Jasco RI-2031 Instruction Manual

MODEL RI-2031

INTELLIGENT REFRACTIVE INDEX

DETECTOR

INSTRUCTION MANUAL

P/N: 0302-0555A

Safety Considerations

To ensure operation safety, this instrument must be operated correctly and

maintained regularly according to schedule. Carefully read to fully understand

all safety precautions in this manual before operating the instrument. This

manual denotes precautions against actions that can result in hazardous

situations or equipment damage by using the signal words WARNING,

CAUTION, and Note.

(1) Safety symbols

Instruction manual symbol. If the product is marked with this

symbol, refer to the instrument manuals to protect the

instrument against damage.

WARNING A WARNING indicates a potentially hazardous situation which,

if not avoided, could result in death or serious injury.

CAUTION A CAUTION indicates a potentially hazardous situation which, if

not avoided, may result in minor or moderate injury. It may also

be used to alert against unsafe practices.

Do not proceed beyond a WARNING or CAUTION notice until

you understand the hazardous conditions and have taken the

appropriate steps.

Note A Note provides additional information to aid the operator in

obtaining optimal instrument performance.

Pressurized, hazardous solvents are used in high-performance liquid

chromatography. Always follow the proper laboratory procedures to ensure

operator safety. Always wear goggles, gloves and protective clothing when

operating the instrument, especially when injecting a sample and opening

valves.

(2) Warning Labels

Warning labels are attached at several locations on this instrument. Do not

remove, deface or damage the warning labels. If a warning label peels off the

instrument or becomes illegible, contact your local JASCO distributor for a

replacement label. Be sure to indicate the part number (P/N) on the label.

(1) Fuse and Ground Warning Label (P/N: 0822-0163A)

Figure 1 Figure of the side view

Regulatory Statements

CE Notice

Marking by the symbol indicates compliance of this JASCO system to the EMC (Electromagnetic Compatibility) and Low Voltage Directives of the

European Community. This symbol indicates that this JASCO system meets

the relevant basic safety and health requirements of the EC Directive based on

the following technical standards:

• EN55011 -- ”Limits and Methods of Measurement of Radio Interference Characteristics of Information Technology Equipment.” -- Group 1, Class A.

Warning

This is a Class A product. In a domestic environment this product may cause radi

interference, in which case the user may be required to take adequate measures.

• EN61000-6-1 -- "Electromagnetic compatibility (EMC) Part 6-1:Generic standards – Immunity for residential, commercial and light-industrial environments"

• IEC61000-3-2 -- "Electromagnetic compatibility (EMC) Part 3-2:Limits – Limits for harmonic current emissions (equipment input current up to and including 16A per phase) "

• IEC61010-1 -- "Safety requirements for electrical equipment for measurement, control and laboratory use – Part 1:General requirements"

• A "Declaration of Conformity" in accordance with the above standards has been made and is on file at JASCO EUROPE srl, Via Confalonieri 25, 22060 CREMELLA (LC), Italy.

FCC Statement (for USA only)

Federal Communications Commission Radio Frequency Interference Statement

Warning

This equipment generates, uses, and can radiate radio frequency energy. If it is not

installed and used in accordance with the instruction manual, it may cause

interference to radio communications. It has been tested and found to comply with the

limits for a Class A computing device pursuant to Part 15 of FCC Rules, which are

designed to provide reasonable protection against such interference when operated in

a commercial environment. Operation of this equipment in a residential area is likely to

cause interference, in which case the user at his own expense will be required to take

whatever measures may be required to correct the interference.

iii

Preface

This instruction manual serves as a guidebook for using this instrument. It is

intended to instruct first-time users on how to properly use the instrument, and

to serve as a reference for experienced users.

Before using the instrument, please read this instruction manual carefully, and

make sure that the contents are fully understood. This manual should be easily

accessible to the operator at all times during instrument operation. When not using

the instrument, keep this manual stored in a safe place. Should this instruction

manual be lost, order a replacement from your local JASCO distributor.

Installation Conditions

To ensure safe operation, the following recommendations should be observed:

(1) Do not operate the instrument under voltage fluctuations exceeding

10% of the recommended line voltage. Large fluctuations may cause

the instrument to fail.

(2) Use a three-pronged electrical outlet with a ground. When only a

two-pronged socket is available, use an adapter and be sure to

connect the ground wire of the adapter.

(3) Operate the instrument under a temperature range of 10 ∼ 30°C.

(4) Operate the instrument under a humidity range of 35 ∼ 85% (RH).

If ambient humidity exceeds 85% (RH), water vapor may deteriorate

optical components. If possible, install the instrument in a location

having a humidity of 60% or lower.

(5) Operate the instrument under an atmospheric pressure of 750 ∼

1060 hPa.

(6) Avoid strong magnetic fields and sources of high-frequency waves.

The instrument may not function properly when near strong

magnetic fields or high-frequency wave sources.

(7) Avoid vibrations caused by vacuum pumps, electric motors,

processing equipment and machine tools.

(8) Avoid dust and corrosive gas. Do not install the instrument in a

location where it may be exposed to dust, especially in locations

exposed to outside air or ventilation outlets that discharge dust

particles.

(9) Do not install the instrument in a location where it may be exposed to

direct sunlight.

(10) Do not install the instrument in a location where it may be directly

exposed to the air current from an air conditioner or heater, as such

a location may inhibit stable measurement.

Note: The above conditions do not ensure optimal performance of this

instrument.

Maintenance

Consult your local JASCO distributor regarding maintenance. In addition,

contact your local JASCO distributor when transporting the instrument.

Replacement parts can be ordered according to part number from your local

JASCO distributor. When the part number is not known, inform your local

JASCO distributor of the part name, instrument model name and its serial

number.

Notices

(1) Jasco shall not be held liable, either directly or indirectly, for any

consequential damage incurred as a result of product use.

(2) Software prohibitions:

y Copying of software or related materials for purposes other than

backup is prohibited.

y Transfer or authorization of the use of Jasco software to or by a third

party is prohibited.

y Disclosure of confidential information related to Jasco software is

prohibited.

y Modification of Jasco software is prohibited.

y Use of Jasco software on multiple workstations or terminals, through

a network or through any other means, is strictly prohibited. (This

does not apply to entities with the network license contract)

(3) The content of this manual is subject to change without notice in

accordance with product improvements.

(4) Unauthorized copying of this manual is prohibited.

(5) This manual shall not be used to guarantee or copyright industrial rights or

other rights.

(6) Company and product names listed herein are trademarks or registered

trademarks of their respective owner.

Warranty

This product is warranted for a period of one year from the date of delivery. If

any defects should occur in the product during this period of warranty, JASCO

will repair or replace the defective part(s) or product free of charge.

This warranty does not apply to defects as a result of the following:

(1) USE FOLLOWING IMPROPER OR INADEQUATE INSTALLATION.

(2) IMPROPER OPERATION.

(3) MOVEMENT, MODIFICATION, OR REPAIR BY PERSONS OTHER

THAN AUTHORIZED JASCO PERSONNEL.

(4) USE OF PARTS OTHER THAN THOSE THAT ARE AUTHORIZED BY

JASCO.

(5) INORDINATELY RAPID DETERIORATION DUE TO THE USE OF

CORROSIVE SOLVENTS OR SAMPLES.

(6) NATURAL DISASTERS SUCH AS FIRES, WATER DAMAGE, OR

EARTHQUAKES.

In addition, this warranty does not cover:

(7) CONSUMABLE PARTS OR PARTS THAT HAVE A SEPARATE

WARRANTY OR A WARRANTY PERIOD THAT IS DIFFERENT THAN

THAT SPECIFIED ABOVE.

The warranty period for all parts and repairs supplied under this warranty

expires with the warranty period of the original product.

Jasco Corporation

vii

viii ix

Safety Considerations ...................................................................i

Regulatory Statements ................................................................iii

Preface..........................................................................................iv

Installation Conditions .................................................................v

Maintenance.................................................................................vi

Warranty......................................................................................vii

Table of Contents.........................................................................ix

1. Outline and Specifications...................................................1

1.1 Outline .................................................................................................... 1

1.2 Specifications ........................................................................................ 2

2. Part Names and Functions ..................................................4

2.1 Front panel ............................................................................................. 4

2.2 Operation panel ..................................................................................... 7

2.3 Back panel.............................................................................................. 8

3. Power On/Off and Self-diagnostics...................................10

3.1 Power on and self-diagnostics........................................................... 10

3.2 Power off .............................................................................................. 11

4. Operations in Normal Operation Mode .............................12

4.1 Parameter changes.............................................................................. 12

4.1.1 Range and response changes..................................................... 12

4.1.2 Temperature control ON/OFF and temperature setting ............ 15

4.1.3 Output polarity change method ([SHIFT][6]).............................. 15

4.2 Purge valve open/close (Solvent replacement in the reference cell)

............................................................................................................. 17

4.3 Auto-zero operations........................................................................... 18

4.4 Error and warning messages during monitoring .............................. 18

4.5 Measurement of concentrated sample (Refractive index range

shifting................................................................................................. 19

5. [SHIFT] Key Operations .....................................................21

5.1 Operation summary............................................................................. 21

5.2 Preamplified output display ([SHIFT][1]) ........................................... 22

5.3 Auto-zero operation setting ([SHIFT][3])............................................ 23

5.4 Zero point shift for integrator output ([SHIFT][4])............................. 24

5.5 Lamp operation time ([SHIFT][5])....................................................... 26

5.6 Signal filtering mode ([SHIFT][7]) ....................................................... 27

5.7 Other settings ([SHIFT][MARK]) ......................................................... 27

5.7.1 Marker voltage/polarity changes................................................. 29

5.7.2 Setting to continue/stop self-diagnostics when an error occurs

................................................................................................................ 30

6. Program Mode Operations.................................................32

6.1 Operation summary............................................................................. 32

6.2 Switching between normal operation mode and program mode .... 32

6.3 File number setting (file loading) ....................................................... 33

6.4 Program editing ................................................................................... 34

6.4.1 Initial parameter editing............................................................... 34

6.4.2 Time program editing................................................................... 35

6.5 Time program operation...................................................................... 40

6.5.1 Time program execution.............................................................. 40

7. MEASURE RANGE Setting.................................................41

8. Maximum Flow Rate Changing at the Front Panel...........43

8.1 “ ~ 10mL/min” tubing arrangement and solvent replacement method

for reference cell................................................................................. 43

8.2 “10 ~ 50mL/min” tubing arrangement and solvent replacement

method for reference cell................................................................... 44

9. Maintenance........................................................................45

9.1 Error messages and countermeasures.............................................. 45

9.1.1 Errors during self-diagnostics after power on........................... 45

9.1.2 Self-diagnostics during operation .............................................. 46

9.1.3 Error message meanings and countermeasures....................... 46

9.2 Flow cell bubble removal .................................................................... 48

9.2.1 Baselines when bubbles are generated ..................................... 48

9.2.2 Bubble removal method 1 (high flow rate fluid pump).............. 50

9.2.3 Bubble removal method 2 (syringe fluid injection) ................... 50

9.2.4 Bubble removal method 3 (covering tubing outlet)................... 50

9.2.5 Bubble prevention method .......................................................... 50

9.3 Flow cell cleaning method .................................................................. 51

9.4 Calibration method .............................................................................. 52

9.4.1 Tubing ........................................................................................... 53

9.4.2 Standard solution......................................................................... 53

9.4.3 Replacement of tubing system solvent with water.................... 54

9.4.4 Calibration method....................................................................... 54

9.4.5 Calibration constant confirmation and setting .......................... 56

9.4.6 Alternative calibration method .................................................... 57

9.5 Lamp maintenance time setting ......................................................... 58

9.6 Serial number setting .......................................................................... 59

9.7 Power Fuse replacement..................................................................... 60

10. Appendix.............................................................................62

10.1 Operation Theory............................................................................... 62

10.1.1 Operation theory of deflection differential refractometers ..... 62

10.1.2 Optical system ............................................................................ 63

10.1.3 Signal processing method......................................................... 65

10.1.4 Flow line ...................................................................................... 66

10.1.5 Internal volume of tubing........................................................... 68

xii

1. Outline and Specifications

1.1 Outline

The JASCO RI-2031 Intelligent Refractive Index Detector is an HPLC detector

which offers unprecedented versatility, performance, and stability. The RI-2031

features the following:

High stability

High stability is obtained through an optical system that is not easily influenced

by temperature, an efficient thermal exchanger, and a digital signal processing

system.

Wide dynamic range

10 times larger dynamic range than an ordinary HPLC refractive index

detector.

Maximum flow rate of 50mL/min.

Maximum flow rate is 50mL/min. (Solvent: H2O) Wide dynamic range and

Extended Maximum flow rate are applied to the semi-preparation.

Easy operation

Parameters can be easily set using the LCD display, function keys, and

numeric keys. Self-diagnostics results and warning messages are also

displayed, which allows the condition of the instrument to be accurately

monitored. Optical Zero can be performed precisely using the easy key

operation.

Automatic analysis capability

The internal time program allows automatic switching of sensitivity range,

response and other functions. Using LC-Net, parameters can be set from the

Model HSS-2000 System without an interface.

Compact design

The front panel dimensions are the same as other JASCO 2000 series HPLC

equipment (pump, UV detector), which facilitates a neat stacking arrangement.

Safety measures An internal fluid leak sensor is installed. When a leak from the flow cell occurs,

a signal is output and the pump can be stopped.

1.2 Specifications

Model name: RI-2031 Intelligent Refractive Index Detector

Measurement system: Deflection type

Refractive index range: 1.00 ~ 1.75

Measurement range settings: 1/4, 1/2, 1, 2, 4, 8, 16, 32, 64, 128, 256, 512 x

10-6RIU/full scale (“MEASURE RANGE”: STD)

1/4, 1/2, 1, 2, 4, 8, 16, 32, 64, 128, 256, 512 x

10-5RIU/full scale (“MEASURE RANGE”:

WIDE)

Linearity: 5.0 x 10

5.0 x 10

-4

RIU (“MEASURE RANGE”: STD)

-3

RIU (“MEASURE RANGE”: WIDE)

<Condition> H2O

Noise: 0.2 x 10-8RIU

<Condition> H2O, Flow stopped

Cell capacity: 10µL

Maximum usable flow rate: 10mL/min. (“ ~ 10mL/min.” tubing)

50mL/min. (“10 ~ 50mL/min.” tubing)

<Solvent> H

Maximum pressure: 0.1MPa. (“ ~ 10mL/min.” tubing)

0.3MPa. (“10 ~ 50mL/min.” tubing)

Temperature control: PID control by heater,

Setting range: 0 ~ 45°C in 1°C increments.

Control range: Room temperature +10°C ~

Room temperature +25°C

Zero adjustment: Automatic Optical and electronic auto-zero

functions.

Integrator output zero positioning

Reference selection: Electromagnetic valve control

(“ ~ 10mL/min.” tubing)

Time program: Parameters that can be set are PURGE

ON/OFF, AUTO ZERO, RANGE, and

RESPONSE. Range from 0.1 to 999.9min.

Response FAST, STD, SLOW (TIME ACCUME, DIGITAL

FICTER)

Input and output signals: Recorder output: 10mV/FS

Integrator output: 5.0 x 10-4RIU/1V(SID)

5.0 x 10-3RIU/1V(WIDE)

Marker and leak output: 1 circuit each

Marker, auto-zero, program reset/start: 1

circuit each

LC-Net control: 1 circuit

Liquid wetted material: Quartz, fluoride resin, stainless steel

(SUS316)

Dimensions and weight: 150(W) x 470(D) x 150(H) mm, excluding

Protrusions.

Approximately 13kg

Power requirements: AC100 ~ 240V, AC, 50/60Hz, 50VA max.

Ambient temperature: +10 ~ +35°C for operation

-30 ~ +60°C for storage

* Specifications are subject to change without notice.

2. Part Names and Functions

2.1 Front panel

Operation Panel

Solvent Inlet and Outlet

POWER Switch



Figure 2.1 Front Panel

Name Function Solvent Inlet and Outlet “1” ~ “6”

Operation panel

POWER switch

Sample and Reference In and out connections Refer to Figure 2.2 and Figure 2.3. Panel containing control keys, parameter edit keys, and LCD display showing operating conditions, parameters and various messages. Refer to Section 4 and 5. Power switch for the instrument

Note: Suitable tubing for the Solvent Inlet and Outlet connections must be

selected according to maximum flow rate. Before connecting tubing,

refer to Figure 2.2. and Figure 2.3. “ ~ 10mL/min”. tubing is supplied

with the instrument.

Note: For a “10 ~ 50mL/min” tubing arrangement, the refractive index signal

output (and display) polarity becomes negative. Change the polarity setting

from plus (+) to minus (-) using the polarity setting function. (Refer to 4.1.3

polarity setting.)

Tubing with

OD=1.6mm

ID= 0.8mm

Sample Out (waste)

Flow rate: ~ 10mL/min.

Sample IN (from column)

Figure 2.2 “ ~ 10mL/min” flow rate tubing connections

Tubing

OD=1.6mm

ID=0.8mm

(Same tubing as used

to connect ports

No.1-2 or ports

Sample Out

4 5

Reference IN

Flow rate: 10 ~ 50mL/min.

No.4-5. for the “

10mL/min” tubing

arran

ement.

Tubing

OD=1.6mm

ID=0.8mm

Sample Out

2 3

Sample IN

Reference Out

Tubing OD=1.6mm, ID=0.8mm

Mobile phase

Flow rate: 10 ~ 50mL/min.

Sample IN

Replace solvent in the reference cell

by sucking the mobile phase solvent.

Keep the syringe connected during

analysis in order to maintain solvent

in the reference cell and to facilitate

solvent replacement.

Figure 2.3 “10 ~ 50mL/min” flow rate tubing connections

2.2 Operation panel



Figure 2.4 Operation Panel

Name Function LCD screen Displays operation conditions, setting values, error

messages and other information.

[PRGM RUN] Used to start and stop the time program. Operation status

is indicated by the lamp to the upper left of the button. The

lamp is lit during program operation. [AUTO ZERO] Sets the refractive index unit value (RIU) to zero. [MARK] Outputs a marker signal from the recorder output terminal. [MONIT] Used to return to the monitor screen from other screens

and to switch between monitor screens. [SHIFT] Used in combination with other keys to set parameters that

are not frequently changed. [PURGE] Executes solvent replacement (ON/OFF) for the reference

cell. [PRGM] Switches between normal and time program mode. [0] ~ [9], [.] Numeric keys. Keys 1 ~ 5 are used for special functions in

addition to their numeric function. The letters on these keys

describe the special functions. In other words, when editing

parameters, these keys are used to call up the relevant

functions. Refer to sections 4.1.1 and 6.4.2 for details. [][] keys Used to edit parameters and change screens. [CLEAR] Used to erase incorrect parameter input and clear error

messages. [EDIT/ENTER] Used to edit parameters.

2.3 Back panel

Input/Output Terminals

LC-Net Connectors

RS-232C Terminal

Fuses

AC input

Ground Terminal

Figure 2.5 Back Panel

Name Function Input and output terminals Signal output terminals REC+/G(GND)INT+/G(GND)

MARK OUT +/-

LEAK OUT +/-

Signal input terminals MARK IN+ GNDA/Z IN+ GND-

PRGM RST/ST+ GND-

Cooling fan

AC input Power fuses Ground terminal

LC-Net connector RS-232C terminal

Recorder output terminal (Output level determined by RANGE setting) Integrator output terminal (Fixed scale of 5x10-4RIU/1V(“MEASURE RANGE”: STD), 5x10-3RIU/1V(“MEASURE RANGE”: WIDE). Marker output terminal (Normally open, contact type output is closed when [MARK] key is pressed or MARK IN is input) Fluid leak warning output terminal (Normally open, contact type output is closed when a fluid leak from the flow cell occurs) (Note) The internal fluid leak sensor can only detect a leak of buffer solution.

Marker input terminal (Marker is added on the recorder output when the contact point is closed) Auto-zero input terminal (Recorder and integrator outputs are zeroed when contact type input is closed) Time program input terminal (Time program is reset and immediately started when contact type input is closed) Used for cooling the internal components of the instrument Accepts the power cable. Protects the instrument from excessive currents. Grounds the instrument. This is not the ground terminal for input and output signals. Input and output terminal for the LC-Net. Used when controlling the instrument via a RS-232C cable (optional).

3. Power On/Off and Self-diagnostics

3.1 Power on and self-diagnostics

Turn the power switch, located at the lower left of the front panel, to the ON

position. The self-diagnostics program is automatically executed. The program

examines the following items:

ROM CHECK (Memory)

RAM CHECK (Memory)

DC POWER (Direct current power source)

BACK UP (Memory backed up by battery)

TEMP SENSOR (Temperature sensor)

LAMP CHECK (Lamp energy)

LAMP O.P TIME (Lamp operating time)

ZERO GLASS DRV. (Optical zero glass driver)

An error message will appear if a problem is detected.

Note: When an error occurs, diagnostics will either stop immediately or

continue to the next item depending on the instrument settings (refer to

section 5.7.2).

The screen on the left in Figure 3.1 will appear when diagnostic tests are

complete. Press the [MONIT] key to switch to the screen on the right in Figure

3.1. The heater temperature is displayed in the screen on the right. When the

[MONIT] key is pressed again, the display will return to the screen on the left.

Normal operation mode consists of these two screens.



Mode display (Normal operation mode)

MODE RANGE RESPONSE

Sensitivity

(64)

NORM 64 STD

-0.1 + ON

RIU(x10 ) POLARITY PURGE

Current refractive index (-0.1)

-6

Polarity (Positive)

Normal operation mode monitor screen(1)

Figure 3.1 Normal Operation Mode Screens

3.2 Power off

Response

(standard)

[MONIT]

Purge valve status (ON)

Current Optical bench temperature/setting

temperature

MODE RANGE RESPONSE

Temperature

TEMP: xx.x/yy 

-0.1 + ON

RIU(x10 ) POLARITY PURGE

-6

°C



control mark



blinks when heating

Normal operation mode monitor screen(2)

Turn the power switch, located at the lower left of the front panel, to the OFF

position. The range, response, polarity, temperature, and time program set at

this time will be recorded in C-MOS RAM (memory backed up by battery).

These values will be restored when the power is turned on again.



4. Operations in Normal Operation Mode

The dynamic measurement range of the RI-2031 is 10 times larger than

ordinary HPLC refractive index detectors. The dynamic measurement range of

the RI-2031 depends on the “MEASURE RANGE” setting. When a highly

concentrated sample is analyzed, set the “MEASURE RANGE” to WIDE. Refer

to section 7.

The maximum flow rate of the RI-2031 depends on the tubing connections of

the front cell panel. The “ ~ 10mL/min.” tubing connections are for conventional

analysis and the “10 ~ 50mL/min” tubing connections are for semi-preparative

analysis. Tubing connection configurations are described in section 8.

4.1 Parameter changes

4.1.1 Range and response changes

After the power is turned on and the self-diagnostic tests are complete, the

normal operation mode monitor screen (1) (left in Figure 4.1) will appear.

Range and response settings can be changed here.

Note: Use the [MONIT] key to switch between monitor screens.

Mode display (Normal operation mode)

MODE RANGE RESPONSE

NORM 64 STD

-0.1 + ON

RIU(x10 ) POLARITY PURGE

Current refractive index (-0.1)

-6

Polarity

(Positive)

Sensitivity

(64)

Purge valve status (ON)

Response (standard)

[MONIT]

Current optical bench

temperature/setting temperature

MODE RANGE RESPONSE

TEMP: xx.x/yy 

-0.1 + ON

RIU(x10 ) POLARITY PURGE

-6

°C

 

Temperature control mark

blinks when heating

Normal operation mode monitor screen(1)

Normal operation mode monitor screen(2)

Figure 4.1 Normal Operation Mode Screens

+ 56 hidden pages

Jasco RI-2031 Instruction Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Safety Considerations

Regulatory Statements

Preface

Installation Conditions

Maintenance

Warranty

Table of Contents

1. Outline and Specifications

1.1 Outline

1.2 Specifications

2. Part Names and Functions

2.1 Front panel

2.2 Operation panel

2.3 Back panel

3. Power On/Off and Self-diagnostics

3.1 Power on and self-diagnostics

3.2 Power off

4. Operations in Normal Operation Mode

4.1 Parameter changes

4.1.1 Range and response changes