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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)

Figure 8.2 “10 ~ 50mL/min” tubing arrangement

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
solvent replacement.

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

Reference

IN

Reference

Out

1

Sample Out

Sample IN

Mobile phase

2

3

4

5

6

1

2

3

4

5

6

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Содержание RI-2031

Страница 1: ...P N 0302 0555A MODEL RI 2031 INTELLIGENT REFRACTIVE INDEX DETECTOR INSTRUCTION MANUAL...

Страница 2: ...entially 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 mode...

Страница 3: ...ove 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 numbe...

Страница 4: ...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 U...

Страница 5: ...rienced 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...

Страница 6: ...ower 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...

Страница 7: ...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...

Страница 8: ...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 SOL...

Страница 9: ...viii...

Страница 10: ...on 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 a...

Страница 11: ...ting 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 set...

Страница 12: ...ng 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 wat...

Страница 13: ...xii...

Страница 14: ...mi 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 condit...

Страница 15: ...x 10 3 RIU MEASURE RANGE WIDE Condition H2O Noise 0 2 x 10 8 RIU Condition H2O Flow stopped Cell capacity 10 L Maximum usable flow rate 10mL min 10mL min tubing 50mL min 10 50mL min tubing Solvent H2O...

Страница 16: ...0 x 10 3 RIU 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 SUS...

Страница 17: ...efer 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 f...

Страница 18: ...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...

Страница 19: ...e connected during analysis in order to maintain solvent in the reference cell and to facilitate solvent replacement Flow rate 10 50mL min Tubing OD 1 6mm ID 0 8mm Same tubing as used to connect ports...

Страница 20: ...creens 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 cel...

Страница 21: ...8 2 3 Back panel Input Output Terminals LC Net Connectors RS 232C Terminal Fuses AC input Ground Terminal Figure 2 5 Back Panel...

Страница 22: ...en 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...

Страница 23: ...E 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 t...

Страница 24: ...ure 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...

Страница 25: ...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 w...

Страница 26: ...r 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...

Страница 27: ...lashes 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 Figure 4 3...

Страница 28: ...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...

Страница 29: ...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...

Страница 30: ...nge 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 clo...

Страница 31: ...t 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 o...

Страница 32: ...properly adjusted optical zero is 5 0x10 4 RIU 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 0...

Страница 33: ...ive index range resulting in proper recorder output is 9 9x10 4 RIU 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...

Страница 34: ...ltage 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 beforehan...

Страница 35: ...s 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...

Страница 36: ...ical 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...

Страница 37: ...ting 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 ze...

Страница 38: ...ses 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 shif...

Страница 39: ...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...

Страница 40: ...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 w...

Страница 41: ...erial 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...

Страница 42: ...ETER 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 K...

Страница 43: ...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 oc...

Страница 44: ...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 par...

Страница 45: ...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 Refe...

Страница 46: ...ensitivity 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 P...

Страница 47: ...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...

Страница 48: ...2 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 exa...

Страница 49: ...omplete 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...

Страница 50: ...d 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 chro...

Страница 51: ...y 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 displa...

Страница 52: ...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 Pre...

Страница 53: ...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...

Страница 54: ...e MEASURE RANGE Dynamic range RANGE Inte output STD 5x10 4 RIU 1 4 512x10 6 RIU 5x10 4 RIU 1 0V WIDE 5x10 3 RIU 1 4 512x10 5 RIU 5x10 3 RIU 1 0V Note The baseline noise and drift when set to WIDE is l...

Страница 55: ...he measurable range is 7x10 4 RIU 1 0V MEASURE RANGE STD and 9 9x10 3 RIU 1 0V MEASURE RANGE WIDE When exceeding the linear range connect to the recorder output terminal instead of the integrator outp...

Страница 56: ...ith 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...

Страница 57: ...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 Figure 8 2 10 50mL min tubing arrangement Tubing OD 1 6...

Страница 58: ...ge 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 chromatogram...

Страница 59: ...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...

Страница 60: ...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 d...

Страница 61: ...t 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 AUT...

Страница 62: ...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 Cha...

Страница 63: ...e 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...

Страница 64: ...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 d...

Страница 65: ...because of the optical characteristics of the detector changing This requires resetting the constant K1 and K2 The K1 value is used when MEASURE RANGE is set to STD and the K2 value is used when MEAS...

Страница 66: ...ection 8 Pump Water 1mL loop Injector Internal diameter of 0 25mm or less Integrator or recorder RI 2031 Port No 6 Port No 3 Figure 9 5 Tubing and Wiring Arrangement for Calibration 9 4 2 Standard sol...

Страница 67: ...mL min may be used 2 Set MEASURE RANGE to STD refer to chapter 7 3 Wait for the drift to decrease to 1 0x10 7 RIU min or less Note On the LCD display 0 1x10 6 RIU min or less corresponds to a 0 1 RIU...

Страница 68: ...e PRGM RUN key to execute the built in calibration program The RIU value will be 160 1 RIU Calibration screen Figure 9 6 Calibration screen 2 In the calibration screen once the baseline has stabilized...

Страница 69: ...Note Calibration of constants K1 and K2 is performed by executing build in calibration program at the same time 9 4 5 Calibration constant confirmation and setting After performing calibration outline...

Страница 70: ...VALUE x xxx RIU xxxx x NORM 64 STD 0 000 ON OFF TEMP xx x yy C 0 000 ON OFF MONIT MONIT PARAMETER SET 3 SET K2 VALUE K2 VALUE x xxx RIU xxxx x EDIT ENTER MONIT EDIT ENTER K1 VALUE x xxx RIU xxxx x MO...

Страница 71: ...this will not cause a problem during solvent replacement proper calibration is not possible if bubbles are introduced immediately before or after standard solution injection Display the preamplified...

Страница 72: ...below 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...

Страница 73: ...OFF MONIT Serial number menu Use the keys to display the menu below Figure 9 10 Serial Number Input Method 9 7 Power Fuse replacement Warning When changing the power fuses be sure to disconnect the po...

Страница 74: ...l 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 a...

Страница 75: ...ll and the area to the right is called the reference cell ns Refractive index of sample nR Refractive index of reference solvent Angle of deflection exaggerated in the figure actual value is 10 2 degr...

Страница 76: ...nges then the refractive index changes thereby changing the angle of deflection in accordance with equation 1 The light image striking the primary photodiode will therefore shift in the horizontal pla...

Страница 77: ...wn in the bottom half of Figure 10 3 and a difference between the output of PD1 and the output of PD2 is generated Since the output is proportional to the surface area receiving light the output diffe...

Страница 78: ...ransmittance and both of these factors can change over time On the other hand the sum of the outputs from PD1 and PD2 hereafter called SUM is proportional to the light source intensity and flow cell t...

Страница 79: ...he effluent passes through the sample cell and then through the reference cell before being discharged When the purge valve is OFF the instrument is switched to the flow line indicated by the solid ar...

Страница 80: ...n passes through the heat exchanger and then through the sample cell The reference side flow line is indicated by the dotted arrow in Figure 10 5 When replacing the solvent in the reference cell draw...

Страница 81: ...able 10 1 and Table 10 2 Table 10 1 Internal volume using 10mL min tubing Flow line Volume Port No6 Sample cell ca 70 L Sample cell Port No3 ca 300 L Table 10 2 Internal volume using 10 50mL min tubin...

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