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...
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.
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.
(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.
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.
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.
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...
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.
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.
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...
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 •...
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.
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.
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.
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)
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”...
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...
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 ▲...
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.
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.
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.
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.
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.
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.
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 ...
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.
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.
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. •...
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.
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.
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.
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 ...
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.
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...
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.
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.
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 ...
Need help?
Do you have a question about the CD-1595 and is the answer not in the manual?
Questions and answers