Jasco J-810 User manual

P/N: 0302-0407A March 1999
MODEL J-810
SPECTROPOLARIMETER
Hardware/Function Manual
JASCO Corporation

i
Safety Cautions
Correct operation and scheduled maintenance are essential for safe use
of the instrument. Read the safety cautions in this manual and fully
understand them before operation.
″WARNING″, ″CAUTION″and ″Note″are used throughout this manual
to call operator′s attention to safety.
(1) Meanings of safety notations
WARNING : Failure to comply with this involves the possibility of death
or serious personal injury. Serious personal injury means
loss of sight, injury, burn (high temperature, low
temperature), electric shock, fracture, intoxication, etc.
which can cause sequel or require hospitalization or long-
term treatment at hospital.
CAUTION : Failure to comply with this involves the possibility of minor
personal injury or physical damage. Minor personal injury
means injury that does not require hospitalization or long-
term treatment, and physical damage means damage to the
instrument itself or damage to objects other than the
instrument, such as buildings, properties, etc. (extended
damage).
Note : This contains care to be taken during operation and
information that will be helpful in operation.

ii
(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.
1) WARNINGS! Handling the Xenon Lamp (①of Fig. 1)
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

iii
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.
150W Light Source, Small Sample Chamber
3
2
1
450W Light Source, Large Sample Chamber
3
2
1
Fig. 1

iv
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
/min, pressure : 0.5～2.0 kg/cm2). Cooling water piping : 10 m in length, inside
diameter : 12 mm
Note: Do not use water at more than 2.0 kg / cm2pressure.
. 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.

v
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

1
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 :
θ
π
εε =−
4500 10( ) log
LR e
(1)
where, εLand εRare the molecular extinction coefficients for the right and left circularly-
polarized beams of light. The difference (∆ε) between εLand εRis determined using
the following formula :








=−=∆
L
R
RL I
I
LC 10
log
1
εεε
(2)
[]








=
L
R
eI
I
LC 10
log10log
4500
π
θ
(3)
In equation (2) and (3), L represents the thickness (cm) of the absorbing layer, and C
represents the molar concentration, IR
and ILrepresent 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.ILis nearly 1. To avoid this difficulty, we substitute the
following quantities.
()
LRA III += 2
1(4)
S
I
I
RL
=−
(5)
Since S/2 Ι
Ais less than 1, equation (3) can be re-expressed as follows, by substituting
the expressions from equations (4) and (5) :

2
[]








=












−
+
=
e
I
S
LC
I
S
I
S
LC
A
e
A
A
e
10
10
log10log
4500
2
1
2
1
log10log
4500
π
π
θ
(6)
Thus, the ratio between IAand S can be approximated with an accuracy sufficient for
practical application.
Given that EAand ESrepresent the output voltages of the photomultiplier tubes
corresponding to light intensities IAand S respectively, S/IA= ES/EA. By substituting
this expression, equation (6) can be expressed as follows.
[]








=e
E
E
LC A
S
e10
log10log
4500
π
θ
(7)
Here, if EScan be amplified independently of EA, equation (7) can be expressed as
follows.
[]






















=G
e
E
GE
LC A
S
e
10
log
10log
4500
π
θ
(8)
where G represents the amplification factor of ES. Since the value ESG can be brought
very close to the value of EAby choosing an appropriate value for G, [θ] can be
determined with a high degree of accuracy.
1.1.2 Optical system
Fig. 1.1 shows the optical system of the Model J-810 spectropolarimeter.
Ｓ１
Ｓ２
Ｓ３Ｌ Ｆ CDM
Ｍ３
Ｍ２
Ｍ５
Ｍ４Ｐ１
Ｐ２
ＰＭ
E-ray
O-ray
SH
Ｍ1
Ｍ0
LS
M0, M1, Mp, M2～M
5: Mirrors LS : Light source
S1～S
3: 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

3
A xenon lamp is used as the light source. The light emitted from the xenon lamp is
converged by the M1mirror into the S1entrance slit. The optical system between the
S1entrance slit and the S2intermediate slit is referred to as the first monochromator,
and the optical system between the S2intermediate slit and the S3exit 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 (P1and 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 :
IR
ILIA
S
Time
Intensity
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 ERis smaller or larger than the
value EL. In Fig. 1.2, the solid line represents the case when ERis greater than EL, and
the dotted line represents the case when ERis 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.
1.1.3 Electrical system
The output signal from the detector (PM photomultiplier tube) consists of an AC
component electrically modulated by the modulator and a DC component that
represents the average intensity of the transmission light. The CD value can be derived
from the ratio between the DC component and the AC component. This instrument
varies the PM voltage in order to maintain a constant DC component, and utilizes the
AC component as the CD signal. Therefore, once the AC signal is calibrated using a
standard sample, the correct CD value can be obtained.
Fig 1.3 shows a block diagram of the electrical system. Since the AC and DC
components can be discussed independently, they are described separately in
reference to Figure 1.3.

4
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.
CPU
RS-232C I/F
A/D D/A
RS-232C I/F
PC SVGA
Parallel I/F
PM
Sensor
Light Source Monochromator Sample
Chamber
Light Source
Power Supply
Slit Motor
Driver
Modulator
Driver Preamplifier
Wavelength
Motor Driver Shutter
Driver CD Amplifier PM Power
Supply
I/O External
Input 1
External
Input 2
Buffer Memory
Program Memory
Main Unit
PC
Keyboard CRT Display
Printer
Fig. 1.3 Block diagram of electrical system
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

5
±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

6
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)

7
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.
Table 2.1 List of Components for J-810 Spectropolarimeter
Component Q′ty Remarks
J-810 main unit 1
Modulator element 1
Detector unit 1
Cable 1 set
Nitrogen gas inlet tube 1 3 m
Nitrogen gas outlet tube 1
Nitrogen gas tube band 2
Cooling water tube 1 10 m for the 450W light source
Cooling water tube band 3 For the 450W light source
Sample chamber window 1
Inner sample chamber 1 For large sample chamber
Cell holder 1
Standard samples 1 set Ammonium d-10-camphor sulfonate, etc.
Tools 1 set
Floppy disk 1 set For setup, data, etc.
Instruction manual 1 set For hardware, software, etc.
Tube for accessories 1 set For accessories
2.2 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/min,
pressure : 0.5～2.0 kg/cm2). Cooling water tube : 10 m in length, inside diameter : 12
mm
Note: Do not use water at more than 2.0 kg / cm2pressure.

8
. 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.
2.3.1 Removing the cushion from the main unit
CAUTION : When removing the cushion, be careful not to give an impact to the cam.
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
(2) Remove the cushion and rubber band.
Cushion
Wavelength
lever
Rubber band
Cam
Fig. 2.2 Removing the cushion and rubber band

9
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.
Electrical system cove
r
Pull
Setscrews
Fig. 2.3 Removing the electrical system cover
(2) Open the monochromator lid.
Lift
Monochromator lid
Setscrews
Fig. 2.4 Opening the monochromator lid
(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.

10
Holder
Modulator
element
Solder
Lead wire
Fig. 2.5 Mounting the modulator element
2.3.3 Installation the detector unit
CAUTION : Handle the detector unit with great care. Do not give an impact to the
detector unit.
CAUTION : Do not loosen any screws, except for the lock screw.
CAUTION : Do not expose the detector window to intense light.
Detector unit
Lock screw
Sample chamber
Label
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.

11
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.
"AC INPUT"
"Amp Unit""PS Out"
"PS In" "Optical Unit" "Serial"
"CD In"
Detector unit
Amplifier rear panel
Computer
Line voltage
Conecting plate of
monochromator
Fig. 2.7 Connection of cables
(2) Connecting the cooling water tubes (450W light source)
CAUTION : Bind the tube at the water faucet and the water inlet/outlet ports of the light
source unit, using the supplied tube bands.

12
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.
(4) Connecting the nitrogen gas or leak water outlet port.
The outlet tube for nitrogen gas or leaked circulation water is provided at the
bottom of the sample chamber. Connect the tube to the water outlet port, if
necessary.
Outlet tube for nitrogen
gas or leaked water Notroger gas
inlet tube

13
Fig. 2.9

14
3. Names of Functions of Components
3.1 Overall View
150W light source. Small sample chamber
1
5
2
4
3
8
9
10
6
7
Fig. 3.1 Overall view (150 kW light source. Small sample chamber)