Jasco CD-1595 User manual

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0302-0402B
JASCO MODEL CD-1595
CIRCULAR DICHROISM CHIRAL
DETECTOR
OPERATION MANUAL
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i
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.
(1) Safety symbols
Instruction manual symbol. If the product is marked with this symbol,
refer to the instrument manuals to protect the instrument against
damage.
WARNING A WARNING indicates an potentially hazardous situation
which, if not avoided, could result in death or serious injury
CAUTION A CAUTION indicates a potentially hazardous situation which,
if not avoided, may result in minor or moderate injury. It may
also be used to alert against unsafe practices.
Do not proceed beyond a WARNING or CAUTION notice until
you understand the hazardous conditions and have taken the
appropriate steps.
Note A Note provides additional information to aid the operator in
obtaining optimal instrument performance.
Pressurized, hazardous solvents are used in high-performance liquid
chromatography. Always follow the proper laboratory procedures to ensure
operator safety. Always wear goggles, gloves and protective clothing when
operating the instrument, especially when injecting sample and opening
valves.
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ii
(2) Warning Labels
Warning labels are attached at several locations on this instrument. Do not
remove, deface or damage the warning labels. 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.
(1) Lamp Replacement Warning Label (P/N: 0822-0078A)
The surface temperature of the Hg-Xe lamp can reach more than
200°C when the lamp is lit. The temperatures of the lamp and the
lamp housing do not return to ambient temperature immediately after
the lamp is turned off. Therefore, when replacing the lamp, take
sufficient care to avoid burn injuries.
Refer to the maintenance manual for further details regarding lamp
replacement. Follow the instructions provided therein and perform all
operations carefully.
(2) Danger Warning Label (P/N: 0822-0035A)
This label is located on the high-voltage source used to light the Hg-
Xe lamp. A voltage of 200 V or greater is generated during the
operation of the detector. Inserting one’s hands or other objects into
this area may result in electric shock. Be sure to turn off the power
and unplug the power cord before performing maintenance in this
area.
WARNING
!
Replacethelampafterthelampbulbiscooled.
Replacethelampafterthelampbulbiscooled.Replacethelampafterthelampbulbiscooled.
Replacethelampafterthelampbulbiscooled.
UsethelampspecifiedbyJASCO.
UsethelampspecifiedbyJASCO.UsethelampspecifiedbyJASCO.
UsethelampspecifiedbyJASCO.
Useofotherlampmayresultinblastorother
UseofotherlampmayresultinblastorotherUseofotherlampmayresultinblastorother
Useofotherlampmayresultinblastorother
failure.Failurescausedbywronglamparenot
failure.Failurescausedbywronglamparenotfailure.Failurescausedbywronglamparenot
failure.Failurescausedbywronglamparenot
coveredbythewarranty.
coveredbythewarranty.coveredbythewarranty.
coveredbythewarranty.
HIGH
VOLTAGE
DANGER
DANGERDANGER
DANGER
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iii
警 告
キセノンランプには高圧ガスが封入
されています。機械的衝撃を与えると
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.
!
破裂し怪我をする恐れがあります。
!
WARNING
MAINS PLUG GROUND PIN
OR GROUND TERMINAL
MUST BE CONNECTED
TO GROUND.
(3) Xenon Lamp Warning Label (P/N: 0822-0077A)
When replacing the Xenon lamp,
refer to the operations manual
(P/N 0301-0193A) and follow the
instructions carefully.
(4)

Fuse Warning Label (P/N: 0822-0120A)
(5) Electric Shock Warning Label (P/N: 0822-0124A)
Electric shock may occur if
the instrument is not properly
grounded.
WARNING
ONLY WITH FUSE OF THE SPECIFIED
AGAINST RISK OF FIRE,REPLACE
FOR CONTINUED PROTECTION
TYPE AND CURRENT RATINGS.
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iv
(6) High voltage inside warning Label (P/N: 0822-0145A)
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.
(7) Voltage Select Warning Label (P/N: 0822-0097A)
Before turning on the lamp, confirm “VOLTAGE SELECT” is set to
115V when AC input voltage is 100-115V or “VOLTAGE SELECT” is
set to 230V when AC input voltage is 220-230V. Lamp may be broken
if the above condition is not followed.
WARNING
!
Highvoltageinside!!
Highvoltageinside!!Highvoltageinside!!
Highvoltageinside!!
Disconnectthepowercordbefore
DisconnectthepowercordbeforeDisconnect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.
CAUTION
!
Beforeturningonthelamp,
Beforeturningonthelamp,Beforeturningonthelamp,
Beforeturningonthelamp,
confirm"VOLTAGESELECT"is
confirm"VOLTAGESELECT"isconfirm"VOLTAGESELECT"is
confirm"VOLTAGESELECT"is
setto115V(or230V)when
setto115V(or230V)whensetto115V(or230V)when
setto115V(or230V)when
ACinputvoltageis100/115V
ACinputvoltageis100/115VACinputvoltageis100/115V
ACinputvoltageis100/115V
(or220/240V).Lampmaybe
(or220/240V).Lampmaybe(or220/240V).Lampmaybe
(or220/240V).Lampmaybe
brokeniftheabove
brokeniftheabovebrokeniftheabove
brokeniftheabove
conditionisnotfollowed.
conditionisnotfollowed.conditionisnotfollowed.
conditionisnotfollowed.
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v
(3) 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
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vi
Preface
This instruction manual serves as your guidebook for using this instrument. It
is intended to instruct first-time users on how to properly use the instrument,
and to serve as a reference for experienced users.
Before using the instrument, please read this instruction manual carefully, and
make sure that the contents are fully understood. This manual should be easily
accessible to the operator at all times during instrument operation. 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. This is the operations manual.
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vii
Installation Conditions
To ensure safe operation, the following recommendations should be
observed:
(1) Do not operate the instrument under voltage fluctuations exceeding
10% of the recommended line voltage. Large fluctuations may
cause the instrument to fail.
(2) 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.
(3) Operate the instrument under a temperature range of 10 ∼30°C.
(4) Operate the instrument under a humidity range of 35 ∼85% (RH).
If ambient humidity exceeds 85% (RH), water vapor may deteriorate
optical components. If possible, install the instrument in a location
having a humidity of 60% or lower.
(5) Operate the instrument under an atmospheric pressure of 750 ∼
1060 hPa.
(6) Avoid strong magnetic fields and sources of high-frequency waves.
The instrument may not function properly when near strong
magnetic fields or high-frequency wave sources.
(7) Avoid vibrations caused by vacuum pumps, electric motors,
processing equipment and machine tools.
(8) Avoid dust and corrosive gas. Do not install the instrument in a
location where it may be exposed to dust, especially in locations
exposed to outside air or ventilation outlets that discharge dust
particles.
(9) Do not install the instrument in a location where it may be exposed
to direct sunlight.
(10) Do not install the instrument in a location where it may be directly
exposed to the air current from an air conditioner or heater, as such
a location may inhibit stable measurement.
Note: The above conditions do not ensure optimal performance of this
instrument.
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viii
Maintenance
Consult your local JASCO distributor, listed at the back of this manual,
regarding maintenance. In addition, contact your local JASCO distributor
representative when transporting the instrument.
Replacement parts can be ordered according to part number from local
JASCO distributor. When the part number is not known, inform parts name,
instrucment model name and it’s serial number.
Notices
(1) Jasco shall not be held liable, either directly or indirectly, for any
consequential damage incurred as a result of the use of this product.
(2) Software prohibitions:
yCopying of software or related materials for purposes other than
backup is prohibited.
yTransfer or authorization of the use of Jasco software to or by a third
party is prohibited.
yDisclosure of confidential information related to Jasco software is
prohibited.
yChanges or revisions to Jasco software are prohibited.
yUse of Jasco software on multiple workstations or terminals, through
a network or through any other means, is strictly prohibited. (This
does not apply to entities with the network license contract)
(3) The content of this manual is subject to change without notice in
accordance with product improvements.
(4) Unauthorized copying of this manual is prohibited.
(5) This manual shall not be used to guarantee or copyright industrial rights
or other rights.
(6) Company and product names listed herein are trademarks or registered
trademarks of various companies.
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ix
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.
This warranty does not apply to defects as a result of the following:
(1) USE FOLLOWING IMPROPER OR INADEQUATE INSTALLATION.
(2) IMPROPER OPERATION.
(3) MOVEMENT, MODIFICATION, OR REPAIR BY PERSONS OTHER
THAN AUTHORIZED JASCO PERSONNEL.
(4) USE OF PARTS OTHER THAN THOSE THAT ARE AUTHORIZED
BY JASCO.
(5) INORDINATELY RAPID DETERIORATION DUE TO THE USE OF
CORROSIVE SOLVENTS OR SAMPLES.
(6) NATURAL DISASTERS SUCH AS FIRES, WATER DAMAGE, OR
EARTHQUAKES.
In addition, this warranty does not cover:
CONSUMABLE PARTS OR PARTS THAT HAVE A SEPARATE
WARRANTY OR A WARRANTY PERIOD THAT IS DIFFERENT
THAN THAT SPECIFIED ABOVE.
The warranty period for all parts and repairs supplied under this warranty
expires with the warranty period of the original product.
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x
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xi
Table of Contents
Safety Considerations ....................................................................i
Preface ...........................................................................................vi
Installation Conditions.................................................................vii
Maintenance ................................................................................viii
Notices .........................................................................................viii
Warranty ........................................................................................ix
1. GENERAL DESCRIPTION AND SPECIFICATIONS OF
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. Power-On, Self-Diagnostic Test and Power-Off..................3-1
3.1 Power-on and Self-Diagnostics ........................................................3-1
3.2 Turning power off...............................................................................3-2
4. PREPARATION FOR MEASUREMENT AND BASIC
OPERATION .............................................................................4-1
4.1 Preparation for Measurement ...........................................................4-1
4.2 Setting Parameters ............................................................................4-3
4.2.1 Changing WAVELENGTH..............................................................4-4
4.2.2 Changing GAIN..............................................................................4-5
4.2.3 Changing RANGE..........................................................................4-6
4.2.4 Changing RESPONSE...................................................................4-7
4.3 Measurement......................................................................................4-8
4.4 Error Messages ..................................................................................4-9
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xii
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 and 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
5.7 [SHIFT] [5]: Shifting Integrator Output Zero Level ..........................5-5
5.7.1 Setting integrator output zero level ................................................5-6
5.8 [SHIFT] [6]: Checking Cumulative Lamp Operation Time...............5-7
5.9 [SHIFT][7]: Changing Recorder Output Polarity..............................5-8
5.10 [SHIFT][8]: Selecting Autozero Mode .............................................5-8
5.11 [SHIFT][9]: .........................................................................................5-9
5.12 [SHIFT] [MARK][5]: Setting Flowcell Path-length ..........................5-9
6. Operations in Program Mode ...............................................6-1
6.1 Description .........................................................................................6-1
6.2 File Number Setting (File Loading)...................................................6-1
6.3 Switching Between Normal Operation Mode and Program Mode..6-2
6.4 Editing Programs ...............................................................................6-3
6.4.1 Editing initial parameters................................................................6-3
6.4.2 Editing the time program ................................................................6-4
6.4.3 Program example...........................................................................6-7
6.5 Time Program Operation .................................................................6-10
6.5.1 Running a time program...............................................................6-10
6.5.2 Changing parameters while a program is running........................6-10
7. KEY OPERATIONS IN SPECTRUM MODE ...........................7-1
7.1 Outline.................................................................................................7-1
7.1.1 Principles of Operation...................................................................7-1
7.1.2 Operation .......................................................................................7-1
7.2 Baseline Spectrum Acquisition ........................................................7-3
7.3 Spectrum Measurement ....................................................................7-3
7.4 Spectra Output ...................................................................................7-4
8. Principle.................................................................................8-1
8.1 CD Measurement Principle................................................................8-1
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1-1
1. GENERAL DESCRIPTION AND SPECIFICATIONS OF
INSTRUMENT
1.1 General Description
JASCO has developed the model CD-1595 chiral detector dedicated to HPLC.
It is an innovative detector that offers higher sensitivity for chiral compounds
with more information than a conventional optical rotation (OR) detector.
Chiral separation is now one of the most important application areas in HPLC.
There is increasing demand for chiral chromatography in various fields, such
as drug analysis, drug discovery, biochemical analysis, natural product
analysis, organic synthesis, etc. Recent advances in chiral column
technology are boosting the use of chiral chromatography in more and more
laboratories. 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.
OR detectors have exclusively been used for detection of chiral compounds,
though it is known that a detector based on circular dichroism may offer better
sensitivity. Therefore, a lot of efforts have been made to utilize a regular CD
spectropolarimeter, which is rather big and expensive, as an HPLC detector.
After extensive R&D work, JASCO has successfully developed a compact CD
detector dedicated to HPLC that offers simultaneous detection of CD and UV
absorption, and even CD and UV spectral measurements by stop-flow
scanning.
Most biologically active compounds are chiral. It is well known that chiral
isomers often cause totally different biological effects, e.g., one offers
therapeutic effect but the other has unwanted one such as teratogenic activity.
Most naturally occurring medicines contain only one type of the isomers.
However, when such a compound is artificially synthesized, both isomers are,
in general, equally produced. Therefore, each isomer must be examined for
its biological activity. In such investigation, a conventional CD
spectropolarimeter has been effectively used. In order to analyze samples
with the CD spectropolarimeter, chiral separation needs to be performed and
each isomer must be fractionated. The new CD-1595 detector offers on-line
monitoring of CD signals during chiral separation and gives indication which
peak components should be collected. In addition, the simultaneous CD and
UV monitoring by the detector allows to determine optical purity of unresolved
peaks of chiral compounds. This facilitates researchers to speed up their
investigation on new drug discovery.
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1-2
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 : 0.1 mdeg/cm/h (at 290nm)
Gain: x1, x10
Response : FAST, STD, SLOW
Flow cell path length : 25 mm(1,5,10 mm optional)
Signal outputs : Simultaneous outputs of CD
(circular dichroism) and UV absorption
CD, UV recorder output = 10mV full scale
CD integrator output = 1V/deg
UV integrator output = 1V/AU and 1V/2AU
Spectral measurement : Simultaneous measurement of CD and UV
spectra
Spectral memory : 220~420 nm(both UV and CD),
Memory:10files
Power requirement : 100-240 VAC, 400VA
Dimeniton: 390(W)x 450(D)x250(H)mm
Weight : approx. 21kg
The specifications are subjected to change without notice.
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2-1
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
Figure 2.1 Front panel.
Name of part Description
(1) Flowcell assembly
(2) LCD display and
keypad
(3) “POWER” switch
(4) “OPT. CD ZERO”
knob
This is the cassette type flowcell assembly.
Display operating conditions, CD, UV and other
signal levels, parameters, and various messages.
Parameters necessary for the operation can be
entered through the keypad.
Used to turn the instrument on or off.
Used to adjust optical zero of the CD signal.
1
2
3
4
0
98
3
2
1
7
6
5
4
MODE W.L(nm) GAIN
CD AU RESPONCE
AUTO
ZERO
PRGM
RUN
MARK
MONIT
CLEAR
SHIFT SCAN PRGM
EDIT/ENTER
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2-2
2.2 LCD and Keypad
Figure 2.2 LCD and keypad
Name of part Function
LCD display
[AUTO ZERO]
[PRGM RUN]
[MARK]
[MONIT]
[SHIFT]
[SCAN]
Displays the operation status, parameters, and messages.
Used to set the integrator and recorder outputs to zero.
Starts/stops a time program. When the time program is
running the lamp on the key lights. It is also used for
measuring/outputting CD/UV spectra.
Outputs marker on the recorder output.
Used to return to or change the monitor mode.
Used in combination with the numeric keys to set or
display parameters that are less frequently changed.
Changes to the scan monde.
0
98
3
2
1
7
6
5
4
MODE W.L(nm) GAIN
CD AU RESPONCE
AUTO
ZERO
PRGM
RUN
MARK
MONIT
EDIT/ENTER
CLEAR
SHIFT SCAN PRGM
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2-3
[PRGM]
[0] 〜[9][・]
[▼] , [▲]
[CLEAR]
[EDIT/ENTER
Changes to time program mode.
Numeric keys.
Increment/decrement keys.
Clear erroneous entry of parameters. It also clears error
messages.
Used to edit/enter parameters.
(NOTE)
Perform optical zero adjustment by turning the CD ZERO knob before
activating the Autozero.
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2-4
2.3 Flowcell Assembly
Figure 2.3 Flowcell Assembly
Name of part Description
(1) Cell body
(2) Cell panel
(3) Lock screws
The light passes through the hole of the cell body.
The cell panel is fixed to the cell body.
Used to secure the flowcell assembly in position to
the detector.
(NOTE)
To attach the flowcell assembly to the detector, press the cell panel until the
cell body reaches to the bottom, then alternately tighten the lock screws to
secure the flowcell assembly.
2
3
1
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