MODEL RI-2031
INTELLIGENT REFRACTIVE INDEX
DETECTOR
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)
Regulatory Statements
CE NoticeMarking 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.
• 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 is a Class A product. In a domestic environment this product may cause radio interference, in which case the user may be required to take adequate measures.
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
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
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.
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.
Table of Contents
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
4.5 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
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
1. Outline and Specifications
1.1 OutlineThe 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.
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 10-4 RIU(“MEASURE RANGE”: STD)
5.0 x 10-3 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> H2O
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.
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
2. Part Names and Functions
2.1 Front panelPOWER Switch
Operation Panel
Solvent Inlet and Outlet
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: 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.)
Figure 2.2 “ ~ 10mL/min” flow rate tubing connections
3
4 5 6
2
1 Sample Out (waste)
Sample IN (from column) Tubing with
OD=1.6mm ID= 0.8mm
Flow rate: 10 ~ 50mL/min.
Tubing OD=1.6mm, ID=0.8mm
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
Flow rate: 10 ~ 50mL/min.
Tubing OD=1.6mm ID=0.8mm
(Same tubing as used to connect ports No.1-2 or ports
No.4-5. for the “ ~
10mL/min” tubing arrangement. Tubing OD=1.6mm ID=0.8mm SampleOut Sample IN ReferenceIN Reference Out 1 Sample Out Sample IN Mobile phase 2 3 4 5 1 2 3 4 5 6 6
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.
2.3 Back panel
Input/Output Terminals LC-Net Connectors
RS-232C Terminal
Fuses AC input
Ground Terminal
Name Function Input and output terminals
Signal output terminals REC+/- G(GND)- INT+/- G(GND) MARK OUT +/- LEAK OUT +/-
Signal input terminals MARK IN+ GND- A/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-diagnosticsTurn 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.
NORM 64 STD -0.1 + ON
MODE RANGE RESPONSE
RIU(x10 ) POLARITY PURGE
Mode display
(Normal operation mode)Sensitivity (64) (standard)Response
Polarity
(Positive) Purge valve status(ON)
-6
TEMP: xx.x/yy -0.1 + ON
MODE RANGE RESPONSE
RIU(x10 ) POLARITY PURGE-6
[MONIT]
Current Optical bench temperature/setting temperature Temperature control mark blinks when heating
Normal operation mode monitor screen(1) Normal operation mode monitor screen(2) °C
Current refractive index (-0.1)
Figure 3.1 Normal Operation Mode Screens
3.2 Power off
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.
NORM 64 STD -0.1 + ON
MODE RANGE RESPONSE
RIU(x10 ) POLARITY PURGE
Mode display
(Normal operation mode) Sensitivity (64) Response (standard)
Polarity
(Positive) Purge valve status(ON)
-6
TEMP: xx.x/yy -0.1 + ON
MODE RANGE RESPONSE
RIU(x10 ) POLARITY PURGE-6
[MONIT]
Current optical bench temperature/setting temperature Temperature control mark blinks when heating °C Current refractive index (-0.1)
Input range:
1/4, 1/2, 1, 2, 4, 8, 16, 32, 64, 128, 256, 512, S (Short) x10-6RIU /10mV (“MEASURE RANGE”: STD)
1/4, 1/2, 1, 2, 4, 8, 16, 32, 64, 128, 256, 512, S (Short) x10-5RIU /10mV (“MEASURE RANGE”: WIDE)
Response input range: FAST, STD, SLOW (1) Change method 1
Flashes
Normal operation mode monitor screen(1)
Sensitivity input screen
Values in parentheses are after changes.
Display the desired value [ ][ ][EDIT/ENTER] NORM 64(16) STD(FAST) -0.000 + ON NORM 64 STD -0.000 + ON [EDIT/ENTER]
Response rate input screen
Display the desired value [MONIT]
NORM 16 STD -0.000 + ON
Flashes
[ ][ ][EDIT/ENTER]
Figure 4.2 Change Method (1)
Note: If an incorrect value is entered accidentally, press the [CLEAR] key before pressing the [EDIT/ENTER] key then enter the value again.
Change method 2
When the [RANGE/4] (range) key or the [RSPNS/5] (response) key are pressed, the corresponding parameter will flash and the value can be changed directly.
Sensitivity flashes [RANGE/4] [ ][ ][EDIT/ENTER] NORM 64 STD -0.000 + ON Response flashes [RSPNS/5]
Sensitivity change Response change
NORM 64(16) STD -0.000 + ON NORM 64 STD(FAST) -0.000 + ON NORM 64 STD -0.000 + ON [ ][ ][EDIT/ENTER]
4.1.2 Temperature control ON/OFF and temperature setting
When the normal operation monitor screen (2) (right in Figure 4.1) is displayed, temperature control can be turned ON/OFF and temperature can be set as shown the operations in Figure 4.4.
Input range: 0 ~ 45°C (Operating temperature range: Room temperature + 10°C ~ Room temperature +25°C)
0: OFF (Temperature control not active)
Note: During heating operation, the mark at the top right of the monitor screen will blink. Blinking speed is related to heater power. When 0 is set (control OFF), the mark belong to stop moving.
Flashes
Normal operation mode monitor screen(2)
Temperature input screen
Values in parentheses are after changes.
Values input [zz][EDIT/ENTER] [EDIT/ENTER] [MONIT] TEMP: xx.x/yy(zz) °C -0.0 + ON TEMP: xx.x/yy °C -0.0 + ON
Note:Temperature control will be turned off when 0 is input
Figure 4.4 Temperature Control ON/OFF and Temperature Setting
4.1.3 Output polarity change method ([SHIFT][6])
This operation changes the output polarity of the signal. When “10 ~ 50mL/min.” tubing is used, or negative peak heights exceed the integrator input range, polarity should be set to negative (-).
4.1.3.1 “10 ~ 50mL/min.” tubing arrangement
When “10 ~ 50mL/min.” tubing is used, because of the optical arrangement, the refractive index signal output decreases when the actual refractive index
When the actual negative peak signal exceeds -5.0x10-4RIU, polarity should be set to positive (+). Refer to Table 4.2 (“10 ~ 50mL/min.” tubing connections)
4.1.3.2 Negative peak signal exceeds the integrator input range
The allowable input voltage range of a current integrator is, in general, -10mV ~ +1V. When the negative peak signal is within 5x10-5 RIU (“MEASURE RANGE”: STD) or 5x10-4 RIU (“MEASURE RANGE”: WIDE), integrator output can be prevented from falling below –10mV using the zero point shift function. Refer to section 5.4.
When the negative peak signal exceeds this range, polarity should be changed. The actual allowable refractive index range is shown in Table 4.1 and Table 4.2. Change polarity settings, according to these tables.
Table 4.1 “ ~ 10mL/min.” tubing arrangement (*shifted by 100mV) MEASURE RANGE polarity without zero point shift* with zero point shift* STD + -5.0×10-6~+5.0×10-4 RIU -5.0×10-5~+4.5×10-4 RIU STD - -5.0×10-4~+5.0×10-6 RIU -4.5×10-4~+5.0×10-5 RIU WIDE + -5.0×10-5~+5.0×10-3 RIU -5.0×10-4~+4.5×10-3 RIU WIDE - -5.0×10-3~+5.0×10-5 RIU -4.5×10-3~+5.0×10-4 RIU
Table 4.2 “10 ~ 50mL/min.” tubing arrangement (*shifted by 100mV) MEASURE RANGE polarity without zero point shift* with zero point shift*
STD - -5.0×10-6~+5.0×10-4 RIU -5.0×10-5~+4.5×10-4 RIU STD + -5.0×10-4~+5.0×10-6 RIU -4.5×10-4~+5.0×10-5 RIU WIDE - -5.0×10-5~+5.0×10-3 RIU -5.0×10-4~+4.5×10-3 RIU WIDE + -5.0×10-3~+5.0×10-5 RIU -4.5×10-3~+5.0×10-4 RIU
When polarity is set to negative (-) with a “ ~ 10mL/min” tubing arrangement, the screen display and output (for both the recorder and the integrator) will change as shown in Figure 4.5. When the actual refractive index decreases,
0 0 0 RIU:-20.0 RIU:20.0 RIU:10.0 RIU:-10.0 Polarity:Positive Polarity:Negative Actual refractive index change
− ＋
Figure 4.5 Changes in Peak Appearance and Display Values Caused by Polarity Differences POLARITY +(-) Input screen Flashes [MONIT] [SHIFT] [5]
Output polarity change screen
[EDIT/ENTER]
(-)is the value after the change.
[ ][ ][EDIT/ENTER] NORM 64 STD -0.0 + ON POLARITY + Normal operation mode monitor screen(1)
Figure 4.6 Output Polarity Change
Note: The marker output polarity can also be changed (refer to section 5.7.1).
4.2 Purge valve open/close (Solvent replacement in the reference cell) This section explains the procedures to open and close the purge valve. When the valve is opened during fluid pumping (Screen display: ON), solvent flows to the cells on both the sample and reference side. When the valve is closed (Screen display: OFF), solvent only flows to the sample side. When replacing
Normal operation mode monitor screen NORM 64 STD -0.0 + ON(OFF) TEMP: xx.x/yy °C -0.0 + ON(OFF) [MONIT] PURGE ON 1:ON 0:OFF [PURGE] [1] [0]
:Opens the purge valve and changes the status to ON. Purge valve open/close screen [MONIT]
Current purge valve status
:Closes the purge valve and changes the status to OFF.
Figure 4.7 Purge Valve Open/Close Operations
Note: When using “10 ~ 50mL/min” tubing connections, draw up the mobile phase solvent using a syringe in order to replace solvent in the reference cell. Replacement of solvent in the reference cell can be performed regardless of the PURGE VALVE setting.
4.3 Auto-zero operations
When the [AUTO ZERO] key is pressed, the current refractive index value is set as 0. In other words, the recorder and integrator output are set to 0.
Note: When a signal is input into MARK IN on the back panel, the auto-zero operation can be set to occur automatically. (Refer to section 5.3) Note: When executing optical auto zero, press the [SHIFT][AUTOZERO] key.
monitor screen. If the problem continues, the same message will appear again after approximately 20 seconds. Refer to section 9.1 for countermeasures.
Table 4.3 Error Messages and Their Meanings
Error message Meaning
TROUBLE LEAK IN CELL TROUBLE OVER TEMP
TROUBLE ZERO GLASS DRV WARNING INTENSITY POOR WARNING OUT OF RANGE WARNING LAMP MAINT TIME
Fluid is leaking from the flow cell Heater is overheating
Zero glass drive not move Light intensity has deteriorated
Optical zero adjustment is not correct
Lamp maintenance time has been exceeded
4.5 Measurement of concentrated sample (Refractive index range shifting when the “MEASURE RANGE” setting is STD)
When “MEASURE RANGE” is set to STD, the linear dynamic range of refractive index, with properly adjusted optical zero, is +/-5.0x10-4RIU. Although this range cannot be expanded, it can be shifted in one direction. For example, the allowable refractive index range can be shifted to -3.0x10-4 ~ +7.0x10-4RIU. The method for shifting the range is described below.
(1) Display the preamplified output screen (refer to section 5.2) and press the [ ][ ] keys so that DIFF is within 0±0.03
(2) Return to the monitor screen.
(3) Press the [AUTO ZERO] key to set the RIU value to 0.
(4) Display the preamplified output screen and press the [ ][ ] keys until the RIU value reaches -300.0±30(x10-6RIU) (this assumes the output polarity is set to positive).
(5) Again press the [AUTO ZERO] key to set the RIU value to 0. As long as optical zero adjustment is not executed, the allowable refractive index range will be -3.0x10-4 ~ 7.0x10-4RIU.
range is exceeded, use the recorder output. The refractive index range resulting in proper recorder output is +/-9.9x10-4RIU (with a range setting of 512). However, signal linearity is lowered when above +/- 5.0 X 10-4 RIU.
Note: When the “MEASURE RANGE” is set to WIDE, this refractive index range shifting method is invalid.
5. [SHIFT] Key Operations
5.1 Operation summaryThe operations executed using the [SHIFT] key are summarized in Table 5.1. Table 5.1 [Shift] Key Operations and their Functions
Key operation Function
[SHIFT][1] Preamplified output display (refer to section 5.2).
Used to check for bubbles in the cell and when adjusting optical zero.
[SHIFT][3] Auto-zeroing operation (AUTO and MANUAL) (refer to section 5.3)
AUTO: When a signal is input into MARK IN on the back panel, the autozeroing operation is executed automatically. MANUAL: Auto-zeroing is executed only when the [AUTO ZERO] key is pressed.
[SHIFT][4] Zero point shift for integrator output (refer to section 5.4) The allowable input voltage for the integrator is normally within the range -10mV ~ +1V. The dynamic range on the negative side is therefore small compared to that on the positive side. When the output level is shifted beforehand to the positive side using the zero point shift function, integrator output can be prevented from falling below -10mV.
[SHIFT][5] Lamp operation time (refer to section 5.5) [SHIFT][6] Output polarity change (refer to section 4.1.3) [SHIFT][7] Signal filtering selection (refer to section 5.6) [SHIFT][AUTO
ZERO]
Used to execute optical auto zero
[SHIFT][MARK] Allows the following parameters to be changed. ・”MEASURE RANGE” (refer to chapter 7)
・ Constant K1 (for STD side optics calibration constant) setting (refer to section 9.4.5)
・Marker voltage/polarity change (refer to section 5.7.1) ・ Setting to continue/stop self-diagnostics when an error
occurs (refer to section 5.7.2)
・Serial number setting (refer to section 9.6)
5.2 Preamplified output display ([SHIFT][1])
Preamplified output is used to check for bubbles in the cell and when adjusting optical zero.
Normal operation mode monitor screen NORM 64 STD -0.0 + ON(OFF) [MONIT] DIFF: -0.0200 V (*) SAM : 1.5000 V [SHIFT] [1] [MONIT] TEMP: xx.x/yy °C -0.0 + ON(OFF)
Figure 5.1 Preamplified Output Screen
(1) Checking for bubbles in the cell
The existence of bubbles in the cell is evaluated by monitoring fluctuation of the SUM value. When the third digit after the decimal place is fluctuating, bubbles remain in the cell. When no fluctuation is found, no bubbles are thought to be present. However, final judgement should be made by recording and inspecting the baseline.
For example, when a problem is found with the baseline, check the SUM value. If the value has decreased, it can be assumed that bubbles have been generated. In addition, when the SUM value increases (decreases) while
present, transparency is reduced and the value decreases. If the value falls below 0.1V, the INTENSITY POOR message appears.
(2) Optical zero-adjustment
When “MEASURE RANGE ” is set to STD, be sure to execute optical zero adjustment after solvent replacement. Even when using the same solvent, readjust whenever new solvent is replaced.
Note: When “MEASURE RANGE” is set to WIDE, dynamic measurement range is large. Therefore, the optical zero adjustment function is not equipped in this unit.
(3) Automatic optical zero adjustment
When “MEASURE RANGE ” is set to STD, optical zero can be automatically adjusted by pressing [SHIFT][AUTOZERO]. This key operation causes the DIFF value to fall zero within –0.01xx ~ +0.01xx. When DIFF value is not within –0.01xx ~ +0.01xx, refer to (4) below.
(4) Optical zero adjustment using [ ][ ] keys
When “MEASURE RANGE ” is set to STD, optical zero can also be adjust by [ ][ ] key operations. To increase (decrease) the DIFF value, press [ ] ([ ]) key. Adjustment is satisfactory if the value is within –0.01xx~+0.01xx. When (*) is displayed in the right side of the LCD display, the optical zero adjustment range is limited. In this case, bubbles may exist in the flow cell or replacement of solvent in the flow cell may not be enough.
Note: The value displayed for DIFF is proportional to the difference in the light intensity detected by two photodiodes. The sign of this value may be positive or negative. When the absolute value of DIFF/SUM is greater than 0.8, the instrument will cease to operate normally and the OUT OF RANGE message will appear.
5.3 Auto-zero operation setting ([SHIFT][3])
This setting determines whether or not the auto-zeroing operation will be executed automatically when a marker signal is input into the MARK IN
AUTO
When analyzing samples using an autosampler, the MARK IN signal, input to the detector from the autosampler at the time of sample injection, causes a marker to be overlayed on the chromatogram and auto-zero to be executed. The chromatogram base is therefore set to zero.
MANUAL
Auto-zeroing is not executed when a signal is input into the MARK IN terminal. The auto-zeroing operation is only executed when the [AUTO ZERO] key is pressed.
Note: The [MARK] key function on the front panel causes a marker regardless of this setting.
AUTO ZERO AUTO AUTO ZERO AUTO(MANUAL) Input screen Flashes [MONIT] [SHIFT] [3]
Auto-zero setting screen
[EDIT/ENTER]
(MANUAL)is the setting after the change.
[ ][ ][EDIT/ENTER]
(AUTO or MANUAL can be selected) Normal operation mode monitor screen
NORM 64 STD -0.0 + OFF
TEMP: xx.x/yy °C -0.0 + OFF [MONIT]
Figure 5.2 Setting for Automatic or Manual Auto-zero Execution
Note: The AUTO setting is convenient for analysis, whereas the MANUAL setting is convenient for fractioning.
5.4 Zero point shift for integrator output ([SHIFT][4])
The allowable input voltage range of a current integrator is, in general, -10mV ~ +1V. The dynamic range on the negative side is therefore small compared to that on the positive side. When the output level is shifted beforehand to the
Note 1: The zero point shift setting has no affect on recorder output.
Note 2: The extent of integrator output noise is not changed by the zero point shift setting. However, as the input voltage increases, the signal resolution of the integrator decreases and visible baseline noise increases. Therefore, do not use values that are larger than necessary
(1) Setting of integrator output zero point shift
A. Z POSITION 0 mV A. Z POSITION 0(50)mV Input screen Flashes [MONIT] [SHIFT] [4]
Zero point shift setting screen
[EDIT/ENTER]
(50) is the value after the change
[ ][ ][EDIT/ENTER] Normal operation mode monitor screen
NORM 64 STD -0.0 + OFF
TEMP: xx.x/yy °C -0.0 + OFF [MONIT]
Figure 5.3 Integrator Output Zero Point Shift Setting (2) Example
In t e g r a t o r o u t p u t In t e g r a t o r p r o c e s s i n g n o t p o s s i b l e 0 V - 1 0 m V Z e r o p o i n t s h i ft : 0 m V 0 V Z e r o p o i n t s h i ft : + 5 0 m V In t e g r a t o r o u t p u t
Figure 5.4 Example when Baseline Drifts in Negative Direction
5.5 Lamp operation time ([SHIFT][5])
This function displays the lamp operation time.
LAMP OPERAT . TIME * 3456.7 H
[MONIT] [SHIFT] [5]
Lamp operation time screen Normal operation mode monitor screen
NORM 64 STD -0.0 + OFF
TEMP: xx.x/yy °C -0.0 + OFF [MONIT]
5.6 Signal filtering mode ([SHIFT][7])
The signal filtering method is normally set to “TIME ACCUME”. If a high noise level makes analysis using the “TIME ACCUME” method difficult, switch to the “DIGITAL FILTER” method. Generally, the “DIGITAL FILTER” method decreases noise, but peak shape may be broad. Select the adequate filtering method and response setting in relation to the chromatogram characteristics.
FILTER MODE TIME ACCUME [EDIT/ENTER] Flashes [SHIFT] [7] [MONIT]
Normal operation mode monitor screen NORM 64 STD -0.0 + ON(OFF) TEMP: xx.x/yy °C -0.0 + ON(OFF) [MONIT] FILTER MODE TIME ACCUME [ ][ ][EDIT/ENTER]
(values in parenthesis are after changes)
Figure 5.6 Setting for signal filtering
Note: The digital filtering method is efficient when the full width half maximum value of the peak is wider than 5 seconds. However, when using the digital filtering method, the retention time delay becomes significant. The delay time of a peak for which the full width half maximum value is 10 seconds is described in Table 5.2.
Table 5.2 Retention time delay
Response setting Fast STD SLOW
・ Constant K1 (for STD side optics calibration constant) setting (refer to section 9.4.5)
・ Constant K2 (for WIDE side optics calibration constant) setting (refer to section 9.4.5)
・ Calibration (refer to section 9.4)
・ Lamp maintenance time setting (refer to section 9.5) ・Marker voltage/polarity change (refer to section 5.7.1)
・ Setting to continue/stop self-diagnostics when an error occurs (refer to section 5.7.2)
・Serial number setting (refer to section 9.6)
The calibration constants K1 and K2 must be input when the BACK UP ERROR message appears. Calibration must be performed when a light source, photodiode, or flow cell is replaced. Other items may be input as required. In this section, the marker voltage/polarity change item and the setting to continue/stop self-diagnostics when an error occurs are described. For descriptions of the other items, refer to chapter 9.
When [SHIFT][MARK] is pressed, the “MEASURE RANGE” selection menu screen appears. Press the [ ][ ] keys to scroll between the menu screens as shown in Figure 5.7.
PARAMETER MODE 3:SET K2 VALUE [SHIFT] [MARK] [MONIT] PARAMETER MODE 2:SET K1 VALUE [ ]
Normal operation mode monitor screen NORM 64 STD -0.0 + OFF TEMP: xx.x/yy °C -0.0 + OFF [MONIT] PARAMETER MODE 1:MEASURE RANGE PARAMETER MODE 4:CALIB. K
Measurement range setting menu [ ]
PARAMETER MODE 8:SERIAL NO. PARAMETER MODE 6:MARK OUT MODE PARAMETER MODE 5:L. MAINTE. TIME PARAMETER MODE 7:DIAG. MODE Menu to continue/stop self-diagnostics when an error occurs
Serial number menu Constant K1 setting
Constant K2 setting
K1, K2 Calibration
Lamp maintenance time menu
Marker voltage/polarity menu [ ] [ ] [ ] [ ] [ ] [ ] [ ] [ ] [ ] [ ] [ ] [ ]
Figure 5.7 Other Menus
The procedures required to change the settings outlined in Figure 5.8. Marker voltage input range: 0, 0.5, 1, 2mV
PARAMETER MODE 3:MARK OUT MODE Marker voltage/polarity menu
Voltage input screen MARK OUT MODE
V:(1)2mV P: +(-)
MARK OUT MODE V: 1mV P: +
MARK OUT MODE V: 2mV P: +
Flashes
Polarity input screen (values in parenthesis are
after changes)
Marker voltage/polarity screen [EDIT/ENTER] [EDIT/ENTER] Flashes [MONIT] [SHIFT] [MARK] [MONIT]
Normal operation mode monitor screen
NORM 64 STD -0.0 + ON(OFF) TEMP: xx.x/yy °C -0.0 + ON(OFF) [MONIT] [ ]
(Display the menu below by pressing the key twice)
[ ][ ][EDIT/ENTER]
Figure 5.8 Marker Voltage/Polarity Changes
5.7.2 Setting to continue/stop self-diagnostics when an error occurs This setting is used to determine whether power on self-diagnostics will stop or continue when an error is detected and displayed. The default setting stops self-diagnostics when an error occurs. When diagnostics is set to continue and an error is detected the error message is displayed for 3 seconds then the
Input range: CONFIRM (Stop), SKIP (Continue) [EDIT/ENTER] DIAG MODE CONFIRM(SKIP) [EDIT/ENTER] Flashes [MONIT] PARAMETER MODE 4:DIAG. MODE [SHIFT] [MARK] [MONIT]
Normal operation mode monitor screen NORM 64 STD
-0.0 + ON(OFF)
TEMP: xx.x/yy °C -0.0 + ON(OFF) [MONIT]
Menu to continue/stop self-diagnostics when an error occurs.
[ ]
DIAG MODE CONFIRM [ ][ ][EDIT/ENTER]
(values in parenthesis are after changes) [ ]
(Use the / keys to displaythe menu below)
6. Program
Mode
Operations
6.1 Operation summaryIn program mode the range, response, valve opening and closing, and auto-zero operations can be changed according to a time program. The maximum number of steps in the time program is 64 and the maximum number of program files that can be stored is 10.
The time program operations are described in the following sections.
Switch to program mode Refer to section 6.2 Set file number Refer to section 6.3 Edit initial parameters Refer to section 6.4.1 Edit time program Refer to section 6.4.2
Execute Refer to section 6.5
6.2 Switching between normal operation mode and program mode
Press the [PRGM] key while in the normal operation mode monitor screen. The program mode monitor screen (Figure 6.1) will appear. Press the key again to return to normal mode. The program mode monitor screen consists of three screens. Switch between screens using the [MONIT] key.
[PRGM]
Program mode monitor screen Normal operation mode monitor screen
NORM 64 STD -0.0 + OFF TEMP: xx.x/yy °C -0.0 + OFF [MONIT] PRG2 T:0.0 -0.0 + OFF [MONIT] TEMP: xx.x/yy °C -0.0 + OFF [MONIT] PRG2 64 STD -0.0 + OFF
Figure 6.1 Switching between Normal Operation Mode and Program Mode
The contents of each screen are described in Figure 6.2.
Current time Program mode
(file number 2) Sensitivity
Response
Current refractive index value
Polarity Purge valve
Current heater temperature/setting temperature Temperature control mark
PRG2 T:12.3 -0.0 + OFF [MONIT] TEMP: xx.x/yy°C -0.0 + OFF [MONIT] PRG2 64 STD -0.0 + OFF (12.3 min) (64) (standard)
blinks when heating
(positive) (off)
Figure 6.2 Meanings of Items in the Program Mode Monitor Screen
6.3 File number setting (file loading)
A maximum of 10 files (0 ~ 9) can be stored. The file number can be changed from the normal operation mode or program mode monitor screen using the following operations.
RPOGRAM FILE NO. y
RPOGRAM FILE NO. y(x)
[SHIFT] [PRGM]
[EDIT/ENTER] [x][EDIT/ENTER]
Flashes
File number screen Input screen
(X) is the value after the change [MONIT]
Normal operation
mode monitor screen [PRGM]
Program mode monitor screen
Figure 6.3 File Number Change
Note 1: If an incorrect value is entered accidentally, press the [CLEAR] key before pressing the [EDIT/ENTER] key then enter the value again. Note 2: When a file number already stored in memory is designated, the stored
program will be loaded. After the file number is set and the time program is edited, the file is automatically saved. Since time programs are stored in C-MOS RAM (the memory backed up by battery), they are not erased when the power is turned off.
6.4 Program editing
6.4.1 Initial parameter editing
Range and purge valve open/close (ON/OFF) are set as initial parameters. The setting method is shown in Figure 6.4.
Note: The settings in normal operation mode for response, polarity, and temperature will remain in effect in program mode.
Note: When using a “10 ~ 50mL/min.” tubing arrangement, the solvent replacement in the reference cell is performed by drawing up the mobile phase solvent using a syringe. Solvent replacement is possible
PRG2 INITIAL
R:64(16) PURGE:OFF(ON)
[ ] [ ] [MONIT]
Initial parameter screen
[EDIT/ENTER]
Purge valve
Sensitivity flashes
Purge valve flashes Sensitivity input screen
Purge valve open/close screen Program mode monitor screen
Sensitivity
Note: Values in parentheses are after changes
[EDIT/ENTER][ ][ ] PRG2 T:0.0
-0.0 + OFF
[MONIT] TEMP: xx.x/yy°C
-0.0 + OFF [MONIT] PRG2 64 STD -0.0 + OFF PRG2 INITIAL R:64 PURGE:OFF PRG2 INITIAL R:16 PURGE: OFF [EDIT/ENTER][ ][ ]
Figure 6.4 Initial Parameter Editing
6.4.2 Time program editing 6.4.2.1 Time program input (1) Input example
As an example, a time program will be created with the initial parameters (range: 16, response: STD) held for 1 minute. The range will then be changed to 8 and, after 2 minutes, the response will be changed to FAST.
P2 ST 2 T:0.0 P2 ST 2 T:2.0 RESPONSE STD P2 ST 1 T:1.0 RANGE:16 P2 ST 1 T:1.0 1: PURGE ON P2 ST 1 T:0.0 [ ] [ ] PRG2 ST 1 T:0.0 [EDIT/ENTER] [1][EDIT/ENTER] [RANGE/4][EDIT/ENTER]
(waiting for input) Input 1 minute
(waiting for input) Call up sensitivity
(waiting for input)
Step 1 input complete P2 ST２ T:0.0 [EDIT/ENTER] [2][EDIT/ENTER] [RSPNS/5][EDIT/ENTER]
(waiting for input) Input 2 minutes
(waiting for input) Call up response
(waiting for input) Input FAST Step 2 input complete
Step 1 screen Step 2 screen
[ ]▼ Initial parameter screen
: Shaded values are flashing Time flashes Function flashes Value flashes Time flashes Function flashes Value flashes [EDIT/ENTER][ ][ ] P2 ST 2 T:2.0 RESPONSE FAST PRG2 INITIAL R:16 PURGE:OFF P2 ST 1 T:1.0 RANGE:8 Input 8 P2 ST 2 T:2.0 1: PURGE ON
or [ ]three times [EDIT/ENTER] or [ ] four times [EDIT/ENTER]
[EDIT/ENTER][ ] [ ]
Figure 6.5 Time Program Key Operation Example (2) Time program input method
[xx][EDIT/ENTER] Function will flash next.
d) Input the function. Select a function from Table 6.1. For example [RANGE/4][EDIT/ENTER]
The input function will appear and the value will flash. e) Input a value.
[ ][ ][EDIT/ENTER]
When input is complete, press the [ ] key to move to the next step.
Repeat the operations in steps a) ~ e) to edit the time program. Functions that can be controlled by the time program and the relevant keys for the functions are shown in Table 6.1.
Note: Steps do not have to be input sequentially in respect to time. Even when steps are out of time sequence, they will be rearranged in chronological order once the [MONIT] key is pressed to return to the monitor screen.
Table 6.1 Function Input Keys and Input Range
Function Key Change keys Setting range Purge valve open [P-ON/1]
Purge valve close [P-OFF/2]
Auto-zero [A.ZERO/3]
Range [RANGE/4] [ ][ ] 1/4,1/2,1,2,4,8,16,32,64, 128,256,512,S
Response [RSPNS/5] [ ][ ] FAST, STD, SLOW
[SHIFT][ ]: Moves to the last step in the program [SHIFT][ ]: Moves to the first step in the program
6.4.2.2 Corrections
When time and functions do not agree
1) Use the [ ] key to display the incorrect step. 2) Re-input the step values starting from time.
When only a value, and not time and function, requires changing 1) Use the [ ] key to display the incorrect step.
2) Skip parts that do not require changes by pressing [EDIT/ENTER] until the value input screen is displayed.
3) Change the value.
For example, when changing only the range value, use the operations shown on the left in Figure 6.6. However, when input is corrected starting with time, the function selection screen, shown on the right in the figure, will appear.
P5 ST 3 T:1.0 1: PURGE OFF
[RANGE/4][EDIT/ENTER] Sensitivity call up [1][EDIT/ENTER]
(waiting for input)
(waiting for input)
(Change the value here) Time flashes Function flashes Value flashes [EDIT/ENTER] Time input [EDIT/ENTER] PRG2 ST 3 T:1.0 RANGE : 16 [ ][ ][EDIT/ENTER] PRG2 ST 3 T:1.0 RANGE : 16 PRG2 ST 3 T:1.0 RANGE : 16 PRG2 ST 3 T:1.0 RANGE : 32
Figure 6.6 Correcting a Time Program
6.4.2.3 Deletion Single step deletion
1) Display the step to be deleted using the [ ] key.
2) Set the time in the step to 0 ([EDIT/ENTER][0][EDIT/ENTER]).
3) Press the [MONIT] key to return to the monitor screen. Steps will be rearranged in chronological order and the 0 time step will be deleted.
Deletion of a step and all subsequent steps
3) Press the [MONIT] key to return to the monitor screen.
6.4.2.4 Insertion
1) Display the final step in the program using [SHIFT][ ]. 2) Display a new step using the [ ] key.
3) Follow the procedure described in section 6.4.2.1 and input desired values. 4) Press the [MONIT] key to return to the monitor screen. Steps will be rearranged in chronological order.
6.5 Time program operation 6.5.1 Time program execution
Start the program while the program monitor screen is displayed. (1) Start
After the baseline has stabilized, press the [PRGM RUN] key. The time program will start. The [PRGM RUN] key lamp will light, indicating a time program is in progress.
When the time program reaches the final step, the parameters at that point are maintained and only time advances.
(2) Stop
Press the [PRGM RUN] key during program execution. The [PRGM RUN] key lamp will go out and the time program will stop.
Note: During time program, execution parameters can be freely changed. The changed values will remain in effect until the next setting value is reached in the time program.
(3) Time program execution by external signal
7. MEASURE RANGE Setting
One of the major features of the RI-2031 is that the dynamic measurement range is 10 times wider than an ordinary RI detector. The “MEASURE RANGE” setting is normally set to STD, however when measuring a high concentration sample, “MEASURE RANGE” should be set to WIDE, using the procedure shown in Figure 7.1. The recorder scale and integrator output scale are automatically changed according to the “MEASURE RANGE” setting.
Table 7.1 “MEASURE RANGE” and output scale
“MEASURE RANGE” Dynamic range RANGE Inte. output STD ~ 5x10-4RIU 1/4~512x10-6RIU 5x10-4RIU/1.0V WIDE ~ 5x10-3RIU 1/4~512x10-5RIU 5x10-3RIU/1.0V
Note: The baseline noise and drift when set to WIDE is larger than when set to STD. Set “MEASURE RANGE” to WIDE only when the STD dynamic range makes analysis difficult.
PARAMETER SET 1:MEASURE RANGE [SHIFT] [MARK] [EDIT/ENTER] [MONIT] MEASURE RANGE STD(WIDE) [EDIT/ENTER] NORM 64 STD -0.000 + ON(OFF) TEMP: xx.x/yy °C -0.000 + ON(OFF) [MONIT] MEASURE RANGE STD [MONIT] [ ][ ][EDIT/ENTER] Normal operation mode monitor screen
(WIDE) is the setting after the change. (STD or WIDE can be selected) Flashes
Note: Although signal linearity is reduced gradually when the refractive index value exceeds 5x10-4RIU (“MEASURE RANGE”: STD) or 5x10-3
RIU(“MEAUSRE RANGE”: WIDE), the measurable range is ~ 7x10-4 RIU/1.0V (“MEASURE RANGE”: STD ), and ~ 9.9x10-3RIU/1.0V (“MEASURE RANGE”: WIDE). When exceeding the linear range, connect to the recorder output terminal instead of the integrator output terminal. For example, when the RANGE setting is 128, the
measurable range is 12.8x10-4 RIU/100mV (“MEASURE RANGE”: STD), and 12.8x10-3 RIU/100mV (“MEASURE RANGE”: WIDE).
8. Maximum Flow Rate Changing at the Front Panel
The maximum flow rate depends on the front panel tubing arrangement. The following subsections describe tubing arrangements and the method for replacing solvent in the reference cell.
8.1 “ ~ 10mL/min” tubing arrangement and solvent replacement method for reference cell
Connects ports No.1 and No.2 with outer diameter: 1.6mm, internal diameter:0.8mm tubing and ports No.4 and No.5 with outer diameter:1.6mm, internal diameter:0.8mm tubing. Connect the tubing from the column to port No.6, and connect the tubing for waste to port No.3. To replace solvent in the reference cell, operate purge valve. When replacing the reference cell solvent, set the valve to ON. During analysis, set the valve to OFF. (Refer to section 4.2)
Figure 8.1 “ ~ 10mL/min” tubing arrangement
3
4
2
1 Sample Out (waste)
Sample IN (from column) Tubing
OD=1.6mm ID= 0.8mm
Flow rate: ~ 10mL/min.
8.2 “10 ~ 50mL/min” tubing arrangement and solvent replacement method for reference cell
Connect the tubing from the mobile phase solvent bottle to port No3. Use tubing with an internal diameter of 0.8mm and an outer diameter of 1.6mm. Connect the syringe to port No.6. To replace solvent in the reference cell, draw up mobile phase solvent by pulling the syringe plunger. Make sure the syringe is connected during analysis. Connect the tubing from the column to port No.5, and connect the tubing for waste to port No.2. The refractive index output signal is reversed. Change the Polarity setting. (Refer to section 4.1.3)
Tubing OD=1.6mm, ID=0.8mm
Replace solvent in the reference cell by sucking the mobile phase solvent. Keep the syringe connected during analysis in order to maintain solvent in Tubing
OD=1.6mm ID=0.8mm
(Same tubing as used to connect ports No.1-2 or ports No.4-5. for the
“~10mL/min” tubing arrangement. Tubing OD=1.6mm ID=0.8mm Sample Sample IN ReferenceIN Reference Out 1 Sample Out Sample IN Mobile phase 2 3 4 5 6 1 2 3 4 5 6
9. Maintenance
9.1 Error messages and countermeasures
9.1.1 Errors during self-diagnostics after power on
The self-diagnostics program is automatically executed when the power switch is turned on. The items in Table 9.1 are checked during self-diagnostics. When a problem is found, an error message is displayed on the screen.
When an error message appears, turn the power off, wait 30 seconds, and turn the power on again. If the error message appears again, a problem exists with the instrument and the user should contact your local JASCO distributor.
Note: When the power is turned off then on quickly, a ROM CHECK ERROR or RAM CHECK ERROR may appear.
When an error message appears and self-diagnostics stop, press [SHIFT][ ] to advance to the next item and continue with the self-diagnostics program. When self-diagnostics have been advanced in this way, check that chromatograms (including baselines) are the same as previously obtained results. In particular, when BACK UP ERROR has been skipped in this way, check the following points.
(1) Have the RANGE and other setting values, including Time Program setting, changed?
(2) Have the setting values followed [SHIFT] key operation changed?
(3) Has the K1 value changed to 1.00? (Refer to Figure 9.8 in section 9.4.5)
If setting values have changed or the K1 value has reverted to 1.00, re-input the setting values, turn the power off, wait at least 3 minutes, and turn the power on again. If the re-input values have changed again, the backup battery is dead and the user should contact your local JASCO distributor.
Table 9.1 Self-diagnostics Items and Corresponding Error Messages after Power On
Check item Error message
ROM operation RAM operation C-MOS RAM backup Temperature sensor Zero glass driver Lamp operation time
ROM CHECK ERROR RAM CHECK ERROR BACK UP ERROR TEMP SENSOR NG Z. GLASS ERROR
WARNING LAMP MAINTE. TIME
9.1.2 Self-diagnostics during operation
The instrument checks the following items during operation (Table 9.2). When a problem is detected, an error message is displayed on the screen. Refer to section 9.1.3 for countermeasures.
Table 9.2 Self-diagnostics Items and Corresponding Error Messages
Check item Error message
Fluid leak in cell Heater overheating
Light intensity deterioration Optical zero adjustment Lamp operation time
TROUBLE LEAK IN CELL TROUBLE OVER TEMP WARNING INTENSITY POOR WARNING OUT OF RANGE WARNING LAMP MAINTE TIME
9.1.3 Error message meanings and countermeasures 9.1.3.1 TROUBLE LEAK IN CELL
9.1.3.2 TROUBLE OVER TEMP
This message appears when overheating occurs due to a problem with the temperature control system. The message may also appear when misjudgment happens due to a problem with the temperature detection system. Immediately turn the power off and contact your local JASCO distributor.
9.1.3.3 WARNING INTENSITY POOR
This message appears when the light intensity incident on the photodiodes is insufficient. Specifically, the message appears when the absolute value of the SUM of preamplified outputs falls below 0.1V.
When this message appears, press the [CLEAR] key to clear the message (see note), display the preamplified output screen, and check the SUM value (refer to section 5.2). When the value is smaller than 0.5V, the following problems are possible.
Note: The message will reappear every 20 seconds, until the problem is fixed.
(1) The solvent on the sample side is different from the solvent on the reference side -> Open the purge valve (ON) and pump fluid (refer to section 4.2).
(2) Large bubbles remain in the cell -> Remove the bubbles (refer to section 9.2).
(3) The cell is broken.
When the SUM value is only slightly smaller than normal, the following problems are possible.
(1) Small bubbles remain in the cell -> Remove the bubbles (refer to section 9.2).
(2) The cell is contaminated -> Clean the cell (refer to section 9.3).
value. The following problems are possible when the message appears.
(1) The solvent on the sample side is different from the solvent on the reference side.
(2) Large bubbles remain in the cell -> Remove the bubbles (refer to section 9.2).
(3) Optical zero is not properly adjusted.
When this message appears, press the [CLEAR] key to clear the message (see note), display the preamplifed output screen, and check the DIFF value (refer to section 5.2).
Note: The message will reappear every 20 seconds, until the problem is fixed.
Replace solvent in the reference and sample cell according to the tubing arrangement. (Refer to chapter 8 and section 4.2) Once the DIFF and SUM values in the preamplified output screen have stabilized, press [SHIFT]+[AUTOZERO] key. Adjustment is satisfactory if the DIFF value falls to zero within +/-0.01xx.
9.1.3.5 WARNING LAMP MAINTE TIME
This message appears when the lamp operation time reaches the set maintenance time. Press the [CLEAR] key to clear the message. The instrument may continue to be used.
Note: Refer to section 9.5 for details regarding how to set the lamp maintenance time.
9.2 Flow cell bubble removal
9.2.1 Baselines when bubbles are generated
(1) Irregular noise (Figure 9.1) (2) Increased drift (Figure 9.2)
(3) Irregular ghost peaks (Figure 9.3)
When the above phenomena occur, display the preamplified output screen and check the SUM value (refer to section 5.2). If the third digit after the decimal point of the SUM value is fluctuating, it is possible that bubbles exist in the flow cell. If third digit after the decimal point is within ±1, the bubbles are considered to have been removed.
Characteristics: No periodicity, Reference: Normal noise irregular widths
Figure 9.1 Irregular Noise Caused by Bubbles
Returns to base when bubbles are removed
9.2.2 Bubble removal method 1 (high flow rate fluid pump)
Note: (1) When pumping fluid at a high flow rate, do not connect other detectors to the OUTLET of the RI-2031.
Note: (2) Be sure to connect a line filter to the pump outlet in order to prevent contaminants from entering the flow cell.
When using a “ ~ 10mL/min.” tubing arrangement, connect the pump directly to the RI-2031, then open and close the purge valve (ON/OFF) (refer to section 4.2) while pumping fluid at a high flow rate (up to 10mL/min is possible).
9.2.3 Bubble removal method 2 (syringe fluid injection)
Remove the INLET and OUTLET tubing of the flow cell, connect a syringe to the INLET (or OUTLET), and push solvent in (or pull solvent out).
Note: Do not move the syringe plunger too quickly. For example, if the plunger of a 20mL syringe is depressed for a full stroke in 10 seconds, the internal solvent will be flushed at a rate of 120mL/min. This greatly exceeds the maximum flow rate of the instrument and may damage the flow cell or cause fluid leaks from the electromagnetic valve.
9.2.4 Bubble removal method 3 (covering tubing outlet)
Note: Use a flow rate of 2mL/min or less with this method. If this method is used with a high flow rate, the flow cell may be damaged or fluid leaks may occur from the electromagnetic valve.
Repeatedly cover (for 2 seconds at most) and release the outlet of the OUTLET tubing. When the solvent being used is dangerous to touch, repeatedly pinch (for 2 seconds at most) and release the OUTLET tubing (Teflon tube).
(1) Use a degasser.
(2) Sufficiently check for clogs in the pump inlet filter. When the inlet filter is clogged, bubbles easily enter the flow cell.
(3) Place the waste fluid bottle in a position higher than the instrument.
9.3 Flow cell cleaning method
Note1: Reversing the fluid flow direction is prohibited. Be sure to pump fluid into port No.6.
Note2: Be sure to place a line filter between the pump and the instrument. Note3: When the inlet filter of the pump is clogged, bubbles may be
introduced. This is particularly troublesome when pumping nitric acid and aqueous solutions.
When contaminants adhered to the internal cell wall are known, flush with a solvent that will dissolve the contaminants. Solvents other than the mobile phase solvent are effective.
When contaminants adhered to the internal cell wall are unknown, flush with the following solvents. Use the pump for cleaning and pump fluid at a high rate for at least 12 hours. Prepare 200mL or more of the solvents and recycle the solvents.
(1) When the mobile phase solvent is aqueous, wash with nitric acid.
(2) When the mobile phase solvent is organic, wash with THF (tetrahydrofurane).