to display a correction coefficient at Flowrate Coeff.
5 A correction efficient may also be entered directly at Flowrate Coeff. Enter an
arbitrary value and press ENT . The input range is from 0.800 to 1.200.

[Pump parameter screen 4]


Pump Control Flow rate : 1.000
Measure Flow rate : 1.000
Flow rate Coeff. : 1.000
( Page ) ( Calc.) ( Unit ) ( Back )

For the flow rate measuring method, see 4.1, Checking the Pump Unit
Performance.

2-19
2.12 Controlling the Temperature Control

Temperature control of the pump oven and column oven and change their settings as
described below.
First, display the oven parameter screen by the following procedure:

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT
to display the oven parameter screen.

[Oven parameter screen]

Oven CO Temp.: 40(40.00) Gas: 300( 50)


PO Temp.: 40(40.00) Gas: 300( 50)

<CO Ctr> <PO Ctr> ( Unit ) ( Back )

Temperature Control start/stop

1 To start temperature control on the column oven, press <CO Ctr>.


The CO.TEMP LED lamp turns on the light.
2 To stop temperature control on the column oven, press <CO Ctr> during
temperature control. The CO.TEMP LED lamp turns off the light.
3 To start temperature control on the pump oven, press <PO Ctr>.
The PO.TEMP LED lamp turns on the light.
4 To stop temperature control on the pump oven, press <PO Ctr> during
temperature control. The PO.TEMP LED lamp turns off the light.

Change control temperature and gas sensor threshold

CO Temp. When changing the set temperature of the column oven, enter an
arbitrary numeric value at CO Temp. and press ENT . The input range
is from 30 to 60C.
Set the value of the room temperature +10C or higher.
The actually measured value is displayed in ( ).
PO Temp. When changing the set temperature of the pump oven, enter an arbitrary
numeric value at PO Temp. and press ENT . The input range is from
30 to 50C.
Set the value of the room temperature +10C or higher.
The actually measured value is displayed in ( ).

2-20
2.12 Controlling the Temperature Control

Gas When changing the gas sensor threshold, enter an arbitrary value at
Gas and press ENT . The input range is from 1 to 1,000. The upper
item for the column oven and the lower item is for the pump oven.
The actually measured value is displayed in ( ).

Be careful that tubing or other objects do not enter the hole of a partition
in the pump oven or column oven. This is very dangerous because of a
fan rotating inside.

The gas sensor sensitivity differs with the solvent. To ensure accurate
gas detection, check the gas sensor sensitivity with the solvent to be
used in advance and then check the threshold. A greater displayed value
(gas sensor measured value) indicates a higher gas concentration.

For the gas sensor, record a value measured in an ordinary state and a value
measured when a wiper containing approximately 0.5 mL of a solvent is
inserted into the oven. Then set the intermediate value as the threshold.
Set each oven to room temperature +10C or higher.
For stable flow, the pump oven controls the temperature of the pump unit.
Since a solvent having a low boiling point may make flow unstable, turn the
temperature control OFF for such solvents.
Do not set the temperature in a range where the solvent concentration
changes greatly. For THF, 40C is recommended.

2-21
2.13 Controlling the Auto Sampler

Washing

1 Press WASH
to start washing. The LED lamp lights ON.
2 If WASH is pressed and held for one second, the manual washing volume can
be changed. Enter a volume using the numeric keys and press ENT . The input
range is from 1 to 20,000 L. Manual Wash V. on Sampler parameter screen 1 is
updated with the input value.

Sample rack ejection/insertion

By pressing , a sample rack can be ejected or inserted. When a sample


rack is correctly loaded, the LED lamp lights ON.

Auto sampler setting change

Control the auto sampler and change its settings as described below.
First, display Sampler parameter screen 1 by the following procedure:

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT to display Sample parameter screen 1.

The sample parameter screen consists of three pages. The page changes
each time (Page) is pressed.
Change the injection parameters on the sample queue screen.

Sampler parameter screen 1


The sampler status can be monitored and the syringe speed, presuction volume, and
washing volume can be changed from this screen.

[Sampler parameter screen 1]


AS: Ready PresuctionV. : 150
Sam. Speed : 6( 40) Auto Wash V. : 1000
Wash Speed : 14(350) Manual Wash V. : 1000
( Page ) (Tube.V.) (AirS. ) ( Unit ) ( Back )

2-22
2.13 Controlling the Auto Sampler

AS Displays the sampler status.


Ready : Standby
Sampling : Sampling
Inj.Wait : Waiting for injection
Injection : Injecting
Wash : Washing
Sam. Speed To change the syringe speed at sampling. Enter a numeric value
from 1 to 15 and press ENT . The actual speed [L/s] is displayed
in ( ).
Wash Speed To change the syringe speed at washing. Enter a numeric value
from 1 to 15 and press ENT . The actual speed [L/s] is displayed
in ( ).
Auto Wash V. To change the presuction volume[L]. Enter a numeric value from 1
to 500 and press ENT .
Auto Wash V. To change the washing volume [L] after sampling. Enter a
numeric value from 1 to 5,000 and press ENT
.
Manual Wash V. To change the manual washing volume [L]. Enter a numeric value
from 1 to 20,000 and press ENT .

At shipping, the syringe speed is set to 6 for Sam. Speed and 14 for Wash
Speed. When using THF as the solvent, the settings need not be changed.
When using a solvent of higher viscosity or measuring a sample of great
viscosity, reduce the speed. The relationship between input values and actual
speeds is as follows:

Input value 1 2 3 4 5 6 7 8
Speed (L/s) 5 10 15 20 30 40 50 65

Input value 9 10 11 12 13 14 15
Speed (L/s) 80 100 125 180 250 350 500

For ordinary needle washing, the washing volume from approximately 500 to
1,000 L is sufficient. For solvent replacement, however, set the manual
washing volume to 20,000 L.

2-23
2.13 Controlling the Auto Sampler

Setting the tube volume


The tube volume of the auto sampler is set to the optimum initial value. When the
needle or needle tubing is replaced, however, the volume needs to be changed.

1 Press (TubeV.) on Sampler parameter screen 1 to display the tube volume


measurement screen.
2 Open the column oven door to see the tubing of the injection valve.
3 While checking the air position in the needle tubing, press <Air>, <4 L>, or <1
L> to load air. Once the air has entered the male nut in the injection valve, stop
loading.
4 Press (Set) for confirmation.

[Tube volume measurement screen]


Tube Volume Set : 88
Measure : 0

( Set ) < Air > < 4 L > < 1 L > ( Back )

Set Displays the current setting.


Measure Displays the current measured value.
( Set ) Update the setting with the current measured value.
<Air> Load air to the air sensor position.
<4 L> Load air of 4 L
<1 L> Load air of 1 L

Look here for air

2-24
2.13 Controlling the Auto Sampler

Adjusting the air sensor sensitivity


If the solvent to be used is changed or if the needle tubing or air sensor is replaced,
adjust the air sensor sensitivity.

1 Press (AirS.) on Sampler parameter screen 1 to display the air sensor sensitivity
adjustment screen.
2 Press <Meas.> to measure the transmissive light strength of air and solvent.
The intermediate value between the maximum and minimum is calculated.
3 Press (Set) to confirm the value of Step 2 as the threshold.

[Air sensor sensitivity adjustment screen]


AirSens. Set : 450
Measure : 450 (300 - 600)

( Set ) <Meas. > ( Back )

Set Current air sensor threshold


Measure Measured air sensor threshold (minimum - maximum)
( Set ) To confirm the measured value
<Meas.> To adjust the air sensor sensitivity

When the difference between the maximum and minimum is below 100, the
air sensor may not function well at analysis. Wash the sampler thoroughly and
execute measurement again.
Instead of automatic adjustment, manual input is possible. Enter arbitrary
numeric value after Set, and press ENT .

2-25
2.13 Controlling the Auto Sampler

Changing the loop volume (Sampler parameter screen 2)


This instrument is equipped with a 100-L sample loop. For injection over 100 L,
replace the loop with a larger loop. If the volume of the sample loop is replaced,
change the loop volume setting. When the EcoSEC WorkStation is in use, the loop
volume is recorded as injection volume if the setting volume is greater than the loop
volume.

1 Press (Page) on Sampler parameter screen 1 to display Sampler parameter


screen 2.
2 Enter the new loop volume at Loop Volume using the numeric keys and
press ENT .

[Sampler parameter screen 2]


AS
Loop Volume: 100

( Page ) (PrsOut) ( Unit ) ( Back )

Loop Volume Sample loop volume [L]

For the sample loop replacement method, see 5.8, Replacing the Sample
Loop.
From the viewpoint of the linearity of injection volume and the carry over, we
recommend the use of a sample loop less than 500 uL.

2-26
2.13 Controlling the Auto Sampler

Checking a cup lacking a sample (Sampler parameter screen 3)


If a sample shortage error is found during analysis, this instrument skips the cup
lacking a sample and analyzes the next cup. Skipped cups can be checked on
Sampler parameter screen 3.

1 Press (Page) twice on Sampler parameter screen 1 to display Sampler parameter


screen 3.

[Sample parameter screen 3]


AS Cup Empty 1234567890 1234567890
1 - 20 cccccccccc ccccccccc
21 - 40 ccccccccc cccccccccc
( Page ) ( Up ) ( Down ) ( Unit ) ( Back )

The row of 1 to 20 indicates the status of Cup No. 1 to 20 sequentially from the left. By
pressing (Up) or (Down), the status of Cup No. 1 to 100 can be checked. c indicates a
cup with no sample shortage or no injection and indicates a cup having a sample
shortage.
In the above figure, Cup No. 13 and 25 were lacking a sample.

2-27
2.14 Controlling the Detector (RI)

Auto balance

Press BALANCE . The detector output signal moves to the set balance. UV auto
balance is executed only when an optional UV detector is equipped.

Detector (RI) setting change

Change the settings of the detector (RI) as described below.


First, display the RI detector parameter screen by the following procedure:

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT to display the RI detector parameter screen.

[RI detector parameter screen]


RI: 0.000 Temp. : 2 (40 )
Range : 2 (256) Pola. : 1 (+)
Balance : 0 Resp. : 1 (0.5)
< Temp > <NGlass> ( Unit ) ( Back )

RI Displays the RI detector output value. The display range is from


1,000 to +1,000 [mV].
Range Set the range of analog output from the RI terminal on the right side
of this instrument and digital output by USB communication. Enter 1
(64) or 2 (256) and press ENT . The output value is in the selected
range 10-6RIU/1V.
Balance Setting value at auto balance. Enter the numeric value and
press ENT . The setting range is from 1,000 to +1,000 [mV].
Temp. Set the control temperature of the RI detector optical block. Enter 1
(35C), 2 (40C), or 3 (45C) and press ENT .
Pola. Set the polarity of RI detector output. Change the polarity to output a
negative peak to the positive side.
Enter 0 ( - ) or 1 (+) and press ENT .

2-28
2.14 Controlling the Detector (RI)

RESP. Set the time constant of RI detector output Enter 1 (0.5 s), 2 (1.0 s),
or 3 (3.0 s) and press ENT .
<Temp> Turn optical block temperature control ON or OFF. When the
temperature control is turned ON, the RI.Temp LED lamp lights.
<NGlass> To do the optical auto balancing.

The response is changed according to the half-value width of the peak. The
table gives the reference response for the half-value width of each peak.

Half-value width Response (s)


3 seconds or less 0.5
Approximately 10 seconds 1.0
30 seconds or more 3.0

Auto balancing is electrical adjustment. After solvent replacement, optical


adjustment must be done.
Detector (RI) signals are very sensitive to temperature variation. For the
stable baseline, set the RI optical block temperature equal to or slightly higher
than the column oven temperature.
If auto balance is executed when the detector output (baseline) is not stable
after solvent replacement, for example, an auto balance error may occur. In
this case, flow the solvent adequately and execute auto balance again after
the detector output becomes stable.

2-29
2.15 Setting the Warmup Conditions

Set or change warmup conditions as follows:


1 Press (Seq.) on Monitor screen 1 to display the process screen .
2 Press (Warmup) to display Warmup screen 1.

[Warmup screen 1]
Column: 1(Column1) UVLamp: 1(ON)
Purge: 1(EXEC) 10
WarmupFlow%: 50 (0.300 0.300)
( Page ) ( Back )

Column Set the column switching valve position.


Enter 0 (KEEP), 1 (Column1), or 2 (Column2) and press ENT .
When 0 (KEEP) is set, warmup starts with current position.
This is displayed only when an optional column switching valve is
equipped.
UVLamp Select whether to turn on the UV detector lamp.
Enter 0 (OFF) or 1 (ON) and press ENT
.
This is displayed only when an optional UV detector is equipped.
Purge Select whether to execute purge at warmup.
Enter 0 (OFF) or 1 (EXEC) and press ENT .
The numeric value at right indicates the purge volume. To change the
value, enter a numeric value from 1 to 150 [mL] by the numeric keys
and press ENT
.
WarmupFlow% Enter the flow rate at warmup start by the ratio (1 to 100%) to the set
flow rate at analysis. In ( ), the actual flow rates are displayed in
order of sample and reference.

If liquid is supplied at the analysis flow rate when the column temperature is still
low at the start of warmup, the column may be deteriorated by a great pressure
difference in the column.
Set the flow rate at warmup (WarmupFlow%) lower than the analysis flow rate
(approximately 50% is recommended).

2-30
2.15 Setting the Warm-up Conditions

[Warm-up screen 2]
CO: 1 (ON ) PO: 1 (ON ) RI: 1 (ON )
WarmupTime : 15
SteadyTime : 0
( Page ) ( Back )

CO,PO,RI Select whether to execute temperature control to the column oven,


pump oven, or RI detector. Enter 0 (OFF) or 1 (ON) and press ENT
.
WarmupTime Set the time to change the flow rate from that at the start of warmup
start to that at analysis. To change the time, enter a numeric value
from 0 to 999 [min] by the numeric keys and press ENT .
SteadyTime Set the wait time until the start of analysis when analysis is reserved
during warmup. To change the time, enter a numeric value from 0 to
999 [min] by the numeric keys and press ENT .

If the column oven control temperature is set to 40C, it is recommended to set


the time of changing to the analysis flow rate (WarmupTime) to 15 minutes or later
after the start of warmup.

2-31
2.16 Executing Warmup

To start warmup, press WARMUP on the operator panel. The LED lamp remains lit during
execution. If WARMUP is pressed and held for one second when the LED lamp is lit,
warmup is finished immediately.

During warmup, analysis or shutdown can be reserved.


If ANALYZE is pressed during warmup, analysis is reserved and the LED lamp
starts flashing. Analysis set on the sample queue is executed automatically
after SteadyTime.
Using the weekly timer function, warmup can be executed at specified time on
a specified day of the week.

2-32
2.17 Setting the Shutdown Conditions

Set and change the shutdown conditions as follows:


1 Press (Seq.) on Monitor screen 1 to display the process screen.
2 Press (S.Down) to display Shutdown screen 1.

[Shutdown screen 1]
AfterSeq.Time : 10
ShutdownFlow% : 50(0.300 0.300)
CO: 0 (OFF) PO: 0 (OFF) RI: 0 (OFF)
( Page ) ( Back )

AfterSeq.Time Set the shutdown start time at the end of analysis.


Enter a numeric value from 0 to 999 [min] and press ENT .
ShutdownFlow% Enter the flow rate at shutdown by the ratio (1 to 100%) to set the
flow rate at analysis. In ( ), the actual flow rates are displayed in
order of sample and reference.
CO,PO,RI Select whether to continue or stop temperature control of the
column oven, pump oven, or RI detector optical block. Enter 0
(OFF) or 1 (ON) and press ENT .

If shutdown is reserved during analysis, the instrument waits for AfterSeq.Time


after the end of analysis on the sample queue and executes shutdown
processing.

If temperature control is stopped at the analysis flow rate when analysis using the
column oven is finished, the column may be deteriorated by a great pressure
difference in the column. If the instrument is stopped immediately after analysis, a
temperature drop may cause the solvent to shrinkage and flow back into the
column. After analysis, stop the temperature control of the column oven and keep
flow at a lower flow rate than the analysis flow rate (approximately 50% is
recommended) until the column cools down.

2-33
2.17 Setting the Shutdown Conditions

[Shutdown screen 2]

ShutdownTime: 30
Power: 0 (OFF)
( Page ) ( Back )

ShutdownTime Set the time from the start of shutdown until flow stops. Enter a
ENT
numeric value from 0 to 999 [min] and press .
Power Select whether to turn the power OFF at the end of shutdown. Enter
0 (OFF) or 1 (ON) and press ENT
.

Considering the pressure balance in the column, the ShutdownTime is


recommended to be 30 minutes or later after the start of shutdown when the set
temperature of the column oven is 40C.

2-34
2.18 Executing Shutdown

SHUTDOWN
To start shutdown, press on the operator panel. The LED lamp remains lit
during execution. If the key is pressed and held for one second when the LED lamp is
lit, shutdown is suspended.

If the SHUTDOWN
is pressed during analysis, shutdown is reserved and the
LED lamp starts flashing. When AfterSeq.Time has passed after analysis,
shutdown is executed .
Even during warmup, shutdown can be reserved as during analysis.
By using the weekly timer function, shutdown can be executed at a specified
time on a specified day of the week. However, analysis has priority and
shutdown is not executed during analysis.
If analysis is aborted by an error, error processing has priority and shutdown
is not executed.

2-35
2.19 Setting the Sample Queue

Set or change the sample queue as follows:


1 Press (Seq.) on Monitor screen 1 to display the process screen.

[Process screen]
RunTime: 15.0
Balance : 0 (OFF)

(Warm-up) ( Ana. ) (S.down) (Timer ) ( Back )

RunTime Enter the sample injection interval. Enter a numeric value from 3 to
999.9 [min] and press ENT .
Balance Select whether to execute auto balance automatically.
Enter 0(OFF)/1(INJ)/2(DAC) and press ENT .
OFF : No auto balance
INJ : Auto balance just before sample injection
DAC : Auto balance just before data acquisition (when the
EcoSEC-WorkStation is not used, the timing is the
same as that for INJ).

2 When specifying an injection cup, press (Ana.) to display the sample queue
screen.

[Sample queue screen]


No Cup Repeat Inj.Vol. Wave.
01 1- 1 1 10 254
02 2- 2 1 10 254
( Up ) ( Down ) ( Ins. ) ( Del. ) ( Back )

No Displays the program execution order. This number is automatically


assigned at setting.
Cup Enter the first and last cup numbers. The input range is from 1 to 100,
but the first cup must be equal to or smaller than the last cup. For
analysis under the same conditions, only this line need be set.

2-36
2.19 Setting the Sample Queue

Repeat Enter the number of repetitive injections from a single sample cup.
The input range is from 1 to 9 [times]. Enter a value after checking the
injection volume, the presuction volume, and the injection volume.
Inj.Vol. Enter the injection volume. The input range is from 1 to 1,500 [L].
Wave. Enter the wavelength of the UV detector. The input range is from 195 to
350 [nm].
If the setting is changed here, the wavelength is changed just before the
injection.
This is displayed only when an optional UV detector is used.
( Up ) Move the cursor one line above.
Scroll the screen if there are more lines above.
( Down ) Move the cursor to one line below.
Scroll the screen if there are more lines below.
( Ins. ) Add to the current line. The setting one line above is copied and
inserted.
( Del. ) Delete the current line.

Set the auto balance timing where the baseline is stable. For analysis
(overlap injection) shown in the figure below, auto balance at the injection
timing is actually executed at the negative peak position. If auto balance is
executed there, the baseline position will deviate greatly.

Auto balance Auto balance Auto balance

Acquisition Acquisition Acquisition

If a detector of a different manufacturer is connected, auto balance does not


work.
From the viewpoint of the linearity of injection volume and the carry over, we
recommend the use of a sample loop less than 500 uL.

2-37
2.20 Preparing Samples

Five types of sample cups are prepared for this instrument. (See 11.2, Consumables.)
If evaporation causes a sample concentration problem, seal a sample cup with an
aluminum sheet or a septum packing, as shown below. The aluminum sheet or septum
packing is used once only because it will have a hole after sample injection.
It is recommended to place as much of the sample as possible because bubbles may be
loaded if the sample is not sufficient.
If evaporation causes a sample concentration problem in repetitive injection from a single
sample cup, use a septum-type cup.

Cap (Part No. 022007)


Cap (Part No. 016330)

Packing (Part No. 013717)


Seal for Septum
(Part No. 022009)
Aluminum sheet (Part No. 013718)

Sample cup Sample cup


(Part No. 022006)
Glass (transparence) (Part No. 016315)

Glass (brown) (Part No. 016314)

Glass (taper) (Part No. 016317)

The instrument may not load a sample of high viscosity. Change the syringe
speed or dilute the sample.
At suction, the needle does not reach the bottom of a cup. Place a sample to
10 mm or higher from the bottom of a cup.

2-38
2.21 Loading Sample Cups

Load sample cups on a sample rack as follows:

1 Press to eject the sample rack.


2 Take out the sample rack and load sample cups on a desk.
3 After loading samples, insert the sample rack.
2 Press , and the sample rack will be taken into the instrument.

Eject

Insert

After sample injection, the sample rack may be ejected until the next sampling
operation starts. If the next sampling time comes when the sample rack is
ejected (not inserted correctly), the instrument will pause.
When inserting the sample rack, push the rack in until it clicks. However,
excess force may damage the instrument.
When the sample rack is inserted correctly, the LED lamp lights.

2-39
2.22 Starting and Stopping Analysis

To start or stop analysis, ANALYZE


on the operation-display is used.

Starting or stopping analysis

If ANALYZE on the operation display is pressed not during warmup, analysis is


executed. Then the LED lamp lights ON.
If ANALYZE is pressed and held for one second when the LED lamp is lit, an analysis
stop is reserved to stop the analysis after the current data acquisition. Then the LED
lamp flashes at short intervals.
If ANALYZE is pressed and held again for one second when an analysis stop is
reserved, analysis is forced to end by discarding even the current data acquisition.

Reserving or canceling analysis

If ANALYZE on the operation display is pressed during warmup, analysis is reserved.


Then the LED lamp flashes at long intervals.
If ANALYZE is pressed and held for one second when analysis is reserved, the
reservation is cancelled.

2-40
2.23 Weekly Timer

The weekly timer is a function to execute warmup or shutdown at a specified time on a


specified day of the week.
Set or change the weekly timer as described below. The warmup or shutdown conditions
cannot be changed here. See 2.15, Setting the Warmup Conditions and 2.17, Setting the
Shutdown Conditions.

1 Press (Seq.) on Monitor screen 1 to display the process screen.


2 Press (Timer) to display Weekly timer screen 1.

[Weekly timer screen 1]


Mon W.up: 0(OFF) 09: 00 S.down: 0(OFF) 17: 00
Tue W.up: 1(ON) 09: 00 S.down: 1(ON) 17: 00
Wed W.up: 1(ON) 09: 00 S.down: 1(ON) 17: 00
( Page ) ( Date ) ( Back )

W.up Select whether to reserve warmup with the timer by the day of the week.
Enter 0 (OFF) or 1 (ON) and press ENT .
Enter the warmup start time.
S.down Select whether to reserve shutdown with the timer by the day of the
week. Enter 0 (OFF) or 1 (ON) and press ENT .
Enter the shutdown start time.
(Page) Change the screen. Page 1 is for Monday to Wednesday, Page 2 for
Thursday to Saturday, and Page 3 for Sunday.

When using a weekly timer, keep the main power ON. Also, check the
warmup and shutdown conditions well before use.
If warmup or analysis is in progress at a specified warmup time, priority is
given to the current processing.
If analysis is in progress at a specified shutdown time, priority is given to the
current processing. Shutdown is executed after the analysis.

2-41
2.24 Setting the Clock

Adjust the built-in clock of this instrument as follows:

1 Press (Seq.) on Monitor screen 1 to display the process screen.


2 Press (Timer) to display Weekly timer screen 1.
3 Press (Date) to display the date and time setting screen.

[Date and time setting screen]


Now : 2007/01/01 MON 12: 00
Set : 2007/02/01 2(TUE) 12: 00

( Set ) ( Back )

Now Displays the current date, day of the week, and time.
Set Enter a day of the week and time to set.
Enter 0 (SUN) to 6 (SAT) for a day of the week and time by the
24-hour system.
(Set) Confirm the setting.

2-42
2.25 Checking the Instrument Program Version

The version of the program installed in the instrument can be checked as follows:

1 Press (Option) on Monitor screen 2 to display the option screen.

[Option screen]
PRG Main : 99.99
Sub1 : 99.99
Sub2 : 99.99
(E.Log ) ( Back )

Main Version number of the main program


Sub1 Version number of Slave 1 program
Sub2 Version number of Slave 2 program

TOSOHs service personnel will update the program.

2-43
2.26 Checking Error Logs

This instrument stores the most recent nine error logs. They can be checked as follows:

1 Press (Option) on Monitor screen 2 to display the option screen.


2 Press (E.Log) to display Error log screen 1.

[Error log screen 1]


1 07/01/01 12: 00 E0501
2 07/01/01 11: 00 E0020
3 07/01/01 11: 00 E0501
( Page ) ( Back )

The error history is displayed in order of date, time, and error number.
By changing (Page), you can check up to nine error logs.
For the error numbers and their contents, see Chapter 6, Troubleshooting.

If the EcoSEC WorkStation is connected, all error logs can be stored and
checked.

2-44

Chapter 3

Analysis
3.1 Analysis Notes

About washing liquid

Use a solvent to wash the auto sampler.


When using a salt-containing solvent or a buffer solution, however, select deionized
water for the aqueous type or a salt-free organic solvent for the organic type.
Otherwise, the syringe and other components may become worn or damaged by
precipitation.

Solvent replacement

When replacing a solvent, check that the solvents are miscible with each other.
If the solvents are not miscible, substitute the current solvent with a miscible solvent
and then with the target solvent.

For solvent replacement, it is recommended to drain the solvent from the


degasser system once and purge the solvent to be used, whether or not the
solvents are miscible with each other (see 2.7, Purge Function). Replacement
without drainage is possible but this takes time.

Tubing washing

After a salt-containing solvent or a buffer solution is used, wash the tubing with
deionized water or ion-exchanged water. Without washing, salt may precipitate and
disable further use.
If a chlorine-based organic solvent such as chloroform is used, wash the tubing with
ethanol or isopropanol. If the tubing is not washed, rusting may make accurate
analysis impossible.

Cell withstand pressure

The cell withstand pressure of the detector (RI) is 0.5 MPa.


When connecting another instrument or tubing to an outlet (sample or reference), take
great care not to impose back-pressure on the cell.

3-2
3.1 Analysis Notes

Use from the dry state

If the plunger seal or plunger is dry, be sure to purge it before flow start. (See 2.7,
Purge Function.)

For long-time storage

When not using the instrument for one week or longer, remove the column, wash the
tubing, and replace the solvent with ethanol or isopropyl before storage.

Static electricity

When an inflammable organic solvent is used as a solvent, static electricity may cause
a fire or explosion.
To prevent an accident, the accumulation of static electricity should be suppressed.
(See 13.5, Countermeasures against Static Electricity.)

3-3
3.2 Analysis Flow Chart

This section explains the operating procedure of this instrument from power-on until
power-off.

Power ON Power-ON initializes each section.


Various settings are reset to the values before the previous
power-OFF.

Set warmup Set the warmup conditions.


conditions (See 2.15, Setting the Warm-up Conditions.)

Set shutdown Set the shutdown conditions.


conditions (See 2.17, Setting the Shutdown Conditions.)

Set data processing Set data processing as you desire.


When EcoSEC WorkStation is used, set a method.

Set sample queue Set the sample cup number, injection volume, injection
interval, and injection count for the sample queue.
(See 2.19, Setting the Sample Queue.)

Warmup Execute warmup.


(See 2.16, Executing Warmup.)

Prepare and load Prepare samples and load them on a rack.


samples (See 2.20, Preparing Samples and 2.21, Loading Sample
Cups.)

Analysis Execute analysis.


(See 2.22, Starting and Stopping Analysis.)

Shutdown Execute shutdown.


(See 2.18, Executing Shutdown.)

Power OFF Settings are stored at power-OFF.

3-4

Chapter 4

Performance Check
4.1 Checking Pump Unit Performance

Flow rate precision check

[Conditions]
Flow rate : 0.5 mL/min
Solvent : Deionized water (degassed)
Load : capillary (inner diameter: 0.1 mm, length: 4 m)

[Procedure]
1 Open the column oven door and connect a stainless steel tubing to the
channel on the sample and reference side.
2 Replace the solvent in the system with deionized water and start flow.
3 When the flowing pressure has become stable, collect the discharge liquid
from the sample and reference sides in a measuring cylinder or measuring
flask and measure the time required to collect 5 mL of water. Repeat this
procedure three times.
4 Calculate the actual flow rate as follows:
Actual flow rate = 5 mLMeasuring time (min)
5 Determine the maximum, minimum, and average actual flow rates from the
measurement results and calculate the flow rate precision as follows:
A B
Flow rate precision = 100 (%)
B
A: Maximum or minimum actual flow rate
B: Average actual flow rate
6 Check that the flow rate precision is within 0.4%.

Before replacing the solvent in the system, check the solvent miscibility.

Flow rate accuracy check

[Procedure]
1 From the average actual flow rate obtained by the above measurement,
calculate the flow rate accuracy as follows:
BC
Flow rate accuracy = 100 (%)
C
B: Average actual flow rate
C: Set flow rate
2 Check that the flow rate accuracy is within 4.0%.

4-2
4.2 Checking Pump and Column Oven Performance

Control temperature check

[Procedure]
1 Set the temperatures of the pump oven and column oven at 40C.
(Room temperature: 20 to 25C)
2 Start temperature control of each oven.
3 After 90 min, check the temperature displayed on the monitor.
4 Check that the temperature of each oven is within 400.2C.

Gas sensor check

[Procedure]
1 With the temperature control ON, place a wiper containing approximately 0.5
mL of THF in the oven and close the door.
2 Check that liquid leakage occurs and temperature control stops.
3 With the oven door open, allow the THF gas to sufficiently dissipate from the
oven.

The gas sensor sensitivity differs with the solvent. Check in advance
that the gas sensor detects the gas to use.

4-3
4.3 Checking Detector (RI) Performance

Sensitivity check

[Conditions]
Sample : 0.67 g of sucrose dissolved in 1 liter of deionized water
Injection volume : 500 L
Flow rate : 0.2 mL/min (both sample and reference)
Range : 256
Response (RI) : 0.5 s
Polarity :
Control temperature : 40C
Column : None
Data acquisition time : 0 - 5 min
Sampling interval : 100 ms
Data analysis condition : Column test

[Procedure]
1 Replace the sample loop of the auto sampler with the 500 L sample loop.
(See 5.8, Replacing the Sample Loop.)
2 Replace the solvent in the detector (RI) cell (both sample and reference) with
deionized water.
3 Under the above conditions, inject the sample into the cell and record the RI
output signal.
4 In the peak editor for the EcoSEC WorkStation data analysis, set the baseline
as shown below and check that the peak height is within 390 20 mV.

Check that the peak top becomes flat.


Output

Within
390 mV20 20
390 mV mV

Edit the baseline flat.


4-4
4.3 Checking Detector (RI) Performance

Be sure to check that the peak is flat at the top. The cell must be saturated
with a sample for an accurate sensitivity check.
If the tubing volume between the sample loop and the cell is greater than the
initial volume because an optional column switching valve is used, the cell
may not be saturated with a sample. In this case, remove the valve tubing
and check again.
If the EcoSEC WorkStation is not used, connect an external instrument
(integrator or recorder) through the RI terminal and check that the output
peak height is within 390 20 mV.

4-5
4.4 Checking Auto Sampler Performance

Injection reproducibility check

[Conditions]
Washing liquid and solvent : Deionized water (degassed)
Sample : 0.67 g of sucrose dissolved in 1 liter of
deionized water
Injection volume : 10 L
Flow rate : 0.5 mL/min (both sample and reference)
Load : Capillary (inner diameter: 0.1 mm, length: 4 m)
Range : 256
Response (RI) : 0.5 s
Control temperature : 40C
Injection interval : 4 min
Data acquisition time : 0 - 3 min
Sampling interval : 50 ms
Data analysis condition : Column test

[Procedure]
1 Under the above conditions, prepare two sample cups on a sample rack,
inject the sample five times (10 times) per cup, and record the peak height.
2 Measure each peak height and calculate CV.

(xi x )
2

s=
n 1
s
CV = 100(%)
x
s : Standard deviation
xi : Measured value
x : Average value
n : Data count
CV : Coefficient of variation
3 Check that CV is 1.5 or less.

When the EcoSEC WorkStation is used, the statistical calculation function is


useful. For details, refer to the operators manual of the EcoSEC WorkStation.

4-6
4.5 Comprehensive Inspection

Drift check

[Conditions]
Solvent : THF
Range : 256
Response (RI) : 1.0 s
Control temperature : 40C
Polarity :
Data acquisition time : 0 - 120 min
Sampling interval : 1,000 ms

[Procedure]
1 Turn on the power to the instrument, start temperature control, and flow THF
to both the sample and reference sides at a flow rate of 1 mL/min.
2 Under the above conditions, record the detector (RI) baseline for two hours.
3 Measure the one-hour baseline fluctuation from one hour after power-on and
check that the fluctuation is within 5107RIUh (within 2 mV).

60min

4-7
4.5 Comprehensive Inspection

Noise check

[Conditions]
Range : 256
Response (RI) : 0.5 s
Control temperature : 40C
Polarity :+
Data acquisition time : 0 - 5 min
Sampling interval : 100 ms

[Procedure]
1 After checking the drift, stop flow.
2 After the baseline becomes stable, record the detector (RI) baseline for five
minutes under the above conditions.
3 Divide the baseline into 30-second segments. Measure the noise width in
each segment and obtain the average value of the 10 segments.
4 Check that the average noise width is within 2.510-8RIU (within 0.1 mV).

10
Y
R=1

X1 X2 X3 X4 X5 X6 X7 X8 X9 X10

Y2 Y6 Y7 Y8
Y3 Y5 Y9 Y10
Y1
Y4

5 min

4-8

Chapter 5

Maintenance and Inspection


5.1 Washing the Check Valves

If pulsation or pressure fluctuation increases during flow, wash the check valves.

[Necessary items]
Wrench 810 mm (Part No. ----------) 1 Accessory
Wrench 1214 mm (Part No. ----------) 1 Accessory
Internal-type union (Part No. 0007337) 2
Finger tight fitting (Part No. 0016566) 2
Deionized water or ethanol Appropriate amount
Solvent bottle 1
Beaker 1
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol.
4 Close the stop valve. (See 2.6, Stop Valve.)
5 With a wrench, disconnect the tubing from the check valves.
6 With a wrench, remove the check valves from the pump head.

Check valve
(Outlet)

Check valve
(Inlet)

5-2
5.1 Washing the Check Valves

7 Soak the removed check valves in a beaker containing deionized water or


ethanol and wash them by ultrasonic cleaning.
8 With a wrench, attach the check valves to the pump head.
9 With a wrench, connect the tubing.
10 Execute purge and replace the deionized water or ethanol in the system with
an used solvent.
Check that there is no leakage from tubing joints. (See 2.7, "Purge Function.")

For solvent replacement in the system, check the solvent miscibility in advance.

The stop valve opens automatically during the purge.

5-3
5.2 Replacing the Check Valves

If the pulsation or pressure fluctuation is great even after the check valves of the pump unit
are washed, replace the check valves.

[Necessary items]
Check valve assembly (Outlet) (Part No. 0022012) Necessary quantity
Check valve assembly (Inlet) (Part No. 0022011) Necessary quantity
Wrench 810 mm (Part No. ----------) 1 Accessory
Wrench 1214 mm (Part No. ----------) 1 Accessory
Internal-type union (Part No. 0007337) 2
Fingertight fitting (Part No. 0016566) 2
Deionized water or ethanol Appropriate amount
Solvent bottle 1
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol.
4 Close the stop valve. (See 2.6, Stop Valve.)
5 With a wrench, disconnect tubing from the check valves.
6 With a wrench, remove the check valves from the pump head.
7 With a wrench, attach new check valves to the pump head.
8 With a wrench, connect the tubing.
9 Execute purge and replace deionized water or ethanol in the system with an
used solvent.
Check that there is no leakage from tubing joints. (See 2.7, "Purge Function.")

For solvent replacement in the system, check the solvent miscibility in advance.

The stop valve opens automatically at purge.

5-4
5.3 Replacing the Plunger Seal

If solvent still leaks from the washing block behind the pump head, replace the plunger
seal.

[Necessary items]
Plunger seal (Part No. 0019190) Necessary quantity
Wrench 810 mm (Part No. ----------) 1 Accessory
Hex wrench 4 mm (Part No. ----------) 1 Accessory
Plunger seal replacement tool (Part No. 0018524, 0018525) 1 set Accessory
Internal-type union (Part No. 0007337) 2
Finger tight fitting (Part No. 0016566) 2
Deionized water or ethanol Appropriate amount
Solvent bottle 1
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol.
4 Close the stop valve. (See 2.6, Stop Valve.)
5 With a wrench, remove the tubing from the pump head.
6 With the 4 mm hex wrench, loosen the cap screw at the center of the pump
head holder and remove the right and left mounting screws.
7 Pull the pump head straight out to remove.
Check the plunger for no damage. Replace the plunger if damaged.

5-5
5.3 Replacing the Plunger Seal

Plunger seal

Pump head

Collar

Mounting screw

Washing block

Pump head holder

Cap screw
(Only loosen)

8 Remove the plunger seal from the pump head using the guide bar of plunger
seal replacement tool, as shown below.

Guide bar

Plunger seal

Pump head

5-6
5.3 Replacing the Plunger Seal

9 Set a new plunger seal on the guide bar of plunger seal replacement tool as
shown below.
10 Insert the guide bar into the pump head. (Note the plunger seal insertion
direction.)
11 Hold the guide bar upright and push the plunger seal into the pump head with
the seal holder.
12 While holding the seal holder, extract the guide bar straight.
13 Remove the seal holder.

Seal holder

Plunger seal

Guide bar

Pump head

14 Push the pump head straight in. With the 4 mm hex wrench, attach the right
and left mounting screws to the pump head holder and tighten the cap screw at
the center.
15 With a wrench, connect the tubing.
16 Execute purge and replace the deionized water or ethanol in the system with
an used solvent.
Check that there is no leakage from tubing joints. (See 2.7, "Purge Function.")

For solvent replacement in the system, check the solvent miscibility in advance.

At replacement of the plunger seal, it is recommended that the plunger be


washed. When the pump head is removed, wipe the plunger using a wiper
saturated with deionized water or ethanol.
The stop valve opens automatically at purge.

5-7
5.4 Replacing the Plunger

If solvent still leaks from the washing block even after the plunger seal at the pump unit is
replaced, replace the plunger.

[Necessary items]
Plunger (Part No. 0019762) Necessary quantity
Wrench 810 mm (Part No. ----------) 1 Accessory
Wrench 1214 mm (Part No. ----------) 1 Accessory
Hex wrench 3 mm (Part No. ----------) 1 Accessory
Hex wrench 4 mm (Part No. ----------) 1 Accessory
Internal-type union (Part No. 0007337) 2
Finger tight fitting (Part No. 0016566) 2
Deionized water or ethanol Appropriate amount
Solvent bottle 1
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol.
4 Close the stop valve. (See 2.6, Stop Valve.)
5 With a wrench, remove tubing from the pump head.
6 With the 4 mm hex wrench, loosen the cap screw at the center of the pump
head holder and remove the right and left mounting screws.
7 Pull the pump head straight out to remove.
8 With the 3 mm hex wrench, remove the washing block mounting screws.
9 Pull the washing block straight out to remove.
10 With a wrench, remove the old plunger and attach a new plunger.
11 When the plunger is removed, check the diaphragm for scratches or cracks. If
scratch or crack is found, replace the diaphragm (Part No. 019056).

5-8
5.4 Replacing the Plunger Seal

Diaphragm

Plunger

Washing block

Plunger seal

Collar

Mounting screw
(large)

Washing block mounting


screws
Pump head

Pump head holder

Cap screw
(Only loosen)

12 Push the washing block straight in and attach the washing block mounting
screws with the 3 mm hex wrench.
13 Push the pump head straight in. With the 4 mm hex wrench, attach the right
and left mounting screws to the pump head holder and tighten the cap screw at
the center.
14 With a wrench, connect the tubing.
15 Execute purge and replace the deionized water or ethanol in the system with
an used solvent.
Check that there is no leakage from tubing joints. (See 2.7, "Purge Function.")

For solvent replacement in the system, check the solvent miscibility in


advance.
When attaching the plunger, make sure that the diaphragm is not distorted.

The stop valve opens automatically at purge.

5-9
5.5 Washing or Replacing the Inline Filter

If the pressure becomes higher at flow, the inline filter may be stopped up. Wash or replace
the inline filter.

[Necessary items]
Inline filter element (Part No. 0017714) Necessary quantity
Wrench 1417 mm (Part No. ----------) 2 Accessory
Wrench 810 mm (Part No. ----------) 1 Accessory
Internal-type union (Part No. 0007337) 2
Finger tight fitting (Part No. 0016566) 2
Deionized water or ethanol Appropriate amount
Solvent bottle 1
Beaker 1
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol and check
the pressure.
4 Close the stop valve. (See 2.6, Stop Valve.)
5 With a wrench, remove the tubing from the top of the inline filter.
6 With a wrench, remove the inline filter.
7 Soak the removed inline filter in a beaker containing deionized water or ethanol
and wash them by ultrasonic cleaning. If the filter element has scratches,
cracks, or stains, replace the filter element.
8 With a wrench, attach the inline filter.
9 With a wrench, connect the tubing to the top of the inline filter.
10 Execute purge and replace deionized water or ethanol in the system with an
used solvent.
Check that there is no leakage from tubing joints. (See 2.7, "Purge Function.")

5-10
5.5 Washing or Replacing the Filter

<Inline filter>

Inline filter

Press in

Assembly

Inline filter element

Tighten with

wrench

For solvent replacement in the system, check the solvent miscibility in advance.

The stop valve opens automatically at purge.

5-11
5.6 Replacing the 6way Valve Rotor Seal and Stator

If the reproducibility of injection volume is not well or if liquid leaks from the needle, check
the rotor seal and stator of the 6way valve (sample injection valve) for damage. Replace
the rotor seal and stator if damaged. When changing the rotor seal and stator of the
sampler 4way valve at the same time, see 5.7, Replacing the 4way Valve Rotor Seal and
Stator.

[Necessary items]
Rotor seal(6way) (Part No. 0016415) Necessary quantity
6way Valve for Stator (Part No. 0016451) Necessary quantity
Wrench 810 mm (Part No. ----------) 1 Accessory
Wrench 1/45/16 (Part No. ----------) 1 Accessory
Hex wrench 3 mm (Part No. ----------) 1 Accessory
Beaker 1
Deionized water or ethanol Appropriate amount
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol.
4 Close the stop valve. (See 2.6, Stop Valve.)
5 With a wrench, remove the tubing (other than sample loop) from Ports 2, 3, 5,
and 6 of the 6way valve.
6 With a hex wrench, remove the three bolts securing the stator.

For solvent replacement in the system, check the solvent miscibility in advance.

Loosen the bolts evenly.

Sliding

6way valve stator (Part No. 016451)

5-12
5.6 Replacing the 6way Valve Rotor Seal and Stator

7 Remove the stator from the valve body and check the sliding surface of the
stator. Only if damage is found, replace the stator.
8 If no damage is found, soak the removed stator in a beaker containing
deionized water or ethanol and then wash it by ultrasonic cleaning.

When removing the sample loop for stator replacement, attach the stator to the
valve body.

9 Remove the rotor seal.

Rotor seal(6way) (Part No. 016415)

If the rotor seal is difficult to remove, drive two M3 screws into the holes of the
rotor seal.

Rotor seal

M3 screw

5-13
5.6 Replacing the 6way Valve Rotor Seal and Stator

10 Attach a new rotor seal.


The projection of the rotor seal should be on the stator side.
11 Attach the stator and secure it evenly with three bolts so that there will be no
gap between the stator and valve body.

Hex-socket head bolt

Tighten with no gap

12 With a wrench, connect tubing to each port.

<6way valve connection port>

3: Column
4: Sample loop

2: Pump

5: 4way valve
1: Sample loop

6: Needle

5-14
5.7 Replacing the 4way Valve Rotor Seal and Stator

If the reproducibility of injection volume is not well or if liquid leaks from the needle, check
the rotor seal and stator of the sampler 4way valve (pressure relief valve) for damage.
Replace the rotor seal and stator if damaged. When changing the rotor seal and stator of
the 6way valve (sample injection valve) at the same time, see 5.6, Replacing the 6way
Valve Rotor Seal and Stator.

Before changing the degasser volume, turn the main power OFF. Since
some sections are driven by motors, fingers or objects may be caught or
pulled into the instrument, causing serious injury.

[Necessary items]
Rotor seal(4way) (Part No. 0016414) Necessary quantity
4way Valve Stator (Part No. 0016450) Necessary quantity
Wrench 810 mm (Part No. ----------) 1 Accessory
Wrench 1/45/16 (Part No. ----------) 1 Accessory
Hex wrench 3 mm (Part No. ----------) 1 Accessory
Beaker 1
Deionized water or ethanol Appropriate amount
Capillary (Part No. 0005319) 1

[Procedure]
1 Turn the main power OFF.
2 Stop flow.
3 Remove the column (if attached) and attach the capillary.
4 Replace the solvent in the system with deionized water or ethanol.
5 Close the stop valve. (See 2.6, Stop Valve.)
6 Open the sampler syringe unit on the left side of the main unit.
7 With a wrench, disconnect the tubing from the sampler 4way valve ports.
8 With a hex wrench, remove the three bolts securing the stator.

5-15
5.7 Replacing the 4way Valve Rotor Seal and Stator

For solvent replacement in the system, check the solvent miscibility in advance.

Loosen the bolts evenly. Sliding

4way valve stator (Part No. 016450)


9 Remove the stator from the valve body and check the sliding surface of the
stator. Only if damage is found, replace the stator.
10 If no damage is found, soak the removed stator in a beaker containing
deionized water or ethanol and wash it by ultrasonic cleaning.

When removing the sample loop for stator replacement, attach the stator to the
valve body.

11 Remove the rotor seal.

4way valve rotor seal (Part No. 016414)

If the rotor seal is difficult to remove, drive two M3 screws into the holes of the
rotor seal.

Rotor seal

M3 screw

5-16
5.7 Replacing the 4way Valve Rotor Seal and Stator

12 Attach a new rotor seal.


The projection of the rotor seal should be on the stator side.
13 Attach the stator and secure it evenly with three bolts so that there will be no
gap between the stator and valve body.

Hex-head socket bolt

Tighten with no gap

14 With a wrench, connect tubing to each port.

<4way valve connection port>

3: 6way valve

4: Syringe 2: End plug

5: Degasser chamber

5-17
5.8 Replacing the Sample Loop

This instrument is equipped with a 100-L sample loop. If necessary, replace the sample
loop with a loop of appropriate volume.

[Necessary items]
Wrench 1/45/16 (Part No. ----------) 1 Accessory
Deionized water or ethanol Appropriate amount
Capillary (Part No. 0005319) 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached) and attach the capillary.
3 Replace the solvent in the system with deionized water or ethanol.
4 Loosen the male nuts at Ports 1 and 4 of the 6way valve in the column oven
and remove the sample loop.
5 Attach the sample loop for replacement. Tighten the male nuts while pressing
the sample loop deep inside the port.

Part No. Description


0007035 Sample loop 1,500 L
0005672 Sample loop 1,000 L
0005464 Sample loop 500 L
0005679 Sample loop 100 L
0005462 Sample loop 50 L

For solvent replacement in the system, check the solvent miscibility in advance.

After replacing the sample loop, change the setting of the loop volume.
For details, see 2.13, Controlling the Auto Sampler.
From the viewpoint of the linearity of injection volume and the carry over, we
recommend the use of a sample loop less than 500 uL.

5-18
5.9 Washing the Detector (RI) Cell

[Necessary items]
Internal-type union (Part No. 0007337) 4
Finger tight fitting (Part No. 0016566) 4
Capillary (Part No. 0005319) 2
Waste container 1
When aqueous liquid, saline solution,
or buffer solution is used: Deionized water Appropriate amount
When organic solvent is used: Ethanol or isopropanol Appropriate amount

[Procedure]
1 Stop flow.
2 Remove the column (if attached).
3 Connect a capillary to the sample column IN tubing (S.COL) and the detector
(RI) sample IN tubing (RI.S).
4 Connect a capillary to the reference column IN tubing (R.COL) and the
detector (RI) reference IN tubing (RI.R).
5 Supply the washing liquid from the solvent suction tubing (SOLVENT) at a flow
rate of 1 mL/min for 10 minutes or longer.
6 Replace the washing liquid in the system with an used solvent and flow for 10
minutes or longer.

For solvent replacement in the system, check the solvent miscibility in advance.

5-19
5.10 Washing the Inside of the System

[Necessary items]
Internal-type union (Part No. 0007337) 4
Fingertight fitting (Part No. 0016566) 4
Capillary (Part No. 0005319) 2
Deionized water Appropriate amount
Nitric acid (Regulation of 1 to 3) Appropriate amount
Solvent bottle 2
Waste container 1

[Procedure]
1 Stop flow.
2 Remove the column (if attached).
3 Connect a capillary to the sample column IN tubing (S.COL) and the detector
(RI) sample IN tubing (RI.S).
4 Connect a capillary to the reference column IN tubing (R.COL) and the
detector (RI) reference IN tubing (RI.R).
5 Replace the solvent in the system with deionized water.
6 Replace the solvent with nitric acid.
7 Flow at a flow rate of 1 mL/min. The reference flow time is 2 hours in the case
of Regulation 1 and 40 min in the case of Regulation 3.
8 Replace the nitric acid in the system with deionized water and flow for 10
minutes or longer.
9 Replace the washing liquid in the system with an used solvent and flow for 10
minutes or longer.

When using nitric acid, be sure to wear protective items (gloves and
goggles). If nitric acid gets on your skin, wash it away thoroughly by
flowing water.

For solvent replacement in the system, check the solvent miscibility in advance.

5-20

Chapter 6

Troubleshooting
6.1 Checking Errors

If an error occurs in this instrument, a buzzer will sound and the operation-display will
display an error screen.
Check the error number, error message, and error information (Info 1 to 3). For
troubleshooting, refer to the following pages.
When consulting TOSOHs service engineer, report the error number, error message, and
error information 1 to 3.
After checking the error contents, press <Buzzer> to stop the buzzer and (Back) to return
to Monitor screen 1. The buzzer will also stop if (Back) is pressed.

[Error screen]

Error number Error message Error date and time

E0407 2007/07/07 09:00


Oven (CO) Door Open
Info1 Info2 Info3
<Buzzer> (Back)

Error information 1 to 3 (Supplementary information)

The user can check up to nine logs on this instrument. For checking error
logs, see 2.26, Checking Error Logs.
When the PC control program EcoSEC WorkStation is connected, the PC
displays an error message. In addition, all error logs can be stored for later
checking.

6-2
6.2 Error Messages

Error processing level

Error processing depends on the error level, as follows:


Level Processing
0 Error indication only
Error indication is performed. When an error is not removed in the
1
back for one hour either, programmed shutdown is carried out.
Analysis stop (After the analysis end, the next injection is not
2 performed)
Programmed shutdown is carried out.
Emergency stop (The analysis carrying out is stopped)
3
Pump flow stop, Degasser stop, Temperature control stop

Error contents

The instrument displays an error number and an error message.


When the PC control program EcoSEC WorkStation is connected, the PC displays a
message.
System related errors
Error Message (Instrument)
Troubleshooting Level
No. Message (PC)
0000 USB Communication Error Turn the main power OFF and 0
USB unit ID error occurred. contact TOSOH service engineer.

0001 USB Communication Error Turn the main power OFF and 0
USB command ID error occurred. contact TOSOH service engineer.
0002 USB Communication Error Turn the main power OFF and 0
USB data error occurred. contact TOSOH service engineer.

0003 USB Communication Error Turn the main power OFF and 0
USB timing error occurred. contact TOSOH service engineer.

0013 Master System Load Error Turn the main power OFF and 0
The installed program could not be contact TOSOH service engineer.
read. (Master)

6-3
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)

0014 Slave1 System Load Error Turn the main power OFF and 0
Could not load the slave 1 program. contact TOSOH service engineer.

0015 Slave2 System Load Error Turn the main power OFF and 0
Could not load slave 2 program. contact TOSOH service engineer.

0016 Slave1 Trans Error Turn the main power OFF and 0
Error occurred in the transmission to contact TOSOH service engineer.
slave1 ROM from master ROM.
0017 Slave1 Receive Error Turn the main power OFF and 0
Error occurred in the reception to contact TOSOH service engineer.
slave1 ROM from master ROM.
0018 Slave2 Trans Error Turn the main power OFF and 0
Error occurred in the transmission to contact TOSOH service engineer.
slave2 ROM from master ROM.
0019 Slave2 Receive Error Turn the main power OFF and 0
Error occurred in the reception to contact TOSOH service engineer.
slave2 ROM from master ROM.
0020 Backup Error (Param) Turn the main power OFF and then 0
The backup loss error of the parameter ON again. Then confirm the settings.
occurred. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.
0021 Backup Error (Adjust) Turn the main power OFF and 0
The backup loss error of the instrument contact TOSOH service engineer.
adjustment value occurred.
0022 External Error Check the connected external 3
The error signal was inputted from instrument (integrator or recorder).
external instrument.
0023 Slave1 Communication Error Turn the main power OFF and 0
The internal communication error contact TOSOH service engineer.
occurred. There is no response from a
Slave1.

6-4
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)

0024 Slave2 Communication Error Turn the main power OFF and 0
The internal communication error contact TOSOH service engineer.
occurred. There is no response from a
slave2.
0025 Slave1 Trans Buffer Full Turn the main power OFF and 0
The internal communication error contact TOSOH service engineer.
occurred. The sending buffer of slave1
ROM overflowed.

0026 Slave2 Trans Buffer Full Turn the main power OFF and 0
The internal communication error contact TOSOH service engineer.
occurred. The sending buffer of slave2
ROM overflowed.

0027 Power Fan Stop Turn the main power OFF and 0
The fan of a power supply has stopped. contact TOSOH service engineer.

Pump related errors


Error Message (Instrument)
Troubleshooting Level
No. Message (PC)

0200 Pump (Sam) Pressure High Check the tubing of the sample 3
Pressure upper limit error occurred in channel for no clogging.
the sample pump.

0201 Pump (Sam) Pressure Low Check the tubing of the sample 3
Pressure lower limit error occurred in channel for no leakage.
the sample pump.

0202 Pump (Sam) Motor Error Turn the main power OFF and then 3
Sample pump drive error occurred. It ON again.
may be a cam gap. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0203 Pump (Ref) Pressure High Check the tubing of the reference 3
Pressure upper limit error occurred in channel for no clogging.
the reference pump.

0204 Pump (Ref) Pressure Low Check the tubing of the reference 3
Pressure lower limit error occurred in channel for no leakage.
the reference pump.

6-5
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)

0205 Pump (Ref) Motor Error Turn the main power OFF and then 3
Reference pump drive error occurred. It ON again.
may be a cam gap. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0206 Degasser Error Continue pump flow for 10 minutes. 2


Vacuum pressure error occurred. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0207 Purge Syringe Home Error Turn the main power OFF and then 3
Purge syringe drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0208 Drain Valve Position Error Turn the main power OFF and then 3
Drain valve drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0209 Stop Valve Position Error Turn the main power OFF and then 3
Stop valve drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

6-6
6.2 Error Messages

Auto sampler related errors


Error Message (Instrument)
Troubleshooting Level
No. Message (PC)

0300 Injection Valve Position Error Turn the main power OFF and then 3
6way (injection) valve drive error ON again.
occurred. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.
0301 Syringe Valve Position Error Turn the main power OFF and then 3
4way (syringe) valve drive error ON again.
occurred. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0302 Sample Syringe Home Error Turn the main power OFF and then 3
Syringe drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0303 Sample Rack Home Error Turn the main power OFF and then 3
Sample rack drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0304 Sample Arm Home Error Turn the main power OFF and then 3
Sampling arm drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0305 Sample Needle Home Error Turn the main power OFF and then 3
Sampling needle drive error occurred. ON again.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0306 Sample Short( This Cup Skip In Future) Add a sample as required and 0
Sample shortage. execute measurement again.

6-7
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)

0307 Washer Shortage Add the washer to continue 2


Washer shortage error occurred. washing.
Check the air sensor sensitivity with
the solvent to be used.

0309 Sample Rack Eject Time Out This warning is issued if the rack is 2
The sample rack is left out. Please left out for 10 minutes or longer.
insert the rack. Insert the rack.

Oven related errors


Error Message (Instrument)
Troubleshooting Level
No. Message (PC)

0400 Column Change Valve Position Error Turn the main power OFF and then 3
Valve drive error occurred at column ON again.
switching. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0402 Oven (CO) Temp. High Check that the set temperature is 3
Temperature control upper limit error the room temperature +10C or
occurred in the column oven. higher.
Temperature control stopped because Turn the main power OFF and
the temperature exceeded the set contact TOSOH service engineer.
temperature +7C.

0403 Oven (CO) Temp. Low Check that the oven door is closed 3
Temperature control lower limit error securely.
occurred in the column oven. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0404 Oven (CO) Temp. Heat Error This error occurs when temperature 3
Temperature rise error occurred in the has not reach the control range after
column oven. 1 h from control start. Check that the
oven door is closed securely.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

6-8
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)

0405 Oven (CO) Temp. High Limit Turn the main power OFF and 3
The column oven temperature contact TOSOH service engineer.
exceeded 70C and the upper
temperature limit error occurred.

0406 Oven (CO) Gas Leak If there is any leak, wipe off the 3
Gas leak error occurred in the column solvent and keep the door open for
oven. a time to allow ventilation.
If this error occurs without any leak,
adjust the gas sensor.

0407 Oven (CO) Door Open Close the door. 2


The column oven door was opened
during the temperature control. Close
the door.

0408 Oven (CO) Door Open Close the door to start temperature 2
The column oven door is open. Close control.
the door to start temperature control.

0409 Oven (PO) Temp. High Check that the set temperature is 3
Temperature control upper limit error the room temperature +10C or
occurred in the pump oven. higher.
Temperature control stopped because Turn the main power OFF and
the temperature exceeded the set contact TOSOH service engineer.
temperature +7C.
0410 Oven (PO) Temp. Low Check that the oven door is closed 3
Temperature control lower limit error securely.
occurred in the pump oven. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

0411 Oven (PO) Temp. Heat Error This error occurs when temperature 3
Temperature rise error occurred in the has not reach the control range after
pump oven. 1 h from control start. Check that the
oven door is closed securely.
If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.

6-9
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)
0412 Oven (PO) Gas Leak If there is a leak, wipe off the solvent 3
Gas leak error occurred in the pump and keep the door open for a time to
oven. allow ventilation.
If this error occurs when no leak has
occurred, adjust the gas sensor.
0413 Oven (PO) Door Open Close the door. 2
The pump oven door was opened
during the temperature control. Close
the door.

0414 Oven (PO) Door Open Close the door to start temperature 2
The pump oven door is open. Close the control.
door to start temperature control.
0415 Oven (CO) Temp. Sensor Error Contact TOSOH service engineer. 3
Column oven master sensor
disconnection error.
0416 Oven (CO) Temp. Sensor Error Contact TOSOH service engineer. 3
Column oven slave sensor
disconnection error.
0417 Oven (PO) Temp. Sensor Error Contact TOSOH service engineer. 3
Pump oven sensor disconnection error.

Detector (RI) related errors


Error Message (Instrument)
Troubleshooting Level
No. Message (PC)

0500 RI Leak Turn the main power OFF and 3


Liquid leak error occurred in RI contact TOSOH service engineer.
detector.

0501 RI Temp. Error Turn the main power OFF and 3


Temperature control error occurred in contact TOSOH service engineer.
RI detector.

6-10
6.2 Error Messages

Error Message (Instrument)


Troubleshooting Level
No. Message (PC)

0502 RI Over Flow Error Flow solvent untill Over Flow Error is 0
RI Over Flow Error removed.

Detector (UV) related errors


Error Message (Instrument)
Troubleshooting Level
No. Message (PC)
0600 UV Leak Turn the main power OFF and then 3
Liquid leak error occurred in UV ON again.
detector. If the error recurs, turn the main
power OFF and contact TOSOH
service engineer.
0601 UV Lamp Error Turn the main power OFF and 2
UV lamp lighting error occurred. contact TOSOH service engineer.

0603 UV Grating Home Error Turn the main power OFF and 3
Grating drive error occurred in UV contact TOSOH service engineer.
detector.

6-11
6.2 Error Messages

Analysis related errors


Error Message (Instrument)
Troubleshooting Level
No. Message (PC)

0800 Pump Flow Stop Warm up the instrument and 0


The pump is stopped and analysis execute analysis after instrument
cannot be executed. Start the pump start.
flow.
0802 No Sample Rack Insert a sample rack. 1
There is no sample rack inserted.
Please insert a sample rack.

0803 Set Time Error (Acquire > Runtime) Check the setting and ensure 0
The acquisition time cannot be set (acquisition end time - acquisition
beyond the runtime. Please check the start time) < runtime.
parameters.

0804 Empty Cup Exist Extract the sample rack once to 0


The analysis started with a cup of clear the error. Replace the cup.
sample shortage.

0805 Sample Shortage (Cup Skip) Add a sample as required and 0


A cup with sample shortage is skipped. execute measurement again.
0806 No Sample Rack Insert a sample rack and execute 0
Analysis cannot be started because no analysis again.
sample rack is inserted. Insert a
sample rack and execute analysis
again.

6-12
6.3 Before Seeking Repairs

If this instrument does not operate normally, perform the following checks:

Phenomenon Check Action


Connect the power cable if
Is the power cable connected?
The power does not disconnected.

turn ON. Is the main power switch ON Turn the main power switch ON
()? ().

Is the USB cable connected? Connect the USB cable.

The instrument Disconnect and reconnect the


cannot be controlled USB cable.
from the PC. Did you try the system If the instrument is not found,
configuration? turn the power to the instrument
and the PC OFF and then ON to
attempt system configuration.

The pump cannot Is the solvent reaching the Execute purge.


flow. pump? (See 2.7, "Purge Function.")
Is the solvent suction tubing Check that the inlet filter is not
free of excess negative blocked and that the suction
pressure? tubing is not clogged.

Execute purge.
The flow pressure is Is air trapped?
(See 2.7, "Purge Function.")
not stable.
Wash or replace the check
valves. (See 5.1, Washing the
Are the check valves clean?
Check Valves and 5.2,
Replacing the Check Valves.)

6-13
6.3 Before Seeking Repairs

Phenomenon Check Action


Is there any noise source
(generating a line of magnetic
Remove the noise source.
force or high frequency)
nearby?
The detector (RI)
If the solvent was replaced, flow
output contains
Was the solvent replaced? the solvent until the baseline
great noise.
becomes stable.

Does the noise become small


If the noise becomes small,
when the pump flow is
check the pump pulsation.
stopped?

If the drift is periodic, check the


installation environment
Is the drift periodic?
(temperature, voltage
fluctuation, etc.).

If the solvent was replaced, flow


Was the solvent replaced? the solvent until the baseline
becomes stable.
The detector (RI) Is the column oven temperature If not, turn temperature control
output drifts greatly. controlled? ON.
Check the boiling point of the
Is the oven temperature setting solvent and set the oven
appropriate? temperature to the room
temperature +10C or higher.

Does the drift become small If the drift becomes small,


without the column? replace the column.

Is the solvent flowing out from If there is no outflow, check the


the drain tubing? tubing for leakage.
Is the instrument in an overflow Flow the solvent until the
No peak can be state? overflow state is cleared.
identified. If the USB cable or analog Connect the cable if
signal cable disconnected? disconnected.
Is the sample loaded in to the Check that the needle tubing is
sample loop? not damaged or trapping air.

6-14
6.3 Before Seeking Repairs

Phenomenon Check Action


Is there any noise source
(generating a line of magnetic
Remove the noise source.
force or high frequency)
nearby?
If the solvent was replaced, flow
The detector (UV) Was the solvent replaced? the solvent until the baseline
output contains becomes stable.
great noise. Is the lamp energy in the
If the Ref. lamp energy is 10 mV
instrument validation
or less, replace the lamp.
information sufficient?
Does the noise become small
If the noise becomes small,
when the pump flow is
check the pump pulsation.
stopped?
If the drift is periodic, check the
installation environment
Is the drift periodic?
(temperature, voltage
fluctuation, etc.).
The detector (UV) If the solvent was replaced,
output drifts greatly. Was the solvent replaced? supply the solvent until the
baseline becomes stable.

Does the drift become small If the drift becomes small,


without the column? replace the column.

Increase the washing volume.


Was the washing volume
(See 2.13, Controlling the Auto
sufficient?
Sampler.)
Increase the presuction volume.
Is the presuction volume
(See 2.13, Controlling the Auto
The injection sufficient?
Sampler.)
reproducibility is
low. Reduce the syringe speed.
Is the syringe speed too fast? (See 2.13, Controlling the Auto
Sampler.)
Replace the rotor seal if worn.
Is the rotor seal of the 6way or (See 5.6, Replacing the 6way
4way valve worn? Valve Rotor Seal and Stator and

6-15
6.3 Before Seeking Repairs

Phenomenon Check Action


Execute purge.
(See 2.7, "Purge Function.")
Wash or replace the check
Is the pump pulsation great?
valves. (See 5.1, Washing the
Check Valves and 5.2,
Is the elution time Replacing the Check Valves.
reproducibility low? In case of liquid leakage,
Is there any liquid leakage from replace the plunger seal. (See
the washing block of the pump? 5.3, Replacing the Plunger
Seal.)
Is there any liquid leakage from
Check the tubing for leakage.
the channel?
Tighten the leaking component,
Did liquid leakage occur in the
wipe off the solvent, and
oven?
ventilate well.
A pump oven liquid
Is a lot of solvent used around
leakage error Ventilate the laboratory well.
the instrument?
persists.
Is there any liquid leakage from Replace the plunger seal. (See
the washing block behind the 5.3, Replacing the Plunger
pump head? Seal.)
Tighten the leaking component,
Did liquid leakage occur in the
A column oven wipe off the solvent, and
oven?
liquid leakage error ventilate well.
persists. Is there a lot of solvent used
Ventilate the laboratory well.
around the instrument?

6-16

Chapter 7

Installation
7.1 Installation Environment

Install this instrument on a level desk free of harmful gas, dust, or vibration where it is not
exposed to direct sunlight or wind and use it under the following environmental conditions:

Temperature 15 to 35C
Humidity 40 to 80% (No condensation)
Altitude 2,000 m max
Dust General office environment
Power supply AC 100 to 240 V, 50/60 Hz, 500 VA

When moving this instrument, need two or more people and hold the
bottom right and left of the instrument.

7-2
7.2 Installation Place

Do not install the instrument under the following environmental conditions:

Direct sunlight Drastic temperature change

Direct wind Very dusty place

Frequent vibration Unstable place

7-3
7.2 Installation Place

Very humid place Near an open flame

Unventilated and narrow place Power fluctuation

Locations that will be subjected to strong Poorly ventilated place

electromagnetic radiation or high-frequency sound

7-4
7.3 Installation Space

The outside dimensions of this instrument are 680W 580H 500D mm. To place the
accessory solvent tray (width: 240 mm), an installation space of approximately 1,000 650
mm is necessary.
When using the EcoSEC WorkStation PC control program, installation space for a personal
computer (PC) is also necessary.

<Installation space (plane)>

680 mm
240 mm

650 mm

PC
Tray HLC-8320GPC

1,000 mm

Since this instrument has a cooling fan blow port on the back, be
sure to allow for a space of approximately 100 mm behind the
instrument.
This instrument weighs 95 kg. Considering the weight, install the
instrument in a stable place.

7-5
MEMO

7-6

Chapter 8

Connection
8.1 Connecting the Power Cable

Connect the power cable by the following procedure:

1 Check that the main power switch on the right side of this instrument is OFF ().
2 Plug in one end of the power cable to the power inlet on the right side of this
instrument.
3 Plug in the other end of the power cable to a power socket with a ground.

When connecting the power cable, check that the main power switch on
the right side of this instrument is OFF ().

8-2
8.2 Removing the Auto Sampler Fixture

At the shipping of this instrument, the drive section of the auto sampler is secured.
When using this instrument, remove the fixture by the following procedure:

Before removing the fixture, turn the main power OFF and remove the
power cable.

1 Unscrew the two screws at the top of this instrument.


2 Slide the top plate back and pull it up to remove.

3 Unscrew the sample rack securing screw.


4 Unscrew the needle Z-axis securing screw.
Sample rack securing
screw

Needle Z-axis securing


screw

5 Slide the top plate to the side for attachment.


6 Attach the two screws to the top of the instrument.

8-3
8.3 Connecting a PC

When using the PC control program EcoSEC WorkStation to control this instrument and to
acquire data, connect a PC to the PC terminal on the right side of this instrument with a USB
cable.
Before connecting, add ferrite cores to both side of the USB cable.
With the PC connected, turn ON the main power to this instrument in order to activate the
acquisition control application and to find the instrument. For details, refer to the operators
manual of the EcoSEC WorkStation.

ferrite core for USB


(parts No.022064)

Add ferrite cores to both side of USB cable.


(Turn USB cable two times)

Right side

8-4
8.4 Tubing

Tubing types

The tubing described below protrudes from the left side of this instrument:

Solvent suction tubing (SOLVENT)


This tubing is used to load a solvent from a solvent bottle into the pump unit.
Pass the tubing through the solvent bottle cap and put it into the solvent
bottle.

Washer suction tubing (WASH)


This tubing is used to load a solvent from a solvent bottle into the auto
sampler.
Pass the tubing through the solvent bottle cap and put it into the solvent
bottle.

Drain tubing (DRAIN)


This tubing is used to drain waste liquid from the detector (RI) and a solvent
when the drain valve is opened.
Put the tubing into a waste container.

Wash drain tubing (AS-DRAIN)


This tubing is used to drain solvent used for washing the auto sampler.
Put the tubing into a waste container.

8-5
8.4 Tubing

Waste container installation

If the drain tubing, or the wash drain tubing of the auto sampler, or the waste container
is positioned or installed at an elevated position relative to the instrument, liquid
leakage may occur in the instrument.

Install the waste container lower than the tubing outlet of this instrument.
Ensure that the drain tubing remains lower than the tubing outlet.

<Positions of drain tubing and waste container>

8-6
8.4 Tubing

Solvent bottle cap attachment

The solvent bottle cap is connected by the two methods explained below. Select the
connection that is suitable for use.
A. Ordinary connection
B. Connection to use a salt-containing solvent or a buffer solution

A. Ordinary connection
1 Attach fittings and adapters to the wash suction tubing (WASH) and solvent suction
tubing (SOLVENT) and connect them through the inner cap. Adjust the tubing so
that it protrudes approximately 30 cm beyond the inner cap and fasten the fittings to
secure the tubing. Pass the wash suction tubing (WASH) through the
small-diameter port and pass the solvent suction tubing (SOLVENT) through the
large-diameter port.
2 Attach the suction filter to the end of the solvent suction tubing (SOLVENT) having
an outer diameter of 1/8.
3 Pass the PTFE tubing of the prevention kit of moisture adsorption through the cap
hole and connect it to the large-diameter port.
4 Attach the solvent bottle end plug to the small-diameter port.

Wash suction
Solvent bottle end plug
O.D. 1/16" Cap tubing (WASH)

Solvent suction
tubing (SOLVENT)

O.D. 1/8" Inner cap


Suction filter
Prevention kit of
moisture ad.

8-7
8.4 Tubing

B. Connection to use a salt-containing solvent or a buffer solution


1 Insert the wash suction tubing (WASH) into the wash bottle, but not through the
inner cap.
2 Attach the solvent bottle end plug to the small-diameter port of the inner cap.

To wash bottle Wash suction


tubing (WASH)

Solvent bottle end plug

Inner cap

HLC-8320GPC
WASH
SOLVENT

Solvent bottle (gallon bottle)


Wash bottle

When using a salt-containing solvent or a buffer solution, use deionized water as


an aqueous wash or an organic solvent as an organic wash.

8-8
8.4 Tubing

Column connection

1 Connect the S.COL tubing from Port 3 of the 6way valve to the inlet of the analytical
column. Connect the outlet of the analytical column to the RI.S tubing.
2 Connect the R.COL tubing of the pump unit to the inlet of the reference column.
Connect the outlet of the reference column to the RI.R tubing.

Sample column IN tubing Reference column IN tubing

R.COL
S.COL

Detector (RI) sample IN tubing Detector (RI) reference IN tubing


RI.R
RI.S

8-9
8.4 Tubing

Each column has a tag indicating the grade and the flow direction. When
connecting a column, check the flow direction.
When connecting more than one column, arrange them as shown below.
If the tubing is too short, extend the inlet tubing (valve to column tubing). If the
tubing is connected by a joint such as a union, the performance may
deteriorate. It is recommended that new tubing be created.

Flow direction

Valve

Valve
Column tag

RI.S RI.S

Even number Odd number

8-10
8.4 Tubing

Tubing is connected to a column by using a male nut and a ferrule.


The ferrule securing position (h in the figure below) depends on the
column grade. Dimension h is 4 mm for the H, HXL, and HHR Series
of TOSOH and 2 mm for the Super H, AW, and HZ Series. Dimension
h may also be different for columns of other manufacturers.
Determine the ferrule and male nut securing position according to the
column to use.
When changing the column grade or manufacturer, it is necessary to
create new column IN/OUT tubing. If inappropriate tubing is used,
the dead volume may increase, the column performance may
deteriorate, or the column may be damaged.

H/HXL/HHR Series
h = 4 mm

Swage lock type

Super H/AW/HZ Series h = 2 mm

Screw type

When using TSKgel SuperAW5000, SuperAW6000, or SuperAWM-H,


handle with great care.
When attaching one of the above columns to the instrument,
connect the column outlet to the detector after flowying the liquid of
double the column volume.
If a column is left attached to the instrument for one week or longer,
connect the column outlet to the detector flowying liquid of double the
column volume.
For solvent replacement, disconnect the detector from the column
outlet and flow liquid of four times the column volume. Then connect
the detector.

8-11
8.5 Attaching Washing Tubing to the Rear of the Pump

If the solvent contains salt, the salt may precipitate from the plunger seal of the pump unit
and reduce the life of the plunger seal. To prevent this problem, fill the diaphragm section
with deionized water for periodic washing.

[Necessary items]
Deionized water Approximately 200 mL
Silicon tubing 422 m (Part No. 008851) 1
Disposable syringe 20 mL (Part No. 008571) 1

[Tubing attachment procedure]


1 Remove the rubber stopper on the left side of the instrument.
2 Open the pump oven door and remove the rubber stopper from the left side.
3 Cut the silicon tubing into three pieces and connect them to the washing ports of the
pump as shown below.
4 Insert one end of the silicon tubing into the bottle containing deionized water and
attach a syringe to the other side.
5 Inject deionized water from the syringe.
6 Cut out the rubber stoppers with scissors and attach them to inside and left side of
the oven

For analysis, fill the silicon tubing with deionized water.


After analysis, inject deionized water from the syringe and wash the inside of
the pump unit.

8-12
8.6 Installing the Cases

Install the accessory solvent tray on the left side of the instrument to hold the solvent bottle
and waste container.

The ovens of this instrument have gas sensors. If liquid leakage occurs in an oven, the
temperature control and the flow stop. Since the instrument is designed to drain leaking fluid
from the bottom, install the accessory instrument tray at the bottom of the instrument.

Solvent tray
Instrument tray
Insert from the front of the
instrument until it hits the stopper.

The pump oven and the column oven have drain ports to deal with liquid leakage
if any.
The auto sampler and the degas/suction unit are designed to drain leaking liquid
from the bottom if it should leak.

8-13
8.7 Connecting the I/O Terminals

This instrument has I/O terminals and a communication port on the right side. When using
external instrument (integrator or recorder), connect it to the I/O terminals.
The EcoSEC WorkStation can be used only by USB cable connection.

1 Remove the two screws from the terminal window on the right side of the
instrument, place the cover as shown below, and secure it with a screw.

2 Connect the necessary cables to the accessory analog terminal block.


3 Add ferrite core to the instrument side.
4 Insert the analog terminal block into the connector.

ferrite core
(parts No.022001)

Add ferrite core to instrument side of Signal cable.


(Turn Signal cable two times)

Right side

8-14
8.7 Connecting the I/O Terminals

RI terminal
This terminal outputs a 25610-6 or 6410-6 RIU/1V signal from the detector (RI). By
connecting the input terminal of external instrument (integrator or recorder) here
through an analog signal cable (Part No. 0017546), data can be processed.

UV terminal
This terminal outputs a 0.5, 1.0, 2.0, or 4.0 ABU/1V signal from the detector (UV). By
connecting the input terminal of external instrument (integrator or recorder) here
through an analog signal cable (Part No. 0017546), an output signal from the detector
(UV) can be recorded.
This is valid only when the optional UV-8320 is equipped.

INJ terminal
This terminal outputs a relay contact signal at sample injection by the auto sampler. By
connecting the start signal terminal of an integrator or other external instrument here,
the relay contact signal can be used as a start signal for the instrument.

ERROR terminal
By connecting the contact output terminal of external instrument here, error processing
of this instrument can be executed at signal input. See P6-4 Error No.0022

Connecting an analog signal cable


While pressing the section shown below with the accessory cable insertion tool,
insert the analog signal cable.

Cable insertion
tool

8-15
MEMO

8-16

Chapter 9

Specifications
9.1 Specifications

Degasser system

Degasser system : Vacuum degassing


Volume : 20 mL 2 series for solvent
10 mL for wash
Pressure resistance : 196 kPa
Tubing resistance : 1.96 kPa for solvent (H2O flow at 2 mL/min)
3.92 kPa for washer (H2O flow at 10 mL/min)
Vacuum pressure : 16 kPa (normal)
20 kPa (low)

Pump oven

Temperature control method : Hot-air circulation under PID control


Temperature control range : Room temperature +10 to 50C (1C steps)
Temperature setting accuracy : 0.5C
Temperature control precision : 0.1C
Heater : DC24 V, 60 W
Safety system : Temperature sensor for monitoring the oven
temperature and stopping temperature control
upon detection of an abnormality.
Gas sensor for stopping temperature control.
Thermal fuse (70C) for shutting down the
temperature control circuit.
Door open/close monitor for stopping
temperature control when the door is opened.
Liquid drain in case of liquid leakage.

9-2
9.1 Specifications

Pump Unit

Flow mode : Parallel flow (Quick return)


Flow rate setting range : 10 to 2000 L/min (1 L steps)
(Sample flow rate only. The reference flow rate is
set in terms of the ratio [1, 1/2, 1/3, or 1/4] with the
sample flow rate.)
Flow rate accuracy : Within 2 % or 5 L whichever greater
(H2O, pressure: 1 MPa or more, 1,200 L/min or
less)
Flow rate precision : Within 0.2 % or 1 L whichever greater
(H2O, pressure: 1 MPa or more, 1,200 L/min or
less)
Pressure setting range : 0 to 25 MPa (0.1 MPa steps)
Plunger diameter : 2 mm
Plunger volume : 7.5 L/stroke
Accumulator volume : 3 mL
Safety system : Flow stop above the upper-limit pressure
Flow stop below the lower-limit pressure
Plunger drive count monitoring
Case for liquid leakage

Auto sampler

Measuring system : Syringe measurement


Standard loop : 100 L
Sample injection volume : 1 to 1,500 L (1 L steps)
(Replace the loop for injection of 100 L or more.)
Reproducibility : Within CV0.5 % (at injection of 10 L or more)
# of Samples : 100
Safety system : Bubble detection in the wash and sample solution.
Needle movement only when the sample rack is
Attached.
6way valve drive count monitoring.
4way valve drive count monitoring.

9-3
9.1 Specifications

Column oven

Temperature control method : Hot-air circulation (double structure) under PID


control (cascade control)
Temperature control range : Room temperature +10 to 60C (1C steps)
Temperature setting accuracy : 0.5C (in the internal box)
Temperature control precision : 0.02C (in the internal box)
Maximum number of columns
accommodated : 7.8 mm 30 cm column 8 (TOSOHs product)
Heater : DC24 V, 100 W
Safety system : Temperature sensor for monitoring the oven
temperature and stopping temperature control upon
the detection of an abnormality.
Gas sensor for stopping temperature control.
Thermal fuse (70C) for shutting down the
temperature control circuit.
Door open/close monitor for stopping temperature
control when the door is opened.
Liquid drain for liquid leakage.

Detector (RI)

System : Bryce-type double path or double flow


Light source : Tungsten lamp
Refractive index range : 1.00 to 1.80
Range (FS) : 64,25610-6RIU/1 V
Response : 0.5, 1.0, 3.0 s
Flow cell : Made of quartz glass (volume: 2.5 L, withstand
pressure: 0.5 MPa)
Dynamic range : 510-4RIU
Noise : 210-9RIU (THF sealed in, Response: 3.0 s)
Drift : 110-7RIU/h (THF, flow at 1.0 mL/min)
Temperature control : OFF, 35, 40, 45C
Safety system : Liquid leakage sensor.
Circuit shutdown by thermal fuse(70C).

9-4
9.1 Specifications

Optional valve

Column switching valve : Electric 2-series 4-way switching

Optional detector (UV)

System : Dual beam, single flow cell


Light source : Deuterium lamp
Wavelength range : 195 to 350 nm
Wavelength accuracy : 2 nm
Bandwidth : 8 nm
Range (FS) : 0.5, 1, 2, 4 ABU/1 V
Response : 0.5, 1.0, 3.0 s
Flow cell : Volume 2 L
Withstand pressure 3 MPa
Drift : 310-4ABU/h (254 nm, air in cell, response: 1.0s)
Noise : 2.510-5ABU (254 nm, air in cell, response: 1.0s)
Safety system : Liquid leakage sensor.
Lighting time monitoring.
Liquid leakage case.
Outside dimensions : 160(W)143(H)390(D) mm (excluding projections)
Weight : 7 kg

9-5
9.1 Specifications

I/O terminals

PC communication : USB
RI signal : Analog output (-1 to 1 V)
UV signal : Analog output (-1 to 1 V)
Injection signal output : Contact output
Error signal input : Contact or TTL-level input

Fluid path materials

Stainless steel 316, PTFE, PEEK, zirconia, silica glass, PFA, and carbon-contained
PTFE, Vespel*
*When a column switching valve (option) is used.

Installation environment

Temperature : 15 to 35C
Humidity : 40 to 80% (No condensation)
Altitude : 2,000 m max
Dust : General office environment

Power supply ratings

Voltage : AC 100 to 240 V


Frequency : 50/60 Hz
Power consumption : 500 VA

9-6
9.1 Specifications

Dimensions and weight

Outside dimensions : 680(W)550(H)500(D) mm (excluding projections)


Weight : 95 kg

I/O signal standard

TTL-level or contact input

tc VH

VL

VH : 2.0 V min
VL : 0.8 V max
tc : 100 ms min

Relay contact output

tc High

Low

NORMAL OPEN
Allowable current :1A
tc : 1.0 to 1.2 s

9-7
MEMO

9-8

Chapter 10

About Options
10.1 UV Absorbance Detector (UV-8320)

In addition to the built-in differential refractometer (RI), a UV absorbance detector (UV-


8320) can be installed in the HLC-8320GPC.

Tubing

Connect the IN tubing (UV.IN) of the UV-8320 to the sample column outlet and the
OUT tubing (UV.OUT) of the UV-8320 to the detector (RI) sample IN tubing (RI.S).

UV.OUT

RI.R

UV.IN Internal-type union RI.S Internal-type union

The detector connection order is columnUV-8320detector (RI).


Since the detector (RI) cell cannot withstand great pressure, the
connection order of columndetector (RI)UV-8320 will damage the
detector (RI) cell.

10-2
10.1 UV Absorbance Detector (UV-8320)

Control

The UV-8320 is controlled from HLC-8320GPC.


The screens described in this section are displayed only when the UV-8320 is
equipped.

Executing auto balance

Press BALANC to move the detector output signal to the set balance value. Auto
balance is executed simultaneously on the RI detector.

Changing settings
Change the settings of the UV-8320 as explained below.
First, display UV detector parameter screen 1 by the following procedure:

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press and ENT to display UV detector parameter screen 1.

[UV detector parameter screen 1]


UV: 0.000 Wave.:254
Range :2( 1.0) Pola.: 1(+)
Balance : 0 Resp.: 1 (0.5)
(Page)<Lamp> (Unit)(Back)

UV Displays the UV detector output value or lamp status.


OFF : Lamp OFF
HEAT : Lamp heating (display output after several seconds)
Output : Output value display when the lamp lights ON.
The display range is from 1,000 to +1,000 [mV].
Range Set a range of analog output from the UV terminal on the right side of
this instrument and digital output by USB communication. Enter 4 (0.5
ABU), 3 (1 ABU), 2 (2 ABU), or 1 (4 ABU) and press ENT . The output
value is in the selected range/1 V.
ENT
Balance Setting value at auto balance. Enter the numeric value and press .
The setting range is from 1,000 to +1,000 [mV].

10-3
10.1 UV Absorbance Detector (UV-8320)

WAVE Set the wavelength, enter the wavelength by the numeric keys and
press ENT . The input range is from 195 to 350 [nm].
Pola. Set the polarity of UV detector output, change the polarity to output a
negative peak to the positive side. Enter 0 (-) or 1 (+) and press ENT .
Resp. Set the time constant of UV detector output, enter 1 (0.5 s), 2 (1.0 s), or
3 (3.0 s) and press ENT .
<Lamp> Turns the lamp on or off

10-4
10.1 UV Absorbance Detector (UV-8320)

Performance check

Drift check
[Conditions]
Solvent :THF
Wavelength :254 nm
Range : 1 ABU/FS
Response : 1.0 s
Control temperature : 40C
Polarity :+
Data acquisition time : 0-120 min
Sampling interval : 1,000 ms

[Procedure]
1 Turn on the power of the HLC-8320GPC, start temperature control, and flow
THF by the sample pump at a flow rate of 0.35 mL/min.
2 Under the above conditions, record the detector (UV) baseline for two hours.
3 Measure the one-hour baseline fluctuation from one hour after power-on and
check that the drift is within 5104 ABU/h (within 0.5 mV).

60min

10-5
10.1 UV Absorbance Detector (UV-8320)

Noise check
[Conditions]
Range : 1 ABU/FS
Response : 1.0 s
Control temperature : 40C
Polarity :+
Data acquisition time : 0-5 min
Sampling interval : 100 ms

[Procedure]
1 After checking the drift, stop flow.
2 After the baseline becomes stable, record the detector (UV) baseline for five
minutes under the above conditions.
3 Divide the baseline into 30-second segments. Measure the noise width in
each segment and obtain the average value of the 10 segments.
4 Check that the average noise width is within 510-5 ABU (within 0.05 mV).

10

Y
R=1

X1 X2 X3 X4 X5 X6 X7 X8 X9 X10

Y2 Y6 Y7 Y8
Y3 Y5 Y9 Y10
Y1
Y4

5 min

10-6
10.1 UV Absorbance Detector (UV-8320)

Sensitivity check
[Conditions]
Solvent : Deionized water
Sample :0.05% p-toluenesulfonic acid sodium/water
Injection volume : 500 L
Flow rate : 0.5 mL/min (both sample and reference)
Wavelength : 262 nm
Range : 1ABU/FS
Response : 0.5 s
Polarity :+
Control temperature : 40C
Column : None
Data acquisition time : 0-3 min
Sampling interval : 100 ms
Data analysis condition : Column test

[Procedure]
1 Replace the sample loop of the auto sampler with the 500 L sample loop.
(See 5.8, Replacing the Sample Loop.)
2 Replace the solvent with deionized water and wait until the baseline becomes
stable.
3 Under the above conditions, inject the sample into the cell and record the
output signal.
4 In the peak editor for the EcoSEC WorkStation data analysis, set the baseline
as shown below and obtain the peak height (X).

Check that the top becomes flat.

Output
Peak height (X)

Edit the baseline flat.

10-7
10.1 Ultraviolet Absorbance Detector (UV-8320)

5 Check that the difference between the peak height (X) and the theoretical
output conversion value (Y) = 332 mV is 5 %.

XY
100 < 5
Y

Be sure to check that the peak is flat at the top. The cell must be saturated
with a sample for an accurate sensitivity check.
If the tubing volume between the sample loop and the cell is greater than
the initial volume because an optional column switching valve is used, the
cell may not be saturated with a sample. In this case, remove the valve
tubing and check again.
If the EcoSEC WorkStation is not used, connect an external instrument
through the UV terminal and check that the output peak height satisfies
the above standard.

10-8
10.1 Ultraviolet Absorbance Detector (UV-8320)

Cell washing

[Necessary items]
Finger tight fitting (Part No. :016566) 2
Internal-type union (Part No. :007337) 2
Capillary 1
Waste container 1
When aqueous liquid, saline solution,
or buffer solution is used: Deionized water Appropriate amount
When organic solvent is used: Ethanol or isopropanol Appropriate amount

[Procedure]
1 Stop flow.
2 Remove the column (if attached).
3 Connect a capillary to the sample column IN tubing (S.COL) and the detector
(UV) sample IN tubing (UV.IN).
4 Supply the washing liquid from the solvent suction tubing (SOLVENT) at a
flow rate of 1 mL/min for 10 minutes or longer.
5 Replace the washing liquid in the system with an used solvent and flow for 10
minutes or longer.

Flow the washing liquid to the sample pump only.


For solvent replacement in the system, check the solvent miscibility in
advance.

10-9
10.2 External Detector

When using a detector other than the UV-8320 as an external detector or when using
a fraction collector, contact TOSOH service engineer.

The recommended installation location is to the right side of the HLC-8320GPC.


Connect the IN/OUT tubing through the hole on the right side of the instrument.

When attaching an external detector, note the attachment order. Since


the detector (RI) can only withstand pressures of up to 0.5 MPa,
connect the detector such that it will not be pressurized.

10-10
10.3 Column Switching Valve

The HLC-8320GPC allows a column-switching valve (Part No. :021793) to be equipped in


the column oven. For equipment, contact TOSOH service engineer.

The column switching valve is a 2-series 4-way valve.


When this valve is equipped, a column can be selected from two series according to the
purpose. At the position of COL.1, Analytical column 1 is for sample and Analytical column
2 is for reference. At the position of COL.2, Analytical column 2 is for sample and
Analytical column 1 is for reference.

<Flow channel>
Auto sampler
injection valve

5
6
1

4
2 Column switching
3
valve
3 2
1
Analytical column 1 4 Analytical column 2
8
5
6 7

When using a column of a different size, note the flow rate at valve switching.
Since a different flow rate can be set for each column switching valve
position, set the flow rate for Analytical column 2 according to the column.
(See 2.11, Controlling the Pump Unit.)

10-11
10.3 Column Switching Valve

Connect the column switching valve by referring to the following diagram:

<Example of tubing>

COL1 COL2

Even number : 250 mm Even number : 350 mm


Odd number : 600 mm Odd number : 600 mm

250 mm 350 mm

INJ RI.S
135 mm 600 mm

450 mm 600 mm
REF RI.R

10-12
10.3 Column Switching Valve

Valve position switching

Change the column switching valve position as explained below.


First, display the column switching valve screen by the following procedure.
The screens described in this section are displayed only when a column switching
valve is equipped.

1 Press (Param.) on Monitor screen 1 to display the unit selection screen.


2 Press
and ENT
to display the column switching valve screen.

[Column switching valve screen]


Column Change
Column:1

<Change> (Unit) (Back)

Column Indicates the current column switching valve position by 1 (Column1) or


2 (Column2).
<Change> Change the column switching valve position.

During flow, the column switching valve position cannot be changed.

When a column switching valve is equipped so as to use a column of a


different size, switching the value without changing the flow rate may
damage the column. Set a flow rate that is appropriate for the column
size in advance.

10-13
MEMO

10-14

Chapter 11

Parts List
11.1 Accessories

If the accessories are purchased as maintenance parts, their quantities may be different.

Part No. Name and Standard Shape and Specifications Quantity


Operator's manual 1

Inspection certificate 1

Warranty card 1

Power cable 1

Wrench 8 mm 10 mm 1

Wrench 12 mm 14 mm 1

Wrench 1/4 5/16 1

Wrench 14 mm 17 mm 1

11-2
11.1 Accessories

Part No. Name and Standard Shape and Specifications Quantity


Hex wrench 3 mm 1

Hex wrench 4 mm 1

Screw driver(+) 100 mm 1

0008290 File (double edge) 1

0018524 Plunger seal replacement tool 1 set


0018525

0006160 Nut, 1/16 4

11-3
11.1 Accessories

Part No. Name and Standard Shape and Specifications Quantity


016180 Ferrule, 1/16 4

016566 Finger-tight fitting 2


1/16 PEEK

006574 Inlet filter 5 m 1 set

022002 Solvent cap assembly 1 set

018118 Prevention kit of moisture ad. 1 set

005464 Sample loop 1 set


500 L

008851 Silicon tube 1


4 mm2 mm2 m

016618 Sample cup assembly 5


(transparence, 2-SV, 2 mL)
(Cap+aluminum sheet+packing
+ cup)

11-4
11.1 Accessories

Part No. Name and Standard Shape and Specifications Quantity


022014 Solvent tray 1

022013 Instrument tray 1

022003 Analog terminal 1

022004 Cable insertion tool 2

022015 Sample rack 1

022001 Ferrite core 1

022064 Ferrite core for USB 2

11-5
11.2 Consumables

Part No. Name and Standard Shape and Specifications Quantity


019190 Plunger seal (GFP) 1

018517 Plunger seal (PE) 1

019762 Plunger(zirconia) 1

022012 Check valve assembly (outlet) 1

022011 Check valve assembly (inlet) 1

019056 PTFE Diaphragm(plunger) 2

017714 Inline filter 10 m 1

021220 Syringe 2,500 L O-ring seal 1

*For replacement, contact TOSOH


service engineer.

11-6
11.2 Consumables

Part No. Name and Standard Shape and Specifications Quantity


016414 Rotor seal (4way) 1
PEEK

016415 Rotor seal (6way) 1


PEEK

016450 4way valve stator 1

016451 6way valve stator 1

022016 Drain block seal 1

*For replacement, contact TOSOH


service engineer.

013718 Sample cup aluminum sheet 100


(For sample cup 016315,
016314, and 016317)

013717 Sample cup packing 100


(For sample cup 016315,
016314, and 016317)

11-7
11.2 Consumables

Part No. Name and Standard Shape and Specifications Quantity


016315 Sample cup 1,000
(transparence, 2-SV, 2 mL)

016618 Sample cup assembly 500


(transparence, 2-SV, 2 mL)
(Cap+aluminum sheet+packing
+ cup)

016314 Sample cup (brown, 2-SV,CA, 1,000


2 mL)

016317 Sample cup 1,000


(taper, 1.1-STVG, 1.1 mL)

016316 Sample cup 1,000


(polyethylene, 0.65 mL)

016330 Cap 1,000


8-SCJ

11-8
11.2 Consumables

Part No. Name and Standard Shape and Specifications Quantity


022006 Sample cup for septum 1,000
2 mL

022007 Cap for septum 1,000

022009 Seal for septum 1,000

022008 Sample cup assembly for septum 500


2 mL
(Cap + packing + cup)

018445 Deuterium Lamp 1

* This is valid only when UV


detector (option) is equipped.

11-9
11.3 Options

Part No. Name and Standard Shape and Specifications Quantity


022000 EcoSEC WorkStation 1 set

021227 USB cable (3 m) 1

021792 UV-8320 1 set

*For equipment, contact TOSOH


service engineer.

021793 Column switching valve unit 1 set

*For equipment, contact TOSOH


service engineer.

007035 Sample loop 1 set


1,500 L

005672 Sample loop 1 set


1,000 L

005679 Sample loop 1 set


100 L

11-10
11.3 Options

Part No. Name and Standard Shape and Specifications Quantity


005462 Sample loop 1 set
50 L

022010 Low dead volume tubing assembly 1 set

017546 Analog signal cable (2 m) 1

022017 Solvent cap assembly for 1 L 1 set

019615 Ground kit (A) 1 set

019616 Ground kit (B) 1 set

005319 Accumulator 1 set

11-11
11.3 Options

Part No. Name and Standard Shape and Specifications Quantity


008571 Disposable syringe 20 mL 1

017545 Micro cell for UV 1

017556 Cell sheet 5

014243 Cell lens for UV 2

017558 Cell lens cover for UV 2

006814 Column end plug 10

Stainless steel tubing


Part No. Name Standard Quantity
006167 Stainless steel tubing 1/160.1 mm2 m 1

006168 Stainless steel tubing 1/160.2 mm2 m 1

006630 Stainless steel tubing 1/160.25 mm2 m 1

006039 Stainless steel tubing 1/160.4 mm2 m 1

006169 Stainless steel tubing 1/160.6 mm2 m 1

006170 Stainless steel tubing 1/160.8 mm2 m 1

006171 Stainless steel tubing 1/16.0 mm2 m 1

11-12
11.3 Options

PTFE tubing
Part No. Name Standard Quantity
006587 PTFE tubing 2.0 mm.0 mm2 m 1

006448 PTFE tubing 3.0 mm2.0 mm2 m 1

Special tube
Part No. Name Standard Quantity
016481 Silicon tubing 2.5 mm1.5 mm2 m 1

Parts for stainless steel tubing


Part No. Name and Standard Shape and Specifications Quantity
006160 Nut 1/16 5

Material: SUS316
008299 Long nut 1/16 5

Material: SUS316
016180 Ferrule 1/16 10

Material: SUS316
006163 Internal-type union 1/16, 0.35 5

Material: SUS316

11-13
11.3 Options

Part No. Name and Standard Shape and Specifications Quantity


007337 Internal-type union 1/16, 1 5

Material: SUS316
022005 Internal-type union 1/16, 1 5
short

Material: SUS316
007539 T-joint 1/16, 0.4 1

Material: SUS316
007055 T-joint 1/16, 1 1

Material: SUS316
008878 Male nut 1/8 5

Material: SUS316
006176 Ferrule 1/8 10

Material: SUS316

11-14
11.3 Options

Parts for stainless steel tubing and PTFE tubing


Part No. Name and Standard Shape and Specifications Quantity
007540 S-T union 0.35 1

Material: SUS316
013656 S-T union 1 mm 1

Material: SUS316

Parts for PTFE tubing


Part No. Name and Standard Shape and Specifications Quantity
006811 Flanged fitting 10
2.0 mm 1/4-28UNF screw

Material: PCTFE (with ring)


006812 Flanged fitting 10
3.0 mm 1/4-28UNF screw

Material: PCTFE (with ring)


006815 Coupling 10
1/4-28UNF screw

Material: PCTFE
008278 T-joint 1
1/4-28UNF screw

Material: PCTFE
013652 T-joint, stainless steel 1 set
1/4-28UNFscrew

Material: SUS316

11-15
MEMO

11-16

Chapter 12

Theory
12.1 Instrument Configuration

General flow diagram

The general flow diagram of this instrument is shown below. The flow channel is of the
reference flow type using two pumps. To prevent performance deterioration when a
semi-micro column such as Tosohs Super H type, this instrument is designed to
minimize the dead volume between injection valve, column, and detector.

Stop valve Drain valve


Purge pump
Auto sampler Column oven

Drain block

Prevention kit of Degasser


system
moisture ad.

Pump oven

Pump unit Detector (UV) Detector (RI)

12-2
12.2 Pump Unit

This pump unit is the reference flow type using two pumps as below.

<Pump unit diagram>


Auto sampler wash

Drain
(To drain block)
Drain valve

Stop valve
Vacuum Inline filter Inline filter
chamber (sample) (reference)

Vacuum Vacuum Pressure gauge Pressure gauge


Solvent bottle end (sample) (reference)
chamber chamber
plug

Prevention kit of Pressure sensor Accumulator Accumulator


moisture ad. (sample) (reference)

Solenoid
valve NC
Vacuum pump Purge pump
COM Pump Pump
NO (sample) (reference)
Inlet coil

12-3
12.3 Auto Sampler

The sampler of this instrument employs a method whereby the sample is loaded to the
sample loop connected to the injection valve, and the valve is switched to inject the
sample into the column.

<Injection operation>
With the needle connected to the syringe, wash solvent loaded to the syringe is
discharged from the needle that has moved to the washing port. (washing)
In order to prevent the sample from mixing with the wash solvent while it is being
loaded to the syringe, a volume of air equivalent to the air volume is loaded from
the end of the needle.
The needle drops into the specified sample cup, the sample is loaded to the
syringe, and the tube between the needle and the injection valve is filled with
sample.
The injection valve is switched, causing the needle, sample loop, and syringe to be
connected together, and the set injection volume of the sample is loaded to the
sample loop. (LOAD)
When the injection valve switches, the sample inside the sample loop is pushed
out by the solvent from the pump, and injected into the column. (INJECTION)

Sample loop

4way valve
Needle
Washing port

Injection valve

Pump Column
Syringe

Wash solvent

The sample loading volume is the sum of the injection volume and the presuction
volume.

12-4
12.4 Detector (RI)

The Bryce-type differential refractometer (RI) uses the phenomenon whereby a ray passing
through two media of different refractive indexes is deflected at their border.
A ray passing through the two cells containing sample and the reference filled with solvent
is deflected at the cell border because of a difference in the refractive indexes of the
solvents. The ray deflection is detected by the light-receiving element as a change
(displacement ) of ray position. Since the displacement is proportional to the difference
in refractive index between the two solvents, the differential refractive index can be
obtained by measuring the displacement .

Reference cell

Displacementment

Ray

Light receiving
element

Sample cell

12-5
12.4 Detector (RI)

A ray emitted from the tungsten lamp passes through the slit and the lens and enters the
cell. The ray deflected in the cell is reflected in the mirror and then enters the cell again.
After passing through the cell, the ray passes through the lens and the null glass and forms
a slit-shaped image on the light-receiving element. The light-receiving element consists of
two light receivers and the light-receiving quantity of the light receivers varies with changes
of the image position caused by ray deflection. A differential refractive index can be
obtained from the difference in output between the light receivers.

Tungsten lamp
Slit
Mirror
Lens

Ray
Cell
Light receiving element

Light receivers

12-6
12.5 Detector (UV)

The detector (UV) measures the absorbency of a substance.


The Monk Gilson spectroscope divides the light from the light source (deuterium lamp)
according to wavelengths.
Light of a set wavelength the passes through the flow cell.
The flow cell has two light pass holes. The hole at the center is intended for solvent and
sample flow (sample side) and the off-center hole is for the reference light equivalent of the
incident light to flow through (reference side).
The light passing through the flow cell enters the photodiode, where the light is converted
from optical energy into electric energy for handling as an electric signal. Absorbency A is
the result of log conversion from the reciprocal of permeability T. If the sample output is
Vsam and the reference output is Vref, absorbency A can be expressed as follows:

1 Vsam
A = log (T = )
T Vref

Sample photodiode
Reference photodiode

Sample pass hole

Reference pass hole

Divided light

12-7
MEMO

12-8

Chapter 13

References
13.1 Solvent Miscibility

Before solvent replacement, check the miscibility of both solvents using the table below.
When replacing the solvent with a non-miscible solvent, substitute the solvent with a
solvent that is miscible with both solvents.

NAME
ACETIC ACID
ACETONE Not miscible
ACETONITRILE
BENZENE
Miscible
BUTYL ALCOHOL
CARBON TETRACHLORIDE
CHLOROFORM
CYCLOHEXANE
CYCLOPENTANE
DICHLOROETHANE
DICHLOROMETHANE
DIMETHYLFORMAMIDE
DIMETHYL SULFOXIDE
DIOXANE
ETHYL ACETATE
ETHYL ALCOHOL
DI-ETHYLETHER
HEPTANE
HEXANE
METHYL ALCOHOL
METHYLETHYL KETONE
1-OCTANE
PENTANE
1-PROPYL ALCOHOL
DI-PROPYLETHER
TETRACHRLOROETHANE
TETRAHYDOROFURANE
TOLUENE
TRICHLORORETHANE
WATER
XYLENE
CARBON TETRACHLORIDE

TETRACHRLOROETHANE
TETRAHYDOROFURANE
METHYLETHYL KETONE
DIMETHYLFORMAMIDE
DIMETHYL SULFOXIDE

TRICHLORORETHANE
1-PROPYL ALCOHOL
DICHLOROMETHANE
DICHLOROETHANE

METHYL ALCOHOL

DI-PROPYLETHER
BUTYL ALCOHOL

ETHYL ALCOHOL
ETHYL ACETATE
CYCLOPENTANE

DI-ETHYLETHER
CYCLOHEXANE
ACETONITRILE

CHLOROFORM
ACETIC ACID

1-OCTANE
ACETONE

HEPTANE

PENTANE

TOLUENE
BENZENE

DIOXANE

HEXANE

XYLENE
WATER

13-2
13.2 Solvent Characteristics

GPC uses some solvents that are harmful to the human body and the environment. This
section introduces some general solvent characteristics. The values may vary with the
measurement conditions.
For details, refer to the MSDS created by the solvent manufacturer.

Solvent Tetrahydrofuran
Mol. formula C4H8O Refractive index 1.4050 (20C)
Mol. mass 72.1 Fusion point -108.5C
Structural formula Boiling point 65C
Specific gravity 0.8892 (20C)
Flash point -14C
Ignition point 321C
Explosion limit 2.0 to 11.8 vol%
CAS No. 109-99-9

Solvent Chloroform
Mol. formula CHCl3 Refractive index 1.4467 (20C)
Mol. mass 119.38 Fusion point -64C
Structural formula Boiling point 62C
Specific gravity 1.484(20C)
Flash point no-data
Ignition point no-data
Explosion limit no-data
CAS No. 67-66-3

Solvent Methl ethyl ketone


Mol. formula CH3COC2H5 Refractive index 1.3788 (20C)
Mol. mass 72.1 Fusion point -86C
Structural formula Boiling point 80C
Specific gravity 0.803
Flash point -5.6C
Ignition point 505C
Explosion limit 1.81 to 11.5 vol%
CAS No. 78-93-3

13-3
13.2 Solvent Characteristics

Solvent Hexafluoro-2-propanol or Hexafluoroisopropylalcohol


Mol. formula C3H2OF6 Refractive index no-data
Mol. mass 168.04 Fusion point -3.3C
Structural formula Boiling point 58.6C
Specific gravity 1.590
Flash point no-data

Ignition point no-data

Explosion limit no-data
CAS No. 920-66-1

Solvent N,N-Dimethylformamide
Mol. formula C3H7NO Refractive index 1.4269 (25C)
Mol. mass 73.1 Fusion point -61C
Structural Boiling point 153.0C
formula Specific gravity 0.9445 (25C)
Flash point 58C
Ignition point 410C
Explosion limit 2.2 to 16 vol%
CAS No. 68-12-2

Solvent Dimethylsulfoxide
Mol. formula C2H6OS Refractive index 1.4783 (25C)
Mol. mass 78.1 Fusion point 18.42C
Structural formula Boiling point 189C
Specific gravity 1.1014 (20C)
Flash point 84C(sealed)

Ignition point 270C

Explosion limit 2.6 to 28.5 vol%
CAS No. 67-68-5

13-4
13.2 Solvent Characteristics

Solvent Toluene
Mol. formula C7H8 Refractive index 1.497 (20C)
Mol. mass 92.14 Fusion point -95C
Structural formula Boiling point 111.6C
Specific gravity 0.867 (20C)
Flash point 4 to 4.4C
Ignition point 116 to 480C
Explosion limit 1.2 to 7.1 vol% (in the
atmosphere)
CAS No. 108-88-3

Solvent N-Methyl-2-pyrrolidone
Mol. formula C5H9NO Refractive index no-data
Mol. mass 99.14 Fusion point -22.97C
Structural Boiling point 204C
formula Specific gravity 1.027 (25C)
Flash point 99C
Ignition point no-data
Explosion limit 0.9 to 3.9 % (in the air)

CAS No. 872-50-4

Solvent m-Cresol
Mol. formula C7H8O Refractive index 1.5438 (20C)
Mol. mass 108.14 Fusion point 11.95C
Structural formula Boiling point 203C
Specific gravity 1.034 (20C)
Flash point 86C

Ignition point 558.9C
Explosion limit 1.06 vol% (lower limit)
CAS No. 108-39-4

13-5
13.2 Solvent Characteristics

Solvent Mol. Boiling Refractive Absorbency Specific gravity


mass point index (Light pass length: 1 cm, (20/20C)
C nD20 object: water)
Acetone 58.08 56 1.359 330 nm:1.00, 340 nm: 0.10 0.790 to 0.793
350 to 400 nm: 0.01

Acetonitrile 41.05 82 1.345 200 nm: 0.22, 210 nm: 0.10 0.782 to 0.784
220 nm: 0.10, 230 nm: 0.02

Benzene 8.11 80 1.501 280 nm: 0.70, 290 nm: 0.10 0.877 to 0.881
300 nm: 0.05

Carbon tetrachloride 153.82 77 1.460 265 nm: 0.80, 270 nm: 0.32 1.594 to 1.599
280 nm: 0.08

Chloroform 119.38 61 1.445 254 nm: 0.30, 270 nm: 0.03 1.477 to 1.494
280 to 400 nm: 0.01

Cyclohexane 84.16 81 1.426 210 nm:1.00, 220 nm: 0.50 0.777 to 0.781
230 nm: 0.20, 240 nm: 0.10

1.2-Dichloroethane 98.96 83 1.445 225 nm:1.00, 230 nm: 0.50 1.255 to 1.260
240 nm: 0.10, 254 nm: 0.02

Dichloromethane 84.93 40 1.425 220 nm: 0.07, 230 nm: 0.50 1.033 to 1.038
240 nm: 0.40, 254 nm: 0.20

Dimethylformamide 73.10 153 1.430 270 nm: 0.70, 275 nm: 0.30 0.949 to 0.954
295 nm: 0.10, 310 nm: 0.05

Dimethyl sulfoxide 78.13 -- 1.476 270 nm: 0.50, 280 nm: 0.25 1.100 to 1.102
290 nm: 0.20, 313 nm: 0.05

Dioxane 88.11 101 1.422 220 nm: 0.70, 230 nm: 0.50 1.033 to 1.038
240 nm: 0.40, 254 nm: 0.20

Ethyl acetate 80.11 77 1.373 254 nm:1.00, 280 nm: 0.02 0.899 to 0.904
260 nm: 0.30, 270 nm: 0.10

Ethyl alcohol 46.07 78 1.362 210 nm: 0.70, 240 nm: 0.10 0.790 to 0.904
220 nm: 0.40, 230 nm: 0.20

13-6
13.2 Solvent Characteristics

Solvent Mol. Boiling Refractive Absorbency Specific gravity


mass point index (Layer length: 1 cm, object: (20/20C)
C nD20 water)
Heptane 100.20 36 1.388 210 nm: 0.08, 230 nm: 0.10 0.683 to 0.685
254 to 400 nm: 0.01

Hexane 86.18 69 1.375 210 nm: 0.30, 220 nm: 0.15


230 nm: 0.05, 240 nm: 0.03

Methyl alcohol 32.04 65 1.329 210 nm: 0.07, 220 nm: 0.30 0.791 to 0.794
230 nm: 0.15, 240 nm: 0.07

Octane 114.23 --- 1.398 210 nm: 0.50, 240 nm: 0.02 0.702 to 0.706
220 nm: 0.15, 230 nm: 0.05

Propanol 60.10 82 1.377 210 nm: 0.70, 230 nm: 0.20 0.785 to 0.788
254 nm: 0.03, 270 nm: 0.02

Tetrahydrofurane 72.11 66 1.408 240 nm: 0.70, 254 nm: 0.20 0.887 to 0.891
280 nm: 0.10, 300 nm: 0.05

Toluene 92.14 111 1.497 285 nm:1.00, 290 nm: 0.50 0.866 to 0.869
300 nm: 0.15, 320 nm: 0.04

Distilled water 18.02 100 1.334

13-7
13.3 Quick Reference for Boiling Point

Before solvent replacement, check both boiling points using the table below. When
replacing a solvent of a high boiling point with a solvent of a low boiling point, cool the
instrument well.
When replacing a solvent of a low boiling point with a solvent of a high boiling point, do not
raise the instrument temperature until replacement is complete.

<Quick reference for boiling point> (One bar)

280

260 1-chloronaphthalene

240

220
1,2,4-trichlorobenzene
N-methylpyrolidone
200
N,N-Dimethylsulfoxide
o-Dichlorobenzene 180
N,N-Dimethyacetoamide
160
N,N-Dimethylformamide

140

Distilled water 120


Tolue
2-Propanol
1,4-Dioxane
Cyclohexane
100
Acetonitrile
Ethyl alcohol
Carbon tetrachloride
Benzene 80
Ethyl acetate
Hexan
Trifluoromethanol
Methyl alcohol
Tetrahydrofurane
60
Chlorofor

Aceto Hexafluoroisopropanol
Heptan
40

20

If a solvent boils in the instrument, the instrument or column may be damaged.

13-8
13.4 Waste Liquid Treatment

This section introduces the general waste liquid treatment methods. The treatment method
may differ depending on the entrusted agent. For details, refer to the related legal
regulations.

Reservoir Type Component Reservoir Notes Treatment Type


Acid waste liquid Mineral acid solution Mineral acid of 5% or 1. Acid and alkali
(5% min) less discharged after solutions are mixed
neutralization for neutralization
Alkaline waste liquid Alkaline solution An alkaline solution of and discharged
(5% min) 5% or less discharged after dilution.
after neutralization 2. Alkali solutions
may be used at
treatment facilities.
Hydrocarbon-c Hexane, benzene, Be careful to avoid 3. This type of
ontaining etc. ignition. solvent is
Combustible Solvent

solvent incinerated by
Oxygen-contai Alcohol, ether, spraying and the
ning solvent ketone, ester, etc. waste gas is
Nitrogen-contai Pyridine, amide, Diluted with C, H, or O washed by alkali.
ning solvent nitrile, etc. type solvent for 5 vol% 4. The amount of
Sulfur-containi Sulfide, sulfoxide, or less of N and S solvent injected
ng solvent etc. into the
combustion
chamber is
Halogen-contai Carbon tetrachloride, 5 vol% or less as a adjusted according
Incombustible waste

ning solvent chloroform, compound containing to the ease of


trichloroethylene, halogen combustion.
etc. If the solvent
liquid

Water-containi Water-soluble contains acid,


ng waste solvent, such as alkali, or metal, the
solvent emulsion instrument will
receive greater
damage.

Legal regulations related to waste liquid treatment may be revised. If the


above-described regulations differ from current legal regulations, follow
the current legal regulations.

13-9
13.5 Countermeasures against Static Electricity

When the mobile phase is a combustible organic solvent, take great care about with regard
to fire or explosions due to static electricity.
If a liquid flows through fine tubing, as in a liquid chromatograph at a high speed, flow
electrification generates static electricity. As a charged liquid accumulates in an insulated
container, the charge level gradually increases and voltage as high as several kV is
generated. As a conductor approaches, a spark may occur and ignite ambient combustible
gas if any.

Countermeasure 1 When using a non-conductive waste liquid container


Connect a ground wire to a conductive metal bar (e.g., tubing for liquid
chromatograph) and insert the bar into the container until its end touches the liquid
inside.

Waste liquid tube


Ground wire

Waste liquid container

(e.g., 3-L glass reagent bottle) Ground terminal

Conductive metal bar

13-10
13.5 Countermeasures against Static Electricity

Countermeasure 2 When using a conductive waste liquid container made of metal


When using a metal container for waste liquid, check the conductivity inside (liquid
surface) in advance. If there is no conductivity, ground the container as explained in
Countermeasure 1.
Connect a ground wire from a ground terminal to inside the container (liquid surface).

Waste liquid tube

Ground terminal

Waste liquid container


Ground wire

For the easy grounding of a waste liquid, the following options are available:
Ground kit A for non-conductive waste liquid container (3-L gallon bottle)
(Part No. 0019615)
Ground kit B for conductive waste liquid container (18-L oil tubing)
(Part No. 0019616)

13-11
MEMO

13-12
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