Operation Manual RI 2031aa

March 27, 2018 | Author: athanasiosm | Category: Electromagnetic Compatibility, Electromagnetic Interference, Electrical Engineering, Electromagnetism, Technology
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MODEL RI-2031INTELLIGENT 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. i (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 Figure 1 (P/N: 0822-0163A) Figure of the side view ii 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 radio 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 Statement Commission Radio Frequency Interference 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 Before using the instrument. and make sure that the contents are fully understood. iv . When not using the instrument. and to serve as a reference for experienced users.Preface This instruction manual serves as a guidebook for using this instrument. please read this instruction manual carefully. It is intended to instruct first-time users on how to properly use the instrument. Should this instruction manual be lost. order a replacement from your local JASCO distributor. This manual should be easily accessible to the operator at all times during instrument operation. keep this manual stored in a safe place. v . (4) Operate the instrument under a humidity range of 35 ∼ 85% (RH). If ambient humidity exceeds 85% (RH). (8) Avoid dust and corrosive gas. especially in locations exposed to outside air or ventilation outlets that discharge dust particles. the following recommendations should be observed: (1) Do not operate the instrument under voltage fluctuations exceeding 10% of the recommended line voltage. (2) Use a three-pronged electrical outlet with a ground. water vapor may deteriorate optical components. When only a two-pronged socket is available. (6) Avoid strong magnetic fields and sources of high-frequency waves. (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. use an adapter and be sure to connect the ground wire of the adapter. as such a location may inhibit stable measurement. processing equipment and machine tools. Large fluctuations may cause the instrument to fail. install the instrument in a location having a humidity of 60% or lower. (7) Avoid vibrations caused by vacuum pumps. If possible. (5) Operate the instrument under an atmospheric pressure of 750 ∼ 1060 hPa. The instrument may not function properly when near strong magnetic fields or high-frequency wave sources.Installation Conditions To ensure safe operation. Do not install the instrument in a location where it may be exposed to dust. Note: The above conditions do not ensure optimal performance of this instrument. (3) Operate the instrument under a temperature range of 10 ∼ 30°C. electric motors. (9) Do not install the instrument in a location where it may be exposed to direct sunlight. for any consequential damage incurred as a result of product use. In addition. instrument model name and its serial number. vi . (6) Company and product names listed herein are trademarks or registered trademarks of their respective owner. Notices (1) Jasco shall not be held liable. either directly or indirectly. Replacement parts can be ordered according to part number from your local JASCO distributor. (2) Software prohibitions: y Copying of software or related materials for purposes other than backup is prohibited.Maintenance Consult your local JASCO distributor regarding maintenance. is strictly prohibited. When the part number is not known. (5) This manual shall not be used to guarantee or copyright industrial rights or other rights. y Modification of Jasco software is prohibited. inform your local JASCO distributor of the part name. y Use of Jasco software on multiple workstations or terminals. y Disclosure of confidential information related to Jasco software is prohibited. through a network or through any other means. contact your local JASCO distributor when transporting the instrument. (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. y Transfer or authorization of the use of Jasco software to or by a third party is prohibited. In addition. This warranty does not apply to defects as a result of the following: (1) USE FOLLOWING IMPROPER OR INADEQUATE INSTALLATION. JASCO will repair or replace the defective part(s) or product free of charge. Jasco Corporation vii . OR REPAIR BY PERSONS OTHER THAN AUTHORIZED JASCO PERSONNEL. (2) IMPROPER OPERATION. (5) INORDINATELY RAPID DETERIORATION DUE TO THE USE OF CORROSIVE SOLVENTS OR SAMPLES. (3) MOVEMENT. WATER DAMAGE. The warranty period for all parts and repairs supplied under this warranty expires with the warranty period of the original product. MODIFICATION. 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. OR EARTHQUAKES.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. (6) NATURAL DISASTERS SUCH AS FIRES. (4) USE OF PARTS OTHER THAN THOSE THAT ARE AUTHORIZED BY JASCO. viii . .........................1 Parameter changes.............ix 1.......................iv Installation Conditions ..............12 4.............................. 17 4..................................... Power On/Off and Self-diagnostics.................................................................................... 18 4.....v Maintenance ........ Part Names and Functions ......................... 12 4...............................................................................................................................................3 Output polarity change method ([SHIFT][6]) .........................................................1..................1 Range and response changes.....................................Table of Contents Safety Considerations .... 10 3.............................................................................i Regulatory Statements ...........................................................1 1...... 11 4.............................. 12 4........................................10 3..............1........................... 7 2........... 15 4...............3 Back panel......................... 18 ix .............................................................................................1 Front panel ... 1 1............................................2 Power off ............... 2 2............................. 15 4.......................................iii Preface................... Outline and Specifications...............2 Purge valve open/close (Solvent replacement in the reference cell) .............................................4 2.....................2 Temperature control ON/OFF and temperature setting ............................................................................... Operations in Normal Operation Mode ......1 Outline .............................................................................................................................................3 Auto-zero operations..................................2 Operation panel .............................................................................................................4 Error and warning messages during monitoring............. 8 3.....................2 Specifications ..vii Table of Contents...........................................vi Warranty ......1 Power on and self-diagnostics ...............................................1........................................................ 4 2...... ...... Maximum Flow Rate Changing at the Front Panel.... 19 5............ 32 6............................................................................. 33 6......... 27 5..............................7.............................4..................5 Time program operation................................................................................ 24 5..........5 Measurement of concentrated sample (Refractive index range shifting..........................................2 Preamplified output display ([SHIFT][1]) .......................................................................................................................... 44 x .................................................1 Time program execution.3 File number setting (file loading) ....................................... 40 6.........................2 Time program editing...............................................21 5.................................... 22 5........................................41 8.................7 Other settings ([SHIFT][MARK]) ................6 Signal filtering mode ([SHIFT][7]) .................................... 35 6.......1 “ ~ 10mL/min” tubing arrangement and solvent replacement method for reference cell...........................1 Operation summary..................1 Marker voltage/polarity changes...2 “10 ~ 50mL/min” tubing arrangement and solvent replacement method for reference cell....................... 27 5........................4...............................7.........................3 Auto-zero operation setting ([SHIFT][3])....................................... 29 5............................ 34 6..43 8.... 26 5................4 Zero point shift for integrator output ([SHIFT][4])........ 43 8............................................. 30 6........................................................1 Initial parameter editing ...........2 Switching between normal operation mode and program mode .... 40 7.......4 Program editing .............2 Setting to continue/stop self-diagnostics when an error occurs . Program Mode Operations.............................................................................................................................. [SHIFT] Key Operations ..................5....................4.. 23 5............... 34 6....................32 6.......... MEASURE RANGE Setting............5 Lamp operation time ([SHIFT][5]) .......... 21 5......... 32 6..............1 Operation summary.............................................. ......1...........................1.. 65 10............... 54 9..... 62 10......................................4 Calibration method ............... 58 9.....1 Baselines when bubbles are generated .............. 50 9.........7 Power Fuse replacement................2... 51 9.....................4............................. 46 9..................4............... 50 9.......................................1 Operation theory of deflection differential refractometers ..................................................................9........................................... 45 9.......... 48 9....................................................................................5 Internal volume of tubing.4.....................3 Replacement of tubing system solvent with water....................................... 48 9... 54 9............ 53 9...................... 66 10....1 Tubing ..............2 Self-diagnostics during operation ............1.........1.. 52 9..........................................4.............4............. 62 10...3 Error message meanings and countermeasures......................... 50 9...1..........................................62 10..........................................2...................................... 50 9.......................................... 59 9... 46 9................5 Bubble prevention method .....................................2........4.......6 Alternative calibration method .3 Flow cell cleaning method .....1 Operation Theory ..........................2 Flow cell bubble removal ...........4 Calibration method....................................................... Maintenance................................... 53 9.. 63 10. 68 xi ........................2 Optical system ..1. 56 9............3 Bubble removal method 2 (syringe fluid injection) ......3 Signal processing method...........................................................1 Errors during self-diagnostics after power on................45 9..........................................................................2 Bubble removal method 1 (high flow rate fluid pump)...2 Standard solution ....................2.......5 Lamp maintenance time setting ......................1.....4 Bubble removal method 3 (covering tubing outlet)............................. Appendix ......6 Serial number setting ...2........1.....................................1 Error messages and countermeasures................................. 45 9.................4 Flow line ...... 57 9..........5 Calibration constant confirmation and setting ............... 60 10.......................................................................................... xii . 1 . an efficient thermal exchanger.1. Self-diagnostics results and warning messages are also displayed. Maximum flow rate of 50mL/min. response and other functions. Maximum flow rate is 50mL/min. When a leak from the flow cell occurs. Wide dynamic range 10 times larger dynamic range than an ordinary HPLC refractive index detector. which allows the condition of the instrument to be accurately monitored. Easy operation Parameters can be easily set using the LCD display. Automatic analysis capability The internal time program allows automatic switching of sensitivity range. UV detector). performance. and a digital signal processing system. Outline and Specifications 1. a signal is output and the pump can be stopped. Using LC-Net. 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. function keys. Optical Zero can be performed precisely using the easy key operation. parameters can be set from the Model HSS-2000 System without an interface. and numeric keys. which facilitates a neat stacking arrangement. Safety measures An internal fluid leak sensor is installed. (Solvent: H2O) Wide dynamic range and Extended Maximum flow rate are applied to the semi-preparation. Compact design The front panel dimensions are the same as other JASCO 2000 series HPLC equipment (pump.1 Outline The JASCO RI-2031 Intelligent Refractive Index Detector is an HPLC detector which offers unprecedented versatility. Flow stopped Cell capacity: 10µL Maximum usable flow rate: 10mL/min. 1. (“10 ~ 50mL/min. (“ ~ 10mL/min. 2.” tubing) 50mL/min.2 Specifications Model name: RI-2031 Intelligent Refractive Index Detector Measurement system: Deflection type Refractive index range: 1.00 ~ 1. 16.0 x 10-3 RIU (“MEASURE RANGE”: WIDE) <Condition> H2O Noise: 0. 512 x 10-6RIU/full scale (“MEASURE RANGE”: STD) 1/4. 8.75 Measurement range settings: 1/4.” tubing) Temperature control: PID control by heater. 32. 16.1MPa. 256. 32. 64.2 x 10-8RIU <Condition> H2O. 2. 1/2. 1/2. Integrator output zero positioning Reference selection: Electromagnetic valve control (“ ~ 10mL/min.0 x 10-4 RIU (“MEASURE RANGE”: STD) 5. 256. Control range: Room temperature +10°C ~ Room temperature +25°C Zero adjustment: Automatic Optical and electronic auto-zero functions. 128.1. 64. Setting range: 0 ~ 45°C in 1°C increments. 1. 128.” tubing) 2 . 4. (“ ~ 10mL/min.” tubing) 0. (“10 ~ 50mL/min.3MPa. 4.” tubing) <Solvent> H2O Maximum pressure: 0. 8. 512 x 10-5RIU/full scale (“MEASURE RANGE”: WIDE) Linearity: 5. Range from 0. 50VA max. 50/60Hz.0 x 10-3RIU/1V(WIDE) Marker and leak output: Marker. AUTO ZERO.0 x 10-4RIU/1V(SID) 5.9min.1 to 999. SLOW (TIME ACCUME.Time program: Parameters that can be set are PURGE ON/OFF. STD. 3 . Response FAST. excluding Protrusions. and RESPONSE. Approximately 13kg Power requirements: AC100 ~ 240V. RANGE. fluoride resin. Ambient temperature: +10 ~ +35°C for operation -30 ~ +60°C for storage * Specifications are subject to change without notice. DIGITAL FICTER) Input and output signals: Recorder output: 10mV/FS Integrator output: 5. program circuit each LC-Net control: Liquid wetted material: 1 circuit each reset/start: 1 1 circuit Quartz. stainless steel (SUS316) Dimensions and weight: 150(W) x 470(D) x 150(H) mm. auto-zero. AC. parameter edit keys. and LCD display showing operating conditions. and Figure 2. “ ~ 10mL/min”.1 Front panel Operation Panel Solvent Inlet and Outlet POWER Switch Figure 2. refer to Figure 2. Part Names and Functions 2.3.1 Front Panel Name Solvent Inlet Outlet “1” ~ “6” Operation panel POWER switch Note: Function and Sample and Reference In and out connections Refer to Figure 2. Before connecting tubing. tubing is supplied with the instrument.2 and Figure 2. 4 .3.2.2. Panel containing control keys. Refer to Section 4 and 5. parameters and various messages. Power switch for the instrument Suitable tubing for the Solvent Inlet and Outlet connections must be selected according to maximum flow rate. (Refer to 4.6mm ID= 0.1.8mm Sample IN (from column) Figure 2.) Tubing with 1 2 3 4 5 6 Sample Out (waste) Flow rate: ~ 10mL/min. Change the polarity setting from plus (+) to minus (-) using the polarity setting function. OD=1.2 “ ~ 10mL/min” flow rate tubing connections 5 .3 polarity setting.Note: For a “10 ~ 50mL/min” tubing arrangement. the refractive index signal output (and display) polarity becomes negative. No. Keep the syringe connected during analysis in order to maintain solvent in the reference cell and to facilitate solvent replacement. Sample IN Reference Out Tubing OD=1.4-5.6mm Mobile phase ID=0.8mm 1 2 3 4 5 6 (Same tubing as used to connect ports No.6mm. for the “ ~ 10mL/min” tubing arrangement. Figure 2.8mm Flow rate: Sample IN 10 ~ 50mL/min.1-2 or ports Flow rate: 10 ~ 50mL/min.Sample Out Reference IN Tubing OD=1.3 “10 ~ 50mL/min” flow rate tubing connections 6 .8mm Sample Out 1 2 3 4 5 6 Tubing OD=1. ID=0. Replace solvent in the reference cell by sucking the mobile phase solvent.6mm ID=0. [.4.2 for details. In other words.2.2 Operation panel Figure 2. Used to edit parameters and change screens. The letters on these keys describe the special functions. setting values. Operation status is indicated by the lamp to the upper left of the button. Refer to sections 4. Used to edit parameters. Used in combination with other keys to set parameters that are not frequently changed. The lamp is lit during program operation. Numeric keys. Used to return to the monitor screen from other screens and to switch between monitor screens. Used to erase incorrect parameter input and clear error messages.] [ ][ ] keys [CLEAR] [EDIT/ENTER] Function Displays operation conditions.1 and 6. Used to start and stop the time program. Sets the refractive index unit value (RIU) to zero.1. 7 . when editing parameters. these keys are used to call up the relevant functions. Keys 1 ~ 5 are used for special functions in addition to their numeric function.4 Operation Panel Name LCD screen [PRGM RUN] [AUTO ZERO] [MARK] [MONIT] [SHIFT] [PURGE] [PRGM] [0] ~ [9]. Switches between normal and time program mode. Executes solvent replacement (ON/OFF) for the reference cell. error messages and other information. Outputs a marker signal from the recorder output terminal. 2.3 Back panel Input/Output Terminals LC-Net Connectors RS-232C Terminal Fuses AC input Ground Terminal Figure 2.5 Back Panel 8 . 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. Protects the instrument from excessive currents. 5x10-3RIU/1V(“MEASURE RANGE”: WIDE). contact type output is closed when [MARK] key is pressed or MARK IN is input) Fluid leak warning output terminal (Normally open. 9 . Used when controlling the instrument via a RS-232C cable (optional). Grounds the instrument.Name 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+ GNDPRGM RST/ST+ GNDCooling fan AC input Power fuses Ground terminal LC-Net connector RS-232C terminal Function Recorder output terminal (Output level determined by RANGE setting) Integrator output terminal (Fixed scale of 5x10-4RIU/1V(“MEASURE RANGE”: STD). 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. This is not the ground terminal for input and output signals. Marker output terminal (Normally open. Input and output terminal for the LC-Net. Note: When an error occurs. When the [MONIT] key is pressed again. Power On/Off and Self-diagnostics 3. The heater temperature is displayed in the screen on the right. 10 . 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. The self-diagnostics program is automatically executed.P TIME (Lamp operating time) ZERO GLASS DRV. Press the [MONIT] key to switch to the screen on the right in Figure 3. (Optical zero glass driver) An error message will appear if a problem is detected.1 Power on and self-diagnostics Turn the power switch.7.1.3. diagnostics will either stop immediately or continue to the next item depending on the instrument settings (refer to section 5. located at the lower left of the front panel. The screen on the left in Figure 3. to the ON position.1 will appear when diagnostic tests are complete.2). the display will return to the screen on the left. Normal operation mode consists of these two screens. 11 . response.1) Current Optical bench temperature/setting temperature -6 + ON Temperature control mark blinks when heating ) POLARITY PURGE Purge valve status (ON) Normal operation mode monitor screen(1) Normal operation mode monitor screen(2) Figure 3. to the OFF position. The range.1 ON RIU(x10 RIU(x10 ) POLARITY PURGE Current refractive index (-0. temperature.2 Power off Turn the power switch.x/yy °C -0.Response (standard) Sensitivity Mode display (Normal operation mode) (64) MODE RANGE NORM -0.1 Normal Operation Mode Screens 3. located at the lower left of the front panel. polarity. and time program set at this time will be recorded in C-MOS RAM (memory backed up by battery).1 64 + MODE RESPONSE STD [MONIT] -6 Polarity (Positive) RANGE RESPONSE TEMP: xx. These values will be restored when the power is turned on again. x/yy °C RIU(x10 RIU(x10 ) POLARITY PURGE Polarity (Positive) RANGE -0.4. The dynamic measurement range of the RI-2031 depends on the “MEASURE RANGE” setting.1) Current optical bench temperature/setting temperature -6 + ON Temperature control mark blinks when heating ) POLARITY PURGE Purge valve status (ON) Normal operation mode monitor screen(1) Normal operation mode monitor screen(2) Figure 4.1 Range and response changes After the power is turned on and the self-diagnostic tests are complete. Response (standard) Mode display Sensitivity (Normal operation mode) (64) MODE RANGE NORM -0.1 ON -6 Current refractive index (-0. The maximum flow rate of the RI-2031 depends on the tubing connections of the front cell panel.1.1 Normal Operation Mode Screens 12 . the normal operation mode monitor screen (1) (left in Figure 4. Tubing connection configurations are described in section 8. Note: Use the [MONIT] key to switch between monitor screens. Operations in Normal Operation Mode The dynamic measurement range of the RI-2031 is 10 times larger than ordinary HPLC refractive index detectors.1) will appear. Refer to section 7. When a highly concentrated sample is analyzed.1 64 + RESPONSE STD MODE [MONIT] RESPONSE TEMP: xx.1 Parameter changes 4. Range and response settings can be changed here. The “ ~ 10mL/min. set the “MEASURE RANGE” to WIDE. 4.” tubing connections are for conventional analysis and the “10 ~ 50mL/min” tubing connections are for semi-preparative analysis. -0. press the [CLEAR] key before pressing the [EDIT/ENTER] key then enter the value again. 256. SLOW (1) Change method 1 NORM 64(16) STD(FAST) Normal operation mode monitor screen(1) Values in parentheses are after changes. 256. 8.2 Change Method (1) Note: If an incorrect value is entered accidentally. 128. 32. 1/2. 13 . 64.000 NORM -0. Change method 2 When the [RANGE/4] (range) key or the [RSPNS/5] (response) key are pressed. 1/2. STD. 4.000 [EDIT/ENTER] 64 STD + ON Flashes Sensitivity input screen [ ][EDIT/ENTER] Display the desired value Flashes STD Response rate input screen ON [ ][ 16 + ][ ][EDIT/ENTER] Display the desired value Figure 4. 4. 1.000 + ON [MONIT] NORM -0. S (Short) x10-6RIU /10mV (“MEASURE RANGE”: STD) 1/4.Input range: 1/4. the corresponding parameter will flash and the value can be changed directly. 512. S (Short) x10-5RIU /10mV (“MEASURE RANGE”: WIDE) Response input range: FAST. 64. 16. 2. 8. 2. 512. 16. 128. 32. 1. 000 + -0.3 Change Method (2) 14 ][EDIT/ENTER] .000 64 STD + ON Response flashes NORM -0.NORM 64(16) STD NORM 64 STD(FAST) -0.000 + ON [RANGE/4] [ ][ ][EDIT/ENTER] ON [ [RSPNS/5] ][ Sensitivity flashes NORM -0.000 Sensitivity change 64 STD + ON Response change Figure 4. 1) is displayed. 15 .” tubing arrangement When “10 ~ 50mL/min. the refractive index signal output decreases when the actual refractive index increases.” tubing is used.4. temperature control can be turned ON/OFF and temperature can be set as shown the operations in Figure 4. Therefore. the mark at the top right of the monitor screen will blink. 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 belong to stop moving.x/yy °C -0.3 Output polarity change method ([SHIFT][6]) This operation changes the output polarity of the signal.1 “10 ~ 50mL/min.0 + [MONIT] ON [EDIT/ENTER] TEMP: xx.x/yy(zz) °C -0. the polarity should be set to negative (-) in order to correct the relation between the actual refractive index and the refractive index signal output (for both the recorder and the integrator). 4. + ON Flashes Temperature input screen [zz][EDIT/ENTER] Values input Note:Temperature control will be turned off when 0 is input Figure 4.” tubing is used.1. because of the optical arrangement.1. or negative peak heights exceed the integrator input range.4. When 0 is set (control OFF). When “10 ~ 50mL/min. TEMP: xx. Blinking speed is related to heater power.2 Temperature control ON/OFF and temperature setting When the normal operation monitor screen (2) (right in Figure 4.1.0 Normal operation mode monitor screen(2) Values in parentheses are after changes.4 Temperature Control ON/OFF and Temperature Setting 4.3. polarity should be set to negative (-). the index (RIU) value on the screen will increase and so will output.0×10 ~+5. polarity should be set to positive (+). according to these tables.1.” tubing connections) 4.2 “10 ~ 50mL/min.” tubing arrangement (*shifted by 100mV) MEASURE RANGE polarity STD + STD - WIDE + WIDE - without zero point shift* -6 -4 -4 -6 -5 -3 -3 -5 -5.0×10 ~+4. in general.5.0×10 -5.5×10 -4.4. When the actual refractive index decreases.0×10 -5. integrator output can be prevented from falling below –10mV using the zero point shift function.0×10 ~+5.” tubing arrangement (*shifted by 100mV) MEASURE RANGE polarity STD STD WIDE WIDE + + without zero point shift* -6 -4 -4 -6 -5 -3 -3 -5 -5.6.5×10 ~+5.5×10 -4. 16 . Table 4.5×10 -4.0×10 ~+5.0×10 ~+5.0×10 ~+4. When the negative peak signal is within 5x10-5 RIU (“MEASURE RANGE”: STD) or 5x10-4 RIU (“MEASURE RANGE”: WIDE).When the actual negative peak signal exceeds -5.5 and key operations are shown in Figure 4. Refer to section 5.5×10 ~+5.5×10 ~+5. Changes in peak appearance and display values caused by polarity differences are shown in Figure 4.2 Negative peak signal exceeds the integrator input range The allowable input voltage range of a current integrator is. Change polarity settings.0×10 RIU RIU RIU RIU with zero point shift* -5 -4 RIU -4 -5 RIU -4 -3 RIU -3 -4 RIU -5. Refer to Table 4.3.0×10 -5.0×10 When polarity is set to negative (-) with a “ ~ 10mL/min” tubing arrangement.0×10 -5.0×10 ~+4.0×10 ~+5. -10mV ~ +1V.0×10 Table 4.0×10 -5.2.1 “ ~ 10mL/min.5×10 -4.1 and Table 4.0×10 ~+5.0×10 ~+5.0×10 -5.2 (“10 ~ 50mL/min.0×10 ~+5.0×10 RIU RIU RIU RIU with zero point shift* -5 -4 RIU -4 -5 RIU -4 -3 RIU -3 -4 RIU -5. the screen display and output (for both the recorder and the integrator) will change as shown in Figure 4.0x10-4RIU.0×10 ~+4.5×10 ~+5. polarity should be changed. The actual allowable refractive index range is shown in Table 4.0×10 -5. When the negative peak signal exceeds this range.0×10 -5. Close the valve during analysis.0 64 STD + ON Normal operation mode monitor screen(1) [SHIFT] [5] [MONIT] POLARITY [EDIT/ENTER] +(-) POLARITY + [ ][ ][EDIT/ENTER] (-)is the value after the change. 4.0 0 0 0 RIU:-10.7. The operations are shown in Figure 4.0 Actual refractive index change Polarity:Positive Polarity:Negative Figure 4.1). Flashes Output polarity change screen Input screen Figure 4.0 ＋ RIU:10.RIU:20.0 − RIU:-20. When the valve is opened during fluid pumping (Screen display: ON). When the valve is closed (Screen display: OFF).5 Changes in Peak Appearance and Display Values Caused by Polarity Differences NORM -0. When replacing solvent or removing air bubbles in the flow cell.7.6 Output Polarity Change Note: The marker output polarity can also be changed (refer to section 5. solvent flows to the cells on both the sample and reference side. 17 . solvent only flows to the sample side. open the valve to pass solvent through the reference cell.2 Purge valve open/close (Solvent replacement in the reference cell) This section explains the procedures to open and close the purge valve. (Refer to section 5. Replacement of solvent in the reference cell can be performed regardless of the PURGE VALVE setting. press the [CLEAR] key to return to the 18 .3 Auto-zero operations When the [AUTO ZERO] key is pressed.Normal operation mode monitor screen NORM -0.3.x/yy °C -0. (Refer to section 5. draw up the mobile phase solvent using a syringe in order to replace solvent in the reference cell. press the [SHIFT][AUTOZERO] key. the auto-zero operation can be set to occur automatically. Note: When a signal is input into MARK IN on the back panel. Figure 4.2) 4. the current refractive index value is set as 0. the recorder and integrator output are set to 0. [0] :Closes the purge valve and changes the status to OFF.7 Purge Valve Open/Close Operations Note: When using “10 ~ 50mL/min” tubing connections.0 64 STD [MONIT] TEMP: xx. When an error message is displayed. 4.3) Note: When executing optical auto zero.0 + ON(OFF) + ON(OFF) [MONIT] PURGE 1:ON [PURGE] ON 0:OFF Current purge valve status Purge valve open/close screen [1] :Opens the purge valve and changes the status to ON. In other words.4 Error and warning messages during monitoring The error and warning messages that may occur during monitoring are shown in Table 4. with properly adjusted optical zero. the linear dynamic range of refractive index. If the problem continues.3 Error Messages and Their Meanings Error message Meaning TROUBLE LEAK IN CELL Fluid is leaking from the flow cell TROUBLE OVER TEMP Heater is overheating TROUBLE ZERO GLASS DRV Zero glass drive not move WARNING INTENSITY POOR Light intensity has deteriorated WARNING OUT OF RANGE Optical zero adjustment is not correct WARNING LAMP MAINT TIME 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. it can be shifted in one direction.0x10-4RIU.03 (2) Return to the monitor screen. the allowable refractive index range can be shifted to -3.0x10-4RIU. (3) Press the [AUTO ZERO] key to set the RIU value to 0. (5) Again press the [AUTO ZERO] key to set the RIU value to 0.0±30(x10-6RIU) (this assumes the output polarity is set to positive). the same message will appear again after approximately 20 seconds. Refer to section 9. For example. (1) Display the preamplified output screen (refer to section 5.2) and press the [ ][ ] keys so that DIFF is within 0±0. When this 19 . is +/-5. (4) Display the preamplified output screen and press the [ ][ ] keys until the RIU value reaches -300.0x10-4RIU.0x10-4 ~ +7. taking into consideration the polarity setting. Table 4.0x10-4RIU.1 for countermeasures. Although this range cannot be expanded. As long as optical zero adjustment is not executed.monitor screen. the allowable refractive index range will be -3.0x10-4 ~ 7. Note: The refractive index range resulting in proper integrator output is +/-5. The method for shifting the range is described below. 20 .9x10-4RIU (with a range setting of 512). signal linearity is lowered when above +/. However.5.0 X 10-4 RIU.range is exceeded. this refractive index range shifting method is invalid. Note: When the “MEASURE RANGE” is set to WIDE. use the recorder output. The refractive index range resulting in proper recorder output is +/-9. 5. integrator output can be prevented from falling below -10mV.3) AUTO: When a signal is input into MARK IN on the back panel.4.1. When the output level is shifted beforehand to the positive side using the zero point shift function.5) ・ Constant K2 (for WIDE side optics calibration constant) setting (refer to section 9. MANUAL: Auto-zeroing is executed only when the [AUTO ZERO] key is pressed.5) ・ Calibration (refer to section 9.5) 21 . Table 5.6) [SHIFT][AUTO ZERO] Used to execute optical auto zero [SHIFT][MARK] Allows the following parameters to be changed. Used to check for bubbles in the cell and when adjusting optical zero.1.4) The allowable input voltage for the integrator is normally within the range -10mV ~ +1V.2).5) [SHIFT][6] Output polarity change (refer to section 4. [SHIFT][5] Lamp operation time (refer to section 5.4. [SHIFT][4] Zero point shift for integrator output (refer to section 5. The dynamic range on the negative side is therefore small compared to that on the positive side.3) [SHIFT][7] Signal filtering selection (refer to section 5. the autozeroing operation is executed automatically.1 Operation summary The operations executed using the [SHIFT] key are summarized in Table 5. [SHIFT][3] Auto-zeroing operation (AUTO and MANUAL) (refer to section 5. ・”MEASURE RANGE” (refer to chapter 7) ・ Constant K1 (for STD side optics calibration constant) setting (refer to section 9.1 [Shift] Key Operations and their Functions Key operation Function [SHIFT][1] Preamplified output display (refer to section 5. [SHIFT] Key Operations 5.4) ・ Lamp maintenance time setting (refer to 9. 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. check the SUM value.1) ・ Setting to continue/stop self-diagnostics when an error occurs (refer to section 5.7.2) ・Serial number setting (refer to section 9. Therefore. If bubbles are 22 . When the third digit after the decimal place is fluctuating. When no fluctuation is found. no bubbles are thought to be present. However. final judgement should be made by recording and inspecting the baseline. If the value has decreased. it can be assumed that bubbles have been generated. bubbles are being eliminated (generated).2 Preamplified output display ([SHIFT][1]) Preamplified output is used to check for bubbles in the cell and when adjusting optical zero.0200 V (*) SAM : 1. For example. when a problem is found with the baseline. In addition.5000 V Figure 5.6) 5. when the SUM value increases (decreases) while pumping solvent.0 + ON(OFF) [SHIFT] [1] [MONIT] DIFF: -0. bubbles remain in the cell.x/yy °C -0.7. Normal operation mode monitor screen NORM -0. Note: The SUM value is proportional to the total light intensity detected by two photodiodes installed in the instrument.・Marker voltage/polarity change (refer to section 5.0 64 [MONIT] STD + ON(OFF) TEMP: xx. the greatest value is restored when the cells are free of bubbles. 01xx ~ +0. When DIFF value is not within –0. To increase (decrease) the DIFF value. the optical zero adjustment range is limited.01xx ~ +0.8. the INTENSITY POOR message appears. Note: The value displayed for DIFF is proportional to the difference in the light intensity detected by two photodiodes. (3) Automatic optical zero adjustment When “MEASURE RANGE ” is set to STD. This key operation causes the DIFF value to fall zero within –0. 23 . If the value falls below 0. Note: When “MEASURE RANGE” is set to WIDE. When (*) is displayed in the right side of the LCD display. Adjustment is satisfactory if the value is within –0. transparency is reduced and the value decreases. refer to (4) below. optical zero can be automatically adjusted by pressing [SHIFT][AUTOZERO].1V.01xx.01xx. bubbles may exist in the flow cell or replacement of solvent in the flow cell may not be enough. be sure to execute optical zero adjustment after solvent replacement.01xx~+0. (2) Optical zero-adjustment When “MEASURE RANGE ” is set to STD.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 terminal on the back panel.present. readjust whenever new solvent is replaced. Even when using the same solvent. optical zero can also be adjust by [ ][ ] key operations. press [ ] ([ ]) key. When the absolute value of DIFF/SUM is greater than 0. the optical zero adjustment function is not equipped in this unit. dynamic measurement range is large. The sign of this value may be positive or negative. Therefore. In this case. the instrument will cease to operate normally and the OUT OF RANGE message will appear.01xx. 5. (4) Optical zero adjustment using [ ][ ] keys When “MEASURE RANGE ” is set to STD. 4 Zero point shift for integrator output ([SHIFT][4]) The allowable input voltage range of a current integrator is. When [AUTO ZERO] is operating or when a signal is input into A/Z IN on the back panel. causes a marker to be overlayed on the chromatogram and auto-zero to be executed. or 100mV can be selected. The dynamic range on the negative side is therefore small compared to that on the positive side. The auto-zeroing operation is only executed when the [AUTO ZERO] key is pressed. MANUAL Auto-zeroing is not executed when a signal is input into the MARK IN terminal. integrator output size of 0. 50. The chromatogram base is therefore set to zero. the MARK IN signal. in general. integrator output can be prevented from falling below -10mV. input to the detector from the autosampler at the time of sample injection.x/yy °C OFF -0.2 Setting for Automatic or Manual Auto-zero Execution Note: The AUTO setting is convenient for analysis. 24 .0 [MONIT] 64 + STD [MONIT] TEMP: xx. whereas the MANUAL setting is convenient for fractioning. -10mV ~ +1V. Auto-zero setting screen AUTO Flashes (AUTO or MANUAL can be selected) Input screen Figure 5.0 + OFF [SHIFT] [3] AUTO ZERO AUTO(MANUAL) [EDIT/ENTER] [ ][ AUTO ZERO ][EDIT/ENTER] (MANUAL)is the setting after the change.AUTO When analyzing samples using an autosampler. 5. 10. 5. Normal operation mode monitor screen NORM -0. Note: The [MARK] key function on the front panel causes a marker regardless of this setting. When the output level is shifted beforehand to the positive side using the zero point shift function. Therefore. do not use values that are larger than necessary (1) Setting of integrator output zero point shift Normal operation mode monitor screen NORM -0. Z POSITION 0(50)mV [EDIT/ENTER] [ ][ ][EDIT/ENTER] A.x/yy °C -0.3 Integrator Output Zero Point Shift Setting (2) Example When the baseline drifts to the negative during a long analysis 25 .Note 1: The zero point shift setting has no affect on recorder output.0 + OFF [SHIFT] [4] A. Z POSITION 0 mV Flashes (50) is the value after the change Input screen Zero point shift setting screen Figure 5. as the input voltage increases. the signal resolution of the integrator decreases and visible baseline noise increases. However. Note 2: The extent of integrator output noise is not changed by the zero point shift setting.0 [MONIT] 64 + [MONIT] STD OFF TEMP: xx. In t e g r a t o r o u t p u t 0 V Z e r o p o i n t s h i ft : 0 m V -1 0 m V 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 In t e g r a t o r o u t p u t 0 V Z e r o p o i n t s h i ft : + 5 0 m V Figure 5.0 OFF + OFF [SHIFT] [5] [MONIT] LAMP OPERAT .5 Lamp operation time ([SHIFT][5]) This function displays the lamp operation time.5 Lamp Operation Time Display 26 . Normal operation mode monitor screen NORM -0. TIME * 3456.7 H Lamp operation time screen Figure 5.0 64 + [MONIT] STD TEMP: xx.x/yy °C -0.4 Example when Baseline Drifts in Negative Direction 5. 2 Retention time delay Response setting Fast STD SLOW Delay time ca.0 + ON(OFF) [SHIFT] [7] [EDIT/ENTER] FILTER MODE TIME ACCUME [ ][ FILTER MODE ][EDIT/ENTER] TIME ACCUME (values in parenthesis are after changes) Flashes Figure 5. 13 sec.2. switch to the “DIGITAL FILTER” method.5.0 64 [MONIT] STD TEMP: xx. Generally. but peak shape may be broad. If a high noise level makes analysis using the “TIME ACCUME” method difficult. ・”MEASURE RANGE” (refer to chapter 7) 27 . 7 sec. ca.7 Other settings ([SHIFT][MARK]) Pressing [SHIFT][MARK] allows the following parameters to be changed.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. ca.x/yy °C + ON(OFF) [MONIT] -0. Normal operation mode monitor screen NORM -0. Table 5. when using the digital filtering method. The delay time of a peak for which the full width half maximum value is 10 seconds is described in Table 5. However. 4 sec.6 Signal filtering mode ([SHIFT][7]) The signal filtering method is normally set to “TIME ACCUME”. Select the adequate filtering method and response setting in relation to the chromatogram characteristics. the retention time delay becomes significant. 5. the “DIGITAL FILTER” method decreases noise. When [SHIFT][MARK] is pressed. refer to chapter 9.5) ・Marker voltage/polarity change (refer to section 5.6) The calibration constants K1 and K2 must be input when the BACK UP ERROR message appears.7.4.4.1) ・ Setting to continue/stop self-diagnostics when an error occurs (refer to section 5.5) ・ Constant K2 (for WIDE side optics calibration constant) setting (refer to section 9.7. or flow cell is replaced.2) ・Serial number setting (refer to section 9. Calibration must be performed when a light source. For descriptions of the other items.7. 28 .4) ・ Lamp maintenance time setting (refer to section 9. Other items may be input as required. In this section. Press the [ ][ ] keys to scroll between the menu screens as shown in Figure 5.・ Constant K1 (for STD side optics calibration constant) setting (refer to section 9. the “MEASURE RANGE” selection menu screen appears. photodiode. the marker voltage/polarity change item and the setting to continue/stop self-diagnostics when an error occurs are described.5) ・ Calibration (refer to section 9. 0 + OFF [SHIFT] [MARK] PARAMETER MODE Measurement range setting menu 1:MEASURE RANGE [ ] [ ] PARAMETER MODE 2:SET K1 VALUE [ ] [ ] PARAMETER MODE 3:SET K2 VALUE [ [ ] ] [ Constant K2 setting ] PARAMETER MODE 4:CALIB.Normal operation mode monitor screen NORM -0. 29 . K [ Constant K1 setting K1. MAINTE. MODE [ ] [ Menu to continue/stop self-diagnostics when an error occurs ] PARAMETER MODE 8:SERIAL NO.x/yy °C -0. Serial number menu Figure 5.7 Other Menus 5.1 Marker voltage/polarity changes These operations are used to change the marker output voltage and polarity of Recorder output. K2 Calibration ] PARAMETER MODE Lamp maintenance time menu 5:L.7. TIME [ ] [ ] PARAMETER MODE Marker voltage/polarity menu 6:MARK OUT MODE [ ] [ ] PARAMETER MODE 7:DIAG.0 64 + STD [MONIT] OFF [MONIT] TEMP: xx. The procedures required to change the settings outlined in Figure 5.5. 1. Marker voltage input range: 0.0 + ON(OFF) [SHIFT] [MARK] (Display the menu below by pressing the [ ] key twice) Marker voltage/polarity menu PARAMETER MODE 3:MARK OUT MODE [MONIT] [EDIT/ENTER] MARK OUT MODE MARK OUT MODE [EDIT/ENTER] V: 1mV V:(1)2mV P: +(-) Marker voltage/polarity screen (values in parenthesis are after changes) Flashes P: + [ ][ ][EDIT/ENTER] MARK OUT MODE V: 2mV Voltage input screen P: + Polarity input screen Flashes Figure 5. 0.x/yy °C -0.7. When diagnostics is set to continue and an error is detected the error message is displayed for 3 seconds then the instrument continues on to the next test.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.0 + ON(OFF) [MONIT] [MONIT] TEMP: xx.8. The default setting stops self-diagnostics when an error occurs.9.8 Marker Voltage/Polarity Changes 5. 30 . The procedure for changing the setting to continue/stop self-diagnostics when an error occurs is outlined in Figure 5. 2mV Normal operation mode monitor screen NORM 64 STD -0. 9 DIAG MODE CONFIRM Flashes Setting to Continue/stop Self-diagnostics when an Error Occurs 31 . SKIP (Continue) Normal operation mode monitor screen NORM 64 STD -0. PARAMETER MODE 4:DIAG. MODE [EDIT/ENTER] [MONIT] [EDIT/ENTER] DIAG MODE CONFIRM(SKIP) [ ][ ][EDIT/ENTER] (values in parenthesis are after changes) Figure 5.0 + ON(OFF) [MONIT] (Use the [ [MONIT] TEMP: xx.Input range: CONFIRM (Stop).x/yy °C -0.0 + ON(OFF) [SHIFT] [MARK] ]/ [ ] keys to display the menu below) Menu to continue/stop selfdiagnostics when an error occurs. 1 Operation summary In program mode the range. Program Mode Operations 6.5 6.6.2 Execute Refer to section 6. and auto-zero operations can be changed according to a time program. Switch between screens using the [MONIT] key. The program mode monitor screen consists of three screens. The time program operations are described in the following sections.1 Edit time program Refer to section 6. response. The maximum number of steps in the time program is 64 and the maximum number of program files that can be stored is 10.4.2 Switching between normal operation mode and program mode Press the [PRGM] key while in the normal operation mode monitor screen.1) will appear. The program mode monitor screen (Figure 6.4.2 Set file number Refer to section 6.3 Edit initial parameters Refer to section 6. Switch to program mode Refer to section 6. valve opening and closing. 32 . Press the key again to return to normal mode. The file number can be changed from the normal operation mode or program mode monitor screen using the following operations.0 + OFF TEMP: xx.x/yy°C -0.2.0 + OFF Program mode monitor screen Figure 6.0 + OFF [MONIT] TEMP: xx.0 OFF Current refractive index value Response (standard) 64 + STD Current heater temperature/setting temperature [MONIT] OFF Polarity (positive) Temperature control mark blinks when heating TEMP: xx.0 T:12.3 File number setting (file loading) A maximum of 10 files (0 ~ 9) can be stored.3 + Current time (12. Input number range: 0 ~ 9 33 .0 -0.x/yy °C -0.x/yy °C -0.0 + OFF [PRGM] PRG2 T:0.1 Switching between Normal Operation Mode and Program Mode The contents of each screen are described in Figure 6.3 min) [MONIT] Sensitivity (64) PRG2 -0.0 + OFF [MONIT] PRG2 64 STD -0. Program mode (file number 2) PRG2 -0.0 + OFF Purge valve (off) Figure 6.Normal operation mode monitor screen [MONIT] NORM 64 STD -0.2 Meanings of Items in the Program Mode Monitor Screen 6. The setting method is shown in Figure 6. Note: The settings in normal operation mode for response. the file is automatically saved. Note 2: When a file number already stored in memory is designated. press the [CLEAR] key before pressing the [EDIT/ENTER] key then enter the value again. Solvent replacement is possible regardless of whether the purge value is ON or OFF. the stored program will be loaded. polarity.1 Initial parameter editing Range and purge valve open/close (ON/OFF) are set as initial parameters. RPOGRAM FILE NO. 6.4. Since time programs are stored in C-MOS RAM (the memory backed up by battery).4.3 File Number Change Note 1: If an incorrect value is entered accidentally.Normal operation mode monitor screen [MONIT] [PRGM] Program mode monitor screen [SHIFT] [PRGM] [EDIT/ENTER] RPOGRAM FILE NO. Note: When using a “10 ~ 50mL/min. 34 . After the file number is set and the time program is edited. they are not erased when the power is turned off. the solvent replacement in the reference cell is performed by drawing up the mobile phase solvent using a syringe. y(x) y [x][EDIT/ENTER] (X) is the value after the change Flashes File number screen Input screen Figure 6.4 Program editing 6.” tubing arrangement. and temperature will remain in effect in program mode. Follow the procedure in Figure 6. In the initial parameter screen. press the down key.4.0 + OFF [MONIT] INITIAL Initial parameter screen Note: Values in parentheses are after changes Purge valve [EDIT/ENTER] R:64(16) PURGE:OFF(ON) Sensitivity PRG2 INITIAL R:64 PURGE:OFF Sensitivity flashes PRG2 [ ][ ] [EDIT/ENTER] INITIAL R:16 PURGE: OFF [ ][ Sensitivity input screen Purge valve open/close screen Purge valve flashes ] [EDIT/ENTER] Figure 6. a time program will be created with the initial parameters (range: 16.0 + OFF [ -0.4. after 2 minutes. the response will be changed to FAST.1 Time program input (1) Input example As an example.0 ] PRG2 PRG2 [ 64 + ] STD [MONIT] OFF TEMP: xx.5 for subsequent operations.0 -0.2. The step 1 screen will appear. The range will then be changed to 8 and.4 Initial Parameter Editing 6. response: STD) held for 1 minute. 35 .2 Time program editing 6.x/yy°C -0.Program mode monitor screen [MONIT] PRG2 T:0. 0 Time flashes (waiting for input) P2 ST 2 T:2. c) Input the time in minutes (0.0 1: PURGE ON [EDIT/ENTER] Time flashes (waiting for input) Input 1 minute T:1. 36 .0 P2 [EDIT/ENTER] P2 ST 1 T:0.0 RANGE:16 [ ][ Function flashes (waiting for input) P2 ST 1 T:1.0 Input 8 P2 ST 2 RESPONSE [ Step 1 input complete T:2. function.5 Time Program Key Operation Example (2) Time program input method Set the time.1min step). a) Press the [ ] key while in the initial parameter screen (displays step 1). and value in sequence for each step. b) Press [EDIT/ENTER] (the time value flashes).0 RANGE:8 ST 2 T:0.0 [1][EDIT/ENTER] P2 ST 1 T:1.0 1: PURGE ON Input 2 minutes Function flashes (waiting for input) Call up response [RSPNS/5][EDIT/ENTER] or [ ] four times [EDIT/ENTER] Value flashes (waiting for input) ] [EDIT/ENTER] P2 [2][EDIT/ENTER] Call up sensitivity [RANGE/4][EDIT/ENTER] or [ ] three times [EDIT/ENTER] P2 ST 1 Step 2 screen ST２ T:0.0 RESPONSE FAST Value flashes (waiting for input) Input FAST Step 2 input complete : Shaded values are flashing Figure 6.PRG2 INITIAL Initial parameter screen R:16 PURGE:OFF [ ] [ PRG2 ST 1 ] [ ▼] Step 1 screen T:0.0 ][ STD ] [EDIT/ENTER] P2 ST 2 T:2. STD.16.8.256.1/2.1. Select a function from Table 6.64. press the [ ] key to move to the next step. Table 6. they will be rearranged in chronological order once the [MONIT] key is pressed to return to the monitor screen. [ ][ ][EDIT/ENTER] When input is complete.1.S FAST. For example [RANGE/4][EDIT/ENTER] The input function will appear and the value will flash. Functions that can be controlled by the time program and the relevant keys for the functions are shown in Table 6.512.4.2.ZERO/3] Range [RANGE/4] [ ][ ] [RSPNS/5] [ ][ ] 1/4. Repeat the operations in steps a) ~ e) to edit the time program.[xx][EDIT/ENTER] Function will flash next.1. SLOW Response Movement among steps [ ]: Moves to the next step [ ]: Moves to the previous step 37 . 128.32.1 Function Input Keys and Input Range Function Purge valve open Key [P-ON/1] Change keys Setting range Purge valve close [P-OFF/2] Auto-zero [A. Note: Steps do not have to be input sequentially in respect to time. e) Input a value. d) Input the function. Even when steps are out of time sequence. use the operations shown on the left in Figure 6.[SHIFT][ ]: Moves to the last step in the program [SHIFT][ ]: Moves to the first step in the program 6. 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.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. will appear. when input is corrected starting with time. when changing only the range value. 38 .4.2. shown on the right in the figure. However. For example. 3) Change the value.6. the function selection screen. When only a value. and not time and function. 3) Press the [MONIT] key to return to the monitor screen.PRG2 ST 3 T:1.6 Correcting a Time Program 6.0 RANGE : 16 [EDIT/ENTER] PRG2 ST 3 T:1. Deletion of a step and all subsequent steps 1) Display the first step to be deleted using the [ ] key.0 RANGE : 32 Figure 6.0 1: PURGE OFF Function flashes (waiting for input) [RANGE/4][EDIT/ENTER] PRG2 ST 3 T:1.3 Deletion Single step deletion 1) Display the step to be deleted using the [ ] key. Steps will be rearranged in chronological order and the 0 time step will be deleted. 2) Set the time in the step to 0 ([EDIT/ENTER][0][EDIT/ENTER]). 39 .2. The designated step and all subsequent steps will be deleted.0 RANGE : 16 Time flashes (waiting for input) [1][EDIT/ENTER] P5 [EDIT/ENTER] ST 3 Time input T:1.4.0 RANGE : 16 [ PRG2 ST 3 ][ Sensitivity call up Value flashes (Change the value here) ][EDIT/ENTER] T:1. 2) Press [SHIFT][CLEAR]. 2. The [PRGM RUN] key lamp will light. execution parameters can be freely changed. 4) Press the [MONIT] key to return to the monitor screen.5 Time program operation 6. Note: During time program. Steps will be rearranged in chronological order. indicating a time program is in progress.4. The time program will start. the time program will reset and start again immediately. The changed values will remain in effect until the next setting value is reached in the time program.3) Press the [MONIT] key to return to the monitor screen. (1) Start After the baseline has stabilized.1 and input desired values. When the time program reaches the final step.4 Insertion 1) Display the final step in the program using [SHIFT][ ]. When using an autosampler. press the [PRGM RUN] key.5. (3) Time program execution by external signal The time program can be started by shorting the rear panel terminal PRGM RST/ST and GND. the parameters at that point are maintained and only time advances. 3) Follow the procedure described in section 6. the injection signal should be connected to these terminals. If the rear panel terminal PRGM RST/ST and GND are shorted while the time program is running. 40 . 6. 6. (2) Stop Press the [PRGM RUN] key during program execution. 2) Display a new step using the [ ] key.4.2. The [PRGM RUN] key lamp will go out and the time program will stop.1 Time program execution Start the program while the program monitor screen is displayed. The “MEASURE RANGE” setting is normally set to STD.0V 5x10-3RIU/1.1. Set “MEASURE RANGE” to WIDE only when the STD dynamic range makes analysis difficult. using the procedure shown in Figure 7. Table 7. “MEASURE RANGE” should be set to WIDE.7.0V Note: The baseline noise and drift when set to WIDE is larger than when set to STD. 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.x/yy °C -0.000 [MONIT] 64 [MONIT] STD + ON(OFF) TEMP: xx. however when measuring a high concentration sample. The recorder scale and integrator output scale are automatically changed according to the “MEASURE RANGE” setting.000 + ON(OFF) [SHIFT] [MARK] PARAMETER SET 1:MEASURE RANGE [MONIT] [EDIT/ENTER] MEASURE RANGE STD(WIDE) Flashes [EDIT/ENTER] [ ][ MEASURE RANGE ][EDIT/ENTER] (WIDE) is the setting after the change.1 “MEASURE RANGE” “MEASURE RANGE” and output scale Dynamic range RANGE Inte. Normal operation mode monitor screen NORM -0.1 “MEASURE RANGE” setting 41 . output STD ~ 5x10-4RIU 1/4~512x10-6RIU WIDE ~ 5x10-3RIU 1/4~512x10-5RIU 5x10-4RIU/1. STD (STD or WIDE can be selected) Input screen MEASURE RANGE setting screen Figure 7. when the RANGE setting is 128.9x10-3RIU/1. the measurable range is 12. 42 .8x10-3 RIU/100mV (“MEASURE RANGE”: WIDE). connect to the recorder output terminal instead of the integrator output terminal.0V (“MEASURE RANGE”: WIDE). and ~ 9. For example. and 12.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). When exceeding the linear range.0V (“MEASURE RANGE”: STD ). the measurable range is ~ 7x10-4 RIU/1.8x10-4 RIU/100mV (“MEASURE RANGE”: STD). 6mm. operate purge valve. Maximum Flow Rate Changing at the Front Panel The maximum flow rate depends on the front panel tubing arrangement.8mm tubing and ports No.1 “ ~ 10mL/min” tubing arrangement 43 .2 with outer diameter: 1.4 and No.8.6mm ID= 0. The following subsections describe tubing arrangements and the method for replacing solvent in the reference cell.5 with outer diameter:1. set the valve to ON. OD=1.6. Connect the tubing from the column to port No.2) Tubing 1 2 3 4 5 6 Sample Out (waste) Flow rate: ~ 10mL/min. internal diameter:0. and connect the tubing for waste to port No.3. During analysis. internal diameter:0. When replacing the reference cell solvent. set the valve to OFF. 8. To replace solvent in the reference cell.8mm tubing. (Refer to section 4.1 and No.1 “ ~ 10mL/min” tubing arrangement and solvent replacement method for reference cell Connects ports No.6mm.8mm Sample IN (from column) Figure 8. 4-5. for the “~10mL/min” tubing Reference Out arrangement. Sample IN Tubing OD=1.3) Sample Reference IN Tubing OD=1.5.8.1.2 “10 ~ 50mL/min” tubing arrangement 44 .1-2 or 1 2 3 4 5 6 ports No. (Refer to section 4. Use tubing with an internal diameter of 0. Make sure the syringe is connected during analysis.2.8mm and an outer diameter of 1.6mm ID=0. ID=0. draw up mobile phase solvent by pulling the syringe plunger.8mm Replace solvent in the reference cell by sucking the mobile phase solvent.6mm Mobile phase ID=0.8mm (Same tubing as used to connect ports No. The refractive index output signal is reversed. Sample IN Keep the syringe connected during analysis in order to maintain solvent in the reference cell and to facilitate solvent replacement.6mm. Change the Polarity setting.6. Connect the syringe to port No.8mm Sample Out 1 2 3 4 5 6 Tubing OD=1. Figure 8.6mm. and connect the tubing for waste to port No. Connect the tubing from the column to port No. To replace solvent in the reference cell.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. 1 Error messages and countermeasures 9. an error message is displayed on the screen. The items in Table 9. changed? (2) Have the setting values followed [SHIFT] key operation changed? (3) Has the K1 value changed to 1.1 Errors during self-diagnostics after power on The self-diagnostics program is automatically executed when the power switch is turned on. If the error message appears again.8 in section 9.00.1 are checked during self-diagnostics.9. when BACK UP ERROR has been skipped in this way.1. a ROM CHECK ERROR or RAM CHECK ERROR may appear. When an error message appears. turn the power off.00? (Refer to Figure 9. press [SHIFT][ ] to advance to the next item and continue with the self-diagnostics program. turn the power off. If the re-input values have changed again. Maintenance 9. check that chromatograms (including baselines) are the same as previously obtained results.4. When a problem is found. and turn the power on again. wait at least 3 minutes. the backup battery is dead and the user should contact your local JASCO distributor. check the following points. When an error message appears and self-diagnostics stop. wait 30 seconds. When self-diagnostics have been advanced in this way. re-input the setting values. Note: When the power is turned off then on quickly. 45 . (1) Have the RANGE and other setting values.5) If setting values have changed or the K1 value has reverted to 1. including Time Program setting. a problem exists with the instrument and the user should contact your local JASCO distributor. In particular. and turn the power on again. and contact your local JASCO distributor.2). Table 9.1. turn the power off. TIME 9. Refer to section 9. 46 . GLASS ERROR Lamp operation time WARNING LAMP MAINTE.3 Error message meanings and countermeasures 9.2 Self-diagnostics Items and Corresponding Error Messages Check item Error message Fluid leak in cell TROUBLE LEAK IN CELL Heater overheating TROUBLE OVER TEMP Light intensity deterioration WARNING INTENSITY POOR Optical zero adjustment WARNING OUT OF RANGE Lamp operation time WARNING LAMP MAINTE TIME 9.3.1 Self-diagnostics Items and Corresponding Error Messages after Power On Check item Error message ROM operation ROM CHECK ERROR RAM operation RAM CHECK ERROR C-MOS RAM backup BACK UP ERROR Temperature sensor TEMP SENSOR NG Zero glass driver Z.1. When a problem is detected.3 for countermeasures.Table 9. Immediately stop the pump.2 Self-diagnostics during operation The instrument checks the following items during operation (Table 9.1. an error message is displayed on the screen.1.1 TROUBLE LEAK IN CELL This message appears when fluid is leaking from the flow cell. 3. When the value is smaller than 0. (3) The cell is broken. 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). When the SUM value is only slightly smaller than normal. Specifically. Immediately turn the power off and contact your local JASCO distributor. The message may also appear when misjudgment happens due to a problem with the temperature detection system.2).9. the message appears when the DIFF value of preamplified output divided by the SUM value is greater than 0. (1) Small bubbles remain in the cell -> Remove the bubbles (refer to section 9. the message appears when the absolute value of the SUM of preamplified outputs falls below 0.1.2).3 WARNING INTENSITY POOR This message appears when the light intensity incident on the photodiodes is insufficient.4 WARNING OUT OF RANGE This message appears when the light incident on the photodiodes is shifted to one end.3).3. Note: The message will reappear every 20 seconds.1V.5V. press the [CLEAR] key to clear the message (see note).2).2 TROUBLE OVER TEMP This message appears when overheating occurs due to a problem with the temperature control system. 9.1.3. the following problems are possible.8 in absolute 47 . and check the SUM value (refer to section 5. When this message appears. the following problems are possible. 9. (2) The cell is contaminated -> Clean the cell (refer to section 9. (2) Large bubbles remain in the cell -> Remove the bubbles (refer to section 9. Specifically. display the preamplified output screen.1. 3. Replace solvent in the reference and sample cell according to the tubing arrangement. (3) Optical zero is not properly adjusted. 48 . press the [CLEAR] key to clear the message (see note). When this message appears. The following problems are possible when the message appears.1 Baselines when bubbles are generated The following baseline phenomena occur when bubbles are generated in the flow cell. 9. until the problem is fixed.2). press [SHIFT]+[AUTOZERO] key.2). Press the [CLEAR] key to clear the message. The instrument may continue to be used. display the preamplifed output screen. (2) Large bubbles remain in the cell -> Remove the bubbles (refer to section 9.01xx.5 for details regarding how to set the lamp maintenance time.value. (Refer to chapter 8 and section 4.5 WARNING LAMP MAINTE TIME This message appears when the lamp operation time reaches the set maintenance time. Adjustment is satisfactory if the DIFF value falls to zero within +/-0.2) Once the DIFF and SUM values in the preamplified output screen have stabilized.2 Flow cell bubble removal 9. (1) The solvent on the sample side is different from the solvent on the reference side. and check the DIFF value (refer to section 5. Note: The message will reappear every 20 seconds. Note: Refer to section 9. 9.2.1. 2).1 Irregular Noise Caused by Bubbles Returns to base when bubbles are removed Figure 9.2 Baseline Drift Caused by Bubbles Figure 9. it is possible that bubbles exist in the flow cell.(1) Irregular noise (Figure 9. 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. If the third digit after the decimal point of the SUM value is fluctuating.2) (3) Irregular ghost peaks (Figure 9. display the preamplified output screen and check the SUM value (refer to section 5.3) When the above phenomena occur.1) (2) Increased drift (Figure 9.3 Ghost Peaks Caused by Bubbles 49 . Note: (2) Be sure to connect a line filter to the pump outlet in order to prevent contaminants from entering the flow cell.2.2 Bubble removal method 1 (high flow rate fluid pump) Note: (1) When pumping fluid at a high flow rate.4 Bubble removal method 3 (covering tubing outlet) Note: Use a flow rate of 2mL/min or less with this method. Repeatedly cover (for 2 seconds at most) and release the outlet of the OUTLET tubing.9.” tubing arrangement. do not connect other detectors to the OUTLET of the RI-2031.2.5 Bubble prevention method Follow the guidelines below (particularly when using aqueous solvents) to prevent bubble generation. the flow cell may be damaged or fluid leaks may occur from the electromagnetic valve. then open and close the purge valve (ON/OFF) (refer to section 4. 50 . connect a syringe to the INLET (or OUTLET). For example.2. 9. connect the pump directly to the RI-2031. Note: Do not move the syringe plunger too quickly.2) while pumping fluid at a high flow rate (up to 10mL/min is possible). When the solvent being used is dangerous to touch. the internal solvent will be flushed at a rate of 120mL/min.2. repeatedly pinch (for 2 seconds at most) and release the OUTLET tubing (Teflon tube). When using a “ ~ 10mL/min. 9. 9. If this method is used with a high flow rate. and push solvent in (or pull solvent out).3 Bubble removal method 2 (syringe fluid injection) Remove the INLET and OUTLET tubing of the flow cell. This greatly exceeds the maximum flow rate of the instrument and may damage the flow cell or cause fluid leaks from the electromagnetic valve. if the plunger of a 20mL syringe is depressed for a full stroke in 10 seconds. Use the pump for cleaning and pump fluid at a high rate for at least 12 hours. (3) Place the waste fluid bottle in a position higher than the instrument. Prepare 200mL or more of the solvents and recycle the solvents.(1) Use a degasser. wash with THF (tetrahydrofurane). bubbles may be introduced. flush with the following solvents. When contaminants adhered to the internal cell wall are unknown. This is particularly troublesome when pumping nitric acid and aqueous solutions. wash with nitric acid. (2) When the mobile phase solvent is organic.6. 51 . When contaminants adhered to the internal cell wall are known. 9. Note2: Be sure to place a line filter between the pump and the instrument. Note3: When the inlet filter of the pump is clogged. Solvents other than the mobile phase solvent are effective. bubbles easily enter the flow cell. flush with a solvent that will dissolve the contaminants. (2) Sufficiently check for clogs in the pump inlet filter.3 Flow cell cleaning method Note1: Reversing the fluid flow direction is prohibited. (1) When the mobile phase solvent is aqueous. Be sure to pump fluid into port No. When the inlet filter is clogged. these values will be lost and the instrument will revert to the default values. (1) After light source replacement (2) After photodiode replacement (3) After flow cell replacement Note: The K1 and K2 values are recorded in RAM.1.) However. in the following cases.Port No.4. refer to section 10.4 Flow Cell Cleaning Method 9.) 52 . Therefore. (refer to section 9. recalibration is necessary because of the optical characteristics of the detector changing. or by the light absorption caused by a mobile phase solvent or a sample solute. This requires resetting the constant K1 and K2. When the backup battery has deteriorated. when the values have been lost.4.3 RI-2031 Pump Wash fluid Port No. check the K1 and K2 values on the label and re-input.4 Calibration method A sophisticated signal processing system incorporated into the RI-2031 is able to measure refractive index accurately without being affected by variations or fluctuations in lamp emission. The K1 and K2 values are written on a label inside the instrument.2. The K1 value is used when “MEASURE RANGE” is set to STD and the K2 value is used when “MEASURE RANGE” is set to WIDE. (For details.6 Figure 9. 6 Water Figure 9. An injector loop with a capacity of 1mL or more is required.1 Tubing Figure 9. The refractive index of this aqueous saccharose solution is 160x10-6RIU greater than the refractive index of the water.3m or more in length with internal diameter of 1. the capacity of the injector loop does not need to be precise.8mm. However.2 Standard solution (1) Prepare approximately 1000mL of water. 53 .9. Note: Use the same water for the mobile phase and to dissovle the saccharose. Alternatively. prepare a loop using tubing 1. prepare a loop using tubing 2m or more in length with an internal diameter of 0. (refer to section 8) Integrator or recorder Port No.0mm. (2) Dissolve 106.5 shows the tubing and wiring arrangement used for calibration.5 Tubing and Wiring Arrangement for Calibration 9. Sufficiently degas the water to prevent generation of bubbles during calibration. Change to the “ ~ 10mL/min.4. When an appropriate loop is not available.” tubing configuration.25mm or less Port No.3 1mL loop RI-2031 Pump Injector Internal diameter of 0.6mg of saccharose in a 100mL volumetric flask using the water prepared in (1) above. If different water is used.4. the correct refractive index may not be obtained. 5 is used. first replace with acetone then replace with water.9. this corresponds to approximately 1% or less during a 10 minutes period with a range of 64 (x10-6). (4) Pump solvent at a flow rate of 1. 0.4.2 (1) until the solvent in the system is sufficiently replaced. (refer to chapter 7) (3) Wait for the drift to decrease to 1. (1) Pump the water prepared in section 9. when the solvent in the cell is chloroform or THF (oxidation inhibitor is insoluble in water). since no other detectors are connected to the system. When a recorder is used. In addition.2.0mL/min and confirm that the drift is within the limit described in (3) above.1x10-6RIU/min or less corresponds to a 0.4. a flow rate of 10mL/min may be used (2) Set “MEASURE RANGE” to STD. 9.4.1 RIU value per minute. Note: On the LCD display.7).7(refer to section 5. Note: If the tubing shown in Figure 9. The K1 and K2 calibration screen is displayed.4 Calibration method (1) Following the procedure described in Figure 5. For example.0x10-7RIU/min or less. confirm that the fluctuation in the RIU value on the LCD display is less than 0. display the K1 and K2 Calibration menu screen and press the [EDIT/ENTER] key. first replace with an intermediate solvent then replace with water. 54 .3 Replacement of tubing system solvent with water Note: When the solvent in the cell is not miscible with water. Normal operation mode monitor screen NORM -0. (4) If the RIU value on the plateau of peak is within 160. If the value is not within 160.0 ± 1.6 x 10-6 RIU. the instrument is already correctly calibrated. press the [AUTOZERO] key. press the [PRGM RUN] key to execute build-in calibration program. Inject standard solution 0.0 ± 1. press the [AUTO ZERO] key to set the RIU value to zero.0 PRESS RUN KEY Figure 9.x/yy °C -0.6 x 10-6 RIU. Press the [PRGM RUN] key to execute the built in calibration program. The RIU value will be 160±1 RIU.000 + ON(OFF) + ON(OFF) [MONIT] [SHIFT] [MARK] [ ][ ][EDIT/ENTER] PARAMETER SET 4:CALIB K [MONIT] [EDIT/ENTER] K CALIB: xxxx.X PRESS RUN KEY Read the RIU value shown on the screen for the plateau of the peak.6 x 10-6 RIU.0 ± 1. K CALIB: 160.000 64 STD [MONIT] TEMP: xx.x PRESS RUN KEY K CALIB: Calibration screen Once the baseline has stabilized.6 Calibration screen (2) In the calibration screen. Set the chart speed to 10mm/min. 55 . (3) Inject standard solution. once the baseline has stabilized. The RIU value will automatically be set to 160. 9. (5) Repeat the operations in steps (2) ~ (4) and confirm that the RIU value is within 160.8 and re-input the calibration constants.Plateau Figure 9.5 Calibration constant confirmation and setting After performing calibration (outlined in previous section). the recorded values can then be re-input in the following situations. inspect the internal diameter of the tubing from the injector to the detector. These values should be written on a piece of paper and attached inside the instrument.7 Peak Shape Note: When the peak dose not contain a plateau.4. decrease the flow rate. and troublesome calibration operations can be avoided.6 x 10-6 RIU without pressing the [PRGM RUN] key. Note: Adjustment of the integrator or recorder output is not necessary. This way. the calibration constants. When the plateau is short. The outputs will automatically be adjusted when the K1 and K2 values are calibrated. When confirming and setting the calibration constant. (1) When the K1 or K2 values have been changed by mistake 56 . Note: Calibration of constants K1 and K2 is performed by executing build-in calibration program at the same time.0 ± 1. follow the procedure shown in Figure 9. K1 and K2 obtained should be recorded. (2) When the backup battery has deteriorated and the K1 value has reverted to 1.x [MONIT] TEMP: xx.4.1 ~ 9. including the pump.4 is the most accurate method of calibration.00.4.x Figure 9.6 Alternative calibration method The method described in sections 9.000 [ ][ + ON(OFF) ] [ ][ [EDIT/ENTER] ] PARAMETER SET 3:SET K2 VALUE [MONIT] K1 VALUE: x.xxx RIU: xxxx.x [EDIT/ENTER] [MONIT] [EDIT/ENTER] K2 VALUE: x. since the entire flow line.8 Confirming and setting calibration constant 9. This label can be seen when the case is removed.4. Normal operation mode monitor screen NORM -0.xxx RIU: xxxx. the K1 and K2 values are recorded on a label attached inside the instrument.xxx RIU: xxxx. (3) When the PCB (CPU board) has been replaced Note: At the time of shipping.000 [MONIT] 64 + ON(OFF) -0.x/yy°C [SHIFT] [MARK] PARAMETER SET 2:SET K1 VALUE [MONIT] [MONIT] STD [EDIT/ENTER] K2 VALUE: x.xxx RIU: xxxx. must be replaced with 57 . However.x K1 VALUE: x. (1) Do not move the syringe plunger too quickly. In addition. Although this will not cause a problem during solvent replacement. 58 . When the lamp maintenance time is set to 0. When the lamp operation time exceeds the lamp maintenance time. the LAMP MAINTENANCE warning will be displayed. the lamp maintenance time recorded in RAM will be lost. points of caution when using syringe injection are listed below. For example. the operations are troublesome when non-aqueous mobile phases (chloroform for example) are being used. Since lamp replacement is done by service engineer.9 and re-input the lamp maintenance time. 9.2). When this occurs. if the plunger of a 20mL syringe is depressed for a full stroke in 10 seconds. Display the preamplified output on the screen and confirm that no bubbles are present while performing calibration (refer to section 5. follow the procedure in Figure 9. the internal solvent will be flushed at a rate of 120mL/min. the warning is not displayed. It may be possible to replace the solution in the detector using only a syringe. (2) When a syringe is used to inject fluid. This greatly exceeds the maximum flow rate of the instrument and may damage the flow cell or cause fluid leaks from the electromagnetic valve. proper calibration is not possible if bubbles are introduced immediately before or after standard solution injection. contact your local JASCO distributor when this is required. when BACKUP ERROR is displayed due to deterioration of the battery. however. there is a tendency to introduce bubbles into the flow cell.5 Lamp maintenance time setting Lamp maintenance time can be set to inform the operator of the number of hours the lamp has been in use. A detailed description of the procedure will not be given.water. Normal operation mode monitor screen NORM -0.0 64 [MONIT] TEMP: xx.x/yy °C -0.0 + ON(OFF) + ON(OFF) [SHIFT] [MARK] [MONIT] (Use the [ STD ]/[ ] keys to display the menu below) Lamp maintenance time menu PARAMETER MODE 2:L. MAINTE. TIME [MONIT] [EDIT/ENTER] LAMP MAINTE TIMER 10000 H [EDIT/ENTER] [xxxxxx] [EDIT/ENTER] LAMP MAINTE TIMER 10000 H Flashes Figure 9.9 Lamp Maintenance Time Input Method 9.6 Serial number setting The serial number of the instrument is recorded on the label on the right side of the instrument case. When BACKUP ERROR is displayed due to deterioration of the battery, the serial number recorded in RAM will be lost. When this occurs, use the procedure outlined in Figure 9.10 to re-input the serial number. When connecting to a JASCO system controller via LC-Net, the serial number is displayed on the HPLC system configuration screen. 59 Normal operation mode monitor screen [MONIT] NORM 64 STD -0.0 + OFF [MONIT] TEMP: xx.x/yy°C -0.0 + OFF [SHIFT] [MARK] (Use the [ ]/[ ] keys to display the menu below) Serial number menu PARAMETER MODE 6:SERIAL NO. [MONIT] [EDIT/ENTER] SERIAL NO 1234567890 [EDIT/ENTER] [xxxxxxxxxx] [EDIT/ENTER] SERIAL NO 1234567890 Flashes Figure 9.10 Serial Number Input Method 9.7 Power Fuse replacement Warning: When changing the power fuses, be sure to disconnect the power cable from the power cable inlet (refer to Figure 2.5). Warning: For continued protection against risk of fire, replace only with fuses of the specified type and current ratings. Note: When one fuse is blown, replace both fuses. 60 Insert finger under the fuse holder, pinch the holder, and pull forward. The fuses and the fuse holder will come out together. (Figure 9.11) (1) Pull the old fuses out from fuse holder, insert new fuses, and insert the fuse holder back into its original position. If the replaced fuses immediately blow out again, an instrument problem is possible. Contact your local JASCO distributor. Fuse Holder Figure 9.11 Fuse Holder 61 10. Appendix 10.1 Operation Theory 10.1.1 Operation theory of deflection differential refractometers With deflection differential refractometers, light refracted inside the prism flow cell is used to detect the difference in refractive indices between the reference (solvent) and the sample. The flow cell structure and light path are shown in Figure 10.1. nS i i θ r nR Figure 10.1 Horizontal Cross-section of Flow Cell and Light Path The area to the left of the center partition is called the sample cell and the area to the right is called the reference cell. ns : Refractive index of sample nR : Refractive index of reference (solvent) θ: Angle of deflection (exaggerated in the figure: actual value is <10-2 degree.) i: Angle of partition (determined by cell shape) Applying the law of refraction to this light path and assuming θ << 1 (since the actual value is 10-2 or less), θ can be expressed as follows: θ = tan i x(nS-nR)/nR... (1) From this equation, the angle of deflection is proportional to the difference in refractive indices between the reference solvent and the sample. In other words, it is possible to determine the difference in refractive indices between the reference solvent and sample by measuring the angle of deflection. 62 The first and second photodiodes contain identical photo-sensitive surfaces and are referred to as PD1 and PD2.2 Optical System Light from the light source passes through a slit and into the collimator lens where it is made into a parallel beam. The remainder of the light passes through the half mirror and strikes the second photodiode. thereby changing the angle of deflection in accordance with equation (1).. the following equation can be expressed. 63 . passes through the cell again.10. (2) The coefficient of 2 is required in the equation to account for the fact that the light passes through the flow cell twice and is therefore refracted twice. The parallel light then passes through and is refracted by the flow cell. Part of the light is reflected by a half mirror. The amount of shift is proportional to the angle of deflection and the focal length of the lens. s = 2f x θ. respectively. When s is the amount of shift and f is the focal length of the lens.. and strikes the first photodiode.1. The light image striking the primary photodiode will therefore shift in the horizontal plane (direction perpendicular to the plane of this paper). The method for detecting the amount of shift is described below.2 Optical system Collimator lens Slit Second photodiode Light source Flow cell First photodiode Half mirror Zero glass (motor driven) Figure 10. then the refractive index changes. If the concentration of the sample in the cell changes. the difference between the refractive indices of the reference solvent and sample is proportional to DIFF. Therefore.(3) In this equation. as shown in the bottom half of Figure 10. Equations (1) ~ (3) can be combined to give the following.3. and a difference between the output of PD1 and the output of PD2 is generated. Next. Since the electrical output from a photodiode is proportional to the surface area receiving light. flow cell transmittance. the difference between the output of PD1 and the output of PD2 is zero and so DIFF is zero.. the image is shifted. the difference between the refractive indices can be calculated by measuring the difference between the outputs of PD1 and PD2. when there is a difference between the refractive indices. Since the output is proportional to the surface area receiving light..PD1 output PD2 output No difference between refractive indices PD1 output PD2 output Difference between refractive indices Figure 10. photodiode measurable range. the light image overlaps PD1 and PD2 equally as shown in the top half of Figure 10. that is the difference between the outputs from PD1 and PD2..3 Light Image on Photodiodes First. A is a constant determined by the light source intensity. the output difference is proportional to the amount of shift s. 64 . nS-nR = B x DIFF. and amplification of the amplifier.. DIFF = A x s.3.(4) where B = 1/2f tan i x (nR/A) In other words. when there is no difference between the refractive indices of the reference (solvent) and the sample. K1 value is for analytical measurement (first photodiode) and K2 value is for preparative measurement (second photodiode). This means that for the optical arrangement shown in Figure 10. SUM = A x k. and both of these factors can change over time.3 Signal processing method Theoretically. the distance between the flow cell and second photodiode is shorter than that of an optical system with first photodiode. as shown in equation (4). 2f in equation (2) is 10 times smaller and. the dynamic range is 10 times larger. Therefore. Although A in equation (4) is proportional to light source intensity and flow cell transmittance.In the case of an optical system with a second photodiode. The RI-2031 measurement system uses two calibration constants (K1 and K2). On the other hand. therefore.nR .1. the difference between refractive indices can be found by measuring DIFF. nS . the value is not affected by light source deterioration or flow cell contamination.(5) The following can then be obtained using equations (4) and (5).2. 10.. the sum of the outputs from PD1 and PD2 (hereafter called SUM) is proportional to the light source intensity and flow cell transmittance regardless of the value of the refractive index.K x DIFF/SUM where K = knR/(2f tan i) DIFF/SUM is proportional only to the difference between refractive indices and does not change over time. 65 .. In this case. the effluent passes through the sample cell only before being discharged and the reference cell is completely sealed. When the purge valve is ON.4. valve Flow cell Purge ON 1 4 Ref.4. the instrument is switched to the flow line indicated by the solid arrow in Figure 10.3.4 Flow line A flow line diagram for the “ ~ 10mL/min.10.4 Flow Line (“ ~ 10mL/min. In this case.” tubing arrangement.1.6 and waste is discharged from the port No.4. the effluent passes through the sample cell and then through the reference cell before being discharged.” tubing arrangement) 66 . the instrument is switched to the flow line indicated by the dotted arrow in Figure 10. Flow lines are changed using the purge valve. is shown in Figure 10. When the purge valve is OFF. Heat exchanger 6 IN 3 OUT Purge OFF Purge Sam. Effluent form the column is introduced from the port No. Heat exchanger 5 2 During analysis (PURGE OFF) When replacing solvent in the reference cell (PURGE ON) Figure 10. Effluent from the column is introduced from the port No. Heat exchanger 5 Sample IN 2 Sample OUT Sample side flow line Reference side flow line Figure 10.2 (Sample OUT).5 (Sample IN) and waste is discharged from the port No. Heat exchanger 6 Reference OUT Purge OFF 3 Purge valve Ref. The sample side flow line is indicated by the solid arrow in Figure 10.A flow line diagram for the “10 ~ 50mL/min.” tubing arrangement) 67 .5. The reference side flow line is indicated by the dotted arrow in Figure 10.5 Flow Line (“10 ~ 50mL/min. The solvent from the column passes through the heat exchanger and then through the sample cell. The mobile phase passes through the reference cell and then through heat exchanger. from the port No.6 (Reference OUT).3 (Reference IN) and is drawn using the syringe. draw up the mobile phase solvent using a syringe connected to the No.5. is shown in Figure 10.6 port.1 and No. Note: The tubing connection between ports No. When replacing the solvent in the reference cell.4 avoids introducing air into the reference cell. The mobile phase solvent is introduced from the port No.5. Purge ON Reference IN 1 Flow cell 4 Sam. The sample and reference flow lines are independent.” tubing arrangement. 1 Internal volume using “ ~ 10mL/min. 70 µL Sample cell -> Port No3 ca.2.2 Internal volume using “10 ~ 50mL/min.5 Internal volume of tubing Internal volume of tubing is described in Table 10. Table 10.1.10.1 and Table 10. 200 µL 68 . 300µL Table 10.” tubing Flow line Volume Port No5 -> Sample cell ca. 500 µL Sample cell -> Port No2 ca.” tubing Flow line Volume Port No6 -> Sample cell ca.
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