Jasco CD-1595 Operation Manual

Jasco CD-1595 Operation Manual

Circular dichroism chiral detector
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Summary of Contents for Jasco CD-1595

  • Page 1 (217) 352-9330 | Click HERE Find the Jasco CD-1595 at our website:...
  • Page 2 JASCO MODEL CD-1595 CIRCULAR DICHROISM CHIRAL DETECTOR OPERATION MANUAL 0302-0402B Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 3: Safety Considerations

    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.
  • Page 4 If a warning label peels off the instrument or becomes illegible, contact your local JASCO distributor (see list on the back cover of this manual) for a replacement label. Be sure to indicate the part number (P/N) on the label.
  • Page 5 Xenon Lamp Warning Label (P/N: 0822-0077A) 警   告 When replacing the Xenon lamp, refer to the operations manual キセノンランプには高圧ガスが封入 (P/N 0301-0193A) and follow the されています。機械的衝撃を与えると instructions carefully. 破裂し怪我をする恐れがあります。 交換の際は保護具をご使用ください。 WARNING WEAR EYE AND FACE PROTECTION AND PROTECTIVE GLOVES WHEN ACCESSING THE XENON LAMP. THE XENON LAMP CONTAINS HIGH PRESSURE GAS AND CAN BURST UNDER MECHANICAL STRESS.
  • Page 6 (6) High voltage inside warning Label (P/N: 0822-0145A) WARNING High voltage inside!! High voltage inside!! High voltage inside!! High voltage inside!! Disconnect the power cord before Disconnect the power cord before Disconnect the power cord before Disconnect the power cord before removing the instrument cover. removing the instrument cover. removing the instrument cover. removing the instrument cover. A voltage of 200 V or greater is generated during the operation of the detector. Be sure to turn off the power and disconnect the power cord before performing maintenance.
  • Page 7 Carrying the Instrument This instrument weighs approximately 21 kg. When carrying the instrument, be sure to hold the instrument as shown in Fig. 3. Figure 3 Grip Locations for Carrying the Instrument Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 8: Preface

    When not using the instrument, keep this manual stored in a safe place. Should this instruction manual be lost, order a replacement from your local JASCO distributor. The manuals for this instrument consist of an operations manual and a maintenance manual.
  • Page 9: Installation Conditions

    Installation Conditions To ensure safe operation, the following recommendations should be observed: Do not operate the instrument under voltage fluctuations exceeding 10% of the recommended line voltage. Large fluctuations may cause the instrument to fail. Use a three-pronged electrical outlet with a ground. When only a two-pronged socket is available, use an adapter and be sure to connect the ground wire of the adapter.
  • Page 10: Maintenance

    (2) Software prohibitions: Copying of software or related materials for purposes other than backup is prohibited. Transfer or authorization of the use of Jasco software to or by a third party is prohibited. Disclosure of confidential information related to Jasco software is prohibited.
  • Page 11: Warranty

    This product is warranted for a period of one year from the date of delivery. If any defects should occur in the product during this period of warranty, JASCO will repair or replace the defective part(s) or product free of charge.
  • Page 12 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 13: Table Of Contents

    Table of Contents Safety Considerations ..............i Preface ...................vi Installation Conditions..............vii Maintenance ................viii Notices ..................viii Warranty ..................ix 1. GENERAL DESCRIPTION SPECIFICATIONS INSTRUMENT ................1-1 1.1 General Description ................1-1 1.2 Specifications..................1-2 2. NAMES AND FUNCTIONS OF PARTS/ASSEMBLY .....2-1 2.1 Front Panel ..................2-1 2.2 LCD and Keypad................2-2 2.3 Flowcell Assembly ................2-4 2.4 Rear Panel ..................2-5 3.
  • Page 14 5. KEY OPERATION USING [SHIFT] KEY......5-1 5.1 Outline of Key Operation..............5-1 5.2 [SHIFT] [0]: UV Signal output setting for integrator.......5-2 5.3 [SHIFT] [1]: Performing Optical Zeroing Checking Preamplifier Output Level..............5-2 5.4 [SHIFT] [2] : Lamp Off Timer ............5-2 5.4.1 Setting Lamp Off Timer ..............5-3 5.4.2 Turning Lamp On after Lamp Off Timer activated......5-3 5.5 [SHIFT] [3]: Setting Recorder Range ..........5-3 5.6 [SHIFT] [4]: Selecting Recorder Output Mode .........5-4...
  • Page 15: General Description And Specifications Of Instrument

    Advances in chiral detection technology, however, have not yet met these demands in terms of sensitivity and selectivity. The new CD-1595 detector is expected to meet the requirements.
  • Page 16: Specifications

    1.2 Specifications Light source : Hg-Xe lamp(150W) Measurment wavelength range : 220-420 nm Measurement range: 1000 mdeg (300nm) in 12 steps Spectral bandwidth : 20 nm Wavelength accuracy : ±5 nm Sensitivity (S/N=2) : 0.05 mdeg/cm (290 m), 0.1 mdeg/cm (240 nm) 0.1 g (Camphor-10-Sulfonic acid, 290 nm) 0.01 g (Pantoy Lactone, 240 nm) Baseline drift :...
  • Page 17: Names And Functions Of Parts/Assembly

    2. NAMES AND FUNCTIONS OF PARTS/ASSEMBLY This chapter contains the names and functions of the parts on the instrument panels. 2.1 Front Panel MODE W.L(nm) GAIN AU RESPONCE SHIFT SCAN PRGM AUTO ZERO PRGM CLEAR MARK MONIT EDIT/ENTER Figure 2.1 Front panel. Name of part Description (1) Flowcell assembly...
  • Page 18: Lcd And Keypad

    2.2 LCD and Keypad MODE W.L(nm) GAIN RESPONCE SHIFT SCAN PRGM AUTO ZERO PRGM CLEAR MARK MONIT EDIT/ENTER Figure 2.2 LCD and keypad Name of part Function LCD display Displays the operation status, parameters, and messages. [AUTO ZERO] Used to set the integrator and recorder outputs to zero. [PRGM RUN] Starts/stops a time program.
  • Page 19 [PRGM] Changes to time program mode. Numeric keys. [0] 〜[9][・] Increment/decrement keys. [▼] , [▲] Clear erroneous entry of parameters. It also clears error [CLEAR] messages. Used to edit/enter parameters. [EDIT/ENTER (NOTE) Perform optical zero adjustment by turning the CD ZERO knob before activating the Autozero.
  • Page 20: Flowcell Assembly

    2.3 Flowcell Assembly Figure 2.3 Flowcell Assembly Name of part Description (1) Cell body The light passes through the hole of the cell body. (2) Cell panel The cell panel is fixed to the cell body. (3) Lock screws Used to secure the flowcell assembly in position to the detector.
  • Page 21: Rear Panel

    2.4 Rear Panel Terminal Block(1) Terminal Block(2) Parts(3) Connectors(5) Labels(4) Figure 2.4 Rear Panel Terminal Block (1) Terminal Description CD 1V/deg CD signal output for integrator. 1V corresponds to 1 + / - / G deg. AU 1V/AU UV signal output for integrator. 1V corresponds to 1 + / - / G AU.
  • Page 22 230V: 220 – 240V Connectors(5) Connectors Description LC-Net Used when controlling the detector via Jasco system controller. RS-232C Connection for controlling the detector through the RS-232C channel.(Option) Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 23: Power-On, Self-Diagnostic Test And Power-Off

    3. Power-On, Self-Diagnostic Test and Power-Off 3.1 Power-on and Self-Diagnostics Turning the power on will automatically start the power-on self-diagnostics. The following items/functions are checked during the self-diagnostics. • Memories C-MOS RAM • DC power supply • Wavelength drive mechanism •...
  • Page 24: Turning Power Off

    Wavelength, sensitivity range and response shown are those set when the instrument power was turned off in the last use. 3.2 Turning power off To turn off the power, just turn the POWER switch off. Parameters set during the operation such as wavelength, sensitivity range and response are stored on the C-MOS RAM and these values will be automatically resumed when the instrument power is turn on again.
  • Page 25: Operation

    Figure 4.1 Connection of input/output terminals on the rear panel and the other instruments. 2) Connect column outlet tubing to the inlet port of the CD-1595 flow cell. Use 1/16 in. OD x 0.25 mm I.D. tube and 1/16 in. fittings.
  • Page 26 3) Connect a tube (16 in. O.D. x 0.5 mm I.D.) to the outlet port of the flow cell. The total length of the tube should be less than 1m. <CAUTION> The maximum allowable pressure of the flow cell is 15 bar (1.5MPa). Do not use a narrow bore tube, e.g.
  • Page 27: Setting Parameters

    4.2 Setting Parameters In the normal operation mode, the detector monitors CD and UV signal at a set wavelength and with set sensitivity range and response. These parameters must be set at suitable values to the sample to be measured. This section describes how to set WAVELENGTH, GAIN, RANGE and RESPONSE.
  • Page 28: Changing Wavelength

    Changing WAVELENGTH 4.2.1 The wavelength, in general, should be selected so that the CD signal becomes maximum. This wavelength can be found by referring to literature, or to spectra obtained by stop-flow scanning at chromatographic peaks. Wavelength range: 220 – 420nm NORM Monitor Screen (Changing Wavelength to 230nm)
  • Page 29: Changing Gain

    Changing GAIN 4.2.2 The GAIN changes the gain of the CD signal amplifier. Normally, GAIN should be set to “X10”. In case a sample compound gives so strong CD signal that may saturate the amplifier and “CD Sig.: 3.9000 V” is displayed(see Fig.5.2) , the setting “X1”...
  • Page 30: Changing Range

    Changing RANGE 4.2.3 RANGE setting attenuates the output to recorder so that 10mV full scale corresponds to the RANGE parameter value. Input range: CD RANGE: 0.0005〜1.28 deg, S (Short) UV RANGE : 0.001〜2.56 AU, S (Short) (G FACTOR: 1E-5〜2.56E-2, S (Short)) Monitor screen UV RANGE input screen CD   RANGE :   0.0001...
  • Page 31: Changing Response

    Changing RESPONSE 4.2.4 The RESPONSE is the parameter that sets the detector response time. The RESPONSE can be selected from FST(fast), STD(standard) and SLW(slow). Normally, it should be set to STD. Normal Operation Mode Display NORM   291    X10 0.000 0.000  STD [EDIT/ENTER] [EDIT/ENTER] NORM   291    X10 Blinking 0.000 0.000  STD ▲...
  • Page 32: Measurement

    4.3 Measurement After the basic parameters setting completed, start measurement. 1) After the baseline has been stabilized, press [SHIFT] [1] to display the CD/UV signal screen. Monitor Screen NORM    291     X10   0.000  0.000     STD [SHIFT] [1] [MONITOR] Signal Voltage  CD/UV Signal Screen CD Sig:0.000 V UV Sig:0.000 V UV Signal Voltage Figure 4.7 Preamplifier Output 2) Turn OPT.CD ZERO knob(see Fig.2.1) to adjust the CD signal voltage to become within 0±0.03V.
  • Page 33: Error Messages

    4.4 Error Messages Table 4 .1 lists the error messages that can be detected by the CD-1595 during operation. When a problem is detected, a message will appear on the LCD. Press [CLEAR] to return to the monitor screen. If the problem reoccurs, the error message will reappear after approximately ten seconds.
  • Page 34: Key Operation Using [Shift] Key

    5. KEY OPERATION USING [SHIFT] KEY 5.1 Outline of Key Operation Table 5.1 outlines the key operation using [SHIFT] key. Function [SHIFT] [0] UV Signal output screen for Integrator. 1V/AU or 1V/2AU can be selectable. [SHIFT] [1] Preamplifier Output display screen. This function is used to perform optical zeroing as well as checking the conditions of the lamp, other optical elements, presence of air bubbles in the flow cell.
  • Page 35: Shift] [0]: Uv Signal Output Setting For Integrator

    5.2 [SHIFT] [0]: UV Signal output setting for integrator 1V/AU or 1V/2AU can be selectable. NORM    291     X10    Monitor screen 0.000  0.000    STD [SHIFT] [0] [MONITOR] [EDIT/ENTER] INTE OUT SCALE INTE OUT SCALE    1.0V/1AU(2AU)    1.0V/1AU(2AU) [EDIT/ENTER] [▼] [▲]or Blinking Integrator output selection screen Figure 5.1 Integrator output selection 5.3 [SHIFT] [1]: Performing Optical Zeroing and Checking Preamplifier Output Level Pressing [SHIFT] [1] keys will bring up the “preamplifier output level”...
  • Page 36: Setting Lamp Off Timer

    Setting Lamp Off Timer 5.4.1 Input time range: 0(OFF) – 99.9 hours(0.1 hour increment) NORM    291     X10    Monitor screen 0.000  0.000    STD [SHIFT] [2] [MONITOR] [EDIT/ENTER] LAMP  OFF  TIMER LAMP  OFF  TIMER        xx H      xx(yy) H [yy][EDIT/ENTER] Blinking Lanp off timer screen (Time has been set to (yy).) Figure 5.3 Setting Lamp Off Timer When the Lamp Off Timer is set, the lamp will be automatically turned off when the time is up.
  • Page 37: Shift] [4]: Selecting Recorder Output Mode

    CD RANGE:  0.0001 NORM    291      X10 AU RANGE:  0.0100 Monitor screen (G RANGE:  1E‑5) 0.000  0.000    STD   Blinking ][EDIT/ENTER] [MONITOR] ▲  ▼ [SHIFT] [3] ][EDIT/ENTER] ▲  ▼ CD RANGE:  0.0001 CD RANGE:  0.0001 AU RANGE:  0.0100 AU RANGE:  0.0100 Blinking (G RANGE:  1E‑5) (G RANGE:  1E‑5) [EDIT/ENTER]     Figure 5. 5 Setting recorder range Selectable range CD RANGE: 0.0005〜1.28 Degree and S(Short) 13steps AU RANGE: 0.001 〜...
  • Page 38: Shift] [5]: Shifting Integrator Output Zero Level

    5.7 [SHIFT] [5]: Shifting Integrator Output Zero Level The CD signal usually appears both positive and negative directions by its nature. However most integrators can accept an input voltage between – 10mv and +1v. This function allows to shift up the voltage on the integrator output terminal , thus preventing the output from going below the –10mv limit even for negative peak or negative drift.
  • Page 39: Setting Integrator Output Zero Level

    Integrator    output 0 mV 0 V Zero shift  ‑10 mV Integrator out of range Integrator   output +50 mV Zero shift  Data processing  as a negative peak 0 V Figure 5.8 Negative peak vs. integrator dynamic range . Setting integrator output zero level 5.7.1 0,5,10,30,50,100,500,1000mV can be selectable as the integrator output zero level.
  • Page 40: Shift] [6]: Checking Cumulative Lamp Operation Time

    5.8 [SHIFT] [6]: Checking Cumulative Lamp Operation Time The accumulated lamp operation time can be checked to estimate when the lamp should be replaced. NORM    291     X10  0.0000 0.000   STD Monitor screen [SHIFT] [6] [MONITOR] LAMP OPERAT TIME      120.5 H Lamp operation time screen Figure 5.10 Checking cumulative lamp operation time. Artisan Technology Group - Quality Instrumentation ...
  • Page 41: Shift][7]: Changing Recorder Output Polarity

    5.9 [SHIFT][7]: Changing Recorder Output Polarity This function has no effect on the integrator output. NORM     291    X10 Monitor screen 0.000  0.000   STD [SHIFT] [7] [MONITOR] [EDIT/ENTER]     POLARITY     POLARITY         +     +(−) ][EDIT/ENTER] ▲  ▼ Blinking Polarity has been changed to (‑). Setting polarity Figure 5.11 Changing recorder output polarity. 5.10 [SHIFT][8]: Selecting Autozero Mode This function is used to control autozeroing when wavelength or gain parameters is changed or when a signal enters the MARKER IN terminal on the back panel.
  • Page 42: Shift][9]

    5.11 [SHIFT][9]: Pressing [SHIFT] [9] keys will bring up the “g factor monitoring screen”. Calculated g factor is displayed on this screen in real time. CD signal and absorbance are also displayed on this screen. NORM     291    X10 Monitor screen 0.000  0.000   STD [MONITOR] [SHIFT] [9] g factor monitor screen G FACT= X.XXXXXX g factor is displayed at here.
  • Page 43: Operations In Program Mode

    6. Operations in Program Mode 6.1 Description In the program mode, the parameters shown below can be changed according to a time program. Time programs can contain up to 64 steps, and up to 10 program files can be stored in the memory of the instrument. •...
  • Page 44: Switching Between Normal Operation Mode And Program Mode

    Note 1: If an incorrect value is entered, press [CLEAR] while the parameter value is blinking, then enter the correct value. Press [EDIT/ENTER] to enter the value. Note 2: When the file number of a file that already contains a time program is designated, the previous program will be loaded.
  • Page 45: Editing Programs

    Editing Programs Editing initial parameters 6.4.1 Wavelength and Response are set sequentially as initial parameters. Note: Gain set in the normal operation mode remains in effect while the instrument is switched to program mode. Press [▼] key while the program monitor screen is displayed. The Step 0 screen (Fig.
  • Page 46: Editing The Time Program

    Editing the time program 6.4.2 Time program input 6.4.2.1 Time program input example: As an example, the following time program will be created. First, wavelength will be changed to 250 nm one minute after starting the program under the initial parameters. Next, spectrum measurement will be performed at two minutes after starting the program.
  • Page 47 Time program functions and their number 1) Wavelength 1:WAVELENGTH 2) CD output range 2:CD RANGE 3) UV output range 3:AU RANGE 4) Spectrum measurement 4:MEASURE 5) Auto zero 5:AUTO ZERO Time program input method: The input sequence is as follows: time, function, value relative to the function. 1) From the initial conditions screen (Step 0 screen), press [▼] key to advance to the Step 1 screen.
  • Page 48 Correcting time programs 6.4.2.2 When times and functions are incorrect: 1) Use the [▼] key to advance to the incorrect step. 2) Enter the correct settings, starting with time. When changing a setting without changing the time or function: 1) Use the [▼] key to advance to the incorrect step. 2) Skip correct settings by pressing [EDIT/ENTER] until the desired input screen appears.
  • Page 49: Program Example

    3) Press the [MONIT] key to return to the monitor screen. Inserting steps into a time program 6.4.2.4 This section describes how to insert a single step into a time program contained in a file. 1) Press [SHIFT][▼] to advance to the final step in the program. 2) Press [▼] to advance to a blank step.
  • Page 50 Table 6.2 Peak Detection Conditions Peak number/ wavelength TIME RANGE Note Condition (nm) INITIAL 0.04 0.04 20.0 0.04 27.0 1.28 41.0 0.001 44.0 0.001 * (*) Immediately following autozeroing The time program for the above example is shown in Fig. 6.7. Artisan Technology Group - Quality Instrumentation ...
  • Page 51 Program mode monitor screen [MONIT] PRG 5    300   X10 PRG 5      T: 0.0 0.0000 0.000  STD W.L:300 RSPN:STD ▲ ▼ Initial parameter screen   PRG5    INITIAL Wavelength 300 nm Range  0.04  W.L:300  RSPN: STD ▲ ▼ Wavelength changed to 270 nm PRG   ST 1   T: 8.0 after 8 minutes.     W.L  270 nm ▲ ▼ PRG   ST 2   T:20.0 Wavelength changed to 250 nm after 20.0 minutes.     W.L  250 nm ▲ ▼ PRG   ST 3   T:27.0 Range changed to 1.28 after 27.0 minutes.  AU  RANGE   1.28 ▼ ▲ PRG   ST 5   T:41.0 Range changed to 0.001 after 41.0 minutes. AU   RANGE   0.001 ▼ ▲ PRG   ST 6   T:44.0 Autozero executed ...
  • Page 52: Time Program Operation

    6.5 Time Program Operation Running a time program 6.5.1 Start the program from the program monitor screen. Starting the time program: Press the [PRGM RUN] key after the baseline stabilizes. The time program will start. The [PRGM RUN] key lamp will light, showing that a time program is currently in progress.
  • Page 53: Key Operations In Spectrum Mode

    This chapter outlines the operating procedures for the SPECTRUM mode. 7.1 Outline In addition to simultaneous monitoring of CD and UV chromatograms, the CD-1595 chiral detector allows simultaneous CD and UV spectral measurements by stop-flow scanning. Please note that this function is primarily meant to find the optimum wavelength for the compound of interest to be monitored.
  • Page 54 4) Enter "n" and press [EDIT/ENTER] after step 3) to set memory no “n”. Refer to Section 7.3. 5) Press [MONIT] to return to NORMAL OPERATION or TIME PROGRAM mode. [MONIT] Normal operation mode  monitor screen [SCAN] [MONIT] SPECTRUM MEASURE BASE=0  MEAS=1 0 Blinking Spectrum mode initial screen [0] [EDIT/ENTER] [1] [EDIT/ENTER]  BASELINE MEASURE SPECTRUM MEASURE...
  • Page 55: Baseline Spectrum Acquisition

    7.2 Baseline Spectrum Acquisition The measured spectrum will include the spectrum of the sample to be measured as well as the solvent and instrument backgrounds. In order to obtain a spectrum of the sample only, the backgrounds must be subtracted from the measured spectra. This subtraction process is called baseline correction.
  • Page 56: Spectra Output

    Spectrum mode initial screen SPECTRUM MEASURE BASE=0  MEAS=1 1 Blinking Select spectrum  [1] [EDIT/ENTER] measure mode SPECTRUM MEASURE Memory NO. select screen (Input range:0〜9) SET MEMORY NO 0 [5] [EDIT/ENTER] Select memory NO. 5 SPECTRUM MEASURE  PUSH PROG RUN [PRGM RUN] Start spectrum measurement MEAS   XXX MEM5 Measuring spectrum  YY.YY‑Z.ZZZ Figure7.3 Procedure for measuring a spectrum 7.4 Spectra Output This section outlines the procedure for outputting spectra (obtained in Sections 7.2 and 7.3) to the recorder and integrator output terminals.
  • Page 57 NORM   250   X10 Monitor screen 0.000 0.000  STD [SHIFT] [SCAN] [MONIT] SPE.REC.OUT Spectrum output screen  BASELINE [▲]  SPE.REC.OUT Select spectrum memory NO.  MEMORY NO. 5 [EDIT/ENTER] SPECTRUM OUTPUT #5 PUSH PRGM RUN [PRGM RUN] OUTPUT XXX MEM5 Spectrum is outputting  YY.YY‑Z.ZZZ Wavelength Absorbance CD signal Figure7.4 Procedure for outputting a spectrum (NOTE 1) Baseline spectrum has been measured before outputting sample spectrum. If not so, the outputted sample spectrum will not be output.
  • Page 58: Principle

    8. Principle 8.1 CD Measurement Principle Hg-Xe Lamp Lens1 Polarizer Grating Lens 2 Flowcell Detector Fig.8.1  Optical diagram The light emitted from the light source(Hg-Xe Lamp) is collimated by the Lens 1 and directed to the polarizer. The collimated light(unpolarized) is converted to linearly polarized light by the polarizer.
  • Page 59 Electric signal DC signal No CD active component are in the flow cell. Time Fig.8.2  No active components in the flow cell Electric signal AC signal CD active component are in the flowcell. Time Fig.8.3  Active components in the flow cell Artisan Technology Group - Quality Instrumentation ...

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