Shimadzu RID-10A User Manual

228-30179

DIFFERENTIAL REFRACTIVE DETECTOR

RID-1

OA

FOR

SHIMADZU

HIGH

-

PERFORMANCE

LIQUID

CHROMATOGRAPH

USER’S

MANUAL

Read the instruction manual thoroughly before you use the product. Keep

this

instruction

manual

with care

so

that you can use it any time you need it.

SHIMADZU

CORPORATION

CHROMATOGRAPHIC & SPECTROPHOTOMETRIC

INSTRUMENTS DIVISION

KYOTO,

3APAN

Copyright 0 Shimadzu Corporation

1995.

.

All rights are reserved, including those to reproduce

this

publication or

parts

thereof in any

form without permission in writing from Shimadzu Corporation. Information in this publication is subject to change without notice and does not represent

a

commitment on the part of the vendor. Any errors or omissions which may have occurred in this publication despite the utmost care

taken in its production will be corrected

as

soon

as

possible, but not necessarily immediately

upon detection. Note that Shimadzu does not have any obligation concerning the effects resulting from the

application of the contents of this manual.

MS, MS

-

DOS, Microsoft and Visual Basic are registerd trademarks, and Windows is

a

trademark of Microsoft Corporation

in

the USA.

IBM is a registerd trademark

of

International Business Machines Corporation in the USA.

TrueType

is

a

registerd trademark of Apple Computer, Inc in the USA.

The

RID-1

OA

is the differential refractive index detector for the high-performance liquid

chromatograph.

In

order to operate the unit safely, strictly observe the following points.

1.

Do

not

use

the unit for any purpose other than the above mentioned analysis.

2.

Follow the procedures described in the instruction manual.

3.

Observe the warnings and cautions.

4.

Do

not disassemble

or

modify the unit without approval

from

Shimadzu. Failing to do

so

may lead to a dangerous situation or damage of the unit.

5.

For internal repair of the product, contact your Shimadzu Service Representative.

6.

The pink-color pages and the meshed parts are for our service engineers, and are not intended for our clients.

Do

not attempt installation of the instruments

as

serious damage

could result.

WARNING IN

THE

INSTRUCTION MANUAL

This instruction stipulates the content of warnings as follows:

-1

Applied in a case that could result in death or serious injury.

-1

Applied in a case that could result in slight injury or physical damage.

-1

Applied for improvement of operating efficiency or help in understanding.

I

For safety

of

operation, this unit is provided with

the

A

mark

at the portion where special

When operating the

parts

where

this

mark

is

indicated, exercise

special

caution

after

reading

cautions are required.

the

manual.

Replacement

of

fuses

This

unit uses the

following

fuse. Be sure to replace the fuse

of

same

type

and

capacity.

Rated voltage

:

100-24OV

Part

NO.

072-01652-23 250V 5AT

I

CAUTION

I

Do

not bend the optical cable for remote control with the radius

of

35mm

or less.

Bending it with the radius smaller than 35mm may damage the cable,

whith may cause

malfunction

of

the

unit.

m

VAOS

I

AOX-022

VAOSI

A02

I

96-000ZE-822

26-0002€-822

VAOS

I

hpedea

A001

16-000Zf-822

a3NlOS

JaMOd

'ON

lred

8.

Solvent

not

usable

HFIPA

(Hexafluoroisopropyl alcohol) affects the materials used in the flow path and

deteriorate the strength of the material. In the worst case, pipe may explode and high

-

pressure solvent scatters.

As

it is very dangerous, never

use

HFIPA.

9.

Others

The equipment should not be exposed to direct sunlight or strong air currents.

It

is

also

recommended to install in a room where temperature fluctuation

is

small.

N

Liquid chromatography using flammable organic solvents as mobile phase requires proper care against

fire,

explosion, etc. Pakcularly, among various possible accidents, those caused by static electricity are difficult to anticipate, and tend to occur only with unexpected conditions which often make countermeasures insufficient. At a site where preparative liquid chromatography is practiced, a large amount of flammable substances may be used. Therefore, once an accident happens, it could lead to tremendous damage.

The mechanism of accident caused by static electrical discharge and preventive measures are described below. Take due care in safety measures in handling of equipment.

1.

Mechanism

of

Static Electrical Discharge Accident (Example)

Accidents caused by static electricity take place through the following processes.

When liquid is fed at high speed through a small

-

diameter tube like the pipe of a liquid chromatograph, static electrical charge occurs by friction between solid and liquid

as

shown in

Fig.

1.

Occurrence

of

Static

Electricity

1

$

-

Flowing liquid

A

Solid

body

A

:

Electric charge moving with flowing liquid

B

:

Electric charge being fixed

to

the

solid surface.

Fig. 1 Occurrence

of

Static Electricity by Friction between Solid and Liquid

Charging and storage

of

static electricity

t

1

Energy release by

1

I

discharge

I

3.

Ignition

of

combustible

substances

f

When the charged liquid is collected in an insulated vessel, the static charge accumulates gradually, and the voltage can easily reach

a

few kilovolts.

If

some other conductive object

is

brought near the vessel, electricity is discharged at a certain distance from the vessel releasing heat energy. If flammable gas of sufficient concentration exists nearby,

ignition is caused by this energy.

If

air drv

\

Liquid is flowing at high

speed

through a

small

diameter tube.

*Charge is easily accumulated if

bubbles are included in the liquid.

Insulated vessel (like polyethylene)

Spark discharge

-

””;”oyc

I

Ill

/

Inflammable gas is stored in the head space

of

the vessel.

(\

n\

Inflammable organic solvent is

charged

to

a great extent.

e

- - -

-

Floor covered

with

rubber, etc.,

provides unwanted insulation.

Fig. 2 Conditions which may cause Accidents

2.

Preventive Measures against Accidents

The principal preventive measure is the prevention of “charging and storage of static electricity” among those items shown in “Mechanism

of

Static Electrical Discharge Accident.” The preventive measures are shown below. It is recommended to exercise two or more measures simultaneously.

3K

Particularly when a large quantity of flammable solvent is held in a large vessel,

be

sure

to observe the preventive measures

1,2,

and

3.

Preventive measure

1.

Use metallic (conductive) waste liquid vessel which is well grounded.

This

releases the charge of the waste liquid and vessel to ground. The following items are available.

(1)

Grounding

wire

with clip P/N

228-21353-91

(2)

Metallic

18

liter can

P/N

038-00044

(3)

Metallic 4 liter can

P/N

038-00043-01

3K

+E

Be sure to ground the vessel properly. Disconnecting of grounding wire or poor grounding defeat the purpose of using

a

metallic vessel.

There are some metallic cans which have no conductivity

due

to

an

oxidized coating

or lacquer on their surface. Be

sure

to

confirm

the grounding

of

vessels by a tester before application. When a liquid with almost no conductivity (of

10-lOs/m or less) is discharged into the

vessel, it is necessary to

mix

it with another liquid with some conductivity. (The other

liquid can be placed in the vessel

in

advance.)

%

Preventive measure

2.

Minimize the clearance

of

both inlet and outlet

of

vessel to prevent flame from entering the

vessel.

(1)

Cap with three holes for

18

liter and 4 liter cans

(P/N

228-21

354-91)

is available.

Connect clip to metallic

Minimize clearance

by

attaching a cap.

ground the metallic vessel.

Metallic

18

litter can

(A

plated can is recommended.)

Static electricity

of

the liquid

is released via vessel.

Fig. 3 Anti-Static Electricity Measures for Vessel

Preventive measure

3.

Do

not approach the vessel with charged objects including the human body.

Charging prevention measures for human body

a)

b) Grounding

of

human body

c) Make

working floor conductive

Prevention of charging of shoes and clothes

Suitable products to be used for those measures a), b), and c) are available on the market. When persons who use no charge prevention measures approach dangerous sections, they have to be grounded beforehand. (For example, they should contact grounded metal by hand.)

%

Preventive measure

4.

Use pipes with inner diameter of

2mm

or more for waste liquid line for large flow rates.

3%

Inclusion

of

bubbles in the

tube

may increase the amount of charging by ten times.

Check that there is no inclusion

of

air

via

tube

joints.

Preventive measure

5.

When it is impossible to use a conductive vessel, use caution in the following points.

a)

Set the vessel

so

that the pipe outlet will be placed below the liquid

level

in the

vessel. Or, dip a grounded metal (ex. pipe connected

to

the main body of device) in

the liquid.

This

method is not effective

for

liquid with small conductivity (10-I0s/m

or

less).

Use

a

vessel

of

the

smallest possible capacity to minimize the damage by

fire

if it should occur. Prevent the

room

from

being

dry.

Humidity of

65% or

more has charge prevention

effects.

+E

b)

c)

a

1ChapterlI

General

1.1

Outline

..........................................................................................................

1-2

1.2

Features

........................................................................................................

1-3

1.3 Principle

of

Measurement

.............................................................................

1-4

1.4

Row Schematic

............................................................................................

1-6

1

Chapter2 1 Parts List

2.1 Parts and Accessories

...................................................................................

2-2

-1

Component Location and Function

3.1 Front View

....................................................................................................

3-2

3.2 Interior

of

Front Cover. Right Side

..............................................................

3-3

3.3 Rear View

.....................................................................................................

3-4

I

Chapter4 1 Installation

4.1 Basic Installation Requirements

...................................................................

4-2

4.2 Example

of

System Layout

..........................................................................

4-3

4.3

Stacking Modules

.........................................................................................

4-4

4.4 Electrical Connections

..................................................................................

4-5

4.6 Connecting the Recorder and Integrator

.......................................................

4-11

4.7

4.5 Plumbing Connections

..........................................

:

......................................

4-6

Connecting the Drain Tube

for

Solvent Leakage

...........................................

4-13

1-1

Operation

5.1

Precautions

for

Operation

.............................................................................

5-2

5.2 Fundamentals

of

Operation

..........................................................................

5-3

5.3 Plumbing

of

the Flow Selection Block

.........................................................

5-13

5.4

5.5

Creating and Executing

Tie

Programs

.......................................................

5-16

Additional Functions (AUX

-

FUNC)

............................................................

5-21

1

ChaDter

6

I

Initial Performance Test

6.1

System Performance Check

............................................................................

6-2

-1

Control from External Equipment

7.1 Connection with System Controller SCL-1 OA

.............................................

7-2

7.2 Control

form

the SCL-IOA

...........................................................................

7-3

7.3

Connecting External Input and Output Terminals

........................................

7-10

I

Chapter

8 1 Maintenance

8.1

Cleaning the Flow Lines

...............................................................................

8-2

8.2 Span Adjustment

..........................................................................................

8-3

8.3 Replacement

of

Fuse

....................................................................................

8-7

8.4 Periodical Cleaning

......................................................................................

8-8

1-1

Performance Verification

9.1 Component Validation

..................................................................................

9-2

9.1

.

1

Test Procedures

of

Stand-alone Unit

......................................................

9-3

9.1.2

Test Procedures Controlled

from

the

SCL

-

1

OA

......................................

9-5

9.2 System Validation

.........................................................................................

9-9

9.2.1 Test Procedure

of

Isocratic LC System

..................................................

9-9

1-1

Troubleshooting

10.1

10.2

Symptoms. Causes and Remedies

................................................................

10-2

List

of

Error

Messages

..................................................................................

10-4

-1

Specifications

...............................................................................

1 1 . 1

RID-1

OA

Specifications 11-2

[-I

Replacement Parts

12.1

Consumables

and

Repair

Parts

.....................................................................

12-2

12.2 Optional

Parts

...............................................................................................

12-4

rChapterl31

Reference

13.1 Solvent Characteristics

.................................................................................

13-2

.

Chapter

1

General

1.1

Outline

.....................................................................................................

1-2

1.2

Features

...................................................................................................

1-3

1.3

Principle

of

Measurement

.......................................................................

1-4

1.4

Flow

Schematic

.......................................................................................

1-6

1-1

RID-1OA

-

RID-1OA

is

the

differential refractive index detector for the high

performance liquid

chromatogaph developed as a module

of

the

LC

-

1

OA

series.

The

RID-10A

improves analysis productivity and convenience

of

use like a

UV

detector. Its shortened stabilization time, the fact that it covers various applications from high sensitivity analysis to sampling analysis preparation

and

more,

RID-1OA

is much

improved in convenience than conventional models.

Only handling instructions for

RID

- 1 OA

and related accessories

are

described

in

this

instruction manual.

For

handling instructions of

other components, please refer to the pertinent instruction manual.

1-2

-

RID-1OA

1.

Excellent

stability

Stabilization time after turning on the power has been shortened to

reduce the waiting time for

start

of

analysis. Excellent stability has been realized by employing the dual temperature control structure of

the optical system and by improving the thermal design.

-

0

r

t

By adapting the original four-partitioned photodiode,

this

equipment

now covers the wide dynamic range of various applications from

high

sensitive analysis to large scale preparation of high concentration

samples.

2.

Various

applications

3.

Safety measure

4.

Corresponding to the

LC-1OA

series

The standard model is equipped with a leak sensor which enables automatic performance

of

operations such

as

stopping the pump in

the early stage of organic solvent leakage.

This

equipment is designed for the

LC

-

1

OA

series to have excellent

operability

as

a

component of the total system, including control

from the

SCL-1OA

and

data

processing in the

CLASS

workstation,

etc.

1-3

RID-1OA

-

The optical system of this unit is shown in following illustration. The light radiated from the lamp passes through the lens slit and through the cell in the form of parallel rays, which is then reflected by

the

mirror and passed through the cell

to

form an image of the

slit

on

the photodiode.

The

flow

cell consists of the sample side and the reference side.

When

the refractive index

in

the sample side cell varies,

the

image

of the slit moves horizontally.

W

lamp

#

When refractive index

I

When refractive index

,

in the

flow

cell

vanes,

Samole

/

<\-&

~&zf

the

slit

moves.

Dhotodiode

This

unit has a photodiode partitioned in four

as

shown in the figure below. When selecting a piece of photodiode to use among these four, the unit is able to provide measurements for both analytical

and preparative work.

In

modes

P

and

L

In

mode

A

1

A

signal is processed

divided into up and down.

regarding

it

as

two

regarding

it

as

two

elements

A

signal is processed

divided into right and left.

Signal processing

in

mode

A

signal

is

processed using the right and left portions of the

photodiode

as

individual elements. Data processing is performed as

a two

-

partitioned photodiode divided into right and left.

When the refractive index in the

cell

varies,

the

balance of the incident

light intensity into right and left

parts

of

the photodiode changes. The

change

in

the right/left balance

is

converted into refractive index and

then can

be

recorded.

1-4

-

RID-1OA

1.3

Principle

of

Measurement

A-B

RIx

TOTAL

Signal processing in mode

P

-

E

a,

Signal processing is performed using the upper and lower parts of

L

Q

the photodiode

as

individual elements. Since the boundary between

the upper and lower parts

is

slanted against a horizontal line, when

an

image of the slit moves horizontally, the balance of the light

intensity

in

the upper/lower parts

of

the diode changes.

This

change

in balance is converted into refractive index. The change

of

the bal

-

ance against the variation

of

the

refractive index is one-twentieth

that

of

mode

A.

In

mode

A,

when the slit image goes beyond the center line, measurement becomes impossible because the balance value stops varying, while in mode

P,

measurement is possible

under

these

conditions enabling measurement of a sample with high

concentration.

A-B

TQTU

Signal processing in mode L (An optional

flow

selection

block

is necessary)

Signal processing is performed

as

the same

as

in mode

P,

using

each

of

the upper and lower parts of the diode

as

individual ele

-

ments. However, since the reference side with less flow line resis

-

tance is used

as

the sample cell, the image moves in the reverse

direction

of

that

of

mode

P.

Thus polarity is turned over

before

the

change in balance

is

converted into a refi-active index.

B-A

TOTAL

w.

A

1-5

RID-1OA

-

The diagram shows flow lines

in

the RID-10A.

At R flow

OFF

When the R flow switch is

OFT,

the solenoid valve is open at side

A.

The solvent passing through the sample cell flows into the outlet

port, not into the reference cell.

At

R

flow

ON

When the R flow switch

is

ON,

the solenoid valve is open at side

B.

The solvent passing through the sample cell flows into the outlet

port after passing through the reference cell. This

is

used to fill the sample cell and the reference cell with solvent of equal refractive index before starting the measurement.

R

flow

ON

Q

!

Outlet

port

Inlet

port

Tubing

volume (At R flow

OFF)

Inlet port to flow cell

63.5

pL

Flow cell volume

9pL

Flow cell to cell outlet port

280.2

pL

S:

Sample

R:

Reference

1-6

-

RID-1OA

Chapter

2

Parts List

c

v)

3

2.1

Parts

and

Accessories

..............................................................................

2-2

1

CONTENTS

1

2

-

1

RID-1OA

-

1

[Caution]

Part

Name

Signal cable

When connecting the flow line and performing maintenance, be

sure

to use the

parts

described on this page or

“1

2.1,

Consumable

and Repair

Parts

”.

Normal

function

of

the system

is

not

,guaranteed

when

other

parts

are

used.

Parts

No.

Quantity

228-25089-92

1

This equipment consists of the following components. Upon unpacking,

confirm that all

parts

listed below

are

included

in

your

shipment.

0

RID-IOA

Main Body

Power supply cord

(

120V)

(220-240V)

Optical cable

0

Standard Accessories

071-608 14-

01

1

07 1-608 14-06 070

-

92025-5

1

sus

tubing

Teflon tubing

228-22310-00 lm 228-22305-00

50

crn

228- 18495-03 2m

Remote

cable

I

228-28253-91

I

1

Locking plate

Instruction

manual

SC

Coil

ASSY

(220-24OV)

Syringe Syringe adapter

228-15672-91

Coupling 1.6C

228-16004-03

Male nut PEEK

228- 18565

228

-

1875

1

228-301 78

1

228-34050-9

1

Drain tubino

kit

I

228-18495-03

I

1

I

2-2

-

RID-1OA

-

Chapter

3

Component Location

and Function

3.1

Front

View

...............................................................................................

3-2

3.2

Interior

of

Front Cover,

Right

Side

.........................................................

3-3

3.3

Rear View

................................................................................................

3-4

c

0

(D

0

-

c

3-1

RID-1OA

-

w

S

Q,

c

0

E

s

0

I

RID-1OA

I

Front cover

The front cover is opened for mounting

and

dismounting of

flow

cell

and

piping.

~ ~~

I

No-

I

Description

7

Function

~~~

1-0

I

controipanel

I

Performs

parasnetex

setting

and

displays

set

values.

I

@

I

Front cover opening

button

1

Press

this

button

to

open the front cover.

3-2

0

RID-1OA

ON

I

I%

OFF0

No.

0

Description Function

Refer

to

page

Cell inlet

port

Connects the

tube

from

column.

4-8

I II

@I

@ @

@

HI1

I

Cell outlet

port

Tube

holder

Connection

port

for leak

tube

Normally

COM~C~S

back

pressure

tube

(03mm

ID.

x

Im).

4-9

Secures

the connected

tube.

Connects the leak

tube

to

this

port.

4-13

Solvent

leak

sensor

Detects

solvent leaks and

outputs

an

error signal.

10-4

n

I

\

/

S

0

E

3

LL

-

c

3-3

RID-1OA

-

E

0

E

3

LL

.-

c

No.

3

6

@

c9

‘c,

E

Q

Description

Function

Refer

to

page

This

is

the connector for

SCL-IOA.

7-2

7

-

16

REMOTE

connector

External

input and output

texminals

Grounding terminal Power supply cord connector Fuse holder

These terminals connect

external equipment.

This

terminal

is

used

for grounding.

The power supply

cord

is

connected here.

4-8

Two fuses

are

provided

in

this

holder.

8-7

r

I---

I

i

Ta2

I

\

I

3-4

-

RID-1OA

Chapter

4

Installation

~~~ ~~~~ ~

(,,NTENTs

1

4.1

Basic Installation Requirements

.............................................................

4-2

4.2

Example

of

System Layout

....................................................................

4-3

4.3

Stacking Modules

...................................................................................

4-4

4.4

Electrical Connections

............................................................................

4-5

4.5

Plumbing Connections

...........................................................................

4-6

4.6

Connecting the Recorder

and

Integrator

................................................

4

-

1 1

4.7

Connecting the

Drain

Tube for Solvent Leakage

...................................

4-13

4-1

RID-1OA

-

Basic Installation Requirements

pAGiiiq

To

take full advantage of the RID-1OA’s performance capabilities

and

to

ensure its operational stability over a long service life,

verify that

the

selected installation site satisfies the following

requirements.

1.

Ventilation

2.

Fire

3.

Sink

Ventilate the room where

the

high-perfomance liquid chromatograph

is located since the solvent used is flammable

andor toxic.

Never use

fre in the same room where the high performance liquid

chromatograph is installed. Also, avoid installation in the same

room of other devices which may spark.

Always

keep

a

fire

extinguisher nearby

in

case of accident.

Install a sink nearby for flushing eyes

or

skin which have been in

contact with solvent.

4.

Corrosive gas and dust

Avoid installation in a place exposed to corrosive

gases

or dust.

5.

Electromagnetic noise

Avoid locations subject to intense magnetic or electromagnetic fields. Use

an

additional noise filter if power line noise interferes.

6.

Space requirements

This system is designed to be used on a table

or

stand, preferably a

solid and flat surface with

a

depth of 60cm

or

more.

See

“4.2,

Example of System Layout” for typical confi,o;urations of systems and installation space.

7.

Others

Select

an

installation site with

the

following parameters to maintain

full performance of the system. (1)

Maintain

room temperature within

4--35”C,

without extreme

fluctuations.

(2)

Avoid direct output of a heater or a cooler.

(3)

Avoid exposure to direct sunlight.

(4)

Avoid locations subject to strong vibrations

or

prolonged

weak vibrations.

(5)

Maintain relative humidity within

45-85%.

4-2

-

RID-1OA

Example

of

System

Layout

Example

of

liquid chromatograph system layout using this equip

-

ment

and

space requirements

are

shown below.

Detector

(RI

0-1QA)

Column oven (CTO-1OA) Manual injector

(7725)

Pump (LC-IOAD)

Reservoir

box

Chrornatopac (C-RGA)

Degasser

(D

G

U -1

06)

Option

bpx

S

[Caution/

Each component

of

the

LC-1OA

has a little clearance at the bot-

tom. Be careful to keep fingers clear when installing the unit.

4-3

RID-1OA

-

RID-1OA may

be

stacked on the pump (LC-IOASLC-lOAD/

LC- 1 OAT/LC- 1 OAi) or the column oven (CTO

-

1

ON

1 OAC). The

equipment can

be

stacked and locked for safety in case of

an

earthquake, etc. using the supplied locking plate.

(1) Refer to the figure below and remove the screws fastening

the equipment cover.

(2)

Attach the mounting plate using the removed screws.

Tighten the

mounting

plate

using the removed screws.

4-4

-

RID-1OA

piEG@-[

Check the following points before connecting power supply.

Supply voltage and capacity

lOOV 150VA 228-32000-91

120V

150VA 228-32000-92

220

-

240V 150VA 228-32000-94

~ ~~~~~~~

When the power supply

is

not stable or the capacity insufficient, satisfactory performance is not possible. Verify the total power supply for the system before preparing the power supply.

0

Verify that the power switch of the main unit is

turned

OFF.

1.

Connection

to

outlet

(1)

Connect the female connector of the power supply cord

supplied with the unit to the power supply cord connector at the rear

of

the unit, and plug the male connector into a power

supply outlet.

The supplied power cord is a three

-

conductor (3-prong) type.

When connecting to a

twoconductor (2-prong) type power

supply outlet, use the provided power supply adapter.

(2)

2.

Grounding

(1)

(2)

When the three

-

conductor type power supply outlet

is

used, the unit is grounded by the power supply cord. When the

two-conductor type power supply outlet is used,

the unit is not grounded.

In

this

case, ground

from

the

grounding terminal on the

rear

panel of the unit.

piiGi@l

To

prevent electric shock and to secure safe operation of the

system, always ground the unit.

4-5

RID-1OA

-

F

-

7

umbing

Connections

This section describes proper connection in a typical

flow

line as

shown

in the figure below:

1.

Flow

line in the system

Refer to the column oven instruction manual for installation

of

the

manual injector and column oven. When the column oven is

not

used, an injector holder and a column holder are optionally available for installation of the manual injector and the column.

2.

Connecting the solvent delivery pump and manual injector

Connection of the solvent delivery pump and the manual injector

are described below.

Cut the

SUS

pipe

(1.6

x

0.3 supplied

as

a liquid pump accessory) to the necessary length for the pump outlet and injector port

2.

Install

the male nut and ferrule to both ends of the

SUS

pipe.

Attach the male nut

1.6MN

and ferrule

1.6F

(accessories of

the pump)

to

the pump outlet side, and the male nut and

ferrule (accessories of the manual injector) to the manual

injector. Connect

an

end of the

SUS

pipe to the pump outlet and the

other end to the injector.

(Notel

Connect the

drain

tube to the manual injector ports 5 and

6.

Adjust the tip of the

drain

tube to meet the needle port of the injector. For all connections of the manual injector, use the male nut and

ferrule supplied

as

the manual injector accessory.

4-6

-

RID-1OA

4.5

Plumbing

Connections

/

T

Manual

injector

Injector

holder

3.

Connecting injector and column

A typical connection

of

a manual injector and a column is

shown

below:

(1)

Cut the

SUS

pipe

(1.6

x

0.3

supplied to the pump, to the

necessary length for connecting the injector and the column.

(2)

Attach a male nut and a ferrule to the ends

of

this

pipe.

(3)

Connect the ends

of

the

SUS

pipe to the injector and the

column respectively.

Attach the ferrule and the male nut supplied with the injector to the injector and those supplied to the pump to the column.

Make the pipe length between the injector and the column

as

short

as

possible to prevent sample band broadening.

Cut the pipe on the perpendicular and connect

it

securely to

avoid dead volume.

4-7

RID-1OA

-

4.5

Plumbing

Connections

SUS

pipe

PEEK

pipe

Cut perpendicularly

with

a cutter knife.

Cylinder Cut perpendicularly.

&

I

\

d

\

I

Mail nut

1.6MN PEEK

Ferrule

1.6F PEEK

Mail nut

1.6MN

Ferrule

1.6F

Rear

of

manual injector

I

J

To

detector

4.

Connecting detector and column

A

typical connection between the RID-1OA and a column is

described in this section. (1) Cut

the

supplied

SUS

tubing (50cm long) to the necessary

length for connecting the column outlet and the cell inlet

Po*.

Cut the tube on the perpendicular. When the

tube

is cut on a diagonal,

dead volume is generated which deteriorates separation.

When the flow selection block (option) is used, refer to section

5.3

Piping of

Flow

Selection Block (Option).

Connect the tubing between the column and the detector inlet with the supplied male PEEK nut

as

shown in the next fi,we. lighten

the male PEEK nut fmly without using tools.

I

Note

I

Insert the tubing into the column joint and the male union securely until it comes

to

the

end and then tighten the male

PEEK

nut.

Similarly, insert the cell inlet pipe until it comes to the end

and

tighten the male

PEEK

nut

so

that dead volume is minimized.

4-8

-

RID-1OA

4.5

Plumbing

Connections

Tubing

(cut

the 50cmlong tube for use)

Manual injector

Main

body

IN

port

Male

nut

PEEK

(Tighten by

hand)

Manual injector

I

by

hand)

5.

Detector outlet side piping

(1)

Prepare a waste liquid bottle. Connect the

drain

tube to the detector outlet. Select one

from

applied flow rate. Insert the outlet

of

the

drain

tube into the

waste liquid bottle.

the

drain

tubes listed

in

the table below depending on the

C

0

m

-

c

Max.

flow rate

Drain

tube

For extension

Remarks

[Wmin]

Fside diameter (mm) x length

(cm)]

[Inside diameter

(mm)

x

length (cm)]

3

0.3

X

100

1.ox

100

5

0.5

X

100 1.ox 100

20

0.8 X

100 1.6X

100

150

1.6X 100

1.6X

100 At mode L (option)

When using the FFX-1OA fraction collector, connect the inlet tube

of

the FRC-1OA to the detector outlet directly. Note that the

maximum

flow rate varies depending on the preparative head

of

the

FRC.

FRC

-

1OA

inlet pipe

Inside diameter

[m]

x

Length

[cm]

FRC-10A outlet pipe

Inside

diameter

[mm]

x

Length

[cm]

Max.

operating

flow

rate

[mVmin]

Fraction correction head with valve

0.8X

100

1.6X 100

20

(150')

Fraction

correction head with valve

0.3

X

100 1.6X

100

3

Fraction correction head without valve

FRC- 1OA preparative

head

0.3

X

100

*)

An

optional flow selection

block

is necessary.

The solenoid valve and flow cells may

be

damaged by application

of

back

pressure which exceeds the detector resistance pressure.

Do

not use the pipes listed

in

the table which

are

out

of

range.

I

Note

1

To

prevent the detector

from

being damaged by back pressure, it is useful to connect the relief valve (option) to the detector outlet when the

unit

is

used with large flow rate, or the piping

is

clogged.

4-9

RID-1OA

-

4.5 Plumbing

Connections

Main

body

outlet

port

When piping

for

the detector inlet and outlet is completed, secure

the two piping tubes

in

the tube holder

as

shown

in the

figure

below.

I

1

I

RID-1

OA

I

Fit the tubes in the tube holder.

/

When the front cover is

dosed.

4-10

-

RID-1OA

1.

Connection

with

recorder

Connect the

RECORDER

terminal

of

the

RID-1OA

and the

recorder using the supplied

signal cable.

Recorde-

-t

RID-1OA

[

Tk15th terminal

of

RID-1OA

Recorder

Recorder GND

(1

OmV

full

scale recorder)

or

the

6th

terminal

(I

mV

full

scale recorder)

The 7th terminal

of

RID-1OA

Green

~

Green

'

Grounding terminal

When using a stranded wire, twist the end tightly, or tin it with

solder.

Using

a small screwdriver or other tool, depress the rectangular button adjacent to the appropriate terminal hole. Insert the wire and release the button to

clamp

the wire

in

position,

as

shown

in the

flapre below.

Wire

-

Press

4-1

1

RID-1OA

-

4.6

Connecting the Recorder and Integrator

~~

2.

Connecting

with

Chrornatopac (integrator)

Connect the Chromatopac to the

INTEGRATOR

terminals

(TBl

No. 3 and

No.

4)

in

the external inpuvoutput terminals at the rear

of

the

RID

-

1

OA.

The connection procedure is similar to that in

“1.

Connecting with

recorder.” Connect the cable supplied with the Chromatopac to the

Chromatopac side and connect each terminal

of

the signal cable to

the

terminal block supplied with the Chromatopac.

To

Chromatooac

Terminal

Mock

supplied

with

Chromatopac

supplied

with

Chromat

412

-

RID-1OA

Each component

in

the LC-1OA series is designed

so

that solvent

leakage is discharged

from the liquid leak tube connection port

either at

the

right side

or

the lower front side

of

the equipment.

Connect the liquid leak tube if necessary.

1.

Connecting liquid

leak

tube in

LC-1OA

system

Connect the supplied L-type leak tube to the connecting port in each component. Connect the straight type joint to the liquid

leak

tube at the bottom

of the equipment

and

insert it into the drain bottle.

L-type leak tuhe

Liqiud leak tube

U

Connecting port

of

\

liquid leak tube Straight

type

joint

Drain

bottle

Use a T-type joint to connect liquid leak tubes for multiple instruments. Cut

the

supplied

drain

tube

to an appropriate len,ath.

Attach the

L-type

leak tubes horizontally or downward. Secure

them

to

the side panels

of

the equipment with the supplied lock catches. Position

the

waste liquid bottle lower than the bottom

of

the

equipment.

4-13

RID-1OA

-

Chapter

5

Operation

5.1

Precautions for Operation

........................................................................

5-2

5.2

Fundamentals of Operation

.....................................................................

5-3

5.3

Plumbing

of

the

Flow

Selection Block

...................................................

5-1

3

5.5

Additional Functions

(AUX-FUNC)

.......................................................

5-21

1

CONTENTS

1

5.4

Creating and Executing Time Programs

.................................................

5

-

1

6

5

-

1

RID-1OA

-

I

Caution

I

1.

Be sure to close the front cover during measurement. The baseline fluctuates when the front cover is opened or closed during high sensitivity analysis. Noise may be increased when the front door is kept open.

2.

Precautions to prevent clogging

of

the flow cell.

Dusty

or

clogged flow cells are the most frequent causes

of

trouble in any detector. After analyzing a high concen

tration sample, thoroughly flush it from the flow cell, using

a

large amount

of

mobile phase. Buffer solution crystallizes upon drying, and can clog the flow cell and tubing. Never leave buffer solution in the unit

as

mobile phase. Always flush the flow lines prior to

shutdown

of

the instrument.

Turn

ON R flow several times during solvent delivery and replace the reference flow cell with water.

5-2

-

RID-1OA

1.

Turning

power

ON

(1)

Push the power switch

on

the front panel to turn the power

ON

and

OFF.

\

d-

\

"7--

1

Power switch

OFF state

Power switch

ON

state

(2)

When the power is tumed

ON,

the

RID-10A

operates

as

follows:

Turning power

ON

All

of the dots in the display

unit

and all of the indicator

lamps light. Control program version

No.

is displayed.

balance

wn0-I

ranae

mode

f

Rl

D-1

OA

V%.

%

1

The motor for optical balance adjustment is moved to the set position and the instrument

seeks

the home position.

-

M(101

rsnge

mode

f'

S

EE

K

I

N

G

H

O

M

E

The position is adjusted

so

that the optical balance is at

the

optimum

position.

balance

RI(10

range

mode

(10

BALANCE

A

(3)

After turning the power

ON,

a memory check is automatically

performed and when no error is

detected

the following display

appears, indicating

that

operation is possible.

This

is the initial

State.

0

4

shift

progrun

remQte

tanpcolll

Rlbw

pol(-)

t=l~nOot=l

The

balance

and

RI

values vary depending

on

the

types

of

instrument.

E

0

-

c

E

Q)

op

5-3

RID-1OA

-

5.2

Fundamentals

of

Operation

a

(3

@

0

a

0

2.

Display

unit

RI

(

loa)

Displays refractive index (unit

:

X

lo4

FUU)

Displays full scale of refractive index output to the recorder terminal (unit : XlOkIU)

mode Displays measurement mode.

shift Shift key indicator lamp.

prog run

remote

Time

pro,oram operation indicator lamp. Lights when time program is being executed.

Remote mode indicator lamp. Blinks when

contmlled by

SCL-

1OA.

If

[

NOT

PROTECTED

)

message is displayed and an alarm sounds

after turning the power

ON,

press

a

key. When this message is

displayed, the time program

is

initialized.

When any other error message

is

displayed,

turn

the power

OFF

and contact your Shimadzu Service Representative.

temp cont

The display unit consists of display screen and indicator lamps as shown below.

Lights when the power is being supplied

to

the temperature controlled heater for optical

system unit.

P PP?

8

@

No.

1

Display

ordescription

I

Function

R flow

Reference flow indicator

lamp. Lights when the liquid is being supplied to the reference

flow line side.

pol

(-1

Polarity indicator lamp.

@I

balance

I

Displays position of the light on photodiode.

3.

Keyboard

The nineteen keys on the front

are

used for operation and

settings and classified into the following

three

types.

(1)

STD-func keys

Press these keys to perform a specified operation immediately

-

(

[Zero

1

key, etc.)

(2)

Shift-func keys

Press

these keys after pressing a

[

shift

1

key to perform

a

specified opeAtion

((7-1

key, etc.).

1-

5-4

-

RID-1OA

5.2

Fundamentals

of

Operation

(3)

Edit keys Use these keys to input parameters and edit a time program (ten

-

key, etc.).

shift

El

I-1

I.'1

shift

[T]

0

I21

'i

Enter

(1)

STD-func

keys

Auto zero key

(-1

Zero

shift

key

[mark]

Mark key

I.1.)

Run key

(2)

shift-func

keys

(+)key

(shlft)

+

[GGF)

key

(shlftj

+

[R]

key

Press this key to perform zero adjustment. Returns the baseline to the zero position

set

by

[-)

.

Press

this

key to move the zero position on the recorder. It is

moved upward by pressing

A

side and downward by pressing

V

side.

Press this key to add Mark to the data being recorded in the recorder by pressing this key. Mark is not valid in the integrator output.

This key is a switch to

start

and stop a time program.

These keys move

to

time program creation mode.

These keys drive the zero glass and adjust its position to'optimal.

These keys switch the solenoid valve to replace the liquid inside

the reference cell with the mobile phase.

@

+=

key

These keys switch the polarity of recorder output.

[pol

(-1

1

LED

is lit for

(-)

polarity.

E

0

.-

c

f

op

5-5

RID-1OA

-

5.2 Fundamentals

of

Operation

=+

(mode]

key

(shlftJ+

@

key

(3)

edit

keys

-

19)

Numerical keys

CEnfer)

Enter key

@

Clear key

a3

0"

(shlft+m

Delete key

uu

Function key

m+m

Back key

-

4.

Basic

operation

These keys select the measurement mode. The measurement mode changes

from

A

+ P +

L

3

A.

A

:

Analytical mode

P

:

Preparativemode

L

:

Large-scale preparative mode

For

the operation

of

each mode, refer to section

5.3.2,

Changing the

Measurement Mode. These keys can be used to set time constant.

Values from

1

to

10

can be set. For the relation between each value

and time constant, refer to section

5.2.9,

Setting the Response.

Input numerical values.

Sets input values.

Returns the display screen to the initial state.

Press

this key to clear an input value when entering a numerical

value. Press this key to clear the display and alarms when an

error

is

displayed. Equipment failure errors cannot be cleared with this key.

Deletes a line in the time program.

Advances to

the

next item in

the

display screen.

AUX.

FUNC

setting screen

is

forwarded.

Returns to the previous item.

AUX.

FUNC

setting screen

is

scrolled backward.

Before starting analysis, flush the detector flow line with mobile

phase. Supply the mobile phase at a flow rate of

1

mUmin, and

then press

(shlftl

and

B.

The solenoid valve is switched and

the

(R)

lamp is lit. Solvent flows

through

the sample and the

reference sides

of

the

detector cell replacing solvent

in

each. Supply

solvent for approximately

20

minutes with Wow ON. Then,

turn

Rflow ON/OFF several times to drive the bubbles out of the cell. Retum to Mow

OFF

state, and wait

until

the baseline stabilizes.

When the balance value is

more

than

50,

press

and

[F)

to perform optical balance adjustment. When the baseline

is

stabilized,

start

analysis.

5-6

-

RID-1OA

5.2

Fundamentals

of

Operation

I

Note

I

When the liquid inside the flow lines is not sufficiently replaced with the mobile phase, the baseline takes longer to become stabilized and the

drift

becomes large.

To

perform effective replacement, turn

R

flow

ON/OFF

several times at an interval of

two

minutes.

Switching flow lines during solvent delivery at large flow rate in mode

L

may damage the solenoid valve and the flow cell.

Thus, the following message appears when performing

R

flow

in mode

L.

f

CHECK

FLOW

7

Press

[E)

after the flow rate is changed to 1 mumin.

To

avoid trouble caused by bubbles, refer to the following.

When the pump sucks bubbles, degas the solvent with the ultrasonic cleaner. If dirt on

the suction filter is the cause,

clean the filter with the ultrasonic cleaner or replace it. Bubbles may not be easily removed when using

an

aqueous

solvent. Flush the flow lines with methanol

or

acetone. When replacing the aqueous solvent with organic solvent or vice versa, bubbles may be generated successively. If bubbles can be observed, flush the flow lines with thoroughly degassed solvent.

5.

Setting the measurement mode

(Example)

When changing the measurement mode from

A

to

P

Press

[shift)

and

.

The mode is changed to P to perform optical balance adjustment.

balance

RI

(lo)

range

mode

100

BALANCE

P

0

4

P

5-7

RID-1OA

-

5.2

Fundamentals

of

Operation

I

Note

I

Note

I

When the above operation is repeated, the mode is changed form

LA-+P+LJ

.

Mode L is only applicable when an optional

flow selection block is installed. When

the

block is

not

installed, do

not perform measurement in mode

L.

Refer

to

5.3.1 for the mode setting when using the flow selection

block.

Mode

I

Refractive

index

measurement range

I

Input step

0.01

step

for

0.01

to

1

step

for 1 to

500

1 A 1

0.Ol-500X1O4RIU

I

P-L

~1-smx1o"RIu

I

1

step

for

I

to 5000

Select the mode corresponding to the refractive index

of

the

sample

to

be

measured. When the index is

500

x

10"

FUU

or less, use

mode A.

Note that the setting of mode

P

has wider measurement range while

it

has

the larger baseline noise.

The range value will

default to 100 when

the

mode

is

changed

as

described below.

0

When

the

mode

is

switched

to

mode P or L during measurement

with the range

of

0.01

to

1

.OO

in mode

A.

0

When the mode is switched to mode A during measurement with the range of 501

to

5000

in mode

P

or

L.

6.

Setting measuring range

The procedure to set the recorder range is

as

follows:

Changing the range

from 4 to

16 X lo4

FUUFS

(1)

Press

[f..c)

once in the initial state to access the range

parameter (blinking).

balance

wr10-7

Rnpe

mode

(2)

Input

0,

@and

(E.t.f)

ba)uue

warn

rangs

mode

0

16

A

(3)

After a value is input, it

returns

to the initial

state.

5-8

-

RID-1OA

5.2 Fundamentals

of

Operation

7.

Changing

the

range

(1)

When a recorder

is

connected

to

the

RECORDER

terminal,

set the range at a value about

1.2

times as much

as

the expected maximum peak value. Maximum peak will be about

80%

of the full scale ensuring that peaks remain

on

-

scale.

(2)

When a Chromatopac (integrator)

is

connected

to

the

RECORDER terminal

(lOmV terminal),

peaks

having

refractive index up to about

100

times as much

as

the setting

range can be recorded. Set the measurement range at

a

value

about

1/80

of the expected maximum peak refractive index.

Normally, the recorder range

is

set

at

a value

of

about from

1

to 10 and the plot full scale is adjusted by changing

AmN

on

the

Chromatopac side. The relationship

of

the

setting

range and attenuation of Chromatopac

(ATTEN)

for the plot

full

scale

when connected to the RECORDER terminal

(10mV) is

as

follows:

Plot

full

scale

Plot full

scale

=

Setting range

x

2-/10

[

x

IO?RUFS]

5-9

RID-1OA

-

5.2

Fundamentals

of

Operation

AUX RANGE

value

1

2

(Exam

p I e)

When that range

=

1,

ATTEN

=

2

:

Plot full scale

=

1

x

22/10

=

0.4

[

x

lO-kUFS]

(3)

When a Chromatopac is used as a recorder, connect it to the INTEGRATOR terminal and set the range at

A?TEN on the

Chromatopac side.

It

is

also

necessary to make a rough range

setting on the detector side since the dynamic range

of

the

detector is extremely wide. This setting

is

made by setting a

value in

the

parameter AUX RANGE. Relation between

AUX RANGE value and

INTEGRATOR

terminal output

are

listed in the table below:

INTEGRATOR

terminal output

Remarks

1

x

~O~RIUN

1

x

103

RIUN

Compatible

with

AUX-L

of

RID-6A

~

4

I

~

Compatible

with

AUX-H

of

RD6A

2.5

X

lo4

RIUN

Plot full scale for Chromatopac determined by AUX RANGE value and

AmN value is

as

follows

:

Plot full scale refractive index

(X

lo4

RIUIFS)

determined

by

AUX RANGE value and AlTEN value.

I

AUXRANGE

I

O

I

Oel

I

1

I

10

1

0.25

I

1

I

0.21

21

20

I

0.5

I

(Example)

When

AUX

RANGE = 2 and Chromatopac AmN

=

7,

the plot

scale becomes

128~ 1 O%U.

5-10

-

RID-1OA

5.2

Fundamentals

of

Operation

8.

Zero adjustment

of

recorder

Before starting analysis, adjust the zero position of the recorder

as

follows:

(1)

Set the measuring range to 0 to short-circuit the recorder output. SHORT is displayed in the range display. (Refer

to

section

5.2.6,

Setting the Range.)

Adjust the pen position to

0

scale on the chart paper using

the pen position recorder adjusting knob.

(2)

(3)

(4)

Reset the measuring range at a value required for the analysis.

F’ress- ,and the

pen

returns to almost 0 scale on the chart

paper.

(5)

Press

(zeroshiftAV1

to move the baseline to a desired

position and

start

analysis.

(6)

Press the

key to return the baseline to the previous

position.

9.

Setting the

RESPONSE

In

this

equipment, a digital noise filter is used to improve

SIN

ratio. Response improves when setting the filter response low, but the noise reduction effect becomes small.

On

the contrary, response is worsened when setting the response high, but the noise reduction effect becomes large. Ten digital filter response steps are available when setting the parameter to

RESPONSE.

RESPONSE

values and

corresponding time constants for analog filters are

as

shown in the

table below:

c

0

-

c

f

00

5-1

1

RID-1OA

-

5.2

Fundamentals

of

Operation

value

1

E

0

Q

.

-

+.I

5

op

(

Letters in brackets are response

ofRID6A.

)

at half-height

0.05

sec

0.2

sec

RESPONSE

I

Corresponding time constant of analog

CR

filter

I

Minimum peak width

I

2

3

4 5

6

7

0.1

sec

0.4

sec

0.5

xc

(

F

A

S

T

)

2.2

sec

1.0

sec

4.8

sec

1.5

sec

(STD)

7.2

sec

3.0

sec

(SLOW)

13

sec

6.0

sec

26

sec

9

10

18

I

8.0

sec

I

36

sec

I

10.0

sec

45

sec

2.0

sec

9

sec

1

\\ I //

// I \\

5

[

RESPONSE

@

O

Input a value using numeral keys and press

(Enter).

Press

@

to return to the initial display.

(Note)

As

response is increased,

data

processor response

decreases, peak height decreases, and width at half

-

height

increases. It is recommended that response

be

set at a

value such that, for a given half

-

height width, the peak

height drops no more than

10%.

The relation between

response time,

peak

half-height width, and peak height

reduction is shown in the figure below.

To select a response using the figure, determine the width at half

-

height of the narrowest peak of interest. Using the

graph,

find the point of intersection between that width

value and the

90%

height value. Set the response which

corresponds to a value

I

the time constant

as

read

from

the graph. Note that response has no effect on peak

area.

Peak

area

does not change even when a low response

value broadens the peak.

100%

-

I

0)

al

r

05

SCC

Y

([I

al

1.0

Scc

a

3.0

fo~

6.0

scc

_-

0

10

Peak

width

at half-height

5-12

-

RID-1OA

1.

Usage

of

each mode

Refractive index measuring range

(xlobRIU)

Measurement mode

When the RID-1OA is equipped with the flow selection block (option), measurement mode can be selected for high sensitivity

analysis, preparative and large

-

scale preparative mode. Operation

in

the large scale preparative mode requires the optional block.

Flow

rate range Tubing

(mUmin) connection

Mounting of the flow selection block is performed by a service engineer. Refer to section

12.3.

Analytical

(A)

Preparative

(P)

Large-scale preparative

(L)

Preparative

-

500

20

Fig.

1

-

5000

20

Fig.

1

-

5000

150

Fig.2

Large-scale

preparative

Mode Setting Application

Analytical A For general analysis. The flow

lines

are

the same

as

that

of

the

RID-10A without

the

flow selection block. This mode is compatible with the

FUD-6A.

P

For measuring samples of high concentration. Samples ten times

S

as

concentrated

as

those for mode

0

-

c

A can

be

measured.

f

L

For measuring samples of high

op

concentration at large flow rate. Samples

of

the same concentration

as

those of the mode P can be

delivered

at

150

mUmin.

2.

Changing the measurement mode

(1) Selection of mode setting

The

current mode is displayed on the

LED

display. Switch

the

measurement mode by pressing

and

@

.

1

A

:

Analytical mode

L

P

:

Preparative mode

1

L

:

Large-scale preparative mode Mode setting must be accompanied with corresponding tubing connection

as

shown in Figs.1 and

2.

5-13

RID-1OA

-

5.3

Plumbing

of

the

Flow

Selection

Block

~

Max

flow

rate

(mumin)

50

1.50

E

0

I

c.

f

8

~~~~ ~ ~ ~~ ~~

Drain tubing

For

extension

0.

D.

x

1.

D.

x

Length [rnm]

0.

D.

x

1.

D. x Length [mm]

1.6X0.8X lo00

3.2X 1.6x lo00

3.2 X 1.6 X lo00

3.2 x 1.6

X

lo00

Drain

tube

Use the following types

of

drain

tube for large-scale preparative

Max

flow

rate

(mumin)

50

mode. The longer and/or smaller

I.D.

tubing than the specified

one causes

high

back

pressure beyond the value

in

the specifications

of the detector, which may lead to damage of the detector.

FRClOA

inlet tubing

0.

D.

x

1.

D.

x

Length [mrn]

1.6 X 0.8

x

lo00

(FRC-

1OA

accessory)

FRClOA

outlet tubing

0.

D.

x

1.

D. x Length [rnrn]

3.2

X

1.6

X

lo00

(FRC-

1

OA

accessory)

3.2

X

1.6 X lo00

[Note)

When a fraction collector

FRC-1OA

is

used,

use the following tubing.

I

150

I

3.2X 1.6X lo00

I

(FRC- 1

OA

accessory)

When using a fraction collector made by other manufacturer, check

that the back pressure caused by connecting

the

fraction collector does not exceed the limit that the detector can resist. Pay attention to pressure change,

as

well

as

back pressure when switching the

preparative valve.

(2)

Changing the tubing connection Open the front panel and change the piping connection

because large

-

scale preparative mode has different plumbing.

+column

1

Drain

Fig. 1 Tubing connection

in

the

analytical and

preparative

modes.

5-14

-

RID-1OA

5.3

Plumbing

of

the

Flow

Selection

Block

f-

Column

Fig.

2

Do

not

tubing

Tubing connection in the largescale preparative mode

set the instrument to mode L with analytical

and

preparative

connection. Similarly, do not set the instrument to mode

A

t

0

or

P

in

large-scale preparative tubing connection.

-

c

0"

5-15

RID-1OA

-

t

0

-

c

E

a

OQ

Command

ZERO

MARK

RNGA

1.

Command

list

Commands which can be used for a time progam

are

listed below.

Description Setting range Remarks

Execution of zero adjustment Marking on output for recorder Designation

of

output range for recorder (mode A)

Not applicable Not applicable

0,O.Ol-

500

Unit: x106RIUFS,

RNGP

RESP

Designation

of

output range for recorder (mode

P)

Designation

of

output range for recorder (mode

L)

Designation

of

response

0,

1

-

5000

Recorder is short-circuited when set to

0.

Refer

to

section

5.2.

Fundamentals

of Operation.

1

-

10

1

EVNT

1

EVEhToutputON/OFF

0,

1,2,

12

Refer

to

section

5.5,

Additional

Functions

.

1

POL

1

~olaritysetting

STOP

I

O’I

Ends a program. Not applicable

Positive polarity Negative polarity

RNGA

(setting value)

1.40

150

I

LOOP

I

Repeats all preceding steps in

the

pro,.ram.

10-25255

I

Value

0

repeats

a program

256

times.

RNGE

(execution value)

1-00

2.00

[Notel

Setting the RNGA at decimal number RNGA enables increments

of

0.01

unit steps. However, when set

at

a

range more

than

1.00,

fraction

of

5

and over is counted

as

unit

and

the

rest is omitted.

(Example)

I

Note

I

Execution of RNGA and RNGP RNGP setting during

a

time promoram is ignored in mode

A.

RNGA setting during a time program is ignored in mode P or

L.

5-16

-

RID-1OA

5.4

Creating and Executing Time Programs

2.

Explanation

of

display

screen

The edit mode is used to create a time program.

(1)

Press and

@.

A

screen similar

to

the one below

will

be

displayed.

b

Q

0

Number

of

steps already set

0

Number

of

remaining steps

The above example

shows

that the time program is

set

for

10

steps and there are

22

remaining steps.

(2)

PressLEnter 1 to display the following:

I

6

@

Commandname

0

Setvalue

Elapsed time fiom time program

start

(minute)

(3)

Press

[Enfet)

again, to display the following:

The contents in the display are

the

same

as

those

in

(2)

balance

RI(t0

range

mode

\\I//

f

1.00

ZERO

1

The above display shows that

AUTO

ZERO

is.activated

one minute

after

start

of the time program.

E

0

-

c.

E

Q)

8

5-17

RID-1OA

-

5.4

Creating and Executing Time Programs

3.

Flow

of

setting

Flow

in

setting a time program is shown below

:

0

4

A\j

Press lshlftjandm.

I

(CE)

baknce

RI

(104)

ranga

mode

0

USED

32

LEFT

Press

CEnter).

RI

(lo4)

range

mode

\\I I I I

//

//I

I

I I

\\

TIME

FUNC

VALUE

I

J

\\I

I

//’

//I I I

I

\\

0. 00

ZERO

Input time with numerical keys and then press [Enter).

balance

(lo4)

range

mode

10.

00

ZERO

--@

\\I

I

I I

//

//I I I I

\\

Each time

Ifunc>

is

pressed, commands are

displayed sequentially. Press

IEnter)

when the

objective command is displayed to set the command.

batance

(lo4)

range

mode

1

0.

0

RANGA

/ylAL,UIE

\\I I I I I

I//

When a command except

for

ZERO,

MARK,

and

STOP

is selected, input a set value for the command

with

numerical keys

and

then press

(Enter).

I

Next setting

If

no program

is

input (even

a step):

Operation

of

Is1.ft1

and

[fun,,,)

in

this

state returns the display to

the previous setting.

5-18

-

RID-1OA

5.4

Creating and Executing Time Programs

4.

Deleting

a

step

(Example)

5.

Start

and stop

It is unnecessary to set the time order

of

steps as they are

automatically rearranged. Set a

STOP

command at the end

of

a

program unless the

program is to

be

operated continuously.

0

When selecting a function, the previous function is displayed

by

-

pressing and

w.

Display the step to

be

deleted and press

@

and

@

.

Deleting the fmt step

in

the program set in the previous section.

(1)

Display the step

to

be

deleted.

(2)

Press

lshlftl

and

.

120.

00

RANGA

21

The

first

step in the program

is

deleted and the second step is

displayed. When the second step

is

not set, the following is

displayed:

-

m(lo3

law

mode

0

USED

32

LEFT

After setting a time program,

start

and stop the program according

to the following:

(1)

Press

(Nnj

.

The LED for

I

prog

run

1

is lit, and the time

program

starts.

There

are

two

methods

to

stop a time program: forced stop

of a time program in

process, and stop of a time program

using the

STOP

command in the program.

To

stop the time

program forcibly, Press again. The LED for

[El

is

dimmed,

and the program stops.

(2)

5-19

RID-1OA

-

5.4

Creating and Executing

Time

Programs

6.

LOOP

command

A

program can be repeated any number of times using a LOOP

command.

E

0

-

c

f

OP

TIME

mc

VALUE

15.00

ZERO

20.00

MARK

30.00

LOOP

3

According to the above setting, steps

(1)

and

(2)

are repeated

3

times at

an

interval of

30

minutes.

When parameter is changed while executing a time program, the changed value

is

valid only until the end

of

the program. On completion of the time program, the parameter is reset to the value set before executing the time program.

Any

number up to

255

can

be

set

to the

VALUE

for the LOOP

command. When

0

is

set for the value, LOOP

is

repeated

256

times.

The

program

that

was

set

after

the

LOOP

command is not executed.

The program stops at the end of the LOOP command.

5-20

-

RID-1OA

Add

i

ti

ona

I Functions

(A

UX-

FU

N C)

Type

4 4

The following Additional Functions are equipped with the

RID

-

1

OA.

Command Function

TOTAL EN CELL

Indicates the total quantity of light irradiated on the photodiode. Displays the quantity of light irradiated on

each of the right and the

left

side of

photodiode.

1

I

1

I

CELLTEMP

I

Sets the cell temperature.

I

AUX

RANGE

EVENT

EXT-S

Sets output range to

in

integrator.

Controls output relays on

the back of the

FUD-IOA.

Sets

control mode for the control of external equipment

through

the EVENT

I

4

I

ACTTEMP

I

Displays the actual temperature of the optical unit.

I

1

4

3

output relays. Monitors when running a time program. Displays the lamp lit time.

Locks

the keypad, preventing unwanted entries.

MONITTIME

LAMPTIME

CLOSE

KEY

1

~-

-

~

--~___~-~

1

Sets address of the

RID

1OA

for control via system controller.

SPAN

A SPAN P SPAN

L

Inputs the span value of the analysis mode. Inputs the span value

of

the preparative mode

Inputs the span value

of

large-scale preparative mode

(An

optional

flow

selection block is necessary.)

I1

ImAL

I

Selects independent operation or control via system controller.

I

1

LAMPVOLT

I

setting of the lamp voltage

I

“Type”

in

the above table indicates a kind of operating procedure.

Type

1

:

Input a value using numerical key

and

then press[=] key.

Type

3

:

Press

[Enfer)

key to execute the function.

Type

4

:

The status

is

displayed.

2.

Setting procedures for AUX.

FUNC

TOTAL

EN

(Total

lamp energy)

CELL

(Lamp energy of each photodiode.)

[

TOTAL

EN

7000

Displays the total quantity of light irradiated into the photodiodes. (unit

:

mV)

CELL

3550

3450

I

E

0

-

c

f

8

Displays the quantity

of

light irradiated into each of the right and

left photodiode. (unit

:

mV)

5-21

I

RID-1OA

-

5.5

Additional Functions

2

IX~O-~

RIU

N

Compatible

with

AUX-L

of

RIDdA

3

1

x

RIUN

4

25x10a

RIUN

Compatible

with

AUX-H

of

RlD-6A

t

CELL

TEMP

(Cell temperature setting)

ACT TEMP

(Monitors actual cell temperature)

AUX RANGE

(Integrator output

full

scale)

EVENT

(Event output terminals)

balance

wriol

lam

mode

(CELL

TEM

P

40.0

Sets the cell temperature at the measuring

unit.

When the

flow

rate is larger than

3

dmin,

turn

this

OFF.

When the

flow

rate is less than

3

mL/min,

set the temperature to

the room temperature

+

12

“c

balpma

m(103

range

mode

(ACT TEMP

40.0

I

Displays the actual cell temperature

in

the optical unit.

[

AUX

RANGE

-

7

I

1

I

1x10~

RIUN

I

[

EVENT

This

function

sets

the relays

accessed

by the

EVENT

output terminals

on

the back

of

the

FUD-1OA.

OFF

is

an open relay and

ON

is closed. Input the desired value and press

(GI.

Setvalue

I

EVENT1

I

EVENT2

I

5-22

-

RID-1OA

5.5

Additional Functions

Set

value

0

1

EXT-S

(External

starts,

sets specific

Control

mode

Relay contact points

are

controlled by the

EVENT

set

value.

Relay

1

(EVENT

1

terminals) closes

at

the

start

of

a time

pro-

gram.

Useful

starting

data

processors or

zeroing detectors.

bamca

RI(10-7

range

mode

EXT-S

-

2

3

functions for the

EVENT

output

terminals)

This

feature is typically used to control external equipment

through

the

EVENT

output (relay 1 and

2).

Input the desired value, then press

(GI.

Relay

2

(EVENT

2

terminals) closes on detection

of

the error

of

the

RIDlOA.

Useful

for

communicating

to

external equipment

Both functions described above

are

enabled.

MONIT-TIME

(Monitors program elapsed time)

LAMP

TIME

(Monitors the lamp

lit

time)

r

0

Q

d)

-

c

L

When

running

a time program, the time elapsed

from

the

start

of

8

the program is displayed. Input the desired value, and press

(K]

.

Sets

display

of

elapsed

time.

When setting this function, the time program display during operation

is

as

follows:

-

W(f0)

ranee

mode

,

.

\

Elapsed

time

from

the

start

of

the

program.

-

R(103

rage

mode

LAMP

TIME

150

Displays the integration time of the lamp lighting. (unit : hour)

The

life

of

a lamp

is

20,000

hours.

When the lamp life

is

close to the

end, contact your

Shimadzu Service Representative.

I

5-23

RID-1OA

-

i

5.5

Additional Functions

Set

value

0

CLOSE

KEY

(Prohibition of key input)

Function

Allows

control

via

an

SCL

-

10A.

ADRS

(Remote address)

1

C

0

LOCAL

I

c,

Independent

operation

(local

mode).

L;

Q)

(Setting of the local mode)

op

LAMP VOLT

(Lamp voltage)

SPAN

A

(Span factor in mode

A)

SPAN

P

(Span factor in mode

P)

balance

RI(10)

range

mode

CLOSE

KEY

This function locks keypad, preventing entry, and is invoked by pressing

(=]when the above display is shown.

To

restore

-

keypad function, press

and

a

simultaneously.

balmce

RI(10)

range

mode

ADRS

3

Sets a remote address setting (port

No.)

when

this

equipment is

connected to the system controller

(SCL-IOA)

for use. Input the

address number, then press(

Enter

.

For port

No.,

see

section

7.1,

Connection with System Controller

SCL

-

1

OA.

[

LOCAL

Selects independent control or control via an

SCL-1OA

system

controller.

A

set value 1 allows the

RID-1OA

to

be

controlled from

its

own

keypad even when connected to an

SCL

-

1

OA.

Input the desired value, and then press

[GI.

Sets a lamp voltage. (Input range

:

0

to

5.00)

Normally, input the value such that value of

TOTAL

EN

is

within

the range from

6,000

to

9,OOO.

balsra,

RI(10-7

range

mode

(SPAN

A

1.

00

1

Inputs the span value of the analytical mode.

balsra,

W(10-7

me

mode

(SPAN P

1.

00

I

Inputs

the span value of the preparative mode.

5

-

24

-

RID-1OA

5.5

Additional

Functions

SPAN

L

(Span factor

in

mode

L)

baiance

FII(I~

range

mode

SPAN

L

1.

00

Inputs

the

span value

of

large-scale preparative mode.

Large

-

scale preparative mode is applicable when the

flow

selection

block option

is

installed.

I

5-25

1

RID-1OA

-

c

Chapter

6

Initial

Performance

Test

-1

6.1

System

Performance

Check

....................................................................

6-2

6

-

1

RID-1OA

-

This

chapter contains

an

explanation

of

the operation check for the

simple system

in

the

figure

below.

Detector

(RID-1OA)

Column oven (CTO-1OA) Manual injector

(7725)

Pump (LC-IOAD)

Reservoir

box

rchromatopac

(C-RGA)

D

9

sser

(DGU-1OB

I

Option

box

S

L370d

-Approx.

540

DGU-1OB

LC-1

OAD

CTO-1

OA

RID-1OA C-R6A

Helium gas

L---L

__--

J

Manual Column injector

Reservoir

1.

Preparation

2.

Connection

3.

Operation

Prepare

required

reservoirs.

Prepare mobile phase. (Refer to section

4.)

Connect the input cable of the Chromatopac to the

INTEGRATOR

output terminal

of

this

equipment

using

the

signal cable supplied

to

this

equipment through the terminal

block supplied to the Chromatopac.

Turn

ON

the system power.

Open

the

drain

valve of the pump

and

purge the entire flow

line to prime the pump. Suck out about

4OmL

using the

syringe.

Close the

drain

valve and operate the pump at 1 mWmin.

Verify

that pump pressure

is

stable

and

mobile phase

is

flowing

from

the outlet.

Set

the temperature of

CTO-1OA

to

4Q°C.

Set parameter

AUX

RANGE

of

RID-1OA

to

2.

(AUX

output

range

becomes

1

x

~O-~RIUN.)

Set the Chromatopac

AmN

to

4.

(Plot full scale

of

the

Chromatopac becomes equivalent to

16

x

lo-.)

6-2

-

RID-1OA

6.1

System Performance Check

(8)

Press

[ZERO

I,

Is) , lo)

and

[

Enter

1

on the Chromatopac to

center

the

Den Position.

(9)

Press mid

on

the ChromatoDac to dot the

output.

(10) Wait

till

the

baseline becomes stable.

Good

example

0

Stable

Bad

examples

x-

There are

spi kings.

Increases

with

the

X

.-H

lapse of

time.

'-\

Decreases with the

lapse

of time.

'X

Unstable

(11) Set

AmN

to 8 on the Chromatopac. (Chromatopac full

scale becomes equivalent to about

256

x

10-6RIU)

(12)

Press

(5)

,

-

and (=)on

the

Chromatopac.

plotting.

(14) Inject sample to the injector.

(15)

Press [=]of the Chromatopac simultaneously with the sample injection.

4.

Example

of

analysis

result

An example

of

analysis under the following conditions

is

shown

below.

Mobile phase

:

AcetonitrilelWater

=

75/25

Column

:

Asahipak

NH2P-50

4.6mm

0

x

25cm

Flow rate

:

1

mwmin

Column temp

:

40°C.

Sample

:

Fructose

in

loomL

water,

lo&

Grucose 100 mg injection

Sucrose 100 mg Maltose

100 mg

Raffmose

100 mg

RID-1OA

-

6.1

System

Performance

Check

(Example

of

chromatogram)

C

Fructose’i.

379

Grucosel9.349

SucroseiIZ.

664

f

’hia

t

tose/’lj.

324

**

CALCULATION

REPORT

**

CH

PKNO

TIME

AREA

1

-

7.379

s40909

s

9.349 551971

9

11.661

862498

10

15.324

533931

12

22.591

761268

TOTAL

-

3553579

--------

HEIGHT

33027

27933

30889

14479

12786

139055

---

!.IF

IDNO

COSC

XAYE

1

..

Fructose

?’

-

Grucose

3

Sucrose

v

4

31a I t

ose

J

Raf

f

i

nose

7

-

---------_

0

6-4

-

RID-1OA

Chapter

7

Control

from

the

External Equipment

7.1 Connection

with

System Controller

SCL-1OA

.......................................

7-2

7.3 Connecting External

Input

and

Output

Terminals

......................................

7-10

7.2 Control

from

the

SCL-IOA

....................................................................

7-3

I

7

-

1

~

RID-1OA

-

c

t

P

3

U

w

i!

-

1.

Preparation

(1)

Using the supplied optical cable, connect the

REMOTE

connector at the rear panel

of

the RID-1OA and the

REMOTE

connector

of

the

SCL

-

1

OA

r(

RlPlOA

(SIL)

(FRC)

REMOTE

1-17

1-21

1-37

1-47

r5-1

r61

r?l

r87

4

Do

not bend the

remote

control optical cable at less

than

a

120"

I

angle.

(2)

Set a value

for

ADRS

in

AUX.

FUNC.

Input the

port

No.

of

the

SCL-IOA

to

which

the optical cable is connected to the

parameter

ADRS

of

this equipment.

7-2

-

RID-1OA

Refer to the SCL-1OA System Controller Instruction Manual for basic operation of the system controller.

1.

Power

ON

and

CONFIG

screen

Turn

ON

the SCL power switch to display the CONFIG screen.

When the detectors and the

SCL

are properly connected,

(LINKED1

is displayed at the right side of both

[=I

and (when

two

detectors

are

connected).

Equipment connection for controlling the detectors by SCL

is

defined on

this

screen. Highlighting the name of the unit defines

it

as

being present and the system controller will

perform

a link check

upon power up. Unit definitions are displayed only once after the

initial installation. These definitions are stored in the SCL and are

required

only

once unless the system configuration is changed.

Module name

-

SYSTEM

CONFIGURATION

L

INKED

L INKED L INKED

L

INKED

FRC L INKED

~

SUBC

L INKED

.-.

pr.88

MENU

PUMP.

B

LINKED

LOCAL

DET.

B

LINKED LOCAL

,

Function line

Define

the

detector connection according to the following procedure

:

(1) Display line a in the function line

as

in the following

figure. When b is displayed in the function line, press

[G)

once to change the display.

a

CI

I

(2)

Select the detector connected to the function key and the equipment name is highlighted on the screen.

Equipment of display

does

not accept control by

SCL

even when its name is highlighted. Refer to section

5.5,

Additional

Functions to change the local mode to the remote mode.

RID-1OA

-

7.2

Control

from

the SCL-1OA

2.

Main menu screen

Press

(menu)

in

the

CONFTG

screen to display the main menu

screen. Press to access the

main

menu from any screen

.

MENU

ANALYSIS FILE PARAMETERS

:o

TIME PROGRAM

:I

PUMP CONTROL

:2

DET CONTROL

:3

FRACTION COLLECTOR

:4

AUTO !NJECTOR/ANAL SEQUENCE:S MON I TOR

:6

SYSTEM

:7

tus

9999.9

0

/o

0

READY

3.

Setting initial parameters

Press numeric key 0 in the main menu screen or move the cursor

to

the number 0 and press

[s)

to display the parameter screen for analysis file. This screen

also

displays parameters for equipment other than

detectors. These parameters can be reset.

I

ANALYTICAL PARAMETERS FILE

0

-------PUMP-------

- -

- - - -

-

DET.

A

(

ISO.

)

RANGE

100.

00

A. FLOW

0.

000

ml/min

POL

1

8.

FLOW

0.

000

ml/min

CELL. T

40.

0

Detector

Sub-controller

J

I

___-_--

DET.

6-

C. FLOW

0.

000

ml/min

A. PRES

0

k

g/cm2

k

g/cm2

WAVE

195

nm

B.

PRES

0

k

g/cm2

nm

C.

PRES

0

P. MAX

100

kg/cmz

WAVE2

200

P. MIN

0

k

g/cmz

sv

0

RV. A

0

EVENT

0

RV.

B

0

POWER

1

RV.

C

1

Multiple

terminal

box

OVEN.

T

40

t

RV.

D

1

DEGAS

0

Solvent delivery unit

RANGE

2.

5600

AUFS

___________________---__------------------

T. MAX

85

t

SVR.

SI

1

p

I/S

SVR.

SO

1

p

I/t

Solenoid

valve

Contact

output

Column

oven

Help

display

By pressing

Ifunc),

the setting range for the highlighted parameter can

be

displayed on

the screen.

When detectors are connected, the control parameters for the

detectors are displayed in

[DET.AI

and

ml

as in the previous figure. Other parameters necessary for the detector are displayed and set

in

the

DET

CONTROL

screen.

7-4

-

RID-1OA

7.2

Control

from

the

SCL-1OA

4.

DET

CONTROL

screen

Press

I3

I

in the

main

menu screen to select the

I

DETECTOR

CONTROL

I

screen.

The detector parameters, which cannot be input on the

ANALYTICALPARAMETERS

1

screen, can

be

input on the

DETECTOR

CONTROL

1

screen. These detector parameters

control the operation of the detector

from

the

SCL

(described in

section

5.2,

Fundamentals of Operation).

Press

[z)on the

SCL

keyboard to

turn

ON

the

-1

lamp.

men the

v1

lamp is lit,

the

parmeters set in

this

screen

are sent to the detector.

(Example)

If the

FI

parameter is set

to

-

1,

the

LED

for polarity on the

detector is lit and the polarity is reversed.

DETECTOR CONTROL

FILE

0

___-_-. DET.

A

-

---

--

(

RID

RANGE

100.

00

RESP

5

POL

-

1

CELL. T

40

t

MODE

0

AUX

RUG

3

~___

In

the

I

DE-ECToRCONTROL

I

screen above, where the

RID-1OA

is connected

as

detector

A,

the

me

and parameters for

one detector

are

displayed. When no detector is connected, the following display appears in the center of the screen.

L

DETECTOR

IS

NOT CONNECTED

When

two

detectors are connected,

use

the function keys

[

DET.A

I

and

1

DET.B

I

to switch between detectors.

(1)

Press

[z]

to change the function display to the following

display:

7-5

RID-1OA

-

7.2

Control from the

SCL-1OA

Parameter

RANGE

RESP

(2)

Using function key

(

lf41

),

select the detector where parameters are to be set. This is only necessary when two detectors

(e.g., A and

B)

are connected. When

a detector

B

is selected and only one detector is connected,

Description Setting range Minimum Unit

Defaultvalue

Range

for

recorder

in

mode

A

(X

RIU)

0,O.O

1-500

(0.01-1.00)

0.01

100

Range

for

recorder

in

modes

P

and

L

(X

RIU)

0,

1-5000

1

100

Response

1-10

1

5

(1-500)

1

I

DETECTOR

IS

NOT CONNECTED

1

is disulaved.

AUXRNG

(3)

Move the

cursor

to select the parameter with the cursor keys

(

It)

and

11)

),

input a desired value, and press

[s)

.

Set

and select the range and minimum parameter

steps after accessing the help line with the

[fu.c)

key.

To

set the parameters for two detectors, refer

to

item

(2)

above. Parameters which can be set in the

DET CONTROL

screen

are

listed in the table below:

(4)

AUXrange

1-4

1

2

W

Parameter summary

POL

1

Polarity

I I I

11

-

1

or

1

CELL.T

I

Cell

temmrature

setting

I

O(-OFF),30-60

I

0.1

I

401

MODE

I

Measurementmode

I

0-2

I

1

I

OI

(5)

The following operations are possible in the detector control

screen using the function keys.

I I

-

[=I

(I)

Outputs detector parameters being displayed to

the

printer of

the

Chromatopac (requires the current loop interface). Resets the parameters (including parameters for other devices such

as

solvent delivery unit, etc.) in the file

No.

being displayed to the

initial values. Copies parameter values

from

the

currently displayed file to another

file. Performs zero adjustment

of

a detector

A.

-

RID-1OA

7.2

Control

from

the

SCL-1OA

Performs zero adjustment of a detector

B.

6.

Time

program

Program

input line

H

Operation

Sends marker signal to the recorder connected to the detector

A.

Sends marker signal to the recorder connected to

the

detector

B.

Toggles between the detector A or B for parameter display. Disables acceptance of any key input except for

I

KEYLOK

I

(lock

release).

After

setting

the

initial

parameters in the I DET

CONTROL

I

screen,

press

[x)

to

retum

to

the

main

menu

to

select

I

TIME

PROGRAM

I

.

In

the

time program

screen,

similar

program

to

the

time

program

is

set

on the

SCL

side

(refa

to

section

5.4,

Creating

and

Editing

Time

Programs).

In

the time

program

set in this

screen,

commands for the

detector

as

well

as

other instruments

are

included, e.g., solvent delivery

unit,

etc.

TIME PROGRAM FILE

0

(B. GE)

300

STEPS LEFT

#I

TIME I FUNC I VALUE

30. 00

E.

CONC 100

?'

50.

55'RANGE

Ai

4

2

1.6-0 0 0. 0

STOP

I

;

I-

I

51

!I

I

FUNCTION FOR (PUMP DELTXh DET. B OTHER) 31 RESP

134 CELL. TI44

R.

CLOS146 RNG. A

32

MARK

135 ZERO

145

R.

FLOW147 RNG.

P

33 POL

143

BALANCl

I

tlme

a.1110

ampl/lnj

frc

at-tua

9999. 9

0

/O

0

READY

Command

table

3

(1)

When no program

is

set and the cursor flashes in the

[TIME[column

in

step o (see example above), input the

desired time for the

start

of

a command and press

-1.

The cursor then moves to the item

FUNC.

(2)

Press

cfuncl

to change the function to the following display:

I

7-7

RID-1OA

-

7.2

Control

from

the

SCL-1OA

Marks

on the

recorder

output.

Polarity

Cell temperature setting

Performs

zero

adjustment.

Performs optical balance adjustment.

Closes

reference

flow

lines.

-

tu

U

f

%

w

-

--

1

0

(-OFF),

0.1

40

-1 or

1

-

30-60

--

I

-

--

-

--

(3)

Move the cursor to a desired device name in the following line using

-1

(m)

and

-1

(

(f4)).

Recorder range

in

mode

A

(x

io4w

Recorder

range

in

modes P and

L

(X

104Rnr)

~ ~~

FUNCTION

FOR

(PUMP

DET. B OTHER)

I

0,O.Ol-500 0.01 (0.01-1) 100

1

(1-500)

0,

1-5ooo

1

100

Commands corresponding to the selected module are displayed in the command table.

An

example

for

the command table is

shown

below:

31

RESP

134

CELL.

1144

R.

CLOS146 RNG.

A

32

MARK

135

ZERO

145

R.

FLOW147 RNG.

P

33

POL

143

BALANCl

I

Command summary

for

time

program

Parameter

pE

I

-*=

I

R.CLOS

I

R.FLOW

I

RNG.A

Description

I

Settingrange

1

Minimumunit 1 Defaultvalue

Response

I

1-10

I

1

I

5

--

I

-

I

-

Purges reference

flow

lines.

I

The

following

operations are possible in

the

time program screen

using

the

function

keys.

I

7-8

-

RID-1OA

7.2

Control

from

the

SCL-1OA

Outputs the time program on display to the printer connected to the Chromatopac

.

Erases all

of

the time program

in

the file being displayed.

Copies the file being displayed to a different

file.

Moves the cursor at the device name in the command table

to

the

left.

Moves the cursor at

-

the device name

in

the command table to the

right.

Press

(funcl

to

change the function to the following display:

I I

Disables acceptance

of

any key input except

[-I

(lock

release).

7-9

RID-1OA

-

The

two

external input

and

output terminals

are

T.B.

1

and

T.B.

2.

5

(+lOmV

F.S.)

6

(+lmV

F.S.)

7

(-COMMON)

c

S

P

S

W

Q

Q,

X

E

-

E

CI

RECODER

output terminal recorder.

Signal output terminal connected

to

ili

T.B.l

..

External

o

equipment

input

terminal

p

+I

1

+-

7

II

1OmV

full

scale

IL1

recorder

1-i

-

1mV recorder

External

terminal

T.B.2

u

T.

B.

1

of

EVENT

parameter in

AUX.

FUNC.

~

INTEGRATOR

output terminal Chromatooac. (1V

F.S.)

Signal output terminal connected to

Note)

F. S.

stands

for full scale.

7-10

-

RID-1OA

7.3

Connecting External Input and Output Terminals

7.1

Appendix

EVENT2

(

Event output terminal

2

T.

B.

2

Relay contact It is turned

ON/OFF

according to the

program or the set value of

EVENT

parameter in

AUX.

FUNC.

Signalname

I

Explanation

I

START input terminal

Time program is started

by

shorting this terminal

with COM terminal.

09

STOP

nnnnn

QQ\ooooo

I

7

is stopped

by

shorting this terminal

input terminal

I

with COM terminal.

I

COM.

I

COM terminal for START and STOP terminals.

I

(1)

Strip the sheath of the connecting cable for approximately

lOmm in len,@h at

the

end.

(It

is unnecessary for supplied remote cable.) When

the

core

wire is solid, insert it into the hole

of

a terminal

while pressing the button above the hole using a small

screwdriver. When the wire is stranded, twist the end well

and insert it into the hole while pressing the button above

the

hole using a small screwdriver.

To

disconnect the cable,

press the button and remove the cable from the terminal.

(2)

A

remote cable is supplied with the IUD-IOA.

To

protect the

cable wire

from breaking, use stranded cables. When connecting

two

or

more circuits to the terminal, use the following wires

with core diameter

as

indicated below:

Stranded wire Element wire diameter

:

@

0.18 at the minimum

Solid wire

@

0.4-@1.0

(AWG

26-18)

:

0.3mmz-0.75 mm2

(AWG

22-20)

7-1

1

RID-1OA

-

Chapter

8

Maintenance

8.1 Cleaning the

Flow

Lines

.........................................................................

8-2

8.2

Span

Adjustment

.....................................................................................

8-3

8.3 Replacement

of

Fuse

...............................................................................

8-7

Q,

8.4 Periodical Cleaning 8-8

0

f

0

r

C

Q,

c

.................................................................................

CI

-

8-1

RID-1OA

-

Dirty cells and piping may cause phenomena such as an unstable baseline or a large baseline noise due to pulsation

of

the solvent

delivery pump.

In

this

case, clean the flow lines with the following

procedures.

Item

to

be

prepared

Syringe

oty

1

I

Adapter

111

I

Water

Il~I

I

Acetone

I

5OmL

I

0.1N

nitric

acid

I

5OmL

I

-

Mixing nitric acid with organic solvent may

form

an explosive

substance. Be extremely careful when handling

mitric acid.

Deliver acetone from the inlet port using the syringe and adapter. During supply, turn the Mow

on(*)

to deliver

solvent to the reference side.

(*)

The state in which Mow lamp is

lit

when

@

and

Use distilled water to flush the flow lines as in step

1.

Flush the flow lies with

0.1N

nitric acid.

Flush out the nitric acid with distilled water.

Replace with mobile phase. When the mobile phase used for

analysis is not miscible with water, replace the flow lines with acetone and replace

it

with the mobile phase.

(Rflow)

ispmsxi

8-2

-

RID-1OA

F

-

polarity

mode

Span adjustment should be performed over each mode of

A,

P

and

L.

When a Chromatopac is used, refer to

8.2.1,

and when

an

LC

workstation is used, refer to

8.2.2.

Inject

the

standard solution whose refractive index is

known,

and

adjust the detector output

so

that the signal intensity can be verfied.

Following

is

the description for mode A span adjustment.

+

A

(When performing mode A

span

adjustment)

I

Items to be prepared

I

Qty

I

Chromatopac

or

LC

workstation

Sy-ringe

.

Adapter Water

(HPLC

grade)

lmL

I

Refractiveindex standardsample*

I

lOOmL

I

*

Refractive index standard sample:

glycerin solution 0.872

gL

Dissolve 43.6 g of glycerin

(USP

grade or equivalent)

in

the

1L

of

water, and dilute this solution

50

times for the refractive index

standard solution. (Reference document

ASTM

E1303-89) This

sample shows difference of

100

x

10

"

RIU

from that

of

pure water.

8.2.1

When span adjustment

is

performed

using the Chromatopac

(1)

Turn

ON

the power.

(2)

Set the parameters of the detector

as

follows:

I

L

ILOCAL I1

(*I

I

m

E

Q)

E

c

-

*

When the

RID-

1

OA

is

controlled from the system controller

SCL

-

1

OA:

This

adjustment is performed by the detector independently. First, input

LOCAL

=

1

to

separate control

(link)

from the

SCL.

After that, input

each

set

value using the numerical keys of the detector

main

unit

8-3

RID-1OA

-

8.2

Span

Adjustment

AUXRANGE

of the detector

2

4

Set the detector

so

that the plot full scale of the Chromatopac

becomes

128

x

1

0-6

RTU.

AlTEN of

the Chromatopac

7

9

Chromatopac

model

C-R7A

Flow distilled water from the inlet port using the syringe and

the adapter. Make

Mow on(*) to purge the reference side flow lines with

water.

(*)

@and

(Rflow)

is pressed, and

Fl

lamp is lit.

After

the

sample celyreference cell inside is replaced with

distilled water, make

Rflow

OFF.

When the baseline is stabilized, press

Ishlftl

and

[%)

and perform optical balance adjustment.

Press

(zerol

,

and

record the baseline level when the cell

is

fdled with distilled water.

Inject the standard solution from the inlet port. The baseline will move up ward by

80%

of the full scale. Record the base

-

line level in

case

of standard solution. Read the difference between the base line levels of the distilled water and

of

the standard solution, and convert the

value into

RI

unit.

Full

scale

on

chart

paper

150mm

(Example)

When the base line moves

120

mm on the chart paper with the

Chromatopac

C-R7A, the difference value can be converted into

RI

unit with the of following formula.

1 20

128X 10

"

[RIUI

XT

mm=

102.4X 10

"

[RlUI

150

:

Plot scale

of

the C-R7A

(see

following table)

*

When

the

Chromatopac is used, record the value by

pressing

the

(

PLOT

]

key. The plot scale is as follows:

I

C-RSAR6A

I

135m

I

(10)

As a result of measurement, when the refractive index of the standard sample is

R

x

lod

RIIJ,

the span factor can be

calculated by the following equation:

[SPAN

-

A] (new) = [SPAN-A] (old)

x

100/R

8-4

-

RID-1OA

8.2

Span

Adjustment

(Example)

When the measured refractive index is

102.4

R

x

old span factor is

0.90,

the new span factor is:

(1

1)

Input the new span factor obtained by the above formula into

SPAN-A.

(12)

Inject distilled water from the inlet port and finish the span adjustment.

(13)

For

span adjustment of mode P/mode

L,

change the mode

setting in

(2)

above to P or

L,

and follow the procedures

from

(4)

above. Input the span value obtained at each mode

into

SPAN-P

and

SPAN-L

each.

[RIU]

and the

0.90 x 100/102.4

=

0.88

t

New

SPAN-A

8.2.2

When span adjustment

is

performed

using

the

LC

workstation

(1) (2)

Turn

ON

the power

of

the

IUD-1OA

and

LC

workstation.

Set the parameters of the

RID-1OA

as

follows:

Example

1

(CLASS-VP)

'Ddecta A :

RID-IOA

MODE

171

RANGE

vj

WL

ELLT

AUXRNG

I

RIP1

OA

parameters

Q,

0

H

Example

2

(CLASS-LClO)

Eolariir

@GJ

0

-

Measure Mode

0

khairticai

0

1:Preparative

Cell

TernPAC1

140

I I

II

V

3:

1

.LIE

-

5

RIU/mV

I

d+!T-7

RnllmU

8-5

8.2 Span

Adjustment

(3)

Change display ATTEN

so

that the vertical axis

of

the

chromatogram on the analysis screen becomes more than

100

pRru.

(Example)

When AUX

RANGE

setting is 2, set ATTEN

=

7.

(4)

Supply distilled water from the inlet port using the syringe and adapter. Then, replace the reference flow line with distilled water, After both sample cell and reference cell

are

filled with distilled water, close R. flow. Press

ITest/..r.l

and

[El,

and wait until the baseline is stabilized. Adjust the

zero

position, and record the baseline when the

inside of

the

cell is filled with distilled water.

Inject

the

standard sample from the inlet port. The baseline

will move toward

+

direction about 100

mu.

When the baseline is stabilized, move the cursor to read the difference between the levels of

the

distilled water and the

standard sample.

(10) When the refractive index of

the

standard sample

is

R

x

1

Od

RIU,

the span factor

is

calculated by the following equation:

(5)

(6)

(7)

(8)

(9)

[SPAN-A]) (new) = [SPAN-A] (old) x lOO/R

(Example)

When the measured refractive index is 102.4 x 10'

NU]

and the

old span factor

is

0.90,

the new span factor is

as

follows.

0.90

x

100/102.4

=

0.88

t

new SPAN-A

(1 1) Input the SPAN

-

A value in local mode.

Press

(fu..]

several

times and set LOCAL to

1.

Press the

(func)

key several

times and input the value obtained into SPAN

-

A.

After setting a the new value, set LOCAL to

0

again to

return to

the

remote mode.

(12)

Inject distilled water from the inlet port and complete the span adjustment.

(13) As for the adjustment of modes

P

and

L,

change the mode

setting, and repeat procedures from

(4)

to (12). Input the

span value obtained in each mode into SPAN

-

P and

SPAN-L.

8-6

-

RID-1OA

-1

This unit uses two pieces of the following fuses. Be sure to replace the fuses

of

the

same type and capacity.

Rated voltage: 100

-

240 VAC

250V, 5AT

Part

NO.

072-01 652-23

Replace the blown fuse according to the following procedure:

(1)

(2) (3)

Turn

the power switch

OFF.

Disconnect the power cord from the power supply connector. Catch the fuse holder cover with a regular screwdriver and take it out to

this

side.

Fuse

holder

-cover

(4)

Replace

the

fuse and pus it in until it clicks.

Fuse

holder cover

q

Fuses

8-7’

RID-1OA

-

Periodical

Cleaning

If

the cover or the

panel

of

the unit is

stained,

wipe out dirt or dust

with

soft

cloth or a piece

of

paper.

If

necessary, use a non-ionic detergent.

8-8

-

RID-1OA

Chapter

9

Performance Verification

9.1 Component Validation

.............................................................................

9-2

9.1

.I

Test Procedure

of

Stand-alone Unit

.................................................

9-3

9.1.2 Test Procedure Controlled

from the SCL

-

1

OA

.................................

9-5

9.2 System Validation

....................................................................................

9-9

9.2.1 Test Procedure

of

Isocratic

LC

System

............................................

9-9

1

CONTENTS

1

9

-

1

RID-1OA

-

1.

~~~

SCL

-

1OA

2.

Chromatopac

9-6

Overview

Each unit of the RID-10A system has been inspected stringently at the factory during the production process. The inspection procedures

described

m

this

manual

have

been

produced

by

compiling

and indicating the inspection activities that are bothactually necessary and can be practically executed by the user. That is, this

manual

is intended to

serve

as

a reference

book

for inspection procedures that do not require specialized expensive equipment that is used at the factory during

manufacture.

When inspection

results

obtained by the procedure

described in

this

manual meet the acceptance criteria, the

RID-

10A

can

be

used without problem.

Frequency for executing hardware validation

Roughly speaking, perform hardware validation every 6 to

12

month. Adjust the frequency of the inspection based on the actual

operating

conditions

of

the

LC system. When the

LC

unit is

operated

continuously,

day

and night, the intervals between inspections will

necessarily

be

shorter.

As

mentioned above, when the equipment is

judged to be improper, hardware validation must

be

executed

immediately to

comt any possible malfunctions.

3.

Validation item

With the

RID-IOA,

validation is performed

on

the following items.

Statement is made in reference to the regulation

in

the ASTM

(American Society

for

Testing and Materials) E1303-89.

(1)

(2)

Checking the lamp intensity

(3)

(4)

Checking the span

Checking the

lamp

lit time

Checking the temperature control system

4.

Validation procedure

Validation procedure differs depending on the system configuration with which the

RID-1OA

is

used.

This

chapter describes the following

methods of validation.

I

Control

of

the

RID-1OA

I

Data

orocessina

unit

I

Paae

I

Stand

alone

I

Chromatopac

I

9-3

I

9-2

-

RID-1OA

7

9.1

Component

Validation

9.1.1

Test

Procedure

of

Stand-alone Unit

1.

Checking the lamp

lit

time

Content

of

inspection

This

test checks the lamp lit time.

Test procedure

(1)

(2)

Press the

[G]

key several times to display LAMP

TIME.

Record the value

as

the

lamp lit time.

Acceptance criteria

LAMP

TIME

is less than

20,000.

The lamp life is approximately

20,000

hours. This

is

equivalent to

approximately

7

years of use 8 hours a day. It is recommended that

the lamp

be

replaced before the expected end of life to avoid the inconvenience of instrument failure. To replace the lamp, contact your Shimadzu representative or service engineer.

2.

Checking the lamp intensity Content

of

inspection

This

test checks whether the light source intensity is sufficient.

Test procedure

(1)

Fill

the cell with distilled water.

(2)

Press the key several times to display TOTAL

EN.

(3)

Record the light intensity value.

AcceDtance criteria

TOTAL

EN

is

more than

6.000.

When the value does not fall within reference value,

first

clean the flow cell. (Refer to the section 8.1 Cleaning the Flow Lines.) Then increase the value of the LAMP VOLT to

6000

or more. (Refer to

the section

5.5

Additional Functions.)

3.

Checking the temperature control system Content

of

inspection

This

test verifies whether the temperature control is working properly.

Test procedure

(1)

(2)

(3)

(2)

Press the

(funcl

key several times to display CELL TEMP.

Record the value

as

the set temperature.

Press the

Ifunc)

key again to display ACT TEMP.

Record the value

as

the actual temperature.

Acceptance criteria

ACT

TEMP

value is within

+/

-

0.1

"C of CELL TEMP.

The

CELL

TEMP

value must

be

12

(C

higher

than

room temperature.

9-3

RID-1OA

-

9.1

Component Validation

4.

Checking the span Content

of

inspection

This test checks whether the refractive index value

is

accurately measured and displayed by testing the standard sample whose index is already

known.

The test requires the following reagents and equipment.

Distilled water Standard sample (Glycerin solution)

Syringe Data processor

Refer to the section

8.2

Span Adjustment.

Test procedure

(1)

Set the parameters

of

the detector

as

follows.

CELL

TEMP:

40

polarity:

+

mode: A (When performing mode A span adjustment) Set the detector

so

that the plot full scale of the data processor

becomes

128

x

10%.

AUX RANGE of the detector 2 (or

4)

A?TEN of the Chromatopac:

7

(or

9)

Use the syringe and adapter to deliver distilled water to the

(2)

(3)

-

inlet port. During delivery,

press

the and

[

R

flow)

keys

to flow the water to the reference flow lines.

After the inside of the sample

celvreference cell is replaced

with distilled water,

turn

Mow

OFF

by pressing

the

@

and

[R)

keys again.

When the baseline is stabilized, press the

@

and

[G)

keys to perform optical balance adjustment.

Press the

@

key and record the baseline level when the cell is filled with distilled water. Inject the standard solution from

the

inlet port. The baseline

moves up ward by

80%

of

the

full scale.

(4)

(5)

(6)

(7)

Record the baseline level when the cell is filled with standard solution. When

the

Chromatopac is used, press the

[

P

LOT

J

key to record the baseline.

(8)

Read the difference of the baseline level between the distilled water and the standard solution, and convert the value into

RI

unit.

9-4

-

RID-1OA

9.1

Component

Validation

C-R4A

(Example)

When the baseline moves

120

mm

on the chart paper with the

Chromatopac

C-R’IA, the value

can

be

converted into the

RI

unit

with the following formula.

128

X

[Rnr] x 120 [mr11]/15O[mm] = 102.4

x

[RKJ]

150

:

Plot full scale

of

the

C-R7A.

(See the table below.)

160

mm

~______

~ ~~

I

Chromatopac

model

Full

scale

on

chart

paper

I

C-R7A

I

150

mm

I

Acceptance criteria

100+/-5~10-~m1

When the value does not fall within reference value, perform span adjustment according to the section

8.2

Span Adjustment.

9.1.2

Test

Procedure

Controlled

from

the

SCL-IOA

1.

Checking the lamp lit time Content

of

inspection

This

test checks the lamp lit time.

Test procedure

(1)

Select the

[6.

MONITOR]

on the main menu of the

SCL-10A

to open the monitor screen.

(Example

of

MONITOR

screen]

ACT.TMP

40.0

T0TAL.E

7566

BALANCE

10

LAMP.Th4

86

(Lamp lit time)

_____

DET-A

_____________________--

(2)

Record

the value

as

the lamp lit time.

Acceptance criteria

LAMP TIME

is

less than

20,000.

The lamp life is approximately

20,000

hours.

This

is equivalent to

approximately

7

years

of

use

8

hours

a

day.

It

is recommended

that

the

lamp

be

replaced before the expected end of life to avoid the inconvenience of instrument failure. To replace the lamp, contact your

Shimadzu representative

or

service engineer.

c

0

=

-

c

-

E

z

a

0

E

b

‘t

n

a

9-5

9.1

Component

Validation

2.

Checking the lamp intensity

Content

of

inspection

This

test checks whether the light source intensity

is

sufficient.

Test procedure

(1)

Fill the cell with distilled water.

(2)

Select the

[6.

MONITOR]

on the main menu

of

the SCL-IOA

to open the monitor screen.

(Example

of

MONITOR screen]

ACT.TMP

40.0

T0TAL.E

7566

(Lamp intensity)

BALANCE

10

LAh4P.m

86

____

DET.A

__________I______-________

......................................

(3)

Record the light intensity value.

AcceDtance criteria

TOTAL

EN

is

more

than

6,000.

3.

When the value

does

not fall within reference value,

first

clean the flow cell. (Refer to the section 8.1 Cleaning the Flow Lines.) Then increase the value of the LAMP VOLT to

6,000

or more. (Refer to

the section

5.5

Additional Functions.)

Checking the temperature control system Content

of

inspection

This test verifies whether the temperature control is working properly.

Test procedure

(1)

Select the

[3.

DET CONTROL] on the main menu

of

the

SCL-1OA

to

open the parameter control screen

of

the detector.

(2)

Record the value

of

CELL.T

as

the set temperature.

9-6

-

RID-1OA

9.1

Component

Validation

(3)

Select the

[6.

MONITOR]

on the main menu

of

the SCL-1OA

to open the monitor screen.

(Example

of

MONITOR

screen]

ACT.TMP

40.0

T0TAL.E

7566

BALANCE 10

LAMP.TM

86

----DET

A-----------------------------

(4)

Record the value

of

ACT-TMP

as

the actual temperature.

Acceptance criteria

ACT TEMP value

is

within

+

/

-

0.1

"C

of

CELL

TEMP.

The CELL

TEMP

value must be 12 "C higher than room temperature.

4.

Checking the span Content

of

inspection

This

test checks whether the refractive index value

is

accurately

measured and displayed by testing the standard sample whose

index is already

known.

The test requires the following reagents and equipment.

Distilled water

Standard sample (Glycerin solution)

0

Syringe

Data processor

Refer to the section 8.2 Span Adjustment.

Test procedure

(1)

Set the parameters

of

the detector

as

follows.

LOCAL:

1

(*)

CELL

TEMF?

40

(

indicated

as

OFF)

polarity:

+

mode: A (When performing mode A span adjustment)

*This test must be performed in LOCAL mode not in

REMOTE

mode. After changing the operation mode, other

parameters,

such

as

CELL

TEMP,

polarity, and mode,

should be set directly to the detector.

Set the detector

so

that the plot full scale

of

the data processor

becomes 128

x

lo-.

AUX

RANGE

of

the detector: 2 (or

4)

AmN

of

the Chromatopac: 7 (or

9)

(2)

9-7

I

RID-1OA

-

9.1

Component Validation

(3)

Use the syringe and adapter

to

deliver distilled water to the

inlet port. During delivery, press

them and

[s)

keys to flow the water to the reference flow lines. After the inside of the sample

celvreference cell is replaced

with distilled water,

turn Mow

OFF

by pressing the

@

and

[flow)

keys again.

When the baseline is stabilized, press the

(shlft)

and

[F)

keys to perform optical balance adjustment.

Press the

[zero)

key and record the baseline level when the cell is filled with distilled water.

lnject the standard solution from the inlet port. The baseline

moves

to

the

+

direction by

80%

of the full scale. Record the baseline level when the cell is filled with standard solution. When the Chromatopac is used, press the

(E]

key to record the baseline.

(8)

Read the difference of the baseline level between the distilled water and the standard solution, and convert the value into

RI

unit.

(4)

(5)

(6)

(7)

(Example)

When

the

baseline moves 120 mm on the chart paper with the

Chromatopac

C-R7A, the value can be converted into the

RI

unit

with the following

formula.

128

x

lo4

Ifuv]

x

120 [mm]/l50[mm] = 102.4

x

[RIU]

150 : Plot full scale

of

the C-R7A.

(See

the table below.)

I

Chromatopac

model

I

Full

scale

on

chart

paper

I

C-R7A

I

150

mm

I

C-R4A

I

16OmIIl

I

~ ~~~ ~~

~

~~

Acceptance criteria

100+/-5x104~]

When the value does not fall within reference value, perform span adjustment according to

the

section 8.2 Span Adjustment.

9-8.

-

RID-1OA

1.

Outline

For the holistic validation of HPLC system, chromatographic analysis is performed under the analytical conditions specified by the manufacturer. The system status can be judged based on the obtained results.

This

is because the failure

of

the LC system may depend on the analytical conditions. Holistic validation procedure described in

this

manual is the standard for checking the status

of

the LC system, serving as the basis of inspection.

In routine operation, the operators must perform a system suitability test under the predetermined analytical conditions. If any problem

occurs under such conditions, perform holistic

validation first

described in

this

manual. If the result of holistic validation meets

the acceptance criteria, the LC system itself is working properly

and the cause of the problem is relate to the analytical method

itself.

On

the other hand, if the results do not meet the acceptance criteria for holistic validation, it implies that there is a problem in the LC system itself and modular validation should

be

performed

for diagnosis of each LC module.

2.

Procedures for inspection

Details of standard operating procedure for holistic validation are described in

9.2.1.

The repeatability (relative standard deviation) of retention time, peak area, and peak height is measured to check whether the values meet the acceptance criteria.

9.2.1

Test Procedure

of

lsocratic

LC

System

1.

Purpose

The purpose of

this

test is to confirm that the chromatographic data can be obtained with good repeatability for the LC system to be inspected.

An

HPLC System for

this

inspection consists

of

the pump, detector,

column oven, auto injector, system controller, and data processor.

2.

Preparation for Inspection

(1)

Prepare the following parts and reagents.

(a) Isocratic LC system

(b)

(c)

Column

(Shim-pack HRC-ODs or equivalent,

Mobile phase

(acetonitrile/water

=

41

(v/v))

*

Use acetonitrile and water of HPLC grade.

4.6mm

ID

x

15Omm)

9-9

RID-1OA

-

9.2

System Validation

(d)

Sample

*

Anthracene in acetonitrile

[Method for sample preparation]

Place 2OOmg of anthracene in the volumetric flask of

lOOmL capacity and add acetonitrile of HPLC grade

to it.

(e)

(f)

Isopropyl alcohol

Water (HPLC grade or equivalent)

(2)

(3)

Check the connection

of

the units. Refer to the instruction manuals for details of the connection of each unit. Before installing the column, observe tubing connection

of

the LC system. Use tubing with 0.3mm

I.D.

or

less

from

the

outlet of auto injector to the column inlet and

from

the column

outlet

to

the detector inlet. Length of the tubing should

be

30cm or less

to

minimize the extracolumn band broadening.

Flush the flow line with appropriate solvents dependent on

the operation status of the system. General guideline is shown below.

To

flush the flow line with solvents, connect

the inlet and outlet tubing of the column directly using

a

proper

union.

Column should be connected after flushing.

(4)

0

Newly installed system

Flush

the flow line with isopropyl alcohol, then with water at

a flow rate of

2

mL/min

for ten minutes.

0

When

low

polarity solvent (such

as

hexane) is used

as

the mobile phase in the system

Flush the flow line with isopropyl alcohol, then with water at

a

flow rate of 2 Wmin for ten minutes.

0

When mixture of water and organic solvent, or organic solvent miscible with water (methanol, acetonitrile, etc.), or buffer solution is used as the

mobile phase in the system

Flush the flow line with water at a flow rate

of

2

mL/min

for

ten minutes.

(5)

Set the mobile phase (b) and flush the flow line, then connect

the column (c) to the LC system.

9-10

-

RID-1OA

9.2

System

Validation

3.

Procedure

Outline

of

procedure is described

as

below:

(1)

Set the

flow

rate

of

the pump

to

ldmin and column oven

temperature

to

40

"C.

Start

pump

flow

and temperature control.

Then, confirm that the solvent comes out

from the outlet tubing

of

the detector and no leak

of

solvent

is

observed at the

connection.

Set the parameters

of

the

RID

detector.

AUX RANGE

:

2

(1

x

RIUN)

RESPONSE

:

5

WIDTH

:

5 SLOPE

:

loo

DRTFT

:o

h4IN.AREA

:

100,000

T.DBL

:o

STOP.TM

:

7

ATIEN

:4

SPEED

:5

Set the parameters

of

the data processor.

Monitor the baseline. When a stable baseline

is

obtained,

press the zero point adjustment key

of

the detector. Then,

inject

lOuL

of

mobile phase and confirm no peak

is

observed. Inject

10

uL

of

test sample solution. Repeat measurement at least five times. Obtain the chromatographic data

of

retention time, peak

area,

and peak height

from

five successive analyses.

Calculate the average

(X)

of

the data and %RSD

using

the

equations

as

shown below.

SD

=

JF

XA

=

(Xl

+x2

+

......

+

X4+X5)

/

5

%RSD = (SD

/

XA)

*

100

X1

.....X5

:

Data

XA

:

Average

SD

:

Standard deviation

%RSD

:

Relative standard deviation

9-1

1

RID-1OA

-

9.2

System

Validation

1

4.

Parameter Setting for

Parameters

to

be set

for

the equipment at measurement

Inspection

described below.

[LC

parameters]

*

Initial condition

*

LC Time program

FLOW

:1

7.00

STOP

0VEN.T

:40

P.MAX

:

200

*

Auto injector [SIL-10NlOAil

SAMPLING SYRINGE SPEED

:

2

EXCESS VOLUME

:

50

(Use default value

for

others.)

*

Detector

[RID-1OA

]

AUX

RANGE

:

2

(1 x 10'~

m/v)

RESPONSE

:

5

are

5.

Acceptancecriteria

The

acceptance criteria for the %RSD are

shown

below.

Retention time

:

0.5%

or less

Peak area

:

1.0%

or

less

Peak height

:

1

.O%

or

less

9-12

-

RID-1OA

Chapter

10

Troubleshooting

J

10.1

Symptoms,

Causes

and Remedies

.....................................................................

10-2

10.2

List of

Error

Messa~es

........................................................................................

10-4

1

CONTENTS

I

L

10-1

RID-1OA

-

1

Symptoms,

Causes

and

Remedies

When

an

abnormality

occurs

in

the

equipment,

follow

the proce

-

dures

below

for

checking

the

unit.

Symptom

OVER

is

displayed

on

the display for

the refractive index.

Recorder baseline does not change.

Using Chromatopac, the obtained values for

peak

area or height are

different from those obtained

form

the

FUD-6A.

LED of

INT

ALARh4

remains lit.

*

The

LED

is lit when the

TOTAL

EN'

value is larger than

9o00,

or less than

SOOO.

OVER

is displayed on the display

for BALANCE.

Possible

cause

Recorder

terminals

are

saturated

in

the negative end.

No

signal

will

be

output

(1)

Range is set to 0.

(2)

Lamp does not light.

(3)

OVERcondicionexist

seeoVERsymptom

AUX

RANGE

setting

is inappropriate.

(1)

The solution in the reference cell is different

from

that

in

the

sample cell.

(2)

Bubbles

are

stagnant in the

flow cell.

(1) Optical balance adjustment is

requested.

(2) Bubbles

are

stagnant in the

flow

cell.

Remedy

Press

I.

(1)

Set appropriate range.

(2)

Light the lamp.

(3)

Press

I.

Refer to Chapter

5.2.7

Changing the range.

* *

Purge the solution in the reference cell.

Perform optical balance adjustment by

pressing and

(balance).

*

Adjust lamp voltage.

*

Purge the solution in the reference cell.

Perf- optical balance adjustment by

pressing and

(E).

10-2

-

RID-1OA

10.1

Symptoms,

causes,

and

Remedies

spiking

_/L/L/L

Sawtooth baseline

Symptom

of

malfunctions Possible cause

Bubbles flowing

-

Continuous

I.

through

the

cell

-

Bubbles trapped

at every stroke of

Spikin: occumng

1

I

.

I

the pump

-

Swell

No

equilibrationA

of baseline

(4)Check the pump,

Impurities

in

the

-

The

drift

stops after

stopping

mobile phase

liquid

supply.

stained.

1

Drift

~

Noise is

Confirmation

of

cause Countermeasures

With the flow cell tubing connected, remove the cell, and check

it

under flow conditions, then check for bubbles and lens

or

cell fouling.

excessive

2

(1)

Degas the mobile phase.

I

,(2) Use

methanol to rinse the cell interior. Remove the cell inlet tubing connector and force methanol from the outlet side with a syringe, then remove bubbles.

\

Should

any

trouble persist, contact

our

nearest branch office, sales

office

or

agent.

10-3

RID-1OA

-

Shimadzu RID-10A User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual