Jasco J-810
Jasco J-810
Jasco J-810
SPECTROPOLARIMETER
Hardware/Function Manual
JASCO Corporation
i
(2) Location of Warning Labels
The instrument is labeled with the following warnings. Use care not to damage or
tear the labels. Should the labels be stained or torn, contact your local JASCO
distributor with its part number.
Part number:0822-0127A
. The xenon lamp is made of quartz glass and is filled with high-pressure gas (5 to 10
atm. pressure, about four times when the lamp is lit).
Twisting, bending or impact can burst the lamp, causing danger with glass
fragments. Never open the lid of the light source unit if the lamp is lit or hot.
. When handling the xenon lamp, wear protective clothing such as a thick, long-
sleeved shirt, a mask, thick gloves, etc.
. Before replacing the xenon lamp, turn the lamp off and allow it to cool for about 30
minutes.
When replacing the xenon lamp, be careful not to give an impact to the lamp.
Never twist the lamp by holding it at both ends.
. Do not mistake the mounting direction (polarity) of the lamp. The cathode will be
damaged if the lamp is mounted incorrectly, rendering the lamp inoperable.
. Do not touch the glass portion of the xenon lamp with bare skin.
. If the glass portion of the xenon lamp is contaminated, wipe it with clean gauze
moistened with alcohol.
. After removal and before disposal, place the xenon lamp in its case, and store the
case in a safe place. If the case is not available, carefully wrap the lamp in
foamed plastic or other protective wrapping, and store it in a same place.
. When disposing of the xenon lamp, carefully wrap it in a cloth, smash it with a
hammer, and dispose of it as hazardous material.
WARNING! Fuse Rating (②in Fig. 1)
Part number:0822-0102A
ii
Use only fuses of the designated rating to protect both the operator and the
equipment from fire and other hazards. When replacing the fuse, turn OFF the ″
Power″ switch and unplug the power cable from the outlet to avoid electric shock.
WARNING! Grounding (③in Fig. 1)
Part number:0822-0109A
If the instrument is operated without being grounded properly, the operator may be
subjected to electric shock. Correctly ground the instrument using the grounding
terminal on the switchboard. Do not use gas or water pipes for grounding, because
these pipes are often made of non-conductive material.
2
3
2
3
Fig. 1
iii
Introduction
This manual is intended to serve as a guide for using the Model J-810
spectropolarimeter, both for experienced and first-time operators.
Prior to operating the instrument, the operator should carefully read and thoroughly
understand the contents of these manuals. In addition, the ″Measurement″,
″ Analysis ″ and ″ CD-ORD Measurement Method ″ instruction manuals should be
understood in full. These three manuals should be kept at your hand at all time
during operation of the instrument. After operation, keep these manuals in your file.
Should the manuals be lost, contact your local JASCO distributor for an additional
copy.
Installation Requirements
Install the instrument in a location where the following conditions are satisfied. The
instrument should be installed in a room that is maintained at a constant temperature
and humidity, because the spectropolarimeter is sensitive to atmosphere fluctuations.
. Room temperature 20 ±5°C
. Humidity lower than 70%
. Not exposed to direct sunlight
. Not in the proximity of harmful or corrosive gas
. Not exposed to a high-intensity light source
. Not in the direct path of air currents emanating from air conditioners or other
equipment
. Relatively free of vibration
. Not in the proximity of a high-intensity magnetic or electromagnetic field
. For the 450W light source, within the proximity of a water supply (flow rate : 2 λ
2
/min, pressure : 0.5~2.0 kg/cm ). Cooling water piping : 10 m in length, inside
diameter : 12 mm
2
Note: Do not use water at more than 2.0 kg / cm pressure.
. Within the proximity of equipment that supplies nitrogen gas. (flow rate : more
than 3 λ/min). Nitrogen gas tube : 3 m in length, inside diameter : 9.5 mm.
. Within the proximity of nitrogen gas ventilator.
iv
Contents
1. Overview and Specifications .........................................................1
1.1 Overview................................................................................................. 1
1.1.1 Principles of operation ...................................................................... 1
1.1.2 Optical system .................................................................................. 2
1.1.3 Electrical system............................................................................... 3
1.2 Specifications.......................................................................................... 4
2. Unpacking and Installation ............................................................7
2.1 Unpacking ............................................................................................... 7
2.2 Installation Requirements ....................................................................... 7
2.3 Reassembly ............................................................................................ 8
2.3.1 Removing the cushion from the main unit......................................... 8
2.3.2 Installing the modulation element ..................................................... 9
2.3.3 Installation the detector unit ............................................................ 10
2.3.4 Connecting the cables and tubes.................................................... 11
3. Names of Functions of Components ...........................................14
3.1 Overall View.......................................................................................... 14
3.2 Panels................................................................................................... 17
3.3 Sample Chamber .................................................................................. 20
3.4 Detector Unit ......................................................................................... 22
4. MAINTENANCE ..........................................................................23
4.1 Light Source Check and Replacement.................................................. 23
4.2 Energy Check ....................................................................................... 25
4.3 Wavelength Accuracy Check and Adjustment ...................................... 27
4.4 CD Scale Check and Adjustment.......................................................... 28
4.5 Test Signal Check................................................................................. 30
5. TROUBLESHOOTING ................................................................31
v
1. Overview and Specifications
1.1 Overview
1.1.1 Principles of operation
When linearly-polarized light passes through an optically-active substance, its two
circularly-polarized components (right and left circularly-polarized beams of light) travel
at different speeds, and are absorbed in differing degrees by the substance. Thus, the
light passing through the substance is elliptically polarized, and the substance is said to
have ″Circular Dichroism (CD)″. The magnitude of circular dichroism is usually
expressed in terms of molecular elliptically [θ], which is determined according to the
following formula :
4500
θ = ( ε L − ε R ) log e 10 (1)
π
where, εL and εR are the molecular extinction coefficients for the right and left circularly-
polarized beams of light. The difference (∆ε) between εL and εR is determined using
the following formula :
1 I
∆ε = ε L − ε R = log10 R (2)
LC IL
[θ ] = 4500 log e 10 log10 I R (3)
π LC IL
In equation (2) and (3), L represents the thickness (cm) of the absorbing layer, and C
represents the molar concentration, IR and IL represent the intensities of the right and
left circularly-polarized beams of light, respectively, after passing through the substance.
Theoretically, the molecular ellipticity can be derived using equation (3). However, in
practice, determining [θ] with a high degree of accuracy is very difficult using equation
(3), because the value of IR.IL is nearly 1. To avoid this difficulty, we substitute the
following quantities.
1
IA = (I R + I L ) (4)
2
S = IR − IL (5)
Since S/2ΙA is less than 1, equation (3) can be re-expressed as follows, by substituting
the expressions from equations (4) and (5) :
1
S
1+
[θ ] = 4500 log e 10 log10 2SI A
π LC
1− (6)
2I A
4500 S
= log e 10 log10 e
π LC IA
Thus, the ratio between IA and S can be approximated with an accuracy sufficient for
practical application.
Given that EA and ES represent the output voltages of the photomultiplier tubes
corresponding to light intensities IA and S respectively, S/IA = ES/EA. By substituting
this expression, equation (6) can be expressed as follows.
[θ ] = 4500 log e 10 E S log10 e (7)
π LC EA
[θ ] = 4500 log e 10 E S G log10 e (8)
π LC E A G
where G represents the amplification factor of ES. Since the value ESG can be brought
very close to the value of EA by choosing an appropriate value for G, [θ] can be
determined with a high degree of accuracy.
M0
LS
S1 M2
M1
M4 P1
P2 S2 M3
O-ray
E-ray
M5 S3 L F CDM SH PM
M0, M1, Mp, M2 ~ M5 : Mirrors LS : Light source
S1 ~ S3 : Slits P1 : First prism (horizontal optical axis)
P2 : Second prism (vertical optical axis) O-ray : Ordinary ray
E-ray : Extraordinary ray L : Lens
F : Filter CDM : Modulator
SH : Shutter PM : Photomultiplier tube
Fig. 1.1 Block diagram of optical system
2
A xenon lamp is used as the light source. The light emitted from the xenon lamp is
converged by the M1 mirror into the S1 entrance slit. The optical system between the
S1 entrance slit and the S2 intermediate slit is referred to as the first monochromator,
and the optical system between the S2 intermediate slit and the S3 exit slit is referred to
as the second monochromator. Such an optical system, comprised of two
monochromators, is known as a double monochromator. The capability of a double
monochromator reducing stray light makes it indispensable for CD measurement.
The instrument uses crystal prisms (P1 and P2) that have different axial orientations, so
that the light that passes through the monochromator is not only monochromated, but
also linearly polarized, and oscillates in the horizontal direction.
This linearly-polarized light is modulated by the modulator into right and left circularly-
polarized beams of light. The modulator subjects quartz to mechanical stress in order
to produce circular polarization in the crystal, based on the principle of the Piezo effect.
When a sample with circular dichroism is placed in the sample chamber, the intensity, I,
of the transmitted light changes as shown in Fig. 1.2 :
Intensity S
IL IR IA
Time
Fig. 1.2 Intensity of transmission light
The relationship between the minimum and maximum intensities and the right and left
circularly-polarized light depends on whether the value ER is smaller or larger than the
value EL. In Fig. 1.2, the solid line represents the case when ER is greater than EL, and
the dotted line represents the case when ER is smaller than EL. For the definitions of IA
and S, refer to Section 1.1.1 ″Principles of operation″.
When light with intensity fluctuations such as that shown in Figure 1.2 is incident upon
the photomultiplier tube, the output signal consists of DC components equivalent to IA,
and AC components equivalent to S.
3
The DC component is separated between the preamplifier and the CD amplifier, and is
compared with the reference voltage in order to control the voltage of the PM power
supply. This voltage is also applied to the PM detector, changing the PM sensitivity.
The AC component is converted to a digital signal after being amplified by the
preamplifier and the CD amplifier.
The main unit and the personal computer communicate through the RS-232C interface.
All parameters of the main unit are designated from the personal computer. The CD
signal and PM voltage are communicated to the personal computer through the RS-
232C interface after being converted to digital signal and stored in the buffer memory.
Sensor
External
I/O Input 1
A/D D/A
RS-232C I/F
External
Input 2
Buffer Memory
CPU
Program Memory
Main Unit
PC
RS-232C I/F
1.2 Specifications
Light source : 150W air-cooled xenon lamp, or 450W water-cooled xenon
lamp
Detector : Head-on photomultiplier tube
Modulator : Piezoelastic modulator
Measurement wavelength range : 163 to 900 nm (standard detector)
163 to 1100 nm (optional detector)
Wavelength accuracy : ±0.2 nm at 163 to 180 nm
±0.1 nm at 180 to 250 nm
±0.3 nm at 250 to 500 nm
4
±0.8 nm at 500 to 800 nm
±2.0 nm at 800 to 1100 nm
Wavelength repeatability : ±0.05 nm at 163 to 250 nm
±0.1 nm at 250 to 500 nm
±0.2 nm at 500 to 1100 nm
Spectral bandwidth : 0.01 to 15 nm
Slit width : 1 to 3000 µm
Response : 0.5 msec to 32 sec
Scanning system : Continuous scan
Step scan (Fixed response and auto response system)
Scanning speed : to 10000 nm/min (continuous scan)
Data interval : 0.025 to 10 nm (continuous scan)
0.1 to 100 nm (step scan)
0.5 msec to 60 min (time change)
CD full scale : ±10, 200, 2000 mdeg
CD resolution : 0.0005 mdeg (at ±10 mdeg full scale)
0.01 mdeg (at ±200 mdeg full scale)
0.1 mdeg (at ±2000 mdeg full scale)
Stray light : Not more than 0.0003% (200 nm)
RMS noise : 185 nm : 0.050 mdeg (150W light source)
0.045 mdeg (450W light source)
200 nm : 0.040 mdeg (150W light source)
0.035 mdeg (450W light source)
500 nm : 0.035 mdeg (150W light source)
0.035 mdeg (450 light source)
(spectral bandwidth 1nm, response 16 sec)
Baseline stability : 0.03 mdeg/hr
(spectral bandwidth 1 nm, response 32 sec, wavelength 290
nm)
UV measurement : Single beam measurement
Photometric range : 0 to 5 Abs
Photometric accuracy : ±0.01 Abs
(0 to 1 Abs, checked using NIST SRM 930D filter)
External input terminal : Two channels (input range : -1 to 1 V DC)
Shutter : Opens and closes in front of sample
Sample chamber : Small sample chamber dimensions :
140mm wide × 300mm deep × 130mm high
Large sample chamber dimensions :
305mm wide × 420mm deep × 270mm high
Sample stage can be dismounted and remounted and
accepts various accessories.
Equipped with constant temperature water inlet/outlet ports
Nitrogen gas displacement: Atmosphere in the light source unit, monochromator unit,
and sample chamber is displaced using dry nitrogen gas.
Temperature : 20 ±5°C
Humidity : Less than 70%
Dimensions : Main unit (small sample chamber) :
1115mm wide × 570mm deep × 410mm high
5
Main unit (large sample chamber) :
1270mm wide × 570mm deep × 410mm high
Weight : Main unit (small sample chamber): 87 kg
Main unit (large sample chamber):106 kg
Power requirements : 100, 115, 200, 220, 230, 240 V, 50/60 Hz
270 W (150 W light source)
670 W (450 W light source)
6
2. Unpacking and Installation
Note: Hold the monochromater bench when you move the main unit.
2.1 Unpacking
After unpacking the instrument, check the parts received against the list of components
(Table 2.1). If any part is missing or damaged, contact your local JASCO distributor.
7
. Within the proximity of equipment that supplies nitrogen gas. (flow rate : more than 3
λ/min).
. Nitrogen gas tube : 3 m in length, inside diameter : 9.5 mm.
2.3 Reassembly
Note: Reassembly of the instrument is performed by your local JASCO distributor.
The cam and lever on the bottom of the instrument are separated by a cushion and
secured with a rubber band to protect the cam from damage and the wavelength from
shifting during transit.
Remove the cushion and rubber band after installing the main unit.
(1) Remove the side cover from the main unit.
Side cover
Setscrews
Fig. 2.1 Removing the side cover
Cushion
Wavelength
lever
Rubber band
Cam
8
2.3.2 Installing the modulation element
The modulation element has been removed from the main unit before shipment to
prevent damage in transit. Install the modulator element in the main unit after installing
the main unit.
(1) Remove the electrical system cover from the main unit.
Pull
Setscrews
Lift
Monochromator lid
Setscrews
(3) Mount the modulator element in the holder and mount it in the main unit.Solder the
leads to the terminals.
CAUTION : Be careful not to damage the modulator element or break the leads.
CAUTION : See to it that the leads do not come into contact with the holder, cover or
with each other.
9
Solder
Modulator
element
Lead wire
Holder
Fig. 2.5 Mounting the modulator element
CAUTION : Do not loosen any screws, except for the lock screw.
Detector unit
Sample chamber
Fig. 2.6 Installation of detector unit
Install the detector unit on the main unit according to the following procedure.
(1) Remove the cover from the detector mounting hole located in the right side panel
of the main unit
(2) Remove the cover from the detector unit
(3) Gently mount the detector unit on the main unit, and secure it using the lock screw.
CAUTION : Install the detector so that the label faces upward.
10
2.3.4 Connecting the cables and tubes
Connect the cables and tubes according to the following procedure :
(1) Connecting the cables
1) Using a digital voltmeter, confirm that the supplied line voltage corresponds to
the voltage shown on the rating plate.
CAUTION : The line voltage must be confirmed. An outlet can provide an incorrect
voltage due to faulty wiring.
2) Confirm that the ″Power″ switch on the power supply unit is turned OFF.
3) Plug the cables according to Fig. 2.7.
CAUTION: Ground the grounding terminal of the power cable.
CAUTION: For details regarding the wiring and connections of the personal computer
and printer, refer to their respective instruction manuals.
Detector unit
"CD In"
11
Water outlet
Water inlet Cooling water tube
Fig. 2.8
1) Connect the ″Water Inlet″ of the light source cooling water flow sensor to the
faucet using the tube.
2) Connect the ″Water Outlet″ of the light source cooling water flow sensor to the
″Water Inlet″ of the light source unit.
3) Connect the ″Water Outlet″ of the light source unit to the water drain port.
4) Feed cooling water to confirm that the system is free from leakage.
(3) Connecting the nitrogen gas tube
Connect the nitrogen gas cylinder (flow meter) to the nitrogen gas inlet.
Note : Bind the tube with the tube band, if necessary.
12
Fig. 2.9
13
3. Names of Functions of Components
3.1 Overall View
150W light source. Small sample chamber
2
4
5
7
9
10
Fig. 3.1 Overall view (150 kW light source. Small sample chamber)
14
450W light source. Large sample chamber
2
4
5
7 12
9
11 10
Fig. 3.2 Overall view (450kW light source. Large sample chamber)
15
Component Function
① ″Power″ switch Power switch of the main unit.
②Sample chamber Set sample.
③Constant temperature Inlet and outlet ports of constant temperature water.
water ports
④Detector unit Houses the photomultiplier tube and preamplifier.
⑤Amplifier unit Houses the amplifier and other elements.
⑥Sample chamber leak Outlet for the water leaking from sample chamber.
water outlet
⑦Monochromator unit Houses the monochromator and modulator.
⑧Connecting plate Connected to the electrical system.
⑨Nitrogen gas inlet Admits nitrogen gas to displace the air in the
monochromator.
⑩Light source unit Houses the light source.
⑪Light source cooling Cooling water inlet to the light source.
water inlet
⑫Light source cooling Cooling water outlet from the light source.
water outlet
16
3.2 Panels
1
Alarm Lamp Shutter
2 Temperature
Open
(Lamp)
Water Flow
(Lamp)
Water Leak
3 (Sample Chamber)
N2 Flow
6 7
5
Fig. 3.3 Front panel of amplifier unit
Component Function
① ″Temperature (Lamp)″ Lights if the light source temperature becomes
LED abnormally high. The light source is automatically
turned off if an alarm is displayed.
② ″Water Flow (Lamp)″ Lights if the cooling water to the 450W light source is
LED insufficient.
③ ″Water Leak (Sample Lights if water leaks in the sample chamber. The use
of the optional constant temperature water stop valve
Chamber)″ LED
stops water leak automatically.
④ ″N2 Flow″ LED Lights if the nitrogen gas flow rate is insufficient. This
alarm is effective when the optional PC-controlled
flowmeter or the flowmeter with sensor is used.
⑤ ″Lamp″ LED Lights when the light source is turned ON.
⑥ ″Shutter″ LED Lights when the shutter is open.
⑦ ″Shutter″ button Opens/closes the light shield shutter.
17
1 7 8 6 5
4
CD In ORD In Accessory PS In
2 3 9 13 14
10 11 12
Component Function
① ″CD In″ connector Connect to the connector on the detector unit.
② ″Scale Correction ID″ Trimmer for adjusting the CD scale using a standard
sample.
③ ″Offset CD″ trimmer Trimmer for adjusting offset of CD.
④ ″ORD In″ connector Connect the connector for optional ORD unit.
port
⑤ ″ORD Unit″ connector Connect the connector for optional ORD unit.
port
⑥ ″Scale Correction Port for mounting the optional LD/ORD scale
adjustment.
LD/ORD″ adjustment
mounting port
⑦ ″Accessory″ connector Connector for optional accessories.
⑧ ″Ps In″ connector Connect to the ″Ps Out″ connector on the rear panel of
the monochromator unit.
⑨ ″X1/X100″ selector Changes over the ″Ext2″ terminal input voltage gain.
switch Set it at X100 to amplify the gain by a factor of 100.
⑩I/O terminals
″Ext1″ terminal Input terminal for analog signal (-1 to 1 VDC)
″Ext2″ terminal Input terminal for analog signal (-1 to 1 VDC)
″GND″ terminal Grounding terminal (for analog signal)
″DA1″ terminal Output terminal for analog signal (0 to 1 VDC)
″DA5″ terminal Output terminal for analog signal (0 to 5 VDC)
″DGND″ terminal Grounding terminal (for digital signal).
″Trig″ terminal Trigger signal input terminal.
⑪ ″Optical Unit″ connector Connect to the ″Amp Unit″ connector on the rear panel
of the monochromator unit.
⑫ ″I/O 1″ connector Connect to an optional accessory.
⑬ ″I/O 2″ connector Connect to an optional accessory.
⑭ ″Serial″ connector Connect to the connector for communication of the
personal computer.
18
1 4
T10A
T6.3A
Amp Unit
T3.15A
PS Out
AC INPUT
2 3
Component Function
① ″Amp Unit″ connector Connect to the ″Optical In″ connector on the rear panel
of the amplifier unit.
② ″PS Out″ connector Connect to the ″PS In″ connector on the rear panel of
the amplifier unit.
③Receptacle Power inlet receptacle
④Fuse
″T3.15A″ label For 200 VAC line voltage.
″T6.3A″ label For 100 VAC (150W light source) or 200 VAC (450W
light source) line voltage.
″T10A″ label For 100 VAC line voltage.
19
3.3 Sample Chamber
Small sample chamber
4
1
9
7
3
8
1
4
2
5
6
3
10
20
Component Function
①Cell holder Set the cell.
②Cell holder mount Set the cell holder.
③Sample stage sub-base (1) Remove this when a medium-sized accessory like
Peltier type thermostatted cell holder is mounted.
④Sample stage sub-base (2) Remove this when a small-sized accessory like
sample changer is mounted.
⑤Light shield plate Changes over the beam diameter to 8 mm or 13
mm according to the cell to be used.
⑥Detector protective switch Turns OFF the switch and sets the voltage applied
to the detector to zero when the sample chamber lid
is opened.
⑦Constant temperature
water inlet/outlet ports
⑧Joint Removable joint for constant temperature water.
⑨Window plate Attached to the sample chamber window when
measuring a sample that emits harmful gas to
protect the monochromator unit.
⑩Inner sample chamber Sample chamber to displace nitrogen gas more
efficiently.
21
3.4 Detector Unit
1 3
Component Function
①Lock screw Secures the detector unit to the main unit.
②Connector Connect to the ″CD In″ connector located on the rear
panel of the amplifier unit.
③Label Indicates the wavelength range. Install the detector
unit on the main unit with this label facing upward.
22
4. MAINTENANCE
4.1 Light Source Check and Replacement
The service life of the xenon lamp is 300 to 500 hours, but it differs considerably from
one light source to another. It is therefore difficult to predict life expectancy from
operating hours. It is generally predicted from noise on the measured data. Compare
the current data with the data on delivery (data obtained with a new light source) to
make decision.
Note : Noise may also appear if the line voltage fluctuates abruptly.
Observe the following guidelines in order to maximize the service life of the xenon lamp.
. If the light source is not used for an extended period, turn it off. However, if the light
source will be inactive for an hour or less, leave it on Frequently turning the light
source on and off will shorten its service life.
. Always feed cooling water to the light source (450W light source).
<Procedure>
WARNING : Carefully read the ″Safety Cautions″ at the beginning of this manual.
(1) Turn OFF the ″Power″ switch located on the main unit.
(2) For the 150W light source, remove the light source cover and then remove the
anode holder and the light source. For the 450W light source, remove the anode
holder, and then loosen the cathode fixing screw with a screwdriver through the
hole on the side cover to remove the light source.
Note : The 150W light source is attached to the anode holder.
(3) For the 150W light source, remove the anode holder and cathode adapter from the
light source, and attach them to a new light source.
(4) Mount a new light source in the position of the old light source.
CAUTION : Confirm that the glass protrusion of the Xe lamp does not face the M0 and
M1 mirrors.
23
(150W Light source)
Light source cover
Anode holder
Light source
Cathode adaptor
M1 mirror
M0 mirror
Anode holder
Light source
M 1 mirror
M 0 mirror
Fig. 4.1
(5) Tighten the cathode fixing screw (for the 450W light source)
(6) Mount the anode holder (for the 450W light source).
(7) Start up the instrument.
(8) Start up the [Data Monitor] program.
(9) Select the [Parameter...] and [Data Mode...] commands from the [Setting] menu
and designate the monitoring parameters shown in Fig. 4-2.
24
Fig. 4.2 Setting parameters (replacement of light source)
(10) Select the [Move Wavelength...] command from the [Setting] menu and set the
wavelength at ″546.1 nm″.
(11) Remove the cover from the M0 and M1 mirrors. The adjustment screw shown in
Fig. 4.4 will be visible.
Cover
(12) Adjust the adjustment screws for the M1 mirror to minimize the value of channel 2
(HT voltage) when the sample chamber is empty.
(13) Adjust the adjustment screws for the M0 mirror to minimize the value of channel 2
(HT voltage) when the sample chamber is empty.
Note : Normally, the minimum value is 200 to 300 volts.
25
shorter wavelength region (250 nm and less). Check the energy about once a year.
The M0 and M1 mirrors should be replaced every two years, and the M2 through M5
mirrors should be replaced every five years.
Note : If an energy decrease is observed in the long wavelength region, improper optical
alignment or a other trouble is suspected.
<Procedure>
(1) Start up the [Data Monitor] program.
(2) Select the [Parameter...] and [Data Mode...] commands from the [Setting] menu
and designate the monitoring parameters shown in Fig. 4.5.
(3) Select the [Wavelength ...] command from the [Setting] menu and set the
wavelength at ″300 nm″
(4) Confirm that the value of channel 2 (HT voltage) is 180 to 260 volts when the
sample chamber is empty.
(5) Select the [Move Wavelength...] command from the [Setting] menu and set the
wavelength at ″300 nm″.
(6) Confirm that the value of channel 2 (HT voltage) is 500 volts or less when the
sample chamber is empty.
26
4.3 Wavelength Accuracy Check and Adjustment
Note : Before checking wavelength accuracy, warm up the instrument for about one
hour after turning the light source ON.
<Procedure>
(1) Start up the Spectrum Measurement program.
(2) Select the [Parameter...] command from the [Measurement] menu, and designate
the measurement parameters shown in Fig. 4.8.
586±0.8nm
H 0
T 5
6
0
W
a
v
e
l
e
n
g
t
h
[
n
m
]
6
1
0
<Adjustment procedure>
Make adjustment using the adjustment screws on the wavelength lever located at the
bottom of the main unit.
(1) If the main unit is mounted in the optional cabinet, the wavelength cam and
27
wavelength lever will be visible from below, as shown in Fig. 4.10. If the main unit
is mounted on a table or bench, bridge the instrument across two tables or
benches to permit access to the adjustment screws.
Wavelength lever
Cam
Fig. 4.10 Adjustment screws
(2) Correct the wavelength by adjusting the fine and coarse adjustment screws
located on the wavelength lever. Turning the screw clockwise shifts the HT data
to shorter wavelengths, and turning the screw counterclockwise shifts the data to
longer wavelengths.
(3) Measure the HT data of the neodymium glass sample to check the wavelength.
Note : If the instrument is moved, gently move it back to its original position, and check
wavelength accuracy again.
<Procedure>
(1) Start up the [Spectrum Measurement] program.
(2) Select the [Parameter...] command from the [Measurement] menu, and designate
the measurement parameters in Fig. 4.11.
28
Fig. 4.11 Measurement parameters (CD scale check)
(3) Fill the 10mm light path cell with 0.06% aqueous solution of ammonium d-10-
camphor sulfonate (solvent : distilled water), and mount the cell in the sample
chamber.
(4) Select the [Start] command from the [Measurement] menu to make measurement.
(5) Using the spectrum analysis program, confirm that the peak value of Channel 1
(Fig. 4.12) is 190.4 ±1 mdeg (291.0 nm). If the peak value does not fall within this
range, adjust the instrument according to the following procedure.
2
0
0
190.4±1mdeg
C
D
0
2
5
0
W
a
v
e
l
e
n
g
t
h
[
n
m
]
3
5
0
<Adjustment procedure>
Use the ″Scale Correction CD″ knob located on the rear panel of the amplifier unit (Fig.
3.4).
(1) Select the [Move Wavelength...] command from the [Control] menu and designate
the wavelength shown in Fig. 4.13. Click on the <OK> button.
29
Fig. 4.13 Setting wavelength (CD scale adjustment)
(2) Turn the ″Scale Correction CD″ knob located on the rear panel of the amplifier unit
(Fig. 3.4) until the CD value comes within the reference range.
(3) Measure the CD spectrum to check the CD scale.
<Procedure>
(1) Start up the [Data Monitor] program.
(2) Select the [Parameter...] and [Data mode...] commands from the [Setting] menu
and designate the measurement parameters as shown in Fig. 4.14.
(3) Verify that the measurement value of Channel 1 falls within 18 (±10%) mdeg.
(4) After that, set the ″Photometric mode″ at ″CD″.
30
5. TROUBLESHOOTING
If the instrument does not operate properly, the following causes are suspected.
. Erroneous operation
. Deterioration of consumable components
. Failure of instrument
The following table describes basic corrective actions for specific symptoms. If the
difficulty cannot be corrected by performing these actions, failure of the instrument is
suspected. In this case, contact your local JASCO distributor with detailed information
about your difficulty, including the model name, serial number, and date of manufacture
of your instrument.
31
Is the wavelength set to a Set the wavelength to a
value at which the detector is value at which the detector
not sensitive? is sensitive.
Is the nitrogen gas flow rate Increase the nitrogen gas
high enough when the flow rate.
wavelength is set below 180
nm?
Is the ″HT″ switch on the sub- Set the ″HT″ switch to
panel of the amplifier unit in ″Auto″.
the ″Auto″ position?
Noise is high Is the spectra bandwidth Increase the spectra
setting too small? bandwidth.
Does the sample have high Decrease the sample
light absorption? concentration, or shorten
the light path of the cell.
Is noise detected in the HT Replace the Xe lamp.
voltage?
Is the HT voltage at below Adjust the M0 and M1
250 nm too high? mirrors.
Any noise source that Remove the noise source
generates electromagnetic from the proximity of the
waves nearby? instrument.
Is any source of mechanical Remove the source of
vibration nearby? vibration.
Does line voltage vary Use stabilized line voltage.
abruptly.
The baseline curves Is the curvature within ±10 Perform baseline correction.
sharply. mdeg when the baseline is
not corrected?
CD value is displayed Is the sample fluorescent? Decrease sample
although sample is not absorbance to 2 or less.
optically active.
Is the sample a film or liquid False CD signal from the
crystal? sample is suspected.
Does the cell contain any Prepare a new sample.
optically active residue?
The displayed CD Is the ″HT voltage setting″ in Set it at ″Auto″ (not
value is smaller than the ″Detector sensitivity″ ″Manu″).
normal, or no display dialog box set correctly?
appears.
Is the photometric value 18±2 Failure of the electrical
mdeg when the photometric system or modulator
mode is ″Test signal″? element is suspected.
Repeatability of CD Is the instrument warmed up Before performing Cd
values is low. sufficiently? measurement, warm up the
instrument for approximately
one hour after the light
source has lit.
32
Is the sample deteriorated by Use the shutter function or
the light emitted from the light narrow the spectrum
source? bandwidth.
Is the variation of the peak Normal.
value of aqueous solution of
ammonium d-10-camphor
sulfonate (distilled water, 10
nm cell) at 291.0 nm within 2
mdeg/hr?
Are room temperature and Maintain room temperature
humidity variations normal? within 20 ±5°C, and humidity
below 70%.
Is the instrument blown with Install the instrument in a
draft from an air conditioner or position outside of the direct
other? path of air currents.
Is the scanning speed too Slightly lower the scanning
high? speed.
Is noise too high? Increase response. Or,
refer to the ″Noise is high″
symptom.
Wavelength Is the instrument warmed up Measure wavelength
repeatability is low. sufficiently? repeatability after warming
up the instrument for
approximately one hour
after the light source is lit.
Are room temperature and Maintain room temperature
humidity variations too high? within 20 ±5°C, and humidity
below 70%.
No communication Is the RS-232C cable Reconnect the cable
with the computer. connected properly? correctly.
Is the communication port Correctly set the
setting in agreement with the communication ports.
wiring?
33