LC92 Manual
LC92 Manual
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□Osaka Branch: 〒532-0002 5-13-8-303 Higashimikuni, Yodogawaku, Osaka city TEL: 06-6393-8511 FAX: 06-6393-8525
□Nagoya Branch: 〒465-0025 3-609-3D Kamiyashiro, Meitoku, Nagoya city TEL: 052-709-5400 FAX: 052-709-5403
RECYCLING PREPARATIV E HPLC
USER'S MANUAL
Preface
Thank you for introducing Recycling Liquid Chromatograph model LC-92XX NEXT.
This manual contains instruction of the LC-92XX NEXT's operational manual,
technical information and safety information.
Refer the manual thoroughly, for applying LC-92XX NEXT series to your research
and investigation with safety operation.
Keep the manual near by the LC-92XX NEXT Liquid Chromatograph for referring
any time.
Printing information
・No part of this document may be photocopied or reproduced, or translated to
another program language without the prior written consent of Japan Analytical
Industry Co., Ltd.
・Please note that the information contain in this document may be revised without
notice.
・Please contact our representative office or our company to make inquiries about
the information contained in this document.
・Manuals with missing pages or incorrect collating will be replaced.
Warranty Statement
JAI warrants the Recycling Preparative HPLC LC-92XX NEXT series as follows,
only when you operate it correctly following the instructions in this manual and
without remodeling it.
Warranty period
LC-92XX NEXT Products are warranted for a period of one year from the
date of installation.
Warranty detail
Even during the warranty period, the defects caused by the following are
not covered by this warranty:
・Improper use.
・Operations under the condition not authorized in this document or our
company.
・Abnormal power supply or use under the conditions of irregular voltage
or frequency.
・Defect is coming from other factors, not from the LC-92XX NEXT.
・Use under severe environmental conditions such as corrosive gas, high
temperature and humidity, or continuous vibration.
・Flowing a highly corrosive liquid.
・Force majeure such as earthquake, fire, or lightning.
・Removal or transfer of the product after installation.
・Remodeling or Disassembly of the LC-92XX NEXT with not written way
in this manual.
・Using an instrument that is resold without our approval.
・Defects of the consumables or the parts of which the warranty period is
limited are not warranted.
Parts of consumption :
Pump seal, pump plunger, pump plunger guide, pump check valve, line filter, manual
sample injector (rotor seal/stator face), selector valve (solvent selector, recycle flow 1,
recycle flow 2, drain, C/D selector)
The items which are not included in this paragraph are out of the
warranty.
Direct or indirect damages coming from the evident or implied warranties
of this instrument are not compensated.
Direct or indirect damages coming from destroy of the instrument are not
compensated.
How to Use This Document
This document "LC-92XX NEXT SERIES USER'S MANUAL" consists of the following
four volumes.
Choose the volume to use as needed.
Each volume has its own table of contents at the beginning.
Cautions
・Do not use the LC-92XX NEXT series instrument other than a liquid
chromatography.
・Please read and adhere the instruction in this manual.
・Take safety measures to prevent an accident.
・Please note that the LC-92XX NEXT products that are remodeled or
disassembled without our prior notice are not warranted.
・In long term stop of the LC-92XX NEXT, disconnect Power cable. Seal column
ends with correct plugs to prevent column drying. Fill tubing with noncorrosive
solvent to prevent collision of tubing and flow line assemblies, but not flow the
solvent into the column.
・To avoid possible eye injury and skin trouble, wear eye protector and gloves.
・Prevent solvent leakage in the instrument.
・Do adequate ventilation in LC-92XX setting laboratory.
Support
Latest applications and soft ware revisions put on the site. News of our exhibition
and Events also put on the site.
Restart should be carefully to check the instrument performance. If you have any
worry, contact us or our representative.
Emergency stop
This manual includes basic operation of the liquid chromatograph model LC-92XX
NEXT series to control.
For more details of information, installation, and maintenance of the instrument, please
refer to other volumes, "General Information Manual", "Installation Manual", and
"Maintenance Manual" on the tabs.
Cautions for Operation
・If a failure or wrong operation occurs in the LC-92XX NEXT, an error message
appears on the LCD display. At the beginning of the error message, "ERROR" is
displayed followed by a number. Based on this number, refer to a section in
"Volume 4 Maintenance Manual" to resolve the cause of failure.
・If you press the [Co/Dr] key for collecting fractions from a fraction nozzle during
the [RECYCLE] operation, an error message appears and fractions cannot be
collected. Stop the [RECYCLE] operation, and then press the [Co/Dr] key in
[FRACTION] to collect fractions.
・For the keys located on the sheet switches other than [PURGE] and [AUTO
ZERO], you can press a key to execute its function, and press the key again to
cancel the function.
1-1
1-1
Operation Panel Display
This section describes the overview of the operation panel of the LC-92XX NEXT
series.
1-2
Operation Flow
Actual procedure is as follows.
Set parameters.
Recycle separation.
1-3
1-2
1-4
Prepare the solvent, waste reservoir and sample.
Solvent
・Prepare the solvent purer than chemical grade reagent. If Chloroform (CHCL3) for
the solvent is recommended, CHCL3 added ethanol for stabilizer is suitable.(Pure
CHCL3 or CHCL3 added Amylene stabilizer is not recommended.)
・In case of using mix solvent, solvent mixture should be degassed perfectly. For
details of degassing, refer to "Appendix" P.2-48 in "General Information Manual".
・For the properties of typical solvent, refer to Appendix P.2-51 in "General Information
Manual".
・Filter the sample to remove micro particles with a suitable membrane. For details of
solvent's filtration, refer to Appendix P.2-53 in "General Information Manual".
Waste
・A waste reservoir volume should be more than the solvent container. Reservoir
should be chemical proof against the solvent.
Samples
・Sample should be filtered to remove particles before injection. For the recommended
sample filtration, refer to Appendix P.2-54 in "General Information Manual".
1-5
Turn the power switch on.
・Make sure that the receptacle is 100 VAC and enough to supply power for the LC-
92XX. Turn power switch on.
Power Switch
・After 15 seconds from turning the power switch on, the computer in the LC-92XX
boots up to indicate the initial stage.
・Press the [START] key of [CLEAN UP] at the lower right side of the operation panel.
・When the manual operation is required, a message appears on the LCD display with
an intermittent beep.
・After the completion of the [CLEAN UP] operation, turn the Column reject valve back
to its original position ([CONNECT]).
*While the pump is in operation, [CLEAN UP] cannot be executed. Execute the operation when the pump
is stopped.
1-6
Set parameters.
・Use the arrow keys to set the flow rate value to use.
Arrow Keys
1-7
Detector setting
For UV DETECTOR
1-8
Turn on the pump.
1-9
Inject the sample.
・Prepare filtered sample. (For the typical filtering method, refer to "Micro
Particle Elimination in Sample Solution", Appendix P.2-54 in "Volume 2
General Information Manual").
・Wipe the drop out of the syringe needle with clean paper.
・Hold the syringe upwardly, push the plunger gently to purge air from the
syringe. Push the plunger until the air is purged thoroughly.
・Insert the syringe into the manual injector thoroughly until the syringe needle
touches the bottom.
・Turn back the handle to the [INJECT] position and take the syringe.
・Clean the needle port with clean solvent. (For details on how to clean the
needle port, refer to "Needle Port Cleaning", Appendix P.2-54 in "Volume 2
General Information Manual").
1-10
Separate recycles.
1-11
Collect the fractions.
Siphon
Fraction nozzle
・Press in [FRACTION].
1-12
Shut down the LC.
・Press the [START] key of [CLEAN UP] at the lower right side of the operation panel.
・When the manual operation is required, a message appears on the LCD display with
an intermittent beep.
・After the [CLEAN UP] operation, move the reject valve back to its original position to
complete the [CLEAN UP] operation. If the LC-92XX NEXT will not be used for a long
time, stay the valve position at [REJECT].
*If the column stays a long time in the stopped flow line, solvent may be lost by gravity to dry the column
packing and to damage the column.
1-13
VOLUME
2-1
Composition of LC-92XX NEXT Series
The main body, pump, sample injector, column*, detector*, and integrator*
are installed as standard equipment.
*Columns, Detectors, integrator, and recorder are optional accessories. Please select
optional accessories according to your purpose.
For details on using accessories, refer to separate instruction manuals for correct
operation.
2-2
Name and Function of Each Part
Name Function
To press the buttons to set conditions or execute the
Operation Panel
operation.
Manual Injector Valve To inject the sample manually.
Column Reject Valve To disconnect the flow line from the column.
Pump Drain Valve To drain the solvent from the pump outlet.
To collect fractions from the fraction nozzle or the
Siphon Box
siphon, or to collect the waste liquid.
2-3
<Inside of the LC-92XX NEXT Front Door>
Solvent Table
Pump Head
UV Detector
Power Switch
RI Detector
Wave Length
Tuner
Inside of
the Siphon
Box
Front Door
Name Function
Device using suction and pressure to force solvent
Pump Head
into the flow line.
Solvent Table A table to place a solvent reservoir.
Detector for absorption of the light after passing
UV Detector*1
through the UV cell.
Power Switch To turn on/off the power of the UV detector.
Wave Length Tuner*2 A tuner for wavelength range.
*1
RI Detector Detector for refractive index.
To collect fractions from the fraction nozzle or the
Siphon Box
siphon, or to collect the waste liquid.
To protect inner units from damages and leaking
Front Door
solvent.
*1 UV detector and RI detector are sold separately.
*2 Wave-length tuner is only available for variable wave length type UV detector.
2-4
<Inside of the LC-92XX NEXT Right Side Column Cover>
Column Holder
TO COLUMN Connector
Name Function
Manual Injector A place to store sample temporarily right after
Sample Loop syringe injection.
Connector of solvent's flow line from the body
TO COLUMN Connector
to columns.
FROM COLUMN Connector of solvent's flow line from the
Connector columns to the body.
Pre-Column Holder To hold the Pre-Column.
Column Holder To hold the Column.
A slit for switching UV wave length range, in
Cut Filter Exchanger
case of installed UV-600 NEXT*1.
A hole for turning optical null glass to adjust the
Null Glass Adj. Hole optical zero point with screwdriver, in case of
installed RI-700 NEXT*1.
*1 UV detector and RI detector are sold separately.
2-5
<LC-92XX NEXT Left Side>
Output Port
Power Switch
*1
Solvent Out
Name Function
Power Switch To turn on/off the LC-92XX.
To output recognized signals from detectors
Output Port
and valves.
Solvent out being connected to the fraction
Solvent Out*1
collector. (Option)
*1 The fraction collector is an optional product. Normally it is not used.
2-6
<Inside of the LC-92XX NEXT Siphon Box Door>
Siphon
Name Function
2-7
Specification
If the explanation or specification is the same for both LC-9210 NEXT and LC-9225 NEXT, it is written
as 92XX NEXT in this manual.
*In the LC-9225 NEXT, the maximum discharge pressure differs depending on the flow rate to be
used.
2-8
NEXT Series Features
This section describes the functional characteristics of LC-92XX NEXT
series.
Layout
Body size made 1/3 smaller compared to our previous models with
improved functions and performance.
Easy to operate
2-9
Auto-cleaning
Non-diffusion function
2-10
Flow Channel Map
The flow channel map of the LC-92XX NEXT series is as follows.
Pump
Buffer Volume
Collect Valve
Solvent Filter Detector
2-11
<Normal Flow Channel via Siphon>
2-12
<Recycle Flow Channel>
2-13
Operation Panel Display
This section provides the overview of the operation panel of the LC-92XX
NEXT series.
Unit Tab
The unit tabs and their
operation keys
2-14
2-2
2-15
WAKE UP
WAKE UP is the state when the power is turned on.
It refers to the initial screen of the LCD display that starts when the power
switch is turned on.
Power on
Initial screen 1
HE L LO ! H E L L O !
LC-NEXT SER I ES L C - N E X T
( C ) JA I ( C )
Initial screen 2
HE L LO ! HE L LO !
LC-NEXT SER I ES LC- NEX
LC- 9 2 1 0
( C ) JA I (C
HE L LO
LC- NE
Normal screen Flow rate
(
F L OW 09 . 9 0 m l /m i n
Monitoring pressure
PRESS 0 . 0 MP a
UV 00 0 0 UV output
RI 00 0 0
RI output
*The LC-9210 NEXT model is used as example.
*While the initial screens 1 and 2 are displayed, the system performs the initialization,
verification of the previous settings, and preparation.
*Key operations are not available on the initial screen 1 or 2.
2-16
Description of Arrow Keys and [OK] Key
The arrow keys are mainly used to change various setting values.
The up arrow key increments the numerical value at the blinking
cursor, and the down arrow key decrements it. The right arrow key
shifts the blinking cursor to the right, and the left arrow key shifts it
to the left. After setting, press the [OK] key to update the setting
value.
*When the manual [CLEAN UP] operation is required or when an error message is displayed,
the LED blinks at the top of the key.
2-17
Description of Units
PUMP Unit
2-18
<Setting Pump Flow Rate>
F L OW R A T E S E T F L OW R A T E S E T - U P
0 9 . 9 0 m l /m i n 0 9 . 9 0 m l /m i n
( M A X : 1 0 . 0 0 m l /m i n ) ( M A X : 1 0 . 0 0 m l /m i n )
F L OW R A T E S E T - U P F L OW R A T E
0 9 . 9 0 m l /m i n 09
F L OW 09 . 9 0 m l /m i n ( M A X : 1 0 . 0 0 m l /m i n ) ( MA X : 1 0 . 0
PRESS 0 . 0 MP a
UV 00 0 0
RI 00 0 0
Press the [FLOW SET] key to display the setting screen in the LCD
display. Use the arrow keys to set the numerical value at the
blinking cursor. After setting, press the [OK] key to update the
setting value.
2-19
<Setting Pump Pressure Limits>
M A X I M UM S E T M I N I M UM S E T
0 2 . 0 MP a 0 0 . 4 MP a
( M I NS E T V A L : 0 0 . 0 MP a ) ( MA X S E T V A L : 0 2 . 0 MP a )
The current pressure is displayed in the normal screen of the LCD display.
Press the [MAXIMUM SET] key to set the maximum pressure limit.
Press the [MINIIMUM SET] key to set the minimum pressure limit.
M I M I M A M S E T
<Setting Maximum Pressure Limit> 0 0 . 1 M
( M A and
When it's over pressed, this function is to protect columns X : detectors.
5 0 . 0 0 M P a )
Press the [MAXIMUM SET] key to display the setting screen in the LCD
display. Use the arrow keys to set the numerical value at the blinking
cursor. After setting, press the [OK] key to update the setting value. When
the maximum pressure limiter is activated, the whole system stops and an M I M I M
error message appears.
( M
*"(MINSETVAL: 00.0 MPa)" displayed in the setting screen indicates the setting value of the
minimum pressure limit
<Setting Minimum Pressure Limit>
When it's pressed too low, this is to protect columns and solvent from
splitting. Press the [MINIMUM SET] key to display the setting screen in
the LCD display. Use the arrow keys to set the numerical value at the
blinking cursor. After setting, press the [OK] key to update the setting
value. When the minimum pressure limiter is activated, the whole system
stops and an error message appears.
*"(MAXSETVAL: 00.0 MPa)" displayed in the setting screen indicates the setting value of the
maximum pressure limit.
*For details on how to operate the arrow keys, refer to P.2-17.
*In case that the pressure limiter is activated to stop the system, refer to "Volume 4
Maintenance Manual" for trouble shooting.
*The maximum value cannot be less than the minimum value, and they cannot exceed
50.1 MPa.
2-20
Detector Unit
UV DETECTOR RI DETECTOR
・In the [UV DETECTOR] and [RI DETECTOR] units, there are the keys for
adjusting the current UV/RI output to O mV and setting the recorder
signal range.
・In the LCD display, the current UV/RI output is displayed in mV unit.
UV Unit
・In the UV unit, there are the [AUTO ZERO] key for adjusting the UV
output to 0 mV, the [RANGE] key for setting the recorder signal range,
and the [SET] key for setting the detector response speed.
2-21
<Zero Adjustment Key>
・Press the [AUTO ZERO] key to adjust the current UV output to 0mV.
However, when the UV transmittance is too low, the AUTO ZERO
function may not work.
UV RANGE SET
x001
↑ : RANGE UP
↓ : RANGE D OW N
・This function is used for output signal attenuation of pen recorder. Press
the [RANGE] key to display the setting screen in the LCD display.
Press the arrows key to increment the signal range (the peak will
be shown smaller), or to decrement it (the peak will be shown
larger).
*In case of monitoring the chromatogram with integrator, recorder signal range
buttons are without the need for setup.
*In case a peak-sense (sense threshold and peak height) fraction collector
(optional product) is used, the range need to be adjusted.
2-22
<Brightness Check>
UV S E T
*ME NU
P A R AM E T E R
BACK
UV S E T ( M E N U )
* S AMP L E 1000
R E F E R E NC E 1500
BACK
・This function is used to perform the brightness check of the lamp
installed on the UV detector. Press the [SET] key and select [MENU] to
display the output values of [SAMPLE] and [REFERENCE].
*If the [REFERENCE] value is too low, the lamp should be replaced.
D O Y O U S E T
<Setting Detector Response Speed>
Y E S
UV S E T
ME NU
* P A R AM E T E R
BACK
U V S E T ( P A R AM E T E R )
* R E S PONS E MID
( S L OW←→M I D←→F A S T )
BACK
U V S E T
・This function is used to set the detector response speed. Press the
* M E N U
[SET] key and select [PARAMETER] to display the response setting
P A R A M E T E R
screen. You can select the response speed from the three levels,
[SLOW], [MEDIUM], and [FAST]. They mean the time constants of 1.5
sec, 0.5 sec, and 0.05 sec respectively. To change the setting, press
the or arrow key.
U V S E T
M E N U
2-23
* P A R A M E T E R
RI Unit
・In the RI unit, there are the [AUTO ZERO] key for adjusting the RI
output to 0 mV, the [RANGE] key for setting the recorder signal range,
the [PURGE] key for replacing the solvent in the reference cell, and the
keys for selecting the polarity and whether or not to control the
temperature.
・Press the [AUTO ZERO] key to adjust the current RI output to 0mV.
When the optical balance is lost too much, the AUTO ZERO function
may not work.
*If the zero adjustment function does not work, refer to "Volume 4 Maintenance
Manual".
2-24
<Starting PURGE>
・This key starts/stops replacing the solvent in the reference cell. Press
to change the flow channel to the reference cell for one minute. At
the top of the key, the LED is turned off when the fraction is flowing
through the sample cell, and turned on when it is flowing through the
reference cell.
*During the [CLEAN UP] operation, the solvent in the reference cell is also
replaced automatically. This PURGE function may not be used in general
operation.
<Starting TEMP.C>
・There are cases that current RI output is shown in negative, when the
solvent with high index of refraction is used for mobile phase. This key
can be used to reverse the negative signal to positive. When the LED is
turned on, the signal is output as it is. Press the [POLARITY] key to turn
the LED off and reverse the polarity from negative to positive.
2-25
FRACTION Unit
D E A D V O L UM E SET
* UV 0 1 . 9m l
( UV ←
→RI ←
→ ELSE )
・You can use this key to select the detector that detects the peak for
the basis of collecting fractions. Press the or arrow key
to select a detector. The time difference is calculated as dead
volume from the selected detector to a fraction nozzle. If you select
[ELSE], you can set an arbitrary value when pipe lines are extended
or other detectors are installed. To set an arbitrary value, press
and select [ELSE] to display the setting screen. Use the arrow keys
to set the numerical value at the blinking cursor.
2-26
<Siphon/Fraction Nozzle Selection Key>
・You can use this key to collect the fractions of eluent from the detector
by using the siphon or the fraction nozzle. The LED is turned off for the
eluent from the siphon, and turned on for the eluent from the fraction
nozzle. To collect fractions with the fraction nozzle, press when
the LED is off. Then the LED blinks, which indicates that the fraction is
passing through the dead volume specified by [DEAD VOLUME SET].
After passing through the dead volume, the eluent will flow from the
fraction nozzle. If you press again, the LED blinks in the same
way, and the eluent passes through the dead volume and then flows
from the siphon.
RECYCLE Unit
<Starting RECYCLE>
2-27
CLEAN UP
Press the [CLEAN UP] key at the lower right of the operation panel to
execute the flow line cleaning automatically.
50%
S TART E ND CLEAN UP progress
In the LCD display, there are the two sections; one indicates the place
where the [CLEAN UP] operation is being executed, and the other the
operation progress.
<STATUS Display>
The upper section of the LCD display shows the place where the
[CLEAN UP] operation is being executed. For information on what the
display indication means, refer to the following table:
2-28
<CLEAN UP Progress>
S AMP L E L OO P C L E A N I NG
50%
S TART E ND
The lower section of the LCD display shows the progress of the
[CLEAN UP] operation. 100% means the completion of the operation.
<Emergency Stop>
If you press the [CLEAN UP] key during the [CLEAN UP] operation,
the LED is turned off, and the operation is stopped forcibly. Please
press the key only in emergency situation. After the emergency stop,
the display returns to the normal display.
<How to Operate>
When you press the [CLEAN UP] key, the operation procedures are
displayed in the LCD display. Please follow the instruction. When a
manual operation is required or when you need to verify settings, a
message appears in the LCD display with an intermittent beep. The
[CLEAN UP] operation ends in 10 to 15 minutes. After the completion,
turn the column selector valve back to its original position
([COLUMN]) to use it.
2-29
<How to Use Solvent Suction Attachment>
In the LC-92XX NEXT, you must inhale the solvent by using a solvent
suction attachment (standard accessory) at the preparation for the
[CLEAN UP] operation.
<How to Use>
2-30
2-3
2-31
Recycling Separation
Recycling separation:
COLUMN: JAIGEL-1H -F+JAIGEL-2H-F
FROW RATE: 3.5 ml/min
SAMPLE: Polystyrene oligomer (Mw. 495, Mw/Mn 1.20)
2-32
Separation efficiency with n times Recycling is shown following formula.
2(n+1) (TR2-TR1)
Rn+1=
{(n+1) W 12+nW E2}1/2+ {(n+1) W 22+nW E2}1/2
T1 T2
Chromatograph
W2
W1
* When a column more than 20φ i.d. is used, W E does not affect the separation because it is negligible
smaller than the column volume. When Recycling executes many times, turn the MANUAL INJECTOR
2-33
Note of good Recycling Separation
Recycling separation may have the following troubles. Before the real
Recycling, pretest is recommended for the chromatogram acquisition
without Recycling.
When the Recycling area is too wide or the Recycle times are too much,
re-mixture trouble may occur. The top of recycled area will mix with the
tail of the recycled area. Recycling area and times should be suitable
value.
1st Cycle
2nd Cycle
3rd Cycle
5th Cycle
4th Cycle
6th Cycle
Re-mixture
Re-mixture
2-34
<Overlap Trouble>
If the Recycling area is set too fast retention time, 2nd cycle peak get
past the 1st peak (symptom 1) or 2nd cycle peak overlaps with the later
peak (symptom 2). Pretest is recommended for the chromatogram
acquisition without Recycling to avoid overlap troubles.
Symptom 1
Symptom 2
without A
Recycle
chromatograph
Recycle chromatograph
Normal chromatograph
2-35
<Contamination Trouble>
The LC-92XX NEXT series standard specification has the backflow
prevention system. The backflow prevention system works to reduce
contamination during the recycle operation for good recycle separation.
The backflow prevention system has a buffer-volume. The buffer-volume
is cleaned during CLEAN UP operation. When the CLEAN UP is
neglected or high-viscosity sample/low soluble sample is recycled,
shock peak may appear at change over of the Recycling valve. When
the shock peak appears, do CLEAN UP operation again. If the symptom
cannot be remedied, cleaning-maintenance is required. Please refer to
Volume 4 "Maintenance Manual".
0 20 40
Rt (min)
2-36
For good Recycling efficiency
During Recycling separation, recycled sample flows unique flow line that
the normal HPLC is not used, rear flow of the Detector, the Pump, and
the Injector flow line.
Select suitable instrument and turn over the knob of the MANUAL
INJECTOR to LOAD.
To Column
Plunger
pressurized.
LC
Type LC-9210 NEXT LC-9225 NEXT
Plunger volume 32 μL x 2 77μL x 2
2-37
<Turn Over the Knob of the MANUAL INJECTOR to LOAD>
The LC-9210 NEXT has a 3 mL-Sample loop, and the LC-9225 NEXT
has a 10 mL-Sample loop as a standard.
When multiple times Recycling is done, turn over the knob to LOAD to
eliminate the sample loop from the flow line because the recycled
sample diffuse in the sample loop.
Wait the manual injector knob at the [INJECT] position while injecting the
sample, cleaning the needle port, and filling the sample loop with the
new solvent. After that, turn the manual injector knob to the [LOAD]
position.
When the pump flow rate of the LC-9210 NEXT is set at 3.0 mL/min or
more (10 mL/min or more for the pump flow rate of the LC-9130 NEXT),
wait for one minute after the injection, and then turn the manual injector
knob to the [LOAD] position to eliminate the sample loop from the flow
line.
Line
From Pump From Pump
To Column To Column
INJECT LOAD
2-38
2-4
2-39
Setting Operation
Pump setting
Set the pump flow rate and the pump pressure limit in the [PUMP] unit.
The pressure maximum limiter stops the pump when the pump pressure rises over the
limit, so as to prevent a column and detector cell damage from the over pressure coming
from injection of dust and precipitated insoluble in a column. An error message appears
when the limiter works.
The pressure minimum limiter stops the pump when the pump pressure drops below the
limit, so as to prevent a column damage or solvent spill when the solvent loses or leakage
of system occurs. An error message appears when the limiter works.
2-40
<Limit of Setting Value>
The setting values of flow rate and pressure limits is limited in accordance
with the LC model and the set flow rate.
Refer to the following table. When the setting value is over the limitation, an
error message appears.
The flow rate can be set in the ranges of 0.1 to 10.0 mL/min and 0.1 to 30.0
mL/min for LC-9210 NEXT and LC-9225 NEXT, respectively.
To stop a pressure limiter, set [0 MPa].
Caution
When the Pump is running, the flow rate cannot be changed. Stop the Pump and reset the
flow rate. When the pump flow rate is changed, change the [MAXIMUM] pressure limit to
"monitoring pressure + 2.0 MPa" or more, and the [MINIMUM] pressure limit to "monitoring
pressure - 2.0 MPa" or less.
2-41
Setting UV detector
In the [UV] unit, the UV-370 NEXT, UV-254 NEXT, or UV-600 NEXT
function can be set.
*In case of monitoring the chromatogram with integrator, recorder signal range
buttons are without the need for setup.
*In case a peak-sense (sense threshold and peak height) fraction collector
(optional product) is used, the range need to be adjusted.
2-42
<Wavelength Selection>
・Pull the front door forward. UV Detector
Front Door
Pull forward
Wavelength
Selector
Locking Pin
Close
Releas
・Remove the locking pin of wave-length selector inside the front door.
・Turn the wave-length selector to set the wave-length.
・Tighten the locking pin.
・Close to the front door.
・Press the [AUTO ZERO] key in [UV DETECTOR].
2-43
Setting RI detector
In the [RI] unit, the RI-700 NEXT function can be set.
*In case of monitoring the chromatogram with integrator, recorder signal range
buttons are without the need for setup.
*In case a peak-sense (sense threshold and peak height) fraction collector
(optional product) is used, the range need to be adjusted.
*Reverse polarity is profitable when high refractive index solvent like toluene is used for
eluent.
*Please refer P.2-51, for the typical solvent refractive index.
2-44
<Setting TEMP C>
・When the LED is turned on, the temperature controlling heater of the
detector is on to maintain the temperature at 35℃. Press the [TEMP C]
key to turn the LED off, which indicates that the temperature is not
controlled.
*When the LED is turned on, more stable RI signal is obtained. Normally, the LED should
be turned on.
*Using low boiling point solvent, turn the LED off to suppress bubbling of the solvent.
*Please refer P.2-51, for the typical solvent boiling point.
2-45
Setting fraction
In the [FRACTION] unit, the dead volume can be set.
*The default value is preset in case our optional products (UV-254 NEXT, UV-370
NEXT, or UV-600 NEXT for UV detector, and RI-700 NEXT for RI detector) are
installed.
*If [0.0] value is selected, the dead volume (delay time) is neglected. Immediately after
pressing the [Co/Dr] key, the valve to be used is switched between the fraction nozzle
and the siphon.
*When the [RECYCLE] operation is switched to ON/OFF, the dead volume (delay time) is
neglected. Immediately after pressing the [RECYCLE] key, the valve is switched.
2-46
2-5
Chapter 5 Appendix
Degassing, property of typical organic solvent, elimination of micro
particles
2-47
Degassing
Solvent to use an eluent in the LC-92XX should be degassed. Pressure
fluctuation of the peak retention time or the detector noise may occur with
the babble in undegassed solvent. To result best chromatograph without
noise and fluctuation, the solvent to use an eluent should be degassed.
2-48
<Degassing with Ultra Sonic Cleaner>
・Move the solvent into the container. In case of
mixture solvent, stir the solvent thoroughly.
Without stirring the mixture solvent, the
reproducibility of the chromatogram may be lost,
because the lost of the component may occurs.
・Dip the container in the Ultra sonic cleaner. Ultra sonic cleaner should be
half full with water.
・Wipe the drops out of the container and place the container on the solvent
stage in the LC-92XX NEXT.
Dissolvent of the air into the solvent occurs soon after degassing. Do
degassing just before use the solvent.
2-49
<Degassing with Ultra Sonic Cleaner Plus Vacuum>
To aspirator
・Move the solvent into the container. In case of
mixture solvent, stir the solvent thoroughly.
Without stirring the mixture solvent, the
reproducibility of the chromatogram may be lost,
because the lost of the component may occurs.
The solvent container must be vacuum tight. A
conical beaker or conical flask may be
damaged at decompression.
・Vapor from the solvent contains organic vapor. To prevent spill of the
organic vapor to swage, use closed system aspirator to make vacuum.
Waste water should be disposed properly according to laws and
regulations in the same manner as organic solvents.
・Place the container in the ultra sonic cleaner, and seal it with a rubber
stopper that is fitted into the container mouth. Set a vacuum line to the
rubber stopper, and connect its one end to the aspirator.
・Perform the ultra sonic cleaning, and operate the aspirator to reduce the
pressure of the container. Operate both the ultra sonic cleaner and a water
aspirator in 5 min.
time and vacuum condition. Keep the vacuum degree and time in
constant.
・Wipe the drops out of the container and place the container on the solvent
stage in the LC-92XX NEXT.
Dissolvent of the air into the solvent occurs soon after degassing. Do
degassing just before use the solvent.
2-50
Property of typical organic solvent
Pentane 0.00 0.24 200 1.357 36.1 Acetone 0.56 0.30 330 1.359 56.3
Hexane 0.01 0.31 200 1.375 68.7 Methyl ethyl ketone 0.51 0.42 329 1.379 79.6
Heptane 0.01 0.42 200 1.388 98.4 iso-Butyl methyl ketone - 0.54 334 1.396 116.5
2,2,4-triMethylpentane 0.01 0.50 215 1.391 99.2 Diethyl ether 0.38 0.24 218 1.352 34.6
Nonane - 0.72 200 1.405 150.8 Diisopropyl ether 0.28 0.37 220 1.369 69.0
decane 0.04 0.92 210 1.412 174.1 Tetrahydrofuran 0.45 0.55 212 1.407 66.0
Cycropentane 0.05 0.47 210 1.409 49.3 1,4-Dioxane 0.56 1.44 215 1.442 101.3
Cycrohexeane 0.04 0.98 200 1.426 80.7 Propylene carbonate - - - 1.419 240.0
Benzene 0.32 0.65 278 1.501 80.1 Methanol 0.95 0.55 205 1.328 64.7
Toluene 0.29 0.59 284 1.497 110.6 Ethanol 0.88 1.20 210 1.361 78.3
o-Xylene 0.26 0.81 288 1.505 144.4 1-Propanol 0.82 2.26 210 1.386 97.2
m- Xylene 0.26 - 290 1.496 138.5 2-Propanol 0.82 2.86 205 1.377 82.3
Dichloromethane 0.42 0.45 233 1.424 39.8 2-Methoxyethanol - 1.72 210 1.402 124.6
Chloroform 0.40 0.58 245 1.446 61.2 1-Butanol - 2.95 215 1.399 117.7
Carbon tetrachloride 0.18 0.97 263 1.460 76.8 2-Butanol - 4.21 260 1.397 99.6
1,2-Dichloroethane 0.49 0.79 230 1.445 83.4 Isobutanol - 4.70 200 1.396 107.7
Trichloroethylene - 0.57 273 1.477 87.2 2- Ethoxyethanol - 2.05 210 1.408 135.6
Tetrachloroethene - 0.93 295 1.506 121.2 Acetonitrile 0.65 0.34 190 1.344 81.6
n-Butyl chloride - 0.47 220 1.402 78.4 Diethylamine 0.63 0.38 275 1.387 56.0
Chlorobenzene 0.30 0.80 287 1.525 131.7 N,N-Dimethylformamide - 0.92 268 1.430 153.0
o-Dichlorobenzene - 1.32 295 1.551 180.5 N,N-Dimethylacetamide - 2.14 268 1.438 166.1
Disulfide 0.15 0.37 380 1.626 46.3 Pyridine 0.71 0.95 330 1.510 115.3
N- Methyl
Methyl acetate 0.60 0.37 260 1.362 56.3 - 1.67 285 1.488 202.0
-2-Pyrrolidone
Ethyl acetate 0.58 0.46 256 1.372 77.1 Dimethylsulfoxide 0.62 2.20 286 1.478 189.0
Butyl acetate - 0.73 254 1.394 126.1 acetic acid 大 1.31 - 1.372 117.9
2-51
<Miscibility of Solvent>
Acetic acid
Acetone
Acetonitrile Immiscibility
Benzene
Butanol Miscibility
Carbon tetrachloride
Chloroform
Cycrohexeane
Cycropentane
Dichloroethane
Dichloromethane
Dimethylformamide
Dimethylsulfoxide
Dioxane
Methyl acetate
Ethanol
Diethyl ether
Heptane
Hexane
Methanol
Octane
Pentane
Propanol
Dipropyl ether
Tetrachloroethane
Tetrahydrofuran
Toluene
Trichloroethane
Water
Xylene
Acetic acid
Acetone
Acetonitrile
Benzene
Butanol
Carbon tetrachloride
Chloroform
Cycrohexeane
Cycropentane
Dichloroethane
Dichloromethane
Dimethylformamide
Dimethylsulfoxide
Dioxane
Methyl acetate
Ethanol
Diethyl ether
Heptane
Hexane
Methanol
Octane
Pentane
Propanol
Dipropyl ether
Tetrachloroethane
Tetrahydrofuran
Toluene
Trichloroethane
Water
Xylene
Replace solvent for a column should be easy soluble chemical against the
solvent pre-used. Make sure that a solubility is good each other. When
changing solvents are poor solubility each other, select the intermediate
solvent which has good solubility to each other.
In case salt contained solvent, the intermediate solvent which has a good
solubility to salt, then replace the final solvent.
2-52
Micro particle elimination
To come in Micro particles such as dust and insoluble, the LC-09XX and the
column may be damaged. Such micro particles should be eliminated before
the application.
In case clear appearance, some time the solvent contain micro particles,
so make sure to eliminate the micro particles.
2-53
<Micro Particle Elimination in Sample Solution>
・With Membrane filter of 0.45μm, filtrate the
sample solution using pressure of a
syringe.
Filtered Sample
The sample may contain the micro particles. Make sure to eliminate the
micro particles.
After injecting the sample with the manual injector, be sure to rinse and
clean the needle port described as follows.
2-54
Index
(Each number indicates a page number within "Volume 2 General Information Manual". Please refer to
[ E Solution · 54
MINSETVAL · 20
[MAXIMUM SET] Key · 20, 40 Elimination of Micro Particles in Solvent ·
Miscibility of Solvent · 52
[MINIIMUM SET] Key · 20 53, 54
FRACTION Unit · 26
Brightness Check · 23
O
FROM COLUMN Connector · 5
C L Output Port · 6
Overlap Trouble · 35
CLEAN UP · 17, 25, 28, 29, 30
LCD Display · 16, 19, 20, 21, 22, 28, 29, 30,
Column Holder · 5
40, 42, 44
Column Reject Valve · 3
P
Limit of Setting Value · 41
Contamination Trouble · 36
Locking Pin · 43 Power Switch · 4, 6
Cut Filter Exchanger · 5
Luer-lock Syringe · 30 Pre-Column Holder · 5
Pump Head · 4, 28
Degassing with ON-LINE DEGASSER ·
Manual Injector · 5
PUMP Unit · 18
48
Manual Injector Valve · 3
Degassing with Ultra Sonic Cleaner · 49,
Manual Sample Injector · 7, 8, 9, 28, 38, 54
50
R
Maximum Discharge Pressure · 8
24, 42, 44
2-55
RECYCLE Unit · 27 Siphon · 3, 4, 7, 12, 26, 27, 30, 46 U
Recycling Separation · 32 Siphon Box · 3, 4, 7, 30
UV Detector · 4, 23, 26, 46
Relation between Peak Separation and Solvent Property List · 51
UV DETECTOR · 21, 43
the number of Recycling · 32 Solvent Suction Attachment · 30
UV Unit · 21, 24
RI Detector · 4, 25 Solvent Table · 4
RI DETECTOR · 21 Specification · 8
2-56
VOLUME
This manual is for JAI staff to install the LC-92XX NEXT series
properly.
3-1
Installation Location
Place the LC-92XX NEXT series at the location and environment that satisfy the
following conditions for correct operation.
Installation Location
The LC-92XX NEXT requires space at least more than 500 mm (W) x 600 mm (H) x
600 mm (D). Depth may need 750mm for an air vent and power supply parts at the
back of the body. For left and right of the body, may need extra 100mm each for
enough space.
The table to place the body has to be horizontally stable and capable to hold the
weight of the body.
Please prepare an enough space for optional accessories and attachments as well.
Environment
3-2
Installation Conditions
Place the LC-92XX NEXT series at the location that satisfies the following installation
conditions for correct operation.
Power condition
Electrical sockets: It has a 3 pins plug with a ground connection (Type A). In case
of none ground connection socket or different type of plug,
please be advised to use an extension and/or adapter to make
it 2 pins plug and connect ground terminal.
3-3
3-2
3-4
Serial Number Check
<Serial Numbers>
・Check out the serial numbers of the body and detectors.
3-5
Pipe Line Connections
Follow the instructions to connect the pipes appropriately to use the LC-92XX NEXT
series.
1. UV Detector Tray
2. UV Screw
3. RI Detector Tray
・ Take out the plastic bag from inside of the body and unscrew all the seal
plugs.
・ Push back the UV Detector tray into the body thoroughly; make sure the
other pipe lines.
3-6
<Pipe Connection>
<A line: Pump out tee joint – Pump drain valve>
A
・ Connect the A pipe between the tee joint of the
pump out and the pump drain valve.
UVD
Pump
TO UV union
3-7
<UV detector cell (up part) – UV-RI union (IN)>
<C line: UV-RI union – RI detector (IN)>
UVD
UV-RI Union
Siphon Box
・ Connect the F pipe from underneath the pump
RID drain valve to the pump drain port of the siphon
box.
Valve Union
Pump Drain Port (Behind the Pump Drain Valve)
3-8
<Solvent supply port – solvent suction line (with line filter)>
Total Waste
Into a waste
reservoir
3-9
Wiring Connections
Follow the instructions to connect the wiring appropriately to use the LC-92XX NEXT
series.
Unavailable
To AC
AC INLET
power 100V
3-10
<Main Body to Integrator (or Recorder)>
・Connect an integrator (or a recorder) signal
Output Port cable to the output port (16 terminals).
*Minus signals at recycle signal(12), collect valve(14), and siphon counter signal(16) are the same. In use of an
electronic device such as JDS series to read several signals at once, joint the outputs with a jumper wire and
connect as one output port.
3-11
<Connect to JDS Series (Sold as optional accessory)>
<Connect to a JDS signal cable>
・Connect the cable between the D sub-
miniature connector and the JDS signal inputs
[H] and [L].
・In use of 2 different detectors, connect another
signal inputs [H] and [L] to output port + (3)
and – (4) as well.
(The left image shows only the UV detector.)
3-12
3-3
3-13
Preparation for the validation
The items listed below are required to validate that the LC-92XX NEXT series is
installed correctly. * 1 items are standard equipped. * 2 items are prepared by JAI staff.
Those without *1 or *2 should be prepared by customer side.
Upon customer's request, we can execute validation in a different way, after mutual
agreement instead of the following standard validation.
3-14
Sample for Validation
3-15
Pipe Line and Start Cable Test
Check the pipe line connection and the start cable connection of the LC-92XX NEXT
series.
・Remove the column cover from the right side of the instrument, and connect a
dummy pressure sensor between [TO COLUMN] and [FROM COLUMN] using a
wrench.
・Dip the solvent filter into methanol or chloroform. Place the solvent container on
Solvent table located upper shelf of LC-92XX NEXT series.
・When [PUMP PURGE] is displayed on the screen during the [CLEAN UP]
operation, check the solvent out from the pump drain out in the repeat injector box.
In the LC-92XX NEXT, you must inhale the solvent by using a solvent suction
attachment at the preparation for the [CLEAN UP] operation.
・ Settings
Settings
Flow Rate 9.0 mL/min
[MAXIMUM] 0
Pressure Limiter
[MINIMUM] 0
*1 This is the case of the optical pass length of 0.5 mm. With other optical pass length, adjust
the concentration of sample accordingly.
3-16
・ Start Pump.
・ Make sure that the pump pressure is stable.
Check Column Pressure Stability
Column pressure is stable. □
・ Refer to the page 1-8 at Volume 1 to perform the zero adjustment of the
detector.
・Set up the integrator or recorder.
Leak Check
Inside of the front door □
Connectors of dummy pressure sensor □
・When using the integrator, check whether 3 chromatograms are obtained, and
whether the peaks are similar in visual. When using the recorder, check that three
peaks are obtained and that they are similar in visual.
Check Chromatogram
Three chromatograms or peaks are obtained □
Peaks are similar in visual □
3-17
Wiring Connections and Valve Validation
Check the wiring connections and valve operation of the LC-92XX NEXT series.
3-18
・After checking the recycling peak, press in [RECYCLE] to stop the
[RECYCLE] operation. Then press in [FRACTION] and check that the eluent
・ After checking the collect valve, press in [FRACTION] and check that the
3-19
VOLUME
Normally cut off the AC power. Be careful of electrical shock during the
maintenance when power switch turn on.
4-1
4-1
Replacement of Column
If the separation is required with the different type column, replacement of column is
needed.
Surely stop the pump during the replacement of column to prevent solvent spill.
<Installing Column>
Install the column as following.
・Remove the column cover of the LC-92XX NEXT from the chassis.
・Hold the column(s) on the column holder inside of the column cover.
Column
TO COLUMN Connector
Column Holder
FROM COLUMN Connector
・Replace the solvent which is able to use with the replaced column(s), with
before used solvent, thoroughly in the flow line of LC-92XX.
Before the solvent replacement, test the solubility between replaced solvent
and before used solvent.
Use Auto-cleaning function for the solvent replacement in the LC.
・Set the pump flow rate to use with the replaced column(s).
4-2
・Cover the outlet of the pipe with a paper towel or thick paper for absorption of
the over flowed solvent.
And start the pump for purging air in the pipe. Please make sure to protect
the replaced column(s).
If the flow rate is large, solvent may flush and spray. Be careful.
Thick Paper for Absorption
Be careful of the
spray.
TO COLUMN Connector
・Once stop pump and remove the seals of the replaced column(s). Connect
the pipe on inlet of the replaced column(s).
Column Column
Inlet ↑ Outlet
FLOW Seal
・When the column is jointed series two or more, the air in the jumper pipe
jointed columns also should be purged.
・Joint the jumper pipe on the first column outlet. Do not joint the pipe on the
second column inlet on this point.
・Cover the outlet of the jumper pipe with a paper towel or thick paper for
absorption of the over flowed solvent. And start the pump for purging air in
the pipe. If the flow rate is large, solvent may flush and spray. Be careful.
Column Outlet
Be careful of the
spray.
4-3
・Connect the jumper pipe on the second column inlet. Connect the pipe from
the column outlet on the [FROM COLUMN connector].
FROM COLUMN
Connector
・Make sure that no leakage is found when the pump is started, then close the
front door.
4-4
<Removing Column>
To remove columns, refer to the instructions below.
・Remove the outlet pipe column. When the Column pressure is high, you
may have dispersed solvent. Be careful.
・Put the seal plug into the column outlet. Tighten the seal plug 1/4 turns by
hand, and then tighten by a wrench. Use a hand for a PEEK-type seal
plug. Too strong tightening may damage the screws or column. Be
careful.
Seal Plug
Make sure that the column removed the pipe are tightly sealed without
solvent leakage, keep in cool dark place.
・Connect with the U shape pipe between the [TO COLUMN connector]
and [FROM COLUMN connector] of the LC that are removed the pipe
from the Column.
4-5
Cleaning of Solvent Filter
When the pump flow rate is not stable and, when no solvent is supplied at the auto-
cleaning, the Solvent filter may cause clogging of dust or particles.
The Solvent filter is clogged with dirt and dust if the solvent without dust removal is fed
to the solvent reservoir.
・Open the front door. Remove the solvent filter connected on the solvent
supply port.
Front Door Solvent Supply Port
Solvent Filter
・Remove the Solvent filter and pipe from the solvent reservoir, put the
Solvent filter and pipe into a beaker filling the solvent.
・Do clean for 10 minutes with the beaker dipped into an ultrasonic cleaner.
4-6
Maintenance of Manual Injector
After high concentration or low solubility sample injection, the Stator face, and the
Rotor seal of the Injector may dirt or precipitate with the remained sample.
If you do not wash with the needle port cleaner after the injection the symptom may
occur. If solvent start leaking from Manual Injector, or if the ghost peaks appear,
Manual Injector may be improved by maintenance.
Rotor seal and Stator face should be replaced every year.
・Remove the Solvent filter and pipe from the solvent reservoir.
・Remove the column cover of the LC-92XX NEXT from the chassis.
2 1
3 6: RHEODYNE Mark
・Loosen two socket set screws side of the manual injector knob at the
front of the LC-92XX NEXT with a hexagonal wrench.
4-7
・Remove retaining screws of the Manual Injector.
・Move apart the Manual Injector from the back of the LC panel.
・Remove Stator retaining screws. Remove Rotor seal, Stator ring, Stator
face, and Stator face from the Manual Injector body.
Stator Ring
Stator
Stator Retaining
Screws
Rotor Seal
Stator Face
・Install New Rotor seal. Place the Rotor seal to fit the tip of the needle port
tube into the liquid passing hole, and insert pins into the pin holes. Insert
as the mark of RHEODYNE co. on the Rotor seal faced toward Stator
face.
4-8
<Installing Manual Sample Injector>
・Place the Manual Injector on the original position at the back of the LC
panel, and tighten the Manual Injector by retaining screws.
・Replace and tighten the Manual Injector knob. Check the smooth
movement of Sample injection.
・If the movement of the Manual Injector knob is too hard or too loose,
readjust the Manual Injector knob. Loosen two socket set screws side of
the knob again. Readjust and insert the knob as fit perfectly the key into
the groove of the knob.
・Readjust the knob to turn. Appropriately check the movement of the knob
and readjust.
・Tighten the retaining socket set screws to install the Manual Injector knob.
・Connect each pipes restored on the back connection port of the Manual
Injector.
・Start Pump and flow solvent using Auto-cleaning function, and check that
no leakage is appeared at any connector. If the leakage is found, tighten
the connector additionally to stop.
・After the Auto-cleaning, Start Pump and flow solvent into the Column to
pressurize the system and check that no leakage is appeared at any
connector.
4-9
Maintenance of Pump
The pump has the necessary cleaning supplies and replacement parts, after which
period of time.
The pump seal replaced every four months, do cleaning the pump head in same time.
The check valve packing to exchange every six months, please replace with new ones
every two years.
Around the time of consumption may be due to the property and frequency of the
sample.
・Remove the Solvent filter and pipe from the solvent reservoir.
Front Door
・Disconnect the pipes A, B, C, D connected to the pump unit. For the pipes B
and C, remove the pipes while fixing the check valve cases with a wrench.
Pump Head
Turn by hand.
D
If the screw is hard, A
cover the screw with
paper and turn by a
nipper.
4-10
・Loosen the screw of the pump head with a 2.5 mm hexagonal wrench.
Loosen the screws alternately.
・Pull the pump head. Pull horizontally on the front. The tilted pull may damage
the plunger. Be careful.
Loosen the screws
alternately.
Pump Seal G
Backup Ring
(remove with tweezers.)
・Loosen the screw of the pump head guide with a 2.5 mm hexagonal wrench.
Loosen the screws alternately.
・Pull the pump head guide.
*Internal parts may fall out. Be careful not to lose them, especially the
stainless ball.
Stainless Ball
Loosen the screws (keeps on the far
alternately. side with grease.)
4-11
・ Remove the pump seal F attached to the pump head guide by using the seal
removal jig.
Seal Removal
Jig
Use the side with
screw.
Pump Seal F
・Clean the pump head. Put Pump head into the beaker. The most frequently
used solvent fills the beaker. Make ultrasonic cleaning for 5 minutes. Empty
the solvent in the beaker. Fill a beaker of methanol. Make ultrasonic cleaning
for 5 minutes. When methanol is non-miscible with used solvent, use ethanol
instead of methanol. Wash the Pump head attached the check valve without
any problems.
・Also wipe around the plunger with BEMCOT or soft gauze. In severe cases
of contaminated, moisten the gauze with a strong solvent like as HFIP and
wipe the Plunger with the moistened gauze.
・Install the pump seal F on the pump head guide by using the seal removal jig.
Seal Removal Jig
・Install the pump head guide on the pump unit. Insert the pump head guide
horizontally, being careful not to damage the pump seal F with the plunger.
・Tighten the screws of the pump head guide lightly. Tighten two screws on the
pump head alternately by 1/4 turns with a 2.5 mm hexagonal wrench to
tightly fix it.
Install the pump head guide with its holes facing outward.
Hole
Hole
4-12
・Insert the backup ring into the plunger.
・Tighten the screws of the pump head lightly. Tighten two screws on the pump
head alternately by 1/4 turns with a 2.5 mm hexagonal wrench to tightly fix it.
Be careful not to turn upside down.
・ Connect the pipes A, B, C, D on the pump head. For the pipes B and C,
connect them while fixing the check valve cases with a wrench.
A D
・Put the Solvent filter into the solvent reservoir. Fill the Pump head with
the solvent to use the [AUTO CLEAN] operation.
4-13
<Cleaning Check Valve, Replacing Check Valve Seal>
・Remove the Solvent filter and pipe from the solvent reservoir.
Pump Unit
Front Door
・Disconnect the pipes A, B connected to the pump unit. For the pipe B,
remove the pipe while fixing the check valve case with a wrench.
Turn by hand.
If the screw is hard, cover A
the screw with paper and
turn by a nipper.
・Remove the check valve inlet case and the check valve outlet case from the
pump head. Loosen the check valve to turn anti-clockwise. Be careful not to
lose inside parts. Remove the check valve outlet to turn anti-clockwise.
Check Valve Outlet Case
4-14
・The inside parts of the check valve is shown as following figure. Handle as a
unit each as "check valve case", "seat", and "check ball", do not confuse the
parts each other. Place each unit separately in the beakers.
・If dirt remains in the visual, remove the dirt with chloroform, toluene, or HFIP
as strong solvent.
・Assemble the check valve. Assemble the check valve as shown below.
Check Ball
Check Valve Case
Flow direction
・Assemble the check valve inlet. Assemble I part on the on the paper. Cover
gently Assemble part I with the check valve inlet case. Turn over gently by
pinching the corners of the paper.
Cover gently Assemble
part 1 with the check
valve inlet case.
4-15
・Assemble the check valve outlet. Assemble the check valve Ⅱon the paper,
holding your finger on the top of the parts, and turn over assembled check
valve gently by pinching the corners of the paper. Put the assembled parts
gently in the check valve case. Turn over the Cover with the assembled parts.
Turn over gently
by pinching the
Turn over gently by corners of the
Ⅱ
pinching the corners paper.
of the paper.
Check Valve Seat B
Seat
Check Ball
Check Valve Case
Check Valve Seat A
Paper
High hexagon
head type (7
mm)
・Connect the check valve outlet case into the pump head inlet case, and
tighten the case with a 10 mm wrench. The gasket B is fixed tightly into the
case. Remove the case, and make sure that the check valve gasket B
insertion is tight. Then connect the case to the pump head outlet side and
tighten it with a 10 mm wrench.
Connect the check valve outlet Connect the case
case into the pump head inlet into the outlet side,
side, tighten the case with a and fix it with a 10
10 mm wrench, and then mm wrench.
remove the case.
・ Connect the check valve inlet case into the pump head inlet and tighten by a
wrench anchor.
Connect the case into
the inlet side, and fix it
with a 10 mm wrench.
4-16
・The pipe B is connected to the pump unit as before. Tighten the screw of
pipe B. The Check valve outlet case is fixed by a wrench while the screw is
tightening.
・Use Auto-cleaning function for the solvent replacement in the Pump head.
4-17
Pipe Connection
Attached standard pipe PEEK and Stainless steel pipe is a consumable.
Repeated connection and release of Ferrule will be occurred collapse or bite of the
screws. Increased dead volume and leakage or damage of the screws may cause.
Replace with new ones when the connector repeats three times of lock and release.
PEEK pipe has life. If only organic solvent is used, PEEK pipe early decays. Solvent
leakage or splash may occur from the decayed PEEK pipe.
Please replace a new one a month in continuous operation.
Front Ferrule
Back Ferrule
Male Screw
In case of PEEK pipe, insert only D) Fitting for PEEK pipe into the pipe.
4-18
・Insert top of the pipe into a union connector. Pressing the pipe into the
bottom of the connector, turn clockwise by hand.
・ Pressing the pipe into the bottom of the connector, turn 3/4 clockwise by a
wrench.
Union
Turn 3/4 clockwise by a
wrench
In case of PEEK pipe, turn clockwise Fitting for PEEK pipe only by hand, and
do not use a wrench or other tool.
4-19
Adjustment of RI Detector
Optical zero of RI Detector may shift according solvent to use. After turning the power
switch on, the output value that is displayed on the LCD display immediately after the
auto-cleaning operation indicates the optical position. If the monitoring output is over
±200, the optical alignment is recommended with the re-alignment of the NUL glass.
・After the [CLEAN UP] operation, check the RI output value on the LCD display.
・Insert a blade of a screw driver and turn with slot of the alignment screw.
・While checking the RI output value on the LCD display of the main body, turn
the driver to perform zero adjustment.
・Remove the driver from the hole. Close the Column cover.
4-20
Manual Cleaning Instruction of Buffer Volume
The LC-92XX series has the Reverse flow protection during Recycling Separation as a
standard. The Reverse flow protection system has a buffer-volume.
The buffer-volume is automatically cleaned in the CLEAN UP operation. When the LC-
92XX has stopped in long term, or when the high-viscosity or low solubility sample is
injected, the buffer-volume is contaminated and cannot be cleaned with the CLEAN
UP operation.
If the noise from the buffer volume contamination is remarkable, following Manual
Cleaning of the buffer volume is recommended.
・After the CLEAN UP operation, turn the Pump Drain Valve to the [DRAIN].
・Turn the Column reject valve in the middle between [REJECT] position and
[CONNECT] position.
(Refer to below figure.)
REJECT
CONNECT
・Set the flow rate to maximum. Set 10 mL/min for LC-9210 NEXT and 25
mL/min for LC-9225 NEXT.
・Start the pump, and check that the solvent flows steadily from the pump drain
out in the siphon box. If the flow from the Pump Drain is not appeared, stop
the pump as soon as possible. If setting is abnormal in the Pump Drain Valve
or the Column reject valve, the maximum flow may damage the column.
Check the position of two valves, and re-start the pump.
・One minute later, press , and then stop the pump to finish the cleaning
maintenance.
4-21
4-2
4-22
Chromatogram Acquisition Error
If chromatogram is abnormal, refer to following paragraph and to remedy.
If abnormal chromatograph cannot be remedy, please contact us or our representative
at the end of the book.
4-23
<Base Line Wander 2>
Do the CLEAN UP operation with degassed solvent and wait that base line
becomes stable after the column equilibrium. Check the base line again.
!Decay of UV Lamp!
4-24
!Loose connection of the Signal Cable!
4-25
<Base Line Drift>
・Check that wind hit the LC chassis directly, or that there is a temperature
change in the laboratory.
RI Detector is sensitive to fluctuation of temperature.
Fluctuation of temperature may cause the base line drift of the RI Detector.
・Make sure that the time is over 30 to 100 min after the CLEAN UP operation.
Wait that the temperature controller become stable.
4-26
!Leakage of the flow line!
!Decay of UV Lamp!
4-27
<Base Line Drift during Recycling Operation>
・When the selection of the column against the sample is not suitable, the base
line is drifting upward in the Recycling operation. Select suitable column(s)
for the sample.
4-28
<Poor Recycling Efficiency>
0 20 40 Rt (min) 0 20 40 60 Rt (min)
(Normal) (Poor)
・When multiple times Recycling is done, turn over the knob to LOAD to
eliminate the sample loop from the flow line because the recycled sample
diffuse in the sample loop.
When you want to use the manual sample injector to execute the recycling
separation, flow the solvent of 3 mL or more for LC-9210 NEXT or 10 mL or
more for LC-9225 NEXT after the sample injection, and then turn the manual
injector knob to the [LOAD] position.
・When the selection of the column and solvent against the sample is not
suitable, Poor Recycling efficiency appears in the Recycling operation.
Select suitable column(s) and solvent for the sample.
4-29
Abnormal Pressure
Abnormal pressure may occur from decayed flow parts, sample property, or handling
error. Refer to following paragraph and to remedy the abnormal pressure.
When the abnormal pressure cannot be remedy, please contact us or our
representative at the end of the book.
・If the maximum pressure limit is set, an error message screen appears to
inform the emergency stop of the pump.
Check that the [MAXMAM] pressure limit is set to monitoring pressure +
2.0 MPa.
・Press the [OK] key, and turn the column reject valve to [REJECT] to start the
pump.
・If the pressure is significant smaller than before, column clogging may occur.
・Stop the pump.
・Remove the column from the flow line. Turn the Column reject valve to
[CONNECT] position. Re-start the Pump and check the pressure.
・If the pressure is significant large without the Column, the clogging may be
between the LC chassis and the Column inlet. Replace flow line part
between the LC chassis and the Column inlet.
・If the pressure is abnormally high with connection of the Column,
replacement of the Column is need.
・In case using reverse phase column or using high polarity column, the
solvent replacement of the column may occur high pressure. While the
solvent replacement is finished, set the maximum limiter at the suitable value.
4-30
<Abnormal Pressure Fluctuation>
・If the monitoring pressure abnormally fluctuates, the pressure fluctuation may
occur the abnormal chromatogram or decay of the column. Stop the Pump,
check the following items.
4-31
!Babble in the Sample cell of RI Detector, babble in the eluent!
4-32
<Abnormal Low Pressure>
・If the minimum pressure limit is set, an error message screen appears to
inform the emergency stop of the pump.
Check that the [MINIMAM] pressure limit is set to monitoring pressure - 2
MPa or less.
Do the CLEAN UP operation with degassed solvent and wait that base line
becomes stable after the column equilibrium. Check the base line again.
4-33
!Leakage of the flow line!
4-34
Abnormal Signal
The decay of the consumable parts or the property and miss-operation, may occur the
abnormal signal of the Detector.
When the abnormal signal cannot be remedy, please contact us or our representative
at the end of the book.
<Fail Power>
・Make sure the insertion of the POWER Cable at the rear of LC chassis.
・Make sure that the connection of signal cable on the Output terminal block at
the left hand of LC.
Check the input cable connection as same.
4-35
<UV Detector Abnormal Signal>
・If the solvent leaks from the UV detector cell, the chromatogram may cause
fluctuation of base line and the sensitivity loss may cause. In the Recycling
separation, extreme low peaks may appear with the leakage.
If above chromatogram is obtained, please contact us or our representative
at the end of the book.
!Decayed UV Lamp!
・If the UV Lamp decays, the chromatogram may cause fluctuation of base line.
The zero balance of the baseline may not achieve. or the sensitivity loss may
cause. If above symptoms appear, please contact us or our representative at
the end of the book.
・If RI Detector is extremely out of optical alignment, electrical zero may not
achieve or the RI signal causes full- scale in tight range.
Refer to p.4-20 described RI Detector Adjustment, and do re-alignment of RI
Detector.
4-36
Error Message
If a failure or wrong operation occurs in the LC-92XX NEXT, an error message
appears on the LCD display. At the beginning of the error message, "ERROR" is
displayed followed by a number. Based on this number, perform the following
operations to resolve the cause of failure. If the error message appears again, please
contact us or our representative at the end of the book.
<ERROR 01>
!This error occurs if the minimum pressure limit is set to a value larger than
the maximum pressure limit when setting them.
・Set them so that the maximum pressure limit is larger than the minimum
pressure limit.
<ERROR 02>
!This error occurs if the maximum pressure limit is set to a value equal to the
minimum pressure limit when setting them.
・Set them again so that the maximum pressure limit is not equal to the
minimum pressure limit.
4-37
<ERROR 03>
!This error occurs if you press one of the [Co/Dr] key in [FRACTION], the
[START] key in [CLEAN UP], the [ON/OFF] key in [RECYCLE], and the
[FLOW SET] key in [PUMP], during the [PURGE] operation of [RI
DETECTOR].
・These keys are unavailable during the [PURGE] operation. Use them after
the [PURGE] operation.
<ERROR 04>
!This error occurs if you press one of the [START] key in [CLEAN UP], the
[PURGE] key in [RI DETECTOR], and the [FLOW SET] key in [PUMP],
during the [RECYCLE] operation.
・These keys are unavailable during the [RECYCLE] operation. Use them after
the [RECYCLE] operation.
4-38
<ERROR 05>
!This error occurs if you set a value greater than the maximum flow rate of the
pump when changing the flow rate.
・Set a value less than the maximum flow rate of the installed pump.
LC-9210 NEXT(FX-10) : 10.0 mL/min
LC-9225 NEXT(FX-25) : 25.0 mL/min
<ERROR 06>
!This error occurs when normal cleaning is not performed in three minutes
during the buffer tube cleaning of the [CLEAN UP] operation.
・If the error is not solved, please contact us. Followings are possible causes of
the error:
1. The sensitivity of the sensor of the buffer tube is too low.
2. The buffer tube is very dirty.
The error will be solved by replacing these parts.
<ERROR 07>
!This error occurs if you set a value greater than or equal to 50.1 MPa in the
maximum or minimum pressure limit setting screen.
4-39
<ERROR 08>
!This error occurs if you press the [Co/Dr] key in [FRACTION], the [ON/OFF]
key in [RECYCLE], or the [PURGE] key in [RI DETECTOR] when the pump
is stopped.
・Press the [ON/OFF] key in [PUMP] to start the pump, and then press these
keys.
<ERROR 09>
!This error occurs if you press the [ON/OFF] key in [PUMP] during the
[RECYCLE] operation.
<ERROR 10>
!This error occurs when the pressure exceeds 1.5 MPa during the [CLEAN
UP] operation.
・Check that the column reject valve is located at the [REJECT] position.
4-40
<ERROR 11>
!This error occurs if you perform the injection operation using the manual
sample injector (INJECT->LOAD->INJECT) when the pump is stopped.
<ERROR 12>
!This error occurs if you press an irrelevant key when setting a function, or if
you press a key for setting a function when the function is running.
<ERROR 13>
!This error occurs if you press the [START] key in [CLEAN UP] when the
pump is running.
・Stop the pump, and then press the [START] key in [CLEAN UP].
4-41
<ERROR 14>
・As the failure may occur on the parts in the pump, please contact us or our
representative.
<ERROR 15>
!This error occurs when the monitoring pressure exceeds the specified
maximum pressure limit.
・Refer to the page 4-30 of this manual to solve the problem according
<Abnormal High Pressure>. < E R ROR 1 9 >
SOL VE NT E SCAP ED
*The pump is stopped when ERROR(15
C HisE displayed.
C K T H E P UM P )
PUSH "OK " KEY
<ERROR 16>
・Refer to the page 4-33 of this manual to solve the problem according
<Abnormal Low Pressure>.
*The pump is stopped when ERROR 16 is displayed.
!This error occurs when the temperature around the pump control board rises
very high (over 60℃).
・Stop the pump for 30 minutes, and then start the pump again. If the error
occurs again, please contact us or our representative.
*The pump is stopped when ERROR 17 is displayed.
<ERROR 18>
!This error occurs if abnormal rotation is detected at the pump driving part
when the pump is running.
・As the failure may occur on the parts in the pump such as board or sensor,
please contact us or our representative.
4-43
<ERROR 19>
!This error occurs if leakage is found around the suction pipe of the pump.
1. Check that the connectors such as check valve and PEEK screw are
tightened additionally.
2. The leakage is caused by secular change of the pump seal. Refer to the
page 4-10 in this manual to replace the pump seal.
3. Remove the leakage sensor, wipe the liquid out of the sensor, and check
the LED changes from red to green.
If the error is not solved, please contact us or our representative at the end of
the book.
<ERROR 20>
!This error occurs, if you press the [PURGE] key in [RI DETECTOR], the
[FLOW SET] key in [PUMP], or the [START] key in [CLEAN UP], while
fraction collection is being executed by the [Co/Dr] key in [FRACTION].
・Press the [Co/Dr] key in [FRACTION] so that the eluent flows from the siphon,
and then press the desired key.
4-44
<ERROR 21>
!This error occurs if you press the [Co/Dr] key in [FRACTION] 33 times
continuously.
・If you press the key continuously while the solvent is running through the
dead volume, the press timings are stored, and accordingly the valve works.
33 times is the limit that can be saved while running through the dead
volume. So do not press the [Co/Dr] key continuously over 33 times.
4-45
CUSTOMER SERVICE
If you have any questions, or something is wrong with Recycling Preparative HPLC, please
contact to the following.
LC-92XX NEXT Series User's Manual (1.3 Edition) Japan Analytical Industry Co.,
January 31, 2012
Ltd.