gas chromatograph gc-9a edition on...
TRANSCRIPT
221-20587D
Gas Chromatograph
GC-9A
Edition on Installation
SHIMADZU CORPORATION
ANALYTICAL INSTRUMENTS PLANT
KYOTO. JAPAN
CONTENTS
Chapter 1 Installation
Section 1 General Description 1
1.1 General description on the equipment 1
1.2 External view and construction of GC-9 A 3
1.3 Specifications 8
Section 2 Installation and Inspection 12
2.1 Inspection 12
2.2 Conditions for installation and general notes to be taken 13
2.3 Installation 16
Section 3 Preparation for Operation 21
3.1 Installation of column 21
Section 4 Confirmative Operations for Installation 32
1. General Description
1.1 General description on the equipment
Gas chromatograph GC-9A Series in multipurpose high-efficiency gas chromatograph
controlled by micro-computer. This instrument is flexible so that it can be connected
to other systems such as data processors for programmed temperature and isothermal
analyses and automatic analysis.
• Column oven has ambient control flap of unique construction. This flap let the air
outside the chamber inflow when temperature is controlled at near room temperature,
and supply coolant when temperature is controlled at sub ambient temperature.
These operations are precisely controlled by computer.
* When using coolant, a special accessory CRG-9 (221-25347-91) and solenoid valve
(option) are necessary.
• The door of column oven is divided into upper portion and lower portion. The normal
column replacement operation is performed by upper door, while lower door is main-
tained as a space to attach application components for particular analysis.
This application components can be confined in an unit which has a same shape with lower
door and can be attached and detached very easily.
The side of oven is designed in a way similar to other models so that various accessories
can be attached.
• Sample injection block and detector are designed to form one unit. In the case of the
standard unit, each detector is placed on the circumference of a circle whose center is
on-column injection block.
• There are vaious types of detectors such as thermal conductivity detector (TCD),
hydrogen-flame ionization detector (FID), electron capture detector (ECD), flame photo-
metric detector (FPD), and flame thermionic detector (FTD). Standard unit can accom-
modate four types of detectors at the same time.
• Microcomputer can control temperatures of six parts including column oven. In the case
of an standard type equipment with TCD and FID, three external equipments temperature
is to be controlled in addition to column oven, injection block and T.C.D. oven.
* For controlling external equipments, simple driver circuit is necessary.
• For automation of analyzing system, two power relay sockets that drive externally
connected valves, etc., by time program are built-in in the case of standard unit. By adding
expansion circuit board, eight triac outputs can be further installed.
- 1 -
Also software for the operation of automatic sample introduction equipment is accommodated
in the standard unit. Thus it is designed so that program control of the temperature of
column oven, operation by time program and operation by automatic sample injection
equipment are controlled by computer.
There are ten files for GC parameters and time programs. The length of each file is flexible
and one file can accommodate even a long time program. Furthermore automatic file
changeover can be performed from one file to another and can be applied for the continuous
analysis with different analysis conditions that require selection of sample flow lines.
These parameters are backed up by battery even when power is turned off.
External output and input terminals of this instrument include input for abnormality, GC
start input from outside, WAIT signal input as input signals and READY, COOL signals of
column oven temperature and START signal for external equipment as output signals
toward outside. By these signals, sequence and synchronization with other analyzing systems
are possible and also emergency actions are performed for safety purposes.
One of the characteristics, as a computer controlled instrument, is the fact that convenient
software, based on experience of gas chromatograph analysis, can be accommodated.
This equipment has functions such as program control of external oven temperature,
ambient control of external oven, stop watch function, setting of START time, STOP
time and SLEEP time for maintaining the equipment at WAIT state for a certain period
of time, hold function with which all time sequences are stopped for some time, a function
to hold only the temperature, display of retention time, temperature displays for six
temperature controlling sections, function to scan the temperature display and to display
them at an interval.
The equipment can perform self-diagnosis by checking parameters of file when power is
turned on and by checking all areas of RAM. Furthermore there are ten types of
displays to indicate errors during operation. Thus inconveniences including operational
mistakes are supervised and protected against.
The greatest characteristic is the fact that the GC-9A can be connected to SHIMADZU's
Chromatopac C-R2A. By this connection, data processing will be possible as well as
setting of GC parameters from the C-R2A. GC parameters, chromatograph and temperature,
etc. are displayed on the CRT. Furthermore programs can be written using BASIC in the
C-R2A. Thus there is a great possibility for expansion.
* For connection to the C-R2A, a current loop circuit board is necessary.
- 2 -
1.2 External view and construction of GC-9A
Fig. 1 GC-9A Series of Standard Specification with TCD and FID
Symbol Name and Major Constituent Units
©
Oven section: column oven, sample injection port, detector, power controller
Flow control section: carrier gas flow control, FID flow control
Electric control portion: CPU unit, IF unit, power unit, key and display unit, detector control unit
- 3 -
A. Oven section
Fig. 2 Oven Section
It) , (12) are on rear ofcolumn oven
Symbol Name and Others
©
(3)
©
Column oven door: Door is divided into upper and lower portions as shown in the
figure, and the upper door opens and closes at the time of normal
column replacement.
This door can also be attached and detached with hinge.
Column oven subdoor: This door can also be attached and detached when upper door is
opened. Complicated operations in the column oven will be easy if
this door is removed.
Various types of application flow line units with a shape similar to
that of this sub-door are provided. By replacing the unit with
this sub-door the equipment is easily turned into a system GC
that matches the purpose of analysis.
Side of oven: Holes are all for connection with external accessories.
Fixing holes on the equipment: There are fixing holes also on the interior of the right electronic
controller section. Using this hole, the equipment can be fixed
on the installation desk.
- 4 -
Symbol
©©
®
®
®©
©
@
TCD vent:
Sample injection port block:
FID detector:
FID igniter:
TCD and TCD oven:
Door switch:
Power input section and fuse:
Rear cable outlet:
Name and Others
IZZ)
This is for preventing any secondary accidents as a result of
earthquakes and so on.
Fixing is not required during normal operation.
This is the carrier gas outlet from the TCD cell.
The photograph shows the standard type on-column injection
block. A ghost cut injection block is also available as a special
accessory.
FID detector is installed in this position. A signal cable is con-
nected to an electrometer through the inside of the equipment.
Manual type FID igniter is installed in the standard type equip-
ment.
Oven temperature is controlled to within ±0.01°C.
Door switch is a switch that turns off the heater power when the
door of column oven is opened.
Fuse is divided into three and protect the column oven, other
ovens and controller section.
There are the following groups of external connection terminals
when back board is removed.
O Output relay (time program controlled)
o CRG (cryogenic) output signal
o AUX oven control signal
o Emergency signal input
o START signal from external source
o WAIT signal from external source
o READY, COOL, START signals of column oven.
Necessary signals are read out from this outlet.
- 5 -
B. Flow controller
* .Li? \ §1
, ( j ) and Qf) are on the rearand (lO) are on right side.
Fig. 3 Flow Controller for FID
Symbol Name and Others
Primary pressure regulator
Rotameter unit
Carrier gas flow control unit
Hydrogen flow contr.ol unit
Air flow control unit
Carrier gas inlet
Hydrogen gas inlet
Air inlet
Carrier gas stop valve
Hydrogen gas stop valve
Pressure regulating valve, pressure gauge (10kg/cm2G)
He, N2 : 20mK ~ lOOmfi/min.
Mass flow controller, pressure gauge (6kg/cm2G)
Pressure regulator, pressure gauge (2kg/cm2G)
Pressure regulator, pressure gauge (2kg/cm2G)
[GC-9A PTF model standard flow line construction]
Carrier gas
Hydrogen gas o—W
Air o
Fig. 4 Flow line
*• Column 1•> Column 2
FID-1* FID-2
- 6 -
C. Electrical controller section
Fig. 5 Electrical Controller Section
Symbol
®
©®
©
©
Detector controller section:
Setting key board:
Protect switch:
Heater OFF switch:
Power switch:
Name and Others
Four types of detector controllers can be mounted in this
space. An arbitrary number is given to each controller. Using
these numbers it is possible to set the condition of each detector.
The relation between the given number and detector can be
known by monitor key operation.
Necessary conditions are input by this key board.
Memories can be backed up by battery even at the time of AC line
off, when this switch is set at ON.
If this switch is turned OFF, the hardware of heater power circuit
will be OFF.
The content of the file can be confirmed when it is not clear.
If the switch is set at OFF during confirmation, careless increase
of temperature at various positions can be avoided.
This switch turns the AC mains power ON and OFF.
- 7 -
1.3 Specifications
• External dimension, weight, power capacity
External dimension: Width 552, height 540, depth 550 (mm)
Weight: Approximately 50kg
Line voltage: 100/115/220 ~ 240 VAC ±10%
(Line voltage for which instrument is internally
configured is indicated by the label.)
Column oven
• Dimension of the internal column oven: Width 217, height 355, depth 140mm
• Length of the column accommodated:
Stainless steel column (outer diameter 4mm0, inner diameter 3mm0) 10m X 2
Glass column (outer diameter 5mm0, inner diameter 2.6mm0 or inner diameter 3.2mm0)5m X 2
Capillary column (stainless steel, or glass, quartz capillary column) 100m X 1
• Range for linear temperature increase:
30°C/min. up to 150°C
15°C/min. up to 300°C
10°C/min. up to 350°C
5°C/min. up to 399°C
(When line voltage is 100V.)
• Programming for temperature:
Temperature setting: -100 ~ 399, 1°C step
Rate of temperature increase: 0.1°C step up to 0°C ~ 40°C/min.
Temperature hold period: 0.1 min. step up to 0mm ~ 999.8 min.
Multi-stage setting: 5 stages
• Temperature controlling range:
-100°C~+399°C
• Column oven temperature at INJ 300°C is from room temperature -+15°C.
• Column oven temperature at INJ 150°C is from room temperature +10°C.
• Column oven temperature at INJ room temperature +10°C is from room temperature
+2°C.
For the. temperature below this, cryogenic attachment will be used.
(Figures above applies to equipments with FID)
- 8 -
• Cooling:
Approximately 8 min. from 399°C to 100°C
Approximately 15 minutes from 399°C to 55°C (when room temperature is 25°C)
Automatic cooling and automatic recovery of initial temperature are made possible by
ambient control valve.
• Control precision:
±0.1°C
(if air temperature is measured by detector with small thermal capacity, there will be
fluctuation of approximately ±0.2°C for a short period of time.)
• Overheating prevention circuit:
One limit is 420°C and another limit can be set freely by key control. Thus dual setting
is possible.
° if ECD controller section is attached, the limit will automatically go down to about
350°C.
° Protection circuit is attached which prevents the rise in column oven temperature before
the temperature of INJECTION block reaches to the set value.
Sample injection port/detector block
• Range for temperature setting: Room temperature ~ +399°C, 1°C step
• Precision: ±0.1°C
• Overheating prevention: 450°C
350°C in the case of instruments with ECD
TCD oven
• Range for temperature setting
• Overheating prevention:
Other external heat zone
• Air oven connected to AUX1
Temperature range:
Program control:
Room temperature ~ 399°C, 1 C step
(When electric current is applied to TCD filament,
by self-heating, control will be possible from
approximately 90°C.)
450°C
Same as that for column oven except subambient operation
Same as that for column oven
- 9 -
• Heat block connected to AUX2.DET:
Temperature range: Room temperature ~ 399°C
Precision: ±0.1°C (However it may differ depending on the
construction of supplementary heat block.)
Sample injection port
• The type to be used for both glass insert method and for on-column method.
In the case when stainless steel column is used, stainless steel column adapter is to be used.
In the case when capillary column is used, inlet splitter is to be used.
• Ghost cut sample injection chamber: Optional
Installation of detectors
• Following detectors can be installed at a same time.
TCD
FID
ECD
FPD
FTD*
• Two types out of these
Four types in total can be installed at a same time.
Standard FTD is a detector in which FTD components are attached to FID.
Flow controller
• Carrier gas:
Hydrogen gas (for FID)
Air:
ON/OFF valve
Primary pressure regulating valve
Primary pressure gauge (0~10kg/cm2)
Mass flow controller
Rotameter (20~100mfi/cm2)
Pressure gauge (0~6kg/cm2)
ON/OFF valve
Pressure regulating valve
Pressure gauge (0~6kg/cm2)
Pressure regulating valve
Pressure gauge (0~2kg/cm2)
Branch pipe
1 unit
1 unit
1 unit
2 units
2 units
2 unit
1 unit
2 units
2 units
1 unit
1 units
1 unit
- 1 0 -
FID (hydrogen-flame ionization detector)
Collector electrode:
Electrode voltage:
Sensitivity:
Minimum detectable level:
Dynamic range:
Cylindrical shape
±200V
S = 0.015c/g
3 X 10"12g/sec (sample, diphenyl)
107
Maximum operation temperature: 400°C
Igniter: External filament, used for both flow lines
Nozzle: Quartz nozzle
Specifications on electrometer
Range:
Polarity selection:
Zero adjustment:
LAMP of zero:
Maximum sensitivity:
Linearity :
Noise:
° Set by key operation
Set by electrometer
• FID ON/OFF switch:
TCD (thermal conductivity detector)
Detector:
Maximum application temperature
Power source:
Current:
Polarity selection:
Zero adjustment:
Sensitivity:
Protection circuit:
10°, 101, 102, 103, 104
INJ1 (+), INJ2 (+)
±6.4 X 10"10A
±0.01V (LAMP is on within this range)
1 X 10~12A/mV (full scale)
105 minimum
10~14A/h (when room temperature is constant)
range, polarity selection
zero adjustment, ON/OFF switch
When OFF, setting by key operation will not be possible.
The state before being set at OFF will be maintained.
Tungsten rhenium filament (differential semi-
diffusion type of 10012 4 element construction at
room temperature)
400°C
Constant current control method
0~200mA, 1mA step (set by key)
INJ1 (+), INJ2 (+) (set by key)
Precise and rough; one each
7000mV, m£/mg, appoximately
° With filament protection circuit (hardware)
° With overheating prevention circuit (software)
- 1 1 -
2. Installation and Inspection
2.1 Inspection
Equipment is thoroughly packaged to protect the equipment from vibration and shocks
during transportation. However, if there should be any damage found, please inform our
closest branch or agent.
Standard accessories
Following parts are provided as standard accessories to the main equipment.
Accessories are provided for each detector, if recorder is also purchased, it will be separately
packaged.
Standard Accessories
Name
Column gasket (aluminum 100 pieces)
Column gasket (silicon rubber)
Injection port rubber septa (20 units)
Silica wool
r Cap nut (GF)
Blind stopper 4 Nipple (GNO)
[ Washer (WG)
r Cap nut (MF)
Blind stopper -<j Nipple
L Washer (WM)
Glass insert*
O-ring (for glass column)
S.S. column adapter (INJ side)
Joint for glass column
Spanner 12 X 10
Hexagonal wrench 2
Hexagonal wrench 3
Fuse 3A ]Fuse 10A [ 100 ~ 115VAC modelFuse 15A J
Fuse 2A 1Fuse5A I 220 ~ 240VAC modelFuse 7A J
Parts Number
201-35183
201-35184
201-35584
201-47616
201-30006
201-30015
201-30050
201-30008
201-30009
201-30051
221-14093
201-47614
221-14087-91
221-15561-91
086-03011
086-03802
086-03804
072-01026072-01028072-01123
072-01004072-01031-02072-01031-04
Number of Unit
1
1
1
1
2
2
2
2
2
2
4
1
2
2
2
1
1
111
111
< For glass columns with inner diameter of 3mm. If glass column with inner diameter 2.6mm is used,please purchase another glass insert (P/N 221-14094).
- 1 2 -
2.2 Conditions for installation and general notes to be taken
2.2.1 Environmental requirement
A place where equipment will not suffer direct wind and sun-light will be suitable.
Please use the equipment in an environment where the ambient temperature is within
the range of 5 ~ 40°C.
2.2.2 Table for installation
Back wall
Fig. 6 Dimension
o A strong table absent of vibration will be suitable. The fact that the main equipment
weighs approximately 50kg and that there is peripheral equipment to be connected
to the main equipment must be taken into consideration.
(A) Approximately 50cm of space will be required if a special accessory, e.g., automatic
sample introduction equipment, is to be installed.
LB) Approximately 60cm of space will be required if data processor C-R2A is to be
installed,
( c ) As the heat from the column oven will be discharged toward the upper rear area
at the time of cooling, leave more than 30cm between the equipment and the
back wall.
Take special precaution if there is a chemical shelf near the back wall.
2.2.3 AC mains power requirements
A dedicated single phase, AC mains line should be installed to isolated the equipment
from transients or overloads. A minimum of 20 amps with circuit breaker protection
and third wire ground should be installed for the 100 ~ 115VAC model, and 10 amps
for the 220 ~ 240VAC model.
- 1 3 -
The instrument draws current according to the following:
1060W for the column oven, 300W for the INJ/DET heater block, 200W for the TCD
heater block or 100W for the FPD heater (if installed).
The color of wires and distinction between HOT, NEUTRAL and GROUND of power
source are as indicated in the following table. When there is no clear distinction between
HOT and NEUTRAL of the supplying source, make sure to check it with a tester.
Color of Power Cord(220V-240V)
Brown
Blue
Green yellow
Color of Power Cord(100V-115V)
Black
White
Green
Polarity
HOT
NEUTRAL
GROUND
Meaning
Has voltage against grounding.
Has no voltage against grounding.
Grounding
2.2.4 Gas necessary for operation
Types of Detectors and Gas Required
Thermal conductivity detector(TCD)
Hydrogen-flame ionizationdetector (FID) and flamethermionic detector (FTD)
Electron capture detector(ECD)
Flame photometric detector(FPD)
Photoionization detector (PID)-
Type
* Helium*Hydrogen* Nitrogen
^Nitrogen* HeliumHydrogenAir
*Nitrogen
* NitrogenHydrogenAir
* Helium
Notes
BestBetter not to useCan be used
BestCan be usedNecessaryNecessary
Best
BestNecessaryNecessary
Best
Purity
99.99% min.99.99% min.99.99% min.
99.99% min.99.99% min.As pure as possible
99.99% min.
99.99% min.As pure as possible
99.99% min.
Precautions
121
111,23
1
123
1
* sign shows carrier gas.
Precautions
1. When applied for high-sensitivity analysis, please use molecular shieve filter. (Parts number 221-05619-91:optional)
2. Strict precautions must be taken for use as there is danger for explosion.
3. Please use gases that are clean, dry and that does not contain oil. Air compressor to pressurize air (3~5kg/cm2G) and silicagel filter (parts number 221-36688: optional) for removing moisture are provided.
- 1 4 -
2.2.5 How to deal with high pressure gases
Please take special precautions when dealing with high-pressure gas, and for the security
and management of the gas. Please be sure of the following items.
Gas cylinder shall be" placed outdoors where ventilation is good and where there will
be no direct sunlight. Gas shall be lead indoors by pipings. This is obligation
stipulated by law especially in the case of liquefied gases.
2) Care must be taken so that the temperature of gas cylinder will not exceed 40°C.
Also there should be no fire within 2m.
3) When high-pressure gas is to be used, make sure good ventilation is maintained.
Also at the beginning of the operation, check so that there is no gas leakage by the
use of soap solution. Especially when using these gases (acetylene, hydrogen, pro-
pane, oxygen and nitrous oxide etc.), there must be no smoking or fire within
5m from the equipment using the gas. Furthermore efficient fire extinguisher
must be provided.
4) Fix the gas cylinder with rope so that it will not fall. Due care must be taken never
to tumble a liquefied gas cylinder (acetylene, propane, nitrous oxide etc.) down.
When using an oxygen gas cylinder, be sure to use a pressure reducing valve of oilless
type. Also oil should not be introduced to the interior of pipe where oxygen gas
contacts.
6) At the completion of use of gas, the stopcock should be closed immediately.
Inspect the function of pressure gauge more than once in three months.
We have made "precaution plate for hydrogen gas operation" (aluminum sticker
plate) and trying to stick this on our equipment already being delivered, if you
find a need to have this plate, please inform a person in charge at our company, so
that we can send it to you free of charge.
If more than 300m3 of high-pressure gas is to be stocked in bomb, permission is required
by law.* Also if gas with pressure exceeding 10kg/cm2 in the equipment under normal
pressure is to be used, this is regarded as high-pressure gas equipment and registration of
the equipment is required by law. *
Please refer to the high-pressure gas control law, the liquefied petroleum gas security
regulation and also the fire services act.
*Local and Federal laws vary.
-15-
When using hydrogen gas, take good note of the following points for prevention of
danger.
(l_) When equipment is not operated, stopcock of the hydrogen gas cylinder must be
closed and check so that there is no leakage at the stopcock.
(2J The passage of hydrogen gas from the hydrogen gas cylinder to the inside of
equipment, further to the final discharging end must be checked at every use so that
there is no leakage.
(3) In order to prevent explosion due to hydrogen gas leaked at the time of emergency,
good ventilation must be maintained in the room where equipment is installed and
use of fire must be avoided.
(V) On completion of the use of equipment, the stopcock of hydrogen cylinder should be
closed. Then turn off the power of the equipment followed by other works
necessary at the end of operation.
When FID is not used, be sure to close the hydrogen cylinder inlet stop valve.
This can prevent the careless inflow of hydrogen gas into the column oven.
2.3 Installation
2.3.1 Gas piping
Joints for various gas pipes are located at the back of the equipment.
Depending on the combination of detectors there may be no inlet for hydrogen and air.
The piping between equipment to gas cylinder must have sufficient resistance against
pressure (approx. 10kg/cm2 is the maximum limit at the time of general use) and metal
piping is better from the safety point of view.
Piping must be cleaned by solvent and thoroughly dried before connecting to the equip-
ment.
CARRIER GAS Necessary carrier gas will be supplied from here into detector
to be used.
Supplying pressure is 7 ~ 8kg/cm2.
HYDROGEN Hydrogen is supplied from here when FID, FPD and FTD are used.
Supplying pressure is 3 ~ 4kg/cm2.
AIR Air supplied from here when FID, FPD and FTD are used.
Supplying pressure is 3 ~ 4kg/cm2.
- 1 6 -
Following parts are provided as gas piping parts. (Special accessories)
1 ) f 2
(T) Carrier gas pipe (5) Silicagel filter
(2) Gas.bomb decompressor (6) Air pipe
(3) Hydrogen gas pipe (7) Oilless compressor
(4) Gas cylinder pressure regulater
Fig. 7 Piping
Method to inspect gas leakage
(1) For flow lines that have pressure gauge, close the passage using stop valve,
nipple etc., after filling gas to the pressure of application, if there is no reduction
in pressure after a period of time, this means that there is no leakage.
(2) Leakage can also be inspected by applying soap solution onto connections with
brush to see whether or not bubbles are generated.
2.3.2 Looseing of fixing screws for transportation
Fan motor of column oven is installed on the vibration-proof rubber desk in order to
prevent noise production due to vibration of detector during operation.
As this portion is fixed during transportation, remove two screws shown in the figure.
- 1 7 -
2.3.3 Connection of signal cables
2.3.3.1 Data processor — Connection with C-R2A
• Connection of analog signal cables (Signal cables standard accessories)
GC
ooo®
- 9A
oL J
Connect the detector"E" is grounded by C-R2A side.
Fig. 8 Connection of signal cable
• Connection using current loop
For setting GC parameters from C-R2A, for displaying and recording GC parameters
in C-R2A, connection by the use of current loop in performed. (Optional)
Hole for output signal ofdetector
Fig. 9 Connection of current loop
- 1 8 -
Fig. 10 Attachment of Current LoopCircuit Board
Remove side board 1 of electrical controller
section of GC main equipment and back
board 2 , and connect current loop circuit
board to the connector of busline using flat
cable of 60 lines. Connector should be
firmly inserted so that upper and lower locks
will be applied.
Circuit board shall be inserted in the groove of
the plastic rail and shall be fixed by rear attach-
ment board.
2.3.3.2 Data processor — Connection with C-R1B
Connection of REMOTE START
"E" is grounded by C-R1B side.
Fig, 11 Connection to C-R1B
2.3.3.3 Connection with recorder
The standard application form of this instrument is to connect to data processor
C-R2A or C-R1B. Therefore a signal cable for recorder shown in the following is
necessary if recorder is to be used. (Special accessory)
- 1 9 -
Recorder signal cable for ionized detector (all detectors except TCD)
P/N 221-23896-91
"E" is grounded by RECORDER side
o Zero point adjustment (precision)
o Attenuation 1, 2, 4, 8, 16, 31, 64, 128, 256, 512, 1024,
Recorder signal cable for TCD
P/N 221-24442-91
"E" is grounded by RECORDER side
o Attenuation 1, 2, 4, 8, 16, 32, 64, 128, 256, 512, 1024, °°
- 2 0 -
3. Preparation for Operation
3.1 Installation of column
3.1.1 Position for column installation
if the door of column oven is opened, several joints are projecting from the upper
portion. The joint on the right end of the column oven viewing from the front is the
joint for sample injection port of column 2, and the joint on the left end is that of
column 1.
Other joints are joints for various detectors, and all joints are located an equal radius
from the sample injection port. Although there may be slight changes depending
on the combination of detector, the joint on the forefront is the joint for TCD, the one
in the middle is for FID and the furthest one is for FPD or ECD.
The arrangement of the joints when viewed from the top of the column oven is shown
in the following.
Column 1 Column 2
Open
A
(T) Sample injection port joint
© TCD joint
(3) FID joint
(4) Joint for ECD, FPD
Front
Fig. 12 Position for column installation
•:;•:«
Pull up and thenpull frontward.
4
The door of column oven is separated into two as
shown in the figure.
The normal column installation work can be
performed only by opening and closing the upper
door. However if there is any inconvenience in
the installation work, lower door can also be re-
moved easily by sliding it 5mm towards the
direction of arrow (up) in the figure and then
pulling it forward.
Fig. 13 Column oven door
- 2 1 -
3.1.2 How to install column
3.1.2.1 Stainless steel column
For installation and removal of stainless steel column* (inner diameter 3mm,
external diameter 4mm), spanner (12 X 10) (standard accessory) is used.
There are two types of gasket, silicon rubber gasket and aluminum gasket**
(standard accessories). Select the gasket that suits the maximum application
temperature of column.
Silicon rubber gasket max. 250°C
Aluminum gasket max. 400°C
* For connection to sample injection port, and detectors, S.S column adapter
(standard accessory) is to be used.
** When using aluminum gasket, two to three gaskets must be used together.
GasketStainlesscolumn
Stainless column adapter (DET)
Stainless column adapter (INJ)
Fig. 14 Stainless steel column adapter
3.1.2.2 Glass column (outer diameter 5mm)
For installation of glass column, installation parts for glass column ((T) ~ (\5) in
the following figure) and O ring Q6J) (standard accessory) are to be used. Make sure
to place back-ling (Sj in the direction shown in the left figure.
V V V V V V VV I
Cm o o o • L
Fig. 15 Installation of glass column
- 2 2 -
Number
©
Name
Glass column
Cap nut
Washer
Spring
Back-ring
O ring P4
P/N
221-00840
201-30051
221-12184
221-12105
201-47614
(Note) (2) /set, Joints for glass column 221-15561-91 (
As this O ring in made of rubber, the application temperature is maximum 250°C.
Graphite ferrule is to be used for temperature higher than this.
It is sufficient to fasten them with fingers. If fastened tightly using a spanner, the
column may be damaged.
Note
If glass column is used, column may be detached during operation due to
carrier gas pressure or thermal contraction of O ring etc. In order to prevent
such situation, after fastening the jointing tools for the column, a wire through
the hook of upper side of the oven is to be inserted in the spiral of glass
column and to be twisted until the wire will become relatively tense.
Be sure to perform this operation as it is dangerous (especially when hydrogen
is used) if column is detached during operation.
Jointing of glass column by use of graphite ferrule
Insert in the order from cap nut (2), washer \3), spring (4) to back-ling (5) (in the
opposite direction to the case of O ring) and finally the graphite ferrule (6j (it is
attached on the side ring. Be careful of the direction.) in the direction shown in
the left diagram to the neck of glass column. Then this is to be attached to the
column jointing section. As it is stiffer than the case of O ring, it is to be tightened
with attached spanner, after fastening it tightly with fingers. It is necessary to
hold the column with one of the hands until it is fastened sufficiently as it will fall
down. Also it is important to fasten the column gradually, checking the leakage,
as glass column will break if fastened too much. Start fastening from the side of
sample injection chamber. If appropriate amount of carrier gas is flowing, column
inlet pressure will be approximately zero while there is some leakage, but the
- 2 3 -
pressure will start rising gradually when leakage stops. When pressure starts rising,
fasten the column further*. (Pressure will depend on the length of column and
flow rate of carrier gas. If the column length is short, the pressure rise will be easy
to observe if large flow rate is maintained.) Next, jointing section of the detector
side is to be fastened with spanner. When it becomes slightly stiff to fasten, fasten
further to the stiffness experienced in the case of sample injection chamber.
In order to check whether or not there is a leakage after jointing, apply soap solution to
the gap between cap nut and glass column. (Section A shown in the previous page.)
* Use 12 X 10 spanner and fasten it with some force in the thumb.
Washer for graphite P/N 221-16118(to be used when graphite starts reducing)
(T) ~ (5) Same as in the case of O ring (7)
(6) Graphiteferrule P/N 221-15563-91
Fig. 16 Installation of glass column
3.1.2.3 Capillary column (glass and stainless steel)
When using capillary column, splitter and column holder etc. will be necessary.
Please refer to the instruction manual for the capillary column.
Notes
(1) The maximum application temperature of the column will depend on the
packing material filled inside the column. Be sure to set the temperature of
column oven under the maximum temperature.
(2) Newly manufactured column is to be attached to the equipment and used after
aging it sufficiently.
(3) When aging the column, be sure to open the column outlet (detector inlet)
side in order to prevent the effluent from the column from flowing into detectors.
3.1.2.4 Jointing to TCD
(1) In the case of the glass column
Insert nut (6), washer (s), spring (4) and sleeve (3) into the edge of glass column.
Then insert graphiteferrule into the edge of the column. Then pressurize this into
- 2 4 -
the pitting at the sleeve end. Then insert this into the column jointing section of
TCD and fasten it with nut.(as shown in the figure below).
(Glass column) (Stainless steel column)
Fig. 17 Installation of column for T.C.D.
Symbol
©©©©
©
Name of parts
Glass column
Graphiteferrule (TCD)
Sleeve
Spring
Washer
Nut
P/N
221-10074*
221-10073
221-12184
201-30051
221-00840
* P/N for a set of 10 graphiteferrule is 221-10076-91.
For fastening with nut (6), first fasten the nut with hand then fasten it further by
turning it several times. Then sufficient sealing will be attained.
Although graphiteferrule is relatively flexible, it may break if fastened too much.
if fastening is performed, while checking the leakage using soap solution, unnecessary
fastening can be avoided.
if there is a gas leakage after the first programmed temperature analysis, fasten it
further for another half turn. By this further fastening gas leakage will not occur
any more. Be careful not to fasten the nut excessively as glass column and sleeve
may break.
- 2 5 -
(2) In the case of the stainless steel column
In the case of the stainless steel column, (6) ~ (2) are to be attached at the tip
of S.S column adapter P/N 221-10079-91 as in the case of glass tube, and fastening
is to be performed.
3.1.2.5 Attachment of glass column to the sample injection chamber
In GC-9A series, a sample injection chamber that can be used for both on-column
and glass insert method is attached to both columns 1 and 2.
Radiating finNeedle guide
-Injection portrubber septumn
"Spacer
Carrier gasGlass insert
Needle guide: P/N 221-14773
Spacer: P/N 221-14074
The spacer should be attached so that theside of spacer with groove will be on theside of the glass insert.
Glass column
Fig. 18 Injection port
On-column method
Be sure to use a glass column for GC-7A in this case. Attach the glass tube by the
method indicated under 3.5.2, being sure that longer neck will be on the side of
sample injection port and the shorter neck will be on the detector side.
Glass insert method (The sample injection port itself is same as in the case of
on-column method.)
Method of attachment:
First attach the bindings to the necks on the both sides of column in accordance
with the instruction shown in 3.5.2. Then hold it with one hand (right hand in the
case of column 2 side, and left hand in the case of column 1 side), and insert the
glass insert* (P/N 221-14093) from the inner side of the column oven and hold it
there so that the thinner side will be on the column oven side. Then slightly insert
the long neck of glass column to the desired detector jointing section, and rotate it
and move it so that shorter neck of glass column will come right under the glass
insert held with the other hand. Then lower the glass insert gradually so that the
thin side will go into the glass column. Glass insert will be maintained at the
- 2 6 -
portion of glass column where the diameter of the column suddenly increases.
Then insert whole glass column slowly and attach it following the instruction
indicated in 3.5.2.
Method for removal:
First cool down the column oven sufficiently. Stop the carrier gas flow and check
so that column inlet pressure has decreased sufficiently. After opening the door
completely manually, and holding the glass column firmly with one hand, loosen
the glass column connecting nut. When loosening the nut, loosen it slowly and
prevent the nut from falling off with fourth and fifth fingers as loosened nut may
fall and break the shoulder of the glass column. After loosening the nuts on both
injection port side and detector side, remove wire for preventing the fall of the
column and then pull the glass column downwards. If O ring is adhered
due to heat, use razor to cut it off. Glass insert will come down together
with glass column, but as it cannot be pulled out under this situation, use
another hand to raise glass insert slightly so that glass column can be removed.
As glass insert is hot, cool it down sufficiently or wear a glove on a hand that
holds the glass insert when performing this operation. When cleaning only the
insert, leaving column as it is, remove injection port rubber septum and take
out the insert from the top using tweezers.
* When using a glass column with inner diameter of 2.6mm, a special glass insert for
this glass column (P/N 221-14094) is to be used.
Stainless steelcolumn adapter
When using stainless steel column adapter,use it with an attached insert ring asshown in the figure on the left.
Fig. 19 Installation of glass insert
-27-
Note
(1) When installing a stainless steel (SUS) column, first attach SUS column
adapter (P/N 221-14087-91) to the sample injection port side and then
joint them in accordance with the instructions in 3.1.2.1.
(2) In the case of glass column for GC-7A, it can still be used when inlet and outlet
sides are reversed. Thus, it can be used for both on-column and glass insert
methods. When used for both methods, it is necessary to fill only small
amount of packing material to suit on-column method as the column will be
inserted deeper in the case of on-column method.
(3) The glass columns of SHIMADZU GC-4BM, GC-4CM, GC-6A, GC-6AM series
can be used for methods other than on-column method.
(4) If something nonvolatile will attach on the glass insert, base line may change
and sensitivity may be decreased. Be sure to wear a clean glove and handle it
with clean hand. Also if it becomes contaminated with sample, wash it with
solvent.
(5) After installing the column, check the leakage with soap solution.
(6) Attach the spacer so that the side of it with groove will come on the glass insert
side.
3.1.3 Setting of carrier gas flow rate
3.1.3.1 Primary pressure controller section
In order to operate the flow controller of the carrier gas flow rate controller section
correctly, it is necessary to maintain this primary pressure constant.
Make adjustment using primary pressure
adjusting knob (T) so that the primary
pressure gauge (2) will indicate 6kg/cm2.
Thus, the appropriate secondary pressure
(or gas pressure of concentrated piping) of
carrier gas cylinder pressure regulator is
7 ~ 8kg/cm2.
Carrier gas inlet stop valve (3) is used when
stopping the carrier gas introduction into
the instrument.
Fig. 20 Primary pressure regulator
- 2 8 -
3.1.3.2 Carrier gas flow rate controller section
Flow rate is adjusted by carrier gas flow rate adjusting knob (T). When the knob is
turned counterclockwise, the flow rate increases. The flow rate adjuster is the
mass flow controller. Therefore in the case of programmed temperature analysis,
carrier gas flow rate will not change even if the column temperature rises and column
resistance increases. However the column inlet pressure increases in accordance
with the increase in the resistance (rise in the column temperature).
Be careful not to tighten the flow rate adjuster too much.
Flow rate can be read from the rotor meter (2). However when precise measure-
ment of flow rate is required, it is necessary to use soap film flow meter.
The appropriate carrier gas flow rate is 40 ~ 60m£/min in the case of column with
inner diameter of 3mm. In the case of capillary column, decide the flow rate by
referring to the instruction manual on the capillary column holder.
3.1.4 Setting of hydrogen and air flow rate for FID
They are set only when FID is used. When FID is not used stop valve of the hydrogen
flow line is to be closed and furthermore attached metal plug is to be attached on to the
column jointing section of FID for safety.
The sensitivity of detector depending on the hydrogen-air mixture proportion.
There is a mixing ratio in which the sensitivity becomes optimum.
Air flow 1 and 2 \ Hydrogen flow 2
Hydrogen flow 1
Fig. 21 FID controller
- 2 9 -
1.5
1.0
C00 0. 5
N2
Air500m^/min
0 20 30 40 50 60 70 80 90 100-*• H2 flow rate (m£/min)The relation between nitrogen-hydrogen mixing ratio andsensitivity
1.5
f 0.5
H2
N2
0 200 500 1000
-* Air flow rate (mC/min)The relation between airflow rate and sensitivity
In the case of this equipment, pressure regulating method is adopted for controlling
flow rate of hydrogen and air. Draw a calibration curve of pressure and flow rate as
shown below*. And set each flow rate according to the pressure indication on
pressure regulator under normal situation.
.3
B§ 100
uO
0 0.5 1.0Pressure (kg/cm2G)(pressure gauge indication)The relation between hydrogenpressure and flow rate
Pressure (kg/cm2G)(pressure gauge indication)The relation between air pressureand flow rate
Figures above shows typical example. Thus to be strict, there are slight differences
depending on the instrument.
In the case of a column with inner diameter of 3mm, each flow rate is to be set as
follows under the normal situation.
Carrier gas (nitrogen) 50m£/min (40 ~ 60m£/min)
Hydrogen* 50mfi/min (30 ~ 60m£/min)
Air 500mC/min (400 ~ 600mC/min)
* Be careful not to raise the hydrogen pressure beyond lkg/cm2.
-30-
Note:
When using hydrogen-flame ionization detector with a single column, make the
hydrogen pressure of the detector on the side that is not used zero and stop it
firmly by using nipple (standard accessory) on the input side of detector.
Also when replacing columns, stop the hydrogen flow before removing the
column. Or there will be a danger for explosion as hydrogen gas may go into
column oven.
- 3 1 -
4. Confirmative Operations for Installation
This work is same as the start of GC operation for the routine operation. For the further
details of this work, please refer to the second manual, Operation (I).
Fig. 22 Places where confirmation is necessaryat the beginning of the operation.
1) Open the stopcock of the carrier gas:
The supplying pressure to the GC main equipment is 7 ~ 8kg/cm2.
if piped directly from the gas cylinder, adjust the secondary pressure of cylinder regulator
to this pressure.
2) Open the stop valve on the right side of the GC main equipment:
Check so that the primary pressure gauge is indicating 6kg/cm2. Set the primary pressure
regulator so that the primary pressure will be 6kg/cm2.
3) Set the carrier gas flow rate:
Observing the rotor meter, set the flow rate for passage 1 and 2. For the confirmative
operation, set at approximately 50m£/min. if column is connected, the indication on the
column inlet pressure gauge will rise.
4) Turn on the switches of the detectors to be used:
If this switch is turned on, detector number and detector type will be searched automatically
when POWER switch in turned on.
5) Turn on the PROTECT switch:
if this switch is turned on battery backs up even when power is turned off.
The memory adjusted at the plant at the time of shipment is cleared and is initialized.
-32-
6) Turn on the POWER switch:
Fan motor of the column oven will rotate. The fan for cooling transistor in electrical
controller section will rotate.
Approximately one second later, CITP X X is displayed.
At this situation, temperature will not rise yet. The temperature of each section will start
rising only after HEATER switch on the side is turned on and START key is pressed.
7) Supply hydrogen gas and air when using FID :
(7-1) Supply hydrogen gas Supplying pressure to the instrument is 2 ~ 5kg/cm2.
(7-2) Open the stop valve and adjust the hydrogen gas flow rate Set the flow rate at
approximately 50m£/min based on the graph showing the relation between pressure
gauge and flow rate.
Inlet pressure gauge should indicate 0.4 ~ 0.7kg/cm2.
(7-3) Supply air from air source to the main equipment Set the supplying pressure to
the instrument at approximately 3kg/cm2.
-33-
221-20573C
GC-9A/GC-9AMGAS CHROMATOGRAPHINSTRUCTION MANUAL
VOLUME I: INTRODUCTION
SHIMADZU CORPORATION
ANALYTICAL INSTRUMENTS PLANT
KYOTO JAPAN
TOKYO OFFICEP.O.BOX No.209, 40th Floor Shinjuku Mitsui Bldg.,No. 1-1, Nishi-Shinjuku 2-Chome, Shinjuku-ku, Tokyo 160, JapanCable Add.:SHIMADZU TOKYO
SHIMADZU CORPORATION Overseas Telex No-:0232~3291 (SHMDT J)
KYOTO OFFICE1, Nishinokyo-Kuwabaracho, Nakagyo-ku, Kyoto604, Japan.Cable Add.lSHIMADZU KYOTOOverseas Telex No.:05422-166 (SHMDS J)
3500-10400-500TD-E
How to use this manual
This manual is mainly intended to explain the meaning of the main key input operation
in GC-9A/9AM. When a more detailed description of the procedures for the key input
operation is desired, refer to the separate volume, "Operation (II)".
For the connecting method and operation in obtaining expanded functions (optional),
refer to the manual provided with the optional unit.
Contents
Page
1. Classification of Keys 1
1.1 Numerical key 1
1.2 Command keys 2
1.3 Function keys 2
1.4 Monitoring key 2
1.5 Dialog key 3
2. Starting Gas Chromatograph 5
3. Column Oven 7
3.1 Setting the column oven temperature 7
3.2 Setting of the maximum column oven temperature 7
3.3 Starting of column oven temperature control 8
3.4 Power supply to column oven heater and its suspension 8
3.5 How to display setting values and actual values of the column oven
temperature 8
4. Setting of Injection Temperature 9
5. Temperature Programming 10
5.1 Standard one stage temperature programming 10
5.2 Multistage temperature programming (in case of 3 stages) 11
6. Meaning Explanation of Each Key 16
6.1 Temperature setting 16
6.2 Temperature monitoring (when actual temperature is to be known) 17
6.3 Temperature monitoring at 6 places 18
6.4 Parameter setting of detector 19
6.5 Detector monitoring 20
6.6 Timer setting 21
6.7 Timer monitoring 22
6.8 Setting of time program 23
6.9 Time program monitoring 24
6.10 File setting 24
6.11 FUNC setting 25
6.12 List of key explanation 27
7. Control Parameter and Default Value 32
8. Setting and Deletion of File 36
9. Setting of Time Program 37
9.1 Time program 37
9.2 Composition of time program 37
9.3 How to make up time program 37
9.4 When new steps are inserted in the program 39
9.5 How to delete unnecessary steps 39
9.6 How to delete whole time program 39
9.7 Confirmation of time program content 39
10. Meanings of Display Lamps 40
11. Detector 41
11.1 Signals of detector 41
11.2 When the kind of the attached detector is to be known 41
11.3 TCD 42
11.4 TCD control 43
11.5 Protective circuit of TCD filament 45
11.6 TCD VENT (upper left side of main body) 45
11.7 Cautions 45
11.8 Hydrogen flame ionization detector (FID) 46
11.9 FID controller 48
12. Temperature Control of AUX t , AUX2 and DET 52
1. Classification of Keys
GC-9A/9AM is designed to carry out a large number of functions with optimized simple
operation by issuing commands and combining them by means of the function keys and numerical
keys, respectively.
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1.1 Numerical key
With numerical keys depressed, numbers are indicated on display. The numbers on display
will not be input unless [ENT| key is depressed.
CE
ENT
- 1-
A number of 4 digits above the decimal point and 2 places below it can be input.
When the displayed number is of more than 4 digits, the digits subsequent to the top digit are
neglected. When the input number is of more than 2 places below the decimal point, the
places subsequent to the last place are neglected.
Note: When displaying numbers, zero suppression is not performed, (e.g., when "1234" is to
be displayed and "0" is input first, only "0123" is input.)
1.2 Command keys
The following are 11 kinds of keys which carry out this operations when being depressed.
START STOP ENT C.E ESCAPE HOLD
FLOW.M SCAN LOCK SHIFT.D
STOP.W
1.3 Function keys
The keys shown below are the ones which put the function into practice when numerical
keys described in 1.1 are input after all key operation and |ENT~| command key is depressed
last.
I. TEMP I. TIME P. RATE F. TIME F. TEMP
RETRN | [START. T 1 [STOP. T | 1 SLEEP. T
When [ENT| is depressed just after depressing these keys but without depressing numerical
keys, setting stored is indicated on display.
1.4 Monitoring key
[MONll key is used when each measured value of controlled GC is to be indicated on display.
In this case, the keys made effective when being depressed after 1 MONI1 are as follows:
I. TEMP : Actual temperature of column oven
I. TIME : Retention time after start (key) is pressed.
P. RATE : Actual temperature of column oven
F. TIME : Retention time after start (key) is pressed.
- 2 -
F. TEMP : Actual temperature of column oven
COL : Actual temperature of column oven
AUXj : Actual temperature of AUXX (satellite oven)
INJ : Actual temperature of INJ (injection port)
TCD : Actual temperature of TCD (TCD oven)
AUX2 : Actual temperature of AUX2 (additional temperature control unit)
DET. T : Actual temperature of DET (detector unit)
S. NO : Sample number of the AOC (auto-injector)
PRG : Step number of time program to be carried out next
START. T : Time elapsed after shift-down start
STOP. T : Time elapsed after shift-down stop
SLEEP. T : Time elapsed after shift-down stop
RET. T : Retention time after START is pressed.
HOLD. T : Retention time after START is pressed.
When the above keys are pressed just after [MONIJ key, the actual values are immediately
indicated on display.
DET : Displays the type of detector
FLOW : Displays actual value of flow rate (only when flow measure option is con-
nected.)
When depressing [MONll key, JDET[ or [FLOWJ key, numerical key of appropriate number,
and [ENT| key in this order, (e.g., | MONI| JDET) [~T] |ENTl), its content is indicated on display.
1.5 Dialog key
A) For the period between [PRG[ key pressing and 1 ESCAPE! key pressing, display and all
other keys are occupied to make time program.
, DIALOG lamp goes up, "TIME?" is indi-When depressing keys as | SHIFT. DPRG
cated on display and time program making routine starts. In order to escape the dialog
routine and return to normal condition, it is necessary to press the keys 1 SHIFT. D| and
in this order.ESCAPE
B) For the period between the fFUNCl key pressing and the [ESCAPE] key pressing,
FUNC routine is called and contents of selected functions are indicated, on display.
if it is unnecessary to revise the displayed contents (numerical values), depress the [ ENT[
key and recall the next function. It is also possible to depress the | ESCAPE] key so as to
escape FUNC routine. If it is necessary to revise the displayed contents, input
- 3 -
the correct number and depress the |ENTl key. Then the numerical value is revised to new
one and the content of the next function is indicated.
When depressing the keys 1 SHIFT. D| FILEFUNC
(numerical value) [ENT| in this order,
DIALOG lamp goes up and content of function is indicated on display in accordance with the
input numerical value.
- 4 -
2. Starting Gas Chromatograph
When power is supplied to GC-9A/9AM for the first time after the purchase, start it in the
following procedure.
(1) Complete the preparations for power supply such as piping of carrier gas, column connection,
and connection to power source outlet as instructed by the attached installation procedure.
(2) Before turning power on, set 3 switches on the left side of GC-9A/9AM main body (at right
of the viewer) as follows:
PROTECT switch
When this switch is turned "ON", preset analytical conditions are stored as they are even when
the power source of GC-9A/9AM is turned "OFF". When the GC-9A/9AM power source is
turned "ON" next time, condition presettings are unnecessary.
If this switch is turned "OFF" and power source of GC-9A/9AM is turned "OFF", all preset
analytical conditions are erased. When the power source of GC-9A/9AM is turned "ON" next
time, analytical conditions are initialized. (Refer to the table on pages 32 ~ 35 for initial values.)
Normally keep "ON" PROTECT switch.
HEATEPv switch
If this switch is turned "ON", it is possible to supply power to each heater of INJECTION
block, COLUMN oven, TCD and DETECTOR block. When the switch is turned "OFF", power
does not reach the heaters of temperature control zones. Normally keep "ON" HEATER
switch.
POWER switch
This is the main switch to supply power to the main body.
(3) Turn ON the main switch.
(4) For about one second, nothing appears on display. Later CITP. XX is indicated. INITIAL,
ERROR CM and FAULT may be indicated, which will be explained later.
(5) Under this condition, power does not reach the heater of each temperature control zone.
Therefore, set the conditions for the analysis at this point. (When shift to other files is required
during the analysis, set all possible files to be used in analysis or confirm the contents.)
* Always file number is set to zero after power on.
(6) After confirming that condition settings are carried out correctly, select the right file and
depress the 1 START| key. From this point on, power reaches the heater of each connected
temperature control zone and the temperature is controlled in accordance with the presetting
values.
- 5 -
Displayed contents when power is turned on
CITP. XX: Displayed normally and is monitor display of column oven temperature. Since
the | START] key has never pressed after turning power on, actual values are
not displayed. When the 1 START] is depressed, actual values are displayed.
ERROR CM : When the contents of condition settings have been changed while power is
turned "OFF" or when setting conditions have been changed just before the
power is turned OFF, reliability of stored content goes down. At this time,
this display appears. (This display does not appear when PROTECT switch
is turned "OFF".)
INITIAL : When there is critical change in stored information in spite of PROTECT
switch turned "ON", setting conditions are initialized and this display appears.
Therefore reset the setting condition once again.
FAULT : Displayed when a part of program is broken. Since the instrument cannot be
used under this circumstance, make contact with our serviceman.
- 6 -
3. Column Oven
With column oven, it is possible to perform isothermal analysis and five-stage programmed
temperature control analysis. On the analysis around at room temperature, controllable minimum
temperature of column oven changes depending on the temperature of injection block at that
time, if the temperature of injection section is 300°C, the controllable temperature of column
oven is between room temperature plus 15°C and 399°C. Moreover, when analysis is carried out at
low temperature, the analysis at -50°C or more (when liquid carbon dioxide is used) or at -80°C
or more (when liquid nitrogen is used) is possible by connecting with an optional CRG unit.
At the start of column oven temperature control, the temperature always rises from the point of
about 70°C lower than the injection temperature in order to keep the detector away from contami-
nation due to elution from the column. However, if the injection temperature is within the range of
(setting value) ±5°C, the temperature of the column oven is controlled to the set value.
3.1 Setting the column oven temperature
When PROTECT switch is turned OFF when supplying power to the GC-9A/9AM, the column
oven temperature is set to the initial value of 100°C. When PROTECT switch is turned ON, column
oven temperature is the one stored as the analysis conditions of the last time. At first, power
does not reach the column oven heater. In this circumstance, set the column oven temperature
to the specified value.
When column oven temperature is to be set to 200°C, press keys as follows: |COL j 11. TEMP
HD [0] [O] JENTJ The column oven temperature can be set by 1°C.
3.2 Setting the maximum column oven temperature
The GC-9A/9AM sets the maximum column oven temperature to 400°C as the initial value.
However, if the maximum value of column oven is to be set otherwise depending on used
column, it is possible to make input by manipulating FUNC key. When the maximum
temperature is to be set to 250°C, depress the keys as follows:
SHIFT. FILEFUNC 7 ENT 2 5 0 ENT SHIFT. D
ESCAPE
When the column oven temperature reaches the maximum temperature set here, "OVER
COL" is displayed and temperature control of column oven is suspended, leaving column oven
heater OFF (At this time, the flap at the rear of the column oven remains closed.) and the
buzzar continuously sounds for abnormality. When circumstances become abnormal, reset
column oven preset temperature to the appropriate value or revise the maximum column oven
- 7 -
temperature and depress the lCE| key. From this moment the temperature control of
column oven is restarted, if the circumstances are still abnormal with this operation, power
is suspended not to reach the column oven heater again, OVER COL is displayed and buzzer
sounds. This requires rechecking.
3.3 Starting column oven temperature control
Turn ON GC power switch. After setting as instructed in 3.1 and 3.2, depress the 1 START
key. From this time on, all temperature controls are started. But temperature program (AOC
or, time program) does not RUN. The next depressing of the 1 START 1 key, means the start
of temperature program (AOC or time program).
3.4 Power supply to column oven heater and its suspension
When the heater ON/OFF switch on the right side of GC is turned OFF, power does not
supplied to the column over heater. If the switch is turned ON and procedure of 3.3 is com-
pleted, power reaches the column oven heater.
3.5 How to display preset values and actual values of the column oven temperature
When the preset value of the column oven temperature should be displayed, depress the keys
as follows:
[COLifl. TEMPI [ENTl
Then the display "CITP 200" appears. In this case the column oven temperature is set to
200°C.
When actual value of the column oven temperature should be displayed, depress the keys as
follows:
Then the display "CITP. 198" appears. In this case the actual temperature of the column
oven is 198°C. The flickering of period "•" of "CITP." means that the actual measurement is
being monitored.
Note: When the actual values are monitored under the state of GC power switch being turned
ON and START switch never depressed, the display "CITP. XX" appears, indicating that
the temperature control is not carried out. (In general key operations, appearance of XX
on display means that the START key has never been depressed since the power was
turned ON.) When the START key is depressed, ** may appear on display, which indi-
cates that this START key operation is the first after the power is turned ON. When the dis-
play indicate a monitored value such as CITP. XX at the first depression of START key, the
actual value of the designated position will be indicated instead of **•
4. Setting Injection Temperature
The temperature in detector block is the same as the temperature in injection block, which is
usually set to about 50°C higher than the column oven temperature. The setting method is as
follows:flNJl [3][0][0] lENTl
In this case the temperature is set to 300°C. When the actual temperature of injection block
is to be known, depress the keys as [MONIl |INJ| . Then the display "INJT. 300" appears.
Note 1: The temperature does not rise until the 1 START 1 key is depressed for the first time
after power is turned on.
Note 2: Until the injection temperature enters the range of (setting value) ± 5°C, the temperature
of the column oven is always adjusted at the temperature about 70°C lower than the
injection temperature. When the injection temperature has entered the range of (setting
value) ± 5°C, the column oven temperature can be adjusted at the temperature higher than
the injection temperature.
5. Temperature Programming
Temperature of the column oven can be programmed for the multistage, 1 to 5, temperature
rise. Detailed operations are described in the separate manual. Here the general operations are
explained.
5.1 Standard one stage temperature programming
TEMP
TIME
In the above figure, parameters necessary to program one-stage temperature rise are as
follows:
Unit
I. TEMP Setting of T t °C
I. TIME • Setting of a min
P. RATE
F. TIME
F. TEMP
Setting of—^-y-
Setting of c
Setting of T2
" T l °C/min
min
°C
Carry out key inputting as follows:
COL] 1 I. TEMP 1 [61 [0] lENT
fi. TIME! [TIR)] RENT"
P. RATE|[2] R [5] lENT"
F. TEMP 2 0 0 ENT
F. TIME 1 5 ENT
The above operation permits the following settings:
Initial time =10 minutes
Initial temperature = 60°C
Temperature programming rate = 2.5°C/minute
- 10-
Final temperature = 300°C
Final time = 15 minutes
5.2 Multistage temperature programming (for 3 stages)
T3
T2
T,
The relation between parameters for multistage temperature rising and keys is as follows:
I.
I.
p
F
F
TIME
TEMP]
.RATE
.TIME
.TEMP
T,
T2-T, T3-T2 T4-T3
b , d , f
c. e, g
As for the setting method, it is recommendable to list up elements to be preset as shown
below.
Initial
First stage
Second stage
Third stage
Temperaturerising rate
X
5
10
5
Temperature
100
150
175
200
Time
10
5
15
20
Initial Temp, Time
Final Temp, Time
In this case the temperature rises as shown in the figure below.
- 1 1 -
Minute
0 10 20 25
27.5 47.5
The key inputting shall be carried out as follows:
COL I. TEMP 1 0 0 ENT
I. TIME] [HE]
P.RATE 5 ENT 1 0 ENT 5 ENT
F. TEMPI LUL5JLQJ [ENT]
|T|f7ir5l HENTl
F.TIME 5 ENT 1 5 ENT 2 0 ENT
When multistage temperature rise is programmed, by pressing the |COL| key, the stage of
multistage temperature rise is designated to the first stage. From that time on, every setting
makes the stage proceed one by one.
If function to be set is not changed, multistage program can be arranged by inputting the
numerical value and by pressing the [ENT| key sequentially.
If the programming is not correct, the program rate must be completely reprogrammed from
the first stage. When the final temp, or the final time is incorrect, repeat pressing only the
| ENT | key without pressing the numerical keys until the value of one stage earlier is displayed
at display. Then set the correct value with numerical keys and depress the |ENT[ key.
Thus they are revised.
(Example) In the case of 2-stage temperature programming.
300.° C
15 min.
10 min.
First stage
Second stage
P RATE
5
6
F .TEMP
200
300
F. TIME
10
15
In this case there are two methods for programming temperature.
- 1 2 -
How to set the same function alone
COL I Designates the first stages of P.RATE, F.TIME and F.TEMP
1F. TIME I Select F. TIME function.
i
a m1 ) Set the first stage to 10 min. CFM1 10 is displayed.
ENTl
m EIi
lENT
I
F. TEMP
1
EI
ENT
Set the second stage to 15 min. CFM2 15 is displayed.
Selects F. TEMP function.
Sets the first stage to 200°C. CFP1 200 is displayed.
ENT
1
P. RATE
1
El1
ENT
I
Ell
"ENT
Sets the second stage to 300°C. CFP2 300 displayed.
Selects P. Rate function.
Sets the first stage to 5°C/min. CRP1 5 is displayed.
Sets the second stage to 6 C/min. CPR2 6 is displayed.
- 1 3 -
How to set P.RATE, F.TIME and F.TEMP in each stage
[COL I Designates each function at the first stage.
P. RATE
F. TIME
F. TEMP
I
F. TIME
F.TEMP
First-stage setting
Second-stage setting
- 1 4 -
When the final time (15 min.) at the second stage is revised to 20 minutes
COL
1
F. TIME
1ENT
[2 Ei
[ENT
When the |ENT| key is depressed, without depressingthe numerical keys, the preset information isindicated on display.
CFM 1 10
Here the final time at the second stage is set.
CFM 2 20
- 1 5 -
O)
/INITIAL TIME.PROGRAM RATE
\ / Sets temperature
\
INITIAL TEMPERATURE AUXlSets initial temperatureof the column oven
I Sets initial hold time in \ I program rate in pro-l programmed temperature / \ grammed temperature
analysis \ ^ / ^analysis
FINAL TEMPERATURESets hold temperature inprogrammed temperature
FINAL TIME N/ Sets hold time in programmed J\ temperature /\ i • TCD OVEN TEMPERATUREanalysis ^^
Sets temperature of TCD oven
COLUMN OVENr n Indicates that the 5 keys on
the above line are for the _-functions of the column.
[in Designates each function intemperature rising programof column to the first stage.
• - 3
B
crq
CD
"5o
7sCD
AUXl OVEN (option)|~T~| Indicates that the 5 keys on the
above line are for the functionsof AUXl.
I 2 I Designates each function intemperature rising programof AUXl to the first stage
AUX2 BLOCKTEMPERATURESet the tempera-ture of AUX2block (optional)
INJECTIONBLOCKTEMPERATURESets temperatureof injection port
DETECTOR TEMPERATURESets temperature of detectorblock (optional)
When this key is depressed, COL or AUXl isstored until it is revised next.
*Useful in case of setting a temperature program.
to
Displays actual tempera-ture in COLUMN oven
Displays actual temperature inAUXl oven. When AUX1 ovenis not connected -105 C isdisplayed.
Display of actualtemperature in columnoven or AUXl oven
DEL RETN COPY
2 3 SHIFT. D
START.T STOP.T SLEEP T
LOCK SCAN ESCAPE
Display of actual I. ^ ^ ^ ^ Display of actual temperaturetemperature in AUX2 Display of Display of in TCD ovenblock , actual temper-\ actual temperature /When TCD is not/ When AUX2 block \ ( ature in INJ j in DET block ( connected, NON is( is not connected, ) \block / /When DET block \ ^displayed.
' \ is not connected,NON is displayed.is displayed.
H
3
P
3
Note: When the | START | key has never been depressed after POWER switch is turned ON,XX is displayed instead of actual value.
6.3 Temperature monitoring at 6 points
I.TEMP I.TIME P.RATE F.TEMP F.TIME• PRG EVENT S.NOSTART COL INJ TCO
AUX.I AUX.2 DET
DET RANG POL CURR
STOP
DEL RETN COPY
CE
MON
SHIFT. D
O(INJ. I) (INJ.2) (STRK) (REPT) S H i n " START.T STOP.T SLEEP T
FILE FLOW STOP.W HOLD 0 * —
FUNC FLOW.M RET. T HOLD.T L ° C K LOCK SCAN ESCAPE
ENT
Actual temperatures of 6 points (COLUMN, AUXl, AUX2,TCD, DET and INJ) are displayed in sequence. In this casepressing the | MONI | key is not required.
-18-
6.4 Parameter setting for detector
DETECTORSet detectornumber, 1 to 4Once it is set, thedetector number isnot changed untilpower is turned offor it is reset.
I.TEMP I.TIME P.RATE F.TEMP F.TIME
START
AUX.I AUX.2 DET
DET ^RANG ^-POL CURR
DEL RETN COPY
CE
MON
SHIFT. D
ENT
RANGESets range ofdetectorselected bythe | DET |key.
POLARITYSets polarity ofdetector selectedby the JDET|key.
CURRENTSets current ofdetector selectedby the |DETlkey.
Note: When RANGE, POLARITY and CURRENT are set,if there is no applicable function in the selectedDETECTOR, NON is displayed.
- 1 9 -
6.5 Detector monitoring
I.TEMP I.TIME P.RATE F.TEMP F.TIME
START COL INJ TCD STOP
AUX.I AUX.2 DET
DET RANG POL CURR
O
PRG EVENT S.NO
DEL RETN COPY
CE
MON
SHIFT. D
(INJ. I) (INJ.2) (STRK) (REPT) 5 H I F T START.T STOP.T SLEEP.T
0 * — E N TFILE FLOW STOP.W HOLD
FUNC FLOW.M RET.T HOLD.TL ° ° K
LOCK SCAN ESCAPE
When the keys [MQNll 1DET| 1 ~ 4 and [ETN[ are depressedin this order, which detector is selected is indicated on display.
FID Flame Ionization DetectorTCD Thermal Conductivity DetectorPID Photo Ionization DetectorFTD Flame Thermionic DetectorFPD Flame Photometric Detector
ECD Electron Capture Detector
- 2 0 -
6.6 Timer setting
Start of timecounting by timer Tl
I.TEMP I.TIME P.RATE F.TEMP F.TIME
START
Note: In this case STARTand STOP are usedin shift-down mode.
Note: | START I is effectiveonly when it is de-pressed for first timeafter POWER switchis turned ON.
COL INJ TCD STOP
1 1 1 1AUX.i AUX.2 DET
DET RANG POL CURR
FUNC FLOWM RET T HOLD.T
Start of time countingby timer T2timer T3 automaticallyoperates after timer T2completes operation.
O
CE
MON
SHIFT. D
(INJ. I) ( INJ.2) (STRK) (REPT) / b M " " ' rSTART,T STOP.T
FILE FLOW STOP.W HOLD
SLEEP TENT
Sets Tl Sets T2 ' Sets T3(unit: 0.1 min.) (unit: 0.1 min.) (unit: 1 min.)
Note: Time accuracy is±0.1 minute.
Sections where power is supplied toheaters of each temperature adjustingunit and where temperature control iscarried out.
Time when shift-downSTART of GC-9A/9AMis depressed.
Sections where power is not suppliedto heaters of each temperaturecontrol zone.
- 2 1 -
6.7 Timer monitoringSTOP WATCH functionWith this pressed, counting starts in
f the order of 0.1 second. With thispressed again, counting stops.
I.TEMP I.TIME P.RATE F.TEMP•START• COL INJ TCD
AUX.I AUX.2 DET
DET RANG POL / CURR
F.TIME CE
STOPPRG EVENT S.NO
4 5 6
DEL RETN COPY
O(INJ. I) ( INJ.2) (STRK)/ (REPT) b H l h ' START.T STOP.T SLEEP. T
FILE FLOW STOP.W HOLD
FUNC FLOWM RET.T HOLD.T
MON
SHIFT. D
ENT
When these keys are depressed after the [MONll key,the time elapsed in each timer is displayed.(Unit: 1 min.)
- 2 2 -
TIME PROGRAMEnters dialog toarrange time program
Changes range Changes polarity
Designates DET number
to
I.TEMP I.TIME
START COL
P. RATE F.TEMP F.TIME
Designates relay(appropriate) number
CE
TCD STOPPRG EVENT S.NO
4 5 6 MON
SHIFT. D
Number of times ofinjections to injectionport No. 1 in AOC
Designates numberof repetition andfile of analysis
.DELETEDeletes one step intime program
Number of times di Syringe strokeinjections to injection of AOCport No. 2 in AOC
Number of \Possible to berepetition of incorporated in timeAOC program and to suspend
time program
ESCAPEFinish the dialogueof time program
OS
00
COCD
1era
13
O
era
Note 1: Time program is started by the | START | key. When it is necessary to interrupt the operation, depress the |STOP| key.
2: During the execution of time program, it is impossible to arrange and revise time program and to monitor the time program.
3: When the [HOLD! is depressed during the execution of time program, the operation can be held at that time. Depressthe |HOLD] once again to restart.
4: INJl, INJ2, STRK and REPT keys can not be set except during time programming.
6.9 Time program monitoring
When the keys [MONIl 1 SHIFT.D] [ PRG1 are depressed in this order during the execution
of time program, step number of time program to be executed next can be displayed.
When whole time program is completed or when nothing is arranged in time program, zero is
displayed as step number.
6.10 File setting
I.TEMP I.TIME P.RATE F.TEMP F.TIME
START, " ' COL INJ TCD• • • •STOP
PRG EVENT S.NO
-DEL RETN COPY-AUX.I AUX.2 DET
PET RANG POL CURR I• • • • o • __ __(INJ. I) ( INJ.2) (STRK) (REPT) S H I h T START.T STOP.T SLEEP.T
FILE FLOW STOP.W HOLD 0
I I 1 I I I °M&£ f I " 'I V 'I LOCK
FUNC FLOWM RET.T HOLD.T I LOCK SCAN ESCAPE
CE
MON
SHIFT. D
ENT
Is used when file number (0~9)is designated and new file isopened.
Is used when file isdeleted. (Impossibleto delete the presentfile.)
Is used when thepresent file is copiedto other file.
- 2 4 -
6.11 FUNC setting
Functions listed below can be set by the operation of FUNC key. Functions possible to be
set and the code number at that time are made into a table.
Code
1
2
3
4
5
6
7
8
13
14
15
Function
Selection of each parameter of AOC
Demand for list to CR2A of time program
Demand for list to CR2A of AOG parameter
Demand for list to CR2A of GC parameter
Setting the maximum value of temperature in detector and injection sections
Setting the maximum temperature in AUXi oven
Setting the maximum temperature in column oven
Setting link device
Starting self-diagnosis(When this is executed, all preset values are deleted and initialized.)
Setting the value of the fixed number "K" of flow measurement
Demand for list to CR2A of temperature program
*3
*1
*1
*1
*4
*1
*2
*1
* 1 is effective when CR2A is connected.
*2 is effective when flux measurement device (optional) is connected.
*3 is effective when automatic sample injection device (optional) is connected.
*4 is effective when AUXi oven (optional), a satellite oven, is connected.
The example of setting is as follows:
5] [ENT| [3][5]LO]SHIFT. D FILEFUNC
In this case the maximum detector temperature is set to 350°C.
Note: One function is selected by FUNC key, the key operations which follow are all
in dialog method and DIALOG lamp lights up. On going out of dialog by FUNC
key, pressing the ESCAPE key is required.
When 350°C is input, the maximum value of AUXi oven which is preset appears on display.
fENTl .Here the dialog by FUNC key is completed by key inputting | SHIFT. DESCAPE
When the preset value of each function by FUNC key should be displayed, there is no need
to set each time.
The functions described below indicate setting value of the next function on display when-
ever the lENTl key is depressed. When the displayed information is to be revised, key input
- 2 5 -
the correct numerical value and depress the lENT| key. Then the numerical value is newly
set and the value to be preset for the next function is indicated on display.
Whenever pressing the |ENT] key, the function is displayed as follows:
AOC parameter Maximum temperature ofdetector, injection block
Maximum temperatureof AUXi oven
Maximum temperatureof column oven
Setting link device Setting "K" of flow-measurement
However, the list demand function of each parameter of CR2A and function of self-diagnosis
can not be selected even if the jENTj key is continuously depressed.
Moreover, when function of AOC parameter setting is selected, the related parameters are
displayed one after another on one pressing of the jENTj key.
AOC parameter includes the following 10 elements. Refer to the separate manual "option"
for the details.
STRK
ISNO
FSNO
REPT
WASH
WSHT
TWTE
PROD
I JIT
1J2T
Syringe stroke
Initial sample number
Final sample number
Number of sample repetition
Selection of detergent solution
Number of washings
Setting waiting time
Analysis period
Number of injections to injection port 1
Number of injections to injection port 2
- 2 6 -
6.12 List of key explanation
Key name Meaning Example
START (T) When this key is depressed the first timeafter power supply to GC-9A, it meansthe start of power supply to each temper-ature control zone. (Until then, poweris not supplied to each temperaturecontrol zone.)
(2) When this key is depressed the secondtime or later after power supply to GC-9A, it means the start of temperatureprogram, time program and AOC.
START
START
STOP It stops operations started in the meaning of©of the [START| key. When the I START 1key is depressed next, operation start fromthe beginning.
It sets the initial temperature of columnA T TS.7-
I. TEMP ovenor AUXX oven.
COLAUX1
Column oven temperature is set to 100 C.
SHIFT. D COLAUX1
AUXj oven temperature is to 100 C.
I.TIME Sets hold time of initial temperature incolumn oven or AUXj oven.
ICOLl ll.TIMEl [1 ||0||ENT|Initial time of column oven is set to 10 minutes.
SHIFT. DCOL
AUX1Initial time of AUXi oven can be set to 10minutes.
P. RATE Sets temperature programming rate ( C/minute) of column oven or AUXj oven.(Possible to set at maximum of 5 stages.)
P. RATETemperature programming rate at the firststage can be set to 5.2 C/minute. When thevalues are input consecutively, temperatureprogramming rates at the 2nd and 3rd stage canbe set.
F.TIME Sets hold time of intermediate and finaltemperatures in column oven or AUXi oven. Temperature hold time at the first step of
column oven, is set to 20 minutes. When thevalues are input consecutively, the times at 2ndand 3rd steps can be set.
F.TEMP Sets the intermediate or final temperature incolumn oven or AUXi oven. SHIFT.D
COLAUXI
The final temperature at the first step of AUXjoven is set to 210 C. When the values are in-put consecutively, the times (temperatures) at2nd and 3rd steps can be set.
- 2 7 -
Key name Meaning
COL (f) Selects whether each function of I.TEMP,I.TIME, P.RATE, F.TIME, F.TEMP is forcolumn oven or for AUXi oven. Once se-lected, it is memorized.
(2) When temperature programming is set, itreturns the step appointment of P. RATE,F.TIME and F.TEMP to the first step.
Example
INJ Sets temperature of injection block.
TCD Sets TCD temperature.
DET When the value is set on parameters of de-tector, POL, PANG and CURR, this key indi-cates which detector should be set and whatsetting value should be reach with the numeri-cal number of detector numbers 1 to 4.Once it is set, it is memorized until next setting
[DETl[2|lENf|Detector 2 is selected and setting values ofPOL, RNG, and CURR are carried out on de-tector 2.
RANGE Sets range of detector. RANGE|[~2ilENT|102 is selected.
POL Sets polarity of detector.
CURR Sets current of detector.Incase of TCD, 10mA is set.
FILE Sets file number 0 to 9. When the numberwhich has never been selected or once deletedby DEL key is set, the file number is newlyopened and its content is initialized. If al-ready opened file number is set, that file isappointed and its content is controlled inaccordance with GC-9A. Consequently, whenthe file number is shifted during analysis,from that time, control is carried out in accordance with the content of the appointed filenumber. Therefore, it is necessary to be care-ful on setting the file which is not in executionand on monitoring the content.
I FILE! 1 lllENTlAlways file number is to zero after power ON.
FLOW Selects the flow rate when the flow value isset. The values possible to input are 1 to 5which correspond as follows:1. Selects flow of carrier gas 1.2. Selects flow of carrier gas 2.3. Selects flow of Hydrogen gas 1.4. Selects flow of Hydrogen gas 2.5. Selects flow of air.Since value of 1 to 5 set here is not memo-rized, it is necessary to set each time.
lFLOWll2]lENfl|5ll0]|ENT|On carrier gas route 2, the flow is set to 50m£/minute.When flow setting devise (option) is not con-nected, setting value is simply memorized.
INJ1 Sets the number of time when injection iscarried out to GC injection port 1, when AOCis attached. (Setting is possible only duringPRG program.)
- 2 8 -
Key name Meaning
INJ2 Sets number of time when injection is carriedout to GC injection port 2, when AOC isattached. (Setting is possible only duringPRG program.)
Example
STRK Sets syringe stroke, when AOC is attached.(Setting is possible only during PRG program/
REPT Sets number of repetition of the same sampleinjection, when AOC is attached. (Setting ispossible only during PRG program.)
FUNC i) Sets the conditions when AOC is attached,ii) Makes a list of GC conditions in CRT or
plotter, when CR2A is connected.iii) Sets the maximum temperature of each
temperature control zone.iv) Self-diagnosis.The above functions can be set in dialog withdisplay.
Starts measurement of carrier gas flow byattaching the flow measuring unit. (Needsoptional accessories)
FLOW. M It is necessary to set what flow is measuredwith the FLOW key in advance.
RET. T Key for monitoring use only. It indicates ondisplay the time elapsed after the STARTswitch is depressed.
MQNll ISHIFT.Dl |REf-f|
HOLD. T It is used to hold the present temperaturewhen the temperature in column oven orAUXj oven is rising. The present temper-ature is held for the period set by this key.
| SHIFT. D11HOLD-T | \3\ [ENT |In this case, hold is for 3 minutes.
STOP-W Operates stopwatch. With the first pressing,display is cleared and counting starts in theunit of 0.1 second. With the second press-ing, counting is suspended. With the thirdpressing, the state becomes same as that onthe first pressing.
STOP-W 1 - | STOP-W 1
HOLD Suspends time control. With the first press-ing, control is suspended and HOLD is dis-played. With the second pressing, holdoperation is removed and retention time isdisplayed.During hold, the following functions suspend.oAOC operationoPRG operationo Retention timeo In case of hold time state in temperature
programming mode, the counting of thehold time is suspended.
However, during the period of temperatureprogramming in temperature rising mode, thetemperature at that time can not be held.
- 2 9 -
Key name Meaning
PRG When the program of time program is arrangedits dialog starts. After that time, dialog con-tinues until the ESCAPE key is depressed.
Example
1 SHIFT.Dl [PROG 1 [ESCAPE]
EVENT Possible to drive external electromagneticvalve and motor by attaching print board forPRG. The number of elements is 18 in total.
ISHIFT.DlNo. 3 relay or transistor is turned ON.In case of turning OFF, place minus in frontof figure. (If this key operation is carried outexcept in time program, relay operators atthat moment.)
S. NO i.) When AOC is attached, the present samplenumber is indicated on display.
ii) Direct appointment of next sample number.
iMONll ISHIFT.Dl | S. NO
DEL i) Deletion of file content.ii) Used in time program and deletes one step
portion.
ISHIFT.Dl |DEL||3||ENTlContent of file number is all deleted.
RETRN Setting is possible only in PRG program.When time program is carried out and reachesthe step with this RETRN arranged, automaticrepetition starts in that file number as manytimes as set number of execution. After theprogram is repeated as many times as set num-ber, it is shifted to appointed file and carriedout.
ISHIFT-D] [RETRN | [103] |ENT|
103i ^—Following file number to be carried (0~
9)-Number of times of repeated executionsin the present file number (1~99).
COPY Used when the content of the present file iscopied to other file as it is. When the present file is 2, the content of file
2 is copied to file 4.
START. T Sets waiting time from power supply to GC tostart of power supply to heater of each temper-ature control zone. If it is used with monitorkey, it is possible to monitor the time elapsed.
ISHIFT.Dl |START.T||3l|ENTlStart time is set to 3 minutes.
STOP. T Sets time until suspension of power supply toheater of GC temperature control zone.After elapsing this time, GC enters sleep state.
| SHIFT. D| I STOP. T | [311ENT |Stop time is set 3 minutes.
SLEEP. T Sets time after GC entering sleep state until re-start of power supply to heater of temperaturecontrol zones.
ISHIFTTDI [SLEEP.til 5||ENT1Sleep time is set to 5 minutes.
LOCK Each key operation is locked. However, keyssuch as START, STOP, SHIFT. D and LOCKcan be operated during lock. When the LOCKkey is depressed again during lock, lock is re-moved.
SHIFT.D LOCK
SCAN Used when actual temperatures of each temper-ature control zone are displayed in order withthe fixed interval.
SHIFT.D SCAN
ESCAPE Used to escape from the dialog after enteringdialog by FUNC key or PRG key operation.
SHIFT.D ESCAPE
-30-
Key name
MONI
CE
SHIFT. D
E N T
Meaning
Used when actual values are monitored.
Deletes the display content. (This key isused when key operation is carried out in-correctly or when each temperature controlzone is heated and OVER display appears.)
Used when the function mentioned beloweach key name.
Used when the placed values are input orwhen already input values are to be known.
Example
iMONll [COLlThe actual value of column oven is indicatedon display.
- 3 1 -
7. Control Parameter and Initial Value
The table shown below indicates parameter symbols, maximum and minimum values of figures
possible to input and units which are available when conditions are set from the external computer
by connecting current loop interface board (option) and is a list of controllable parameters of
GC-9A.
When the power is supplied in the state of the PROTECT switch turned OFF, each condition
setting value of analysis is initialized and file zero is automatically selected and files 1 to 9 are
deleted. Setting values of initial functions are indicated the right column of the table.
Name
D1RG
D1PL
DlCR
D2RG
D2PL
D2CR
D3RG
D3PL
D3CR
D4RG
D4PL
D4CR
FLW1
FLW2
FLW3
FLW4
FLW5
INJT
DETT
AUXT
CITM
CITP
AITM
AITP
CPR1
CPR2
CPR3
Meaning
DETECTOR 1 RANGE
POLARITY
CURRENT
DETECTOR 2 RANGE
POLARITY
CURRENT
DETECTOR 3 RANGE
POLARITY
CURRENT
DETECTOR 4 RANGE
POLARITY
CURRENT
FLOW CARRIER 1
CARRIER 2
H2 1
H2 2
AIR
INJECTION TEMP.
DETECTION TEMP.
AUX.2 TEMP.
COLUMN INITIAL HOLD TIME
COLUMN INITIAL TEMP.
AUX1 INITIAL HOLD TEMP.
AUX1 INITIAL TEMP
COLUMN PROGRAM RATEl
2
3
Max. • Min.
0, 1, 2, 3, 4
2 (-), 1(+)
0-200
n
"
n
0-999.8
»
0-399
0—399
0-399
0-655
-99.0-399.0
0 - 655
- 9 9 . 0 - 399
0— 40.0
»
Unit
io x
mA
a
"
m^/min
»
»
deg. °C
»
min
deg. °C
min
deg. °C
°C/min
»
"
Initial value
40.0
40.0
30.0
30.0
200.0
200
200
200
0.0
100.0
0.0
100
0.0
»
"
-32 -
Name
CPR4
CPR5
CFP1
CFP2
CFP3
CFP4
CFP5
CFM1
CFM2
CFM3
CFM4
CFM5
APR1
APR2
APR3
APR4
APR5
AFP1
AFP2
AFP 3
AFP4
AFP 5
AFM1
AFM2
AFM3
AFM4
AFM5
TCDT
SNO
STRK
ISNO
FSNO
REPT
WASH
WSHT
TWTE
PROD
Meaning
COLUMN PROGRAM RATE4
5
COLUMN FINAL TEMPI
//
//
2
3
4
5
COLUMN FINAL TIME 1
»
"
2
3
4
5
AUX1 PROGRAM RATE1
//
//
//
»
AUX1 FINAL TEMPI
2
3
4
5
AUX1 FINAL TIME 1
2
3
4
5
TCD TEMP
SAMPLE NUMBER
STROKE
2
3
4
5
INITIAL SAMPLE NOMBER
FINAL SAMPLE NUMBER
REPEAT
WASHING LIQUID
WASHING TIME
TIME WAIT
PERIOD
Max. • Min.
0-
-99.0 -
o-
/
o -
-99.0 -
ti
»
»
»
0 ~
»
"
0 ~
0 ~
1 0 ~
0 ~
0 ~
1 ~
- 40.0
•'
-399.0
• '
•>
- 655
- 40.0
-399
655
-399
- 50
- 80
50
50
10
0 ( SAMPLE )1(SOLVENT )
1, 2, 3,
0 ~
10
, io
999
Unit
°C/min
//
de.g. °C
"
min
»
»
//
//
°C/min
//
//
»
deg.°C
min
"
//
»
deg.°C
min
Initial value
0.0
»
200.0
0.0
//
//
//
0.0
»
//
//
0.0
»
»
»
200
0
//
»
0.0
»
»
//
//
30
1
10
1
49
1
1
1
5
10
-33-
Name
IJ1T
IJ2T
FLWK
DMAX
CMAX
AMAX
HLDA
HLDC
SLPT
STRT
STPT
LDVC
STTS
FILE
STAR
STOP
FLM
AUXF
MONT
SSTR
SSTP
DET1
RT
SCAN
COPY
KLOK
CKSM
VALU
FNC$
DIGN
HOLD
ESCP
EVNT
LPRG
Meaning
INJECTION 1 TIME
INJECTION2 TIME
FLOW K
DETECTOR TEMP MAX
COLUMN TEMP MAX
AUX1 TEMP MAX
HOLD AUX1
HOLD COLUMN
SLEEP TIME
START TIME
STOP TIME
LINK DEVICE
STATUS ( PRINT )
FILE NUMBER
START
STOP
FLOW MEASURE
AUX. FUNCTION ( PRINT )
MONI TOR
SHIFT DOWN START
SHIFT DOWN STOP
DETECTOR 1 ( PRINT )
RETAINTION TIME ( PRINT )
SCAN
FILE COPY
KEY LOCK
CHECK SUM
VALUE C PRINT )
FUNCTION ( PRINT )
DIAGNOSTICS
HOLD
ESCAPE
EVENT
LIST PROGRAM
Max. • Min.
0 — 1 0
0 - 10
0.01 - 9 9 9 . 8
10 — 450
-99 - 400
-99 - 400
0 - 6 5 5
0.1 - 3 0 0 0
0 - 3 0 0 0
0 - 3 0 0 0
0 - 5 5
0 - 9
0 - 9
0 ( UNLOCK)
1 (LOCK )
2 ( INVERSE )
0 ( O N ) , l ( O F F )
3 (INVERSE)
0 - 255
Unit
deg. °C
//
//
min
//
min
//
//
Initial value
1
1
500.0
450
400
//
0.0
//
10
//
//
0
0
- 3 4 -
Name
LAOC
LPRM
AOC
PROG
TIME
DELT
RETN
LTPR
Meaning
LIST AOC PARAMETER
LIST GC PARAMETER
AOC ( PRINT )
PROGRAM
TIME
DELETE
RETURN
LIST TIME PROGRAM
Max. • Min. Unit Initial value
Note: For multistage temperature program, the total time that includesInitial and each Final times, cannot exceed 655min.
- 3 5 -
8. Setting and Deletion of File
10 files in total are prepared with its numbers 0 to 9. Functions possible to arrange in each
file include setting temperature of each temperature control zone, temperature program, condition
setting value of each detector, flow condition and time program. Since the memory area of each
file is not fixed, memory can be occupied in accordance with size of each file. Therefore, if only
a few files are opened, the length of time program to be arranged becomes considerable long.
For example, when only one file is opened, about 250 steps can be stored in the Time Program.
When the new file is opened, its content is all initialized and nothing is arranged in time program.
When the already opened file is deleted, carry out with the |DEL| key. In this case, however,
the file which is executed at present can not be deleted.
LNTl are depressed in order, file 3 is deleted.DEL
When the keys of | SHIFT. Dl
When the file appointed at present is to be copied to other file, carry out with the [COPY] key.A
When the keys of | SHIFT. P] | n r > p v | | 4 | |ENTl are depressed in order, the content of the fileCOPY
appointed at present is copied to file 4.
When LIMIT is displayed during file operation, it means that there is no file in reserve for ex-
pansion and that it is necessary to delete unused files.
Note: Only one file can be always appointed. Therefore, when the file number is revised, from
that time is controlled in accordance with the content of the new file number. When other
file is selected carelessly in analysis, setting temperature will be change in the case of the con-
tent of that file being incorrect. New setting of several files and checking of the content
should be carried out after power is supplied to GC-9A but before the 1 START] key is de-
pressed.
* File number is automatically set to zero after power "ON".
Note: In this example, it's necessary that the file 4 is not opened in the past, if the file 4 is opened
in the past, you should delete the file 4 and copy to the file 4.
- 3 6 -
9. Setting of Time Program
Function keys which can be incorporated in time program are as follows:
RANGE of each detector (1 ~ 4). POL and CURR, EVENT, RETRN, INJj , INJ2, STRK,
REPT, STOP.
9.1 Time program
Time programs realizes automatic operation of the functions related to GC-9A in the course
of time elapse by the advance programming.
9.2 Composition of time program
Components of each program step in time program are operation time, operation function
and its setting value.
(TIME) (FUNCTION) (VALUE)
Value (numerical key)
-Function (function key)
-Time from start switch pressing to operation (Unit: 0.01 minute)
9.3 How to make up time program
Time program is arranged all in dialog method. Thus, depress the PRG key in order to
inform that arrangement of time program will start form now. After that, arrange it in dialog
with display. After the arrangement is complete, depress the ESCAPE key, which indicates
the completion of dialog.
SHIFT. D| iPRGl Dialog start
Time program making
[SHIFT. D] [ESCAPE) Completion of dialog
When no program was arranged in the past, TIME? is displayed after the key operation of
SHIFT. P] [PRG[ . At this time, input the execution time of function to be operated by keys
and depress the [ENT] key. Next, display indicates FNC VLU. Then, depress the key of
function to be operated, key-input its value and depress the |ENT[ key. The above operation
completes the arrangement of program for one step.
- 3 7 -
[Example 1]
Display
TIME?
Key operation
FNC VLU
PET I • ] |ENT
POL | [2] |ENT
TIME?
FNC VLU
TIME ?
SHIFT. D EVNT 3 ENT
By the above operation, polarity of DETi will be changed to 2 after 1.2 minutes and relay (or
transistor) 3 for drive of the external device will be turned ON after 2.5 minutes.
[Example 2]
TIME?
FNC VLU
TIME?
FNC VLU
^ 1 TIM 3.5
FNC VLU
S H E ] lENT
SHIFT. D INJ1 3 ENT
[2] [ENT
SHIFT. D EVNT 2 ENT
SHIFT. D | | EVNT | H I S I ENT
-&2 TIME?
^ 1 Since the time was set to 3.5 minutes in the past, that value is displayed.
^ 2 Since the time is set to 4.5 minutes and time with more than 4.5 minutes has never been
arranged, TIME is displayed.
- 3 8 -
[Example 3]
TIME ?
FNC VLU
^ 1 FNC VLU
^ 1 Since setting mistake on POLj of DET2 occurred, that value is neglected and FNC VLU is
displayed again. (In this case, it is due to setting operation although no detector is con-
nected to DET2 and it is impossible to select.)
9.4 When new steps are inserted in the program
Since order change of time in making time program by dialog method is carried out inside of
device, there is no need to set the order of time in arrangement. Therefore, if new step is
inserted into the already arranged time program, set time when TIME or TIM XX.X (XX.X is
arbitrary number) is displayed. Next when FNC VLU is displayed, input the corresponding
function and value.
9.5 How to delete unnecessary steps
When the time of unnecessary step is displayed, depress the keys [SHIFT. D 1 |DEL| .
Then that step will be deleted.
9.6 How to delete whole time program
There is no method to delete whole time program only from file. Therefore, after deletion
of whole file, open the file and reset the content of file. Otherwise, time program should be
deleted step by step by using the DEL key.
9.7 Confirmation of time program content
When the [ENTl is depressed after [SHIFT. D] jPRGl , content of each step in time program
can be monitored one after another. If the step in time program is turned back, depress the
keys Q ]̂ [ENT[ when time is displayed. Then content of the previous step can be monitored.
- 3 9 -
10. Meanings of Display Lamps
READY Lit when the temperature of column oven is within the range of setting value
±1°C and when time program, temperature program and AOC do not operate.
INITIAL Lit when the temperature of column oven is within the range of setting value
±1°C and initial hold is operated in temperature rising mode or time program
and AOC operate.
RAISE Lit when the temperature of column oven is rising.
FINAL Lit when the temperature of column oven is held in the temperature rising mode.
COOL Lit during the period until the temperature of column oven stabilizes at initial
temperature after reaching the final temperature in the temperature rising mode.
DIALOG Lit when dialog is operated by PRG and FUNC keys.
SHIFT. D When this lamp is lit, it indicates that the key next depressed is in shift down
mode.
LOCK When this lamp is lit, it indicates that each key operation is locked.
-40-
11. Detector
GC-9A/9AM can be attached maximum 4 kinds of detectors simultaneously. (More than 2 of FID
dual, TCD and PID each can not be attached simultaneously.)
11.1 Signals of detector
Signals of each detector are generated by special connector from each detector control.
Analoguerecorder
(R-lll)la)
(b)
When detector is connected to analogue recorder
Detector unit of GC-9A/9AM does not have attenuator and fine adjustment knob for zero
point adjustment. Since option includes the unit with these functions, connect to analogue
recorder through this unit of they are needed. (Fig. (a))
When detector is connected to unit corresponding to C-R2A
When signals from GC-9A/9AM detector is connected to C-R2A, (INP-R2A), or C-R3A,
connect directly because attenuator and zero point adjusting knob are unnecessary.
11.2 When the kind of the attached detector is to be known
GC-9A/9AM can be attached with maximum 4 kinds of detectors. When the conditions of
these detectors are set, it is necessary to select detector with detector numbers 1 to 4. It is possible
to monitor what kinds of detector are attached to detector numbers 1 to 4. For example if
- 4 1 -
you want to know what is attached to detector number 1 depress the keys as follows:
iMONIl | PET | [T] lENTl
if FID is attached, FID is indicated on display. However, if ON/OFF switch of detector
unit corresponding to detector number 1 is turned OFF, NON is displayed. Do not forget to
turn ON this switch.
11.3 TCD
(1) Composition
Thermal Conductivity Detector is composed of the following parts.
Name
TCD constant-temperature bath assembly
Detector
TCD control
TCD parts
Accessories
Stainless column adaptorGlass column jointGraphite ferrule (10 in a pouch)
\2) Specification
Detector : Tungsten (Rheniun
Part number
221-23547-91
201-40034
221-23821-91
221-11386-91
P/N
221-10079-91221-10078-91221-10076-91
I) filament UOOfl
Quantity
1
1
1
1
Quantity
2
2
1
, in room ten
Maximum temperature
Power source
Current
Polarity switch
Zero adjustment
Sensitivity
Differential type of half-diffusion flowing path by 4 element
composition
399°C
Constant-current control method
0 ~ 200mA (1mA step)
(In case of He carrier gas, when polarity is 1, peak of injection
to column 1 appears in positive)
Accurate and rough; one each
with filament protective circuit
About 7000mV'm£/mg (different depending on sample and
condition)
-42-
(3) Application
This detector does not have very high sensitivity, but is applicable to all samples.
This is especially effective for gas analysis.
(4) Theory
When the metal filament heated by current is set in the carrier gas with large heat con-
ductivity such as helium, heat conductivity of sample element is smaller than that of carrier
gas so that the filament temperature will rises as the element passes through. Chromato-
gram can be obtained by measuring charge of filament resistance caused by the temperature
rising.
(5) Setting of flowing quantity of carrier gas
Helium, nitrogen, argon and hydrogen
can be used as carrier gas. Helium with
large heat conductivity is most suitable.
Note: Since use of hydrogen as carrier
gas has danger of explosion, strict
attention should be paid.
Carrier gas shall flow equally in both
flowing paths. Suitable flowing quantity
for column with inner diameter of 3mm
is about 50m£/min. (40~60m£/min.)
(6) Sensitivity property
Sensitivity of detector is changed in proportion to supplied current cubed. In order to
obtain the big peak, manipulate ATTENTION of the plotter*. If the sensitivity is insufficient,
increase current value within the range illustrated in the figure.
When large current is flown to detector, filament temperature rises, causing service life of
filament shortened and noise and drift generated.
* Do not revise setting of current value during the analysis. It requires some period to make
detector stabilized.
11.4 TCD controller
(1) Temperature setting
For temperature setting of TCD oven, depress the |TCD| key on key board, key-input the
setting temperature and finally depress the lENTl key. Since the maximum used temper-
ature is fixed to 399°C, more than that temperature can not be set. Set the temperature to
approx. 20~50°C higher than the column oven temperature (or final temperature in case of
-43-
temperature program).
(2) Temperature control
Temperature control of TCD oven can be obtained temperature stability within setting
value ±0.01°C by microcomputer-optimized control. If the temperature becomes higher
than 450°C due to some abnormality, power supply to heater of TCD oven is suspended.
At that time display shows OVER TCD.
(3) Current setting
Setting of current value flown in TCD filament is carried out at key board. Since TCD is
usually fixed to DET number 4, depress the
keys as follows:
(T) Carrier gas@ Carrier gas(3) Carrier gas
Carrier gas
(In this case, 100mA is set.)
The value possible to set is between 0mA
and 200mA in the step of 1mA. However,
the maximum current value possible to
supply to TCD filament be related to the
kinds of carrier gas and the temperature
setting of TCD oven as shown in the figure.
(4) Polarity
When sample is injected to injection port 1, input 1 1 [ when its signal is recorded to positive
direction and input | 2 [ when its signal is recorded to negative direction in the following
procedure.
HeH2
N2
Ar
200 300 400TCD TEMP °C
PET
PET
FENT
ENT
POL 1 [I
POL 1 [2]
ENT
ENT
(5) Zero point adjustment
In order to adjust the zero point on base line, turn 2 knobs on TCD control panel.
(6) Detector ON/OFF
When TCD is not used, turn OFF this switch.
When this switch is turned off, current is not supplied to TCD filament.
When detector ON/OFF switch of TCD is turned ON after power is supplied to GC, some-
time display lamp of current OVER is lit. In this case, do not forget to input current value
once again from the key board.
- 4 4 -
11.5 Protection circuit of TCD filament
When large amount of air enters in TCD at the time of replacement a septum of column
injection port or gas cylinder, control circuit is operated to prevent damage of filament during
the use of TCD. In this case, OVER TCD is indicated on display and OVER lamp on TCD
panel is lit. After confirming that carrier gas is flowing to detector normally by connecting
a flow meter to VENT of TCD, key-input the current value once again like lCE[ [PET! (~4]
1 CURRl [T][0][0] |ENT| . When the CURRENT OVER lamp is still lit as the result of key
input, key-input the lower setting value of current once again.
Note: When CURRENT OVER lamp of TCD is lit
Since current value is automatically set to OmA, it is necessary to set once again.
When the JCEJ key is depressed, TCD OVER display disappears. However by
these key operation alone, resetting of current vaule is not carried out. So set
the suitable current value once more.
11.6 TCD VENT
Carrier gas passing through TCD comes out here. Before CURRENT is supplied to filament,
confirm surely that carrier gas is flowing here.
if dangerous H2 is used as carrier gas, release it to inside of draft or outdoor by attaching
pipe to VENT.
11.7 Cautions
1) When stainless column is used, use TCD S.S column adaptor (TCD parts) at the column
exit. In the case of glass column, use the sleeve (TCD side).
2) Current flowing to detector should be surely lower than the value mentioned before.
3) Select the site free from draft, direct sunlight and a little temperature change as the environ-
mental conditions. Vibration of device may cause noise.
4) When carrier gas is stopped even temporarily for replacement of column or septum of
injection port, set the current to OmA surely.
5) When the kind of carrier gas is changed or after the operation 4), supply CURRENT, after
sufficient gas replacement.
- 4 5 -
11.8 Hydrogen flame ionization detector (FID)
(1) Composition
Hydrogen flame ionization detector is composed of the following parts.
Name
Detector
Igniter
FID flow controller
FID control
Part number
221-21905-92
221-22986-91
221-22984-91
221-23820-91
Quantity
2
1
1
1
(2) Specification
Collector electrode:
Applied voltage on electrode
Minimum detectable level
Dinamic range
Maximum temperature
Igniter
Nozzle
Cylindrical shape
+200V
3 X 10~12g/sec (sample:
More than 107
400°C
Filament for both flowing paths
Made of quartz
Dual operation is possible by attaching another FID control.
Wide-diameter nozzle can be attached for sample of high density.
Specification of electrometer
Maximum sensitivity : 1 X 10" 12A (full scale)
Noise : Less than 1% in maximum sensitivity
Drift : Less than 2% hr in maximum sensitivity
(Room temperature: constant)
Range : 1, 10, 102, 103, 104
Background compensation : ±8 XI0"10A (NORM position)
Independent of range,
Linearity : More than 105 (in case of no switch of input attenuator)
Output : RECORDER 0~lmV
INTEGRATOR O~1V
(3) Application
This detector has sensitivity only for organic compound but most general, having excellent
properties such as high sensitivity, wide dynamic range and hardly affected by the temperature
and impurity in carrier gas.
- 4 6 -
(4) Theory
When organic compound is burned in hydrogen flame, ion is generated in flame.
Chromatogram can be obtained by collecting ions with direct voltage-applied electrode and
measuring the ion current with electrometer.
(5) Setting of flowing amount of hydrogen and air sensitivity of detector changes in accordance
with the mixture ratio of carrier gas (nitrogen), hydrogen and air. There is the most suitable
mixture ratio for maximum sensitivity.
1.5-
5 i-o-l
0.5-
1.5-
N2 60ml/min
Air 500ml/min
• H2 50ml/min
N2 60ml/min
500 10000 20 30 40 50 60 70 80 90 100 0 200
—* Flowing amount of H2 (mfi/min) —* Flowing amount of air (mfi/min)Ratio comparison of hydrogen and Flowing amount of air and sensitivitysensitivity
In case of column with inner diameter of 3mm, usually set as follows:
Carrier gas (nitrogen) 60m£/min (40 ~ 60m£/min)
Hydrogen* 50m£/min (30 ~ 60mC/min)
Air 500m£/min (400 ~ 600mfi/min)
* Do not raise the hydrogen pressure higher than 1 kg/cm2.
Flowing amount control of hydrogen and air adopts pressure adjusting method. Use the
calibration curves of pressure-flowing amount shown below which is included in FID parts.
I &100H*>2
On Oml/min
50-
1000-
0 0.5 1.0 0.25 0.5—*- Pressure (kg/cm2 G) —» Pressure kg/cm2 G)
(Indication value of manometer) (Indication value of manometer)Relation of hydrogen pressure and flowing amount Relation of air pressure and flowing amount
-47-
The above figure is the typical example. In strict term, there is a little difference
depending on instrument.
11.9 FID controller
(1) Setting of range (RANGE)
Sensitivity switchover of electrometer is carriered out from key board. Peak is expanded
by 10 multiplied step. Sensitivity becomes lower in the order of 1 -• 10 -> 102 -> 103 -• 104.
Setting from key board inputs numerical value of index section. For example, when FID is
connected DET number 1 and range is set to 10, depress the keys as follows:
iDETinn^ENT^ [RNGimfENTi
If range is set to 1, 0 is key-input. Once detector number is set, FID of DET x is selected
until setting is revised. Therefore, when range and polarity are revised, do not operate as
lDET| [F] [ENTl but depress the keys of iRNGl [3] |ENT| directly. Then range of FID is
changed to 103. Content which is now set is displayed on detector control panel. When
display is required on key board display, setting value is displayed by depressing the keys
IRNGl and |ENT[ .
(2) Setting of polarity
Switchover of polarity is also input from key board. When 1 is input, signal terminal
outputs as signals from column 1 becomes positive and when 2 is input, signal terminal
outputs as signals from column 2 becomes positive.
On setting polarity, for example when [PETI |~T] lENTl (these are unnecessary operation
when DETj has already been selected). [POLI [T1 iNETl are depressed and key-input,
signal output appears as the signals of column 1 becomes positive. Setting value is dis-
played on lamp of FID control panel. When©lamp is lit, signals of column 1 becomes
-48-
positive. When setting content is to be displayed on key board display, operate the keys
in the following order.
I POL] fENTl
(3) Backing mode switchover
Backing mode switchover is installed on print board of FID controller. When background
value of FID is too large to carry out zero point adjustment by turning the zero point adjust-
ment knob on panel.
(4) Measurement of flowing amount
Carry out when accurate flowing amount is to be known. Carry out when whole GC
device is sufficiently cooled before starting.
Carrier gas
1) Stop hydrogen by stop valve.
2) Stop air with adjusting knob of air flowing amount.
3) Remove sealed cap on detector's top.
4) Remove collector's top and measure with flow-meter.
Hydrogen
1) Stop carrier gas by stop valve.
2) Stop air with adjusting knob of air flowing amount.
3) Measure the flowing amount in the same method as the carrier gas.
Air
1) Stop carrier gas by stop valve.
2) Stop hydrogen by stop valve.
3) Measure the flowing amount in the same method as the carrier gas and hydrogen.
(5) Ignition
On igniting the detector, decrease air flowing amount to the degree where pressure gauge
indicates 0.1 ~ 0.2kg/cm2 after hydrogen pressure is set to 0.9kg/cm2. Then, turn around
ignition lever to each detector's top and hold for 2 ~ 3 seconds. Filament will be illuminated
and light ignition sound "pop!" can be heard. After ignition, the air flowing amount is
restored to the regular value (usually pressure gauge indicates about 0.5kg/cm2) and hydrogen
flowing amount is also restored to the regular value (pressure gauge indicates about 0.6kg/cm2).
Ignition of detector should be surely confirmed by checking whether the mirror approached
to the detector's top is moistured with water drops.
Note: Since ignition lever does not return to the original position automatically, put it back
to the center position by manually. On ignition, set the hole on the side of FID cap
- 4 9 -
the direction of ignition lever. If not, ignition is not carried out smoothly.
(6) Cleaning of FID cell
FID cell may be contaminated with solvent, sample and column liquid phase.
Contamination can be removed by flowing a little more air or raising temperature of INJ
(and detector) section.
By combustion of silicone steam derived from liquid phase, white powder attaches to
collector surface, causing sensitivity lowering and noise. In this case, it is necessary to clean
FID collector in the following precedure.
1) Remove sealed cap (lj .
2) In the state of signal cable (2) attached, hold external cylinder f 3J and pull it up while
revolving. Then cylinder (~3) can be removed together with collector (4).
-50-
3) After cleaning collector (4j and insulator (jf) with solvent and rubbing off the white
powder attached to collector with sand paper, assemble it as original.
(7) Caution
1) When FID is used in single column, set hydrogen pressure of unused flowing path to
zero and stop firmly by setting blind stopper (standard attachment of main body) to
detector entrance. Column exchange shall also be carried out after stopping firmly with
hydrogen stop valve. Otherwise, hydrogen may enter the column bath and there is danger
of explosion.
2) Inorder to prevent contamination of detector, detector temperature shall be set to 20
to 50°C higher than the column bath temperature (the final temperature in case of
program).
3) When stainless column is used, use FID S.S column adaptor (FID attachment) in
detector entrance.
4) High voltage electrode and nozzle should contact firmly.
- 5 1 -
12. Temperature Control of AUX!, AUX2 and DET
These can be connected to GC-9A/9AM main body as option and controlled. Refer to the
attached instruction manual on attached devices for their connecting method and setting.
-52-
221-20574D
GC-9A/GC-9AM
GAS CHROMATOGRAPH
INSTRUCTION MANUAL
VOLUME D: PROGRAMMING
SHIMADZU CORPORATION
ANALYTICAL INSTRUMENTS PLANT
KYOTO. JAPAN
TOKYO OFFICEP.O.BOX No.209, 40th Floor Shinjuku Mitsui Bldg.,No. 1-1, Nishi-Shin|uku 2-Chome, Shinjuku-ku, Tokyo 160, JapanCable Add.lSHIMADZU TOKYO
SHIMADZU CORPORATION OverseasTelex No-:0232~3291 (SHMDTJ)
KYOTO OFFICE1, Nishinokyo-Kuwabaracho, Nakagyo-ku, Kyoto604, Japan.Cable Add.:SHIMADZU KYOTOOverseas Telex No.:05422-166 (SHMDS J)
3500-10400-500TD-
Contents
Page
START
Operation (II)
1. Description of Keys
1-1
1-2
1-3
1-4
1-5 [ TCD/DET. T
1-6 " '
COL/AUX. 1
INj/AUX. 2
I. TEMP
1-7
1-8
I. TIME
P. RATE]
1-9 1 F. TEMP |
1-10 1 F. TIME |
1-11 |DET| ..,
1-12
1-13
RANG
1-14 CURR
1-15
1-16
1-17
1-18
1-19
1-20
1-21
1-22
1-23
1-24
1-25
1-26
1-27
1-28
1-29
1-30
FILE/FUNC]
FLOW/FLOW. M
STOP-W/RET. T
HOLD/HOLD. T
9/S. NO
8/EVNT
7/PRG~
6/COPY
5/RETRN)
4/DEL
3/SLEEP. T ...
2/STOP. T
I/START. T ...
0/LOCK
•/SCAN
-/ESCAPE
Page
9
9
9
1-34 [ENTl 9
2. Setting of Temperature
2-1 Description 10
2-2 Temperature setting method 11
2-3 To learn the set temperature 14
2-4 Procedure for making up the temperature program 15
2-5 To learn the set program 28
2-6 To alter part of the program 31
2-7 Setting maximum temperature 32
3. Detector
3-1 Introduction 34
3-2 Setting of detector 34
3-3 To learn the set detector 34
3-4 RANGE, POLARITY, CURRENT 35
4. Starting and Ending Temperature Control
4-1 Description 37
4-2 Starting and ending of temperature control 37
4-3 Function of timer 37
4-4 Monitoring of sleep time 40
5. Analysis
5-1 Description 42
5-2 Starting of analysis 42
5-3 Operation during measurement 44
6. Time Program
6-1 Description 51
Page
6-2 Items that can be programmed 51
6-3 Procedure for making up the time program 52
6-4 To see the time program 54
6-5 Alteration of the time program 54
6-6 When the time program is beyond capacity of memory 55
6-7 Starting and ending of the time program 55
7. Files
7-1 Description 56
7-2 Setting files 56
7-3 To know the current file number 57
7-4 Copy 57
7-5 Cancellation of files 57
7-6 When there is insufficient storage area for file extention 58
8. Other Operations
8-1 Lock 59
8-2 Stopwatch 59
8-3 Self-diagnostic function 60
8-4 List 61
9. Option
9-1 Measurement of flow rate 64
9-2 Auto sampler 67
9-3 Connection with exterior data processor 71
Appendix 1 Error Display 74
Appendix 2 Incorrect Keystroke 77
A. When keys are pressed incorrectly 77
B. Effective digit of a numerical value 78
C. Misoperation during Dialogue 79
Operation - Procedure -
This manual is intended to explain operating procedures, section by section, classified according
to the purpose of use of Gas Chromatograph GC-9A/9AM. Each procedure is described so than it
can be understood by refering to the appropriate section alone without reference to others. There-
fore, similar description is repeated at times.
- 1 -
1. Description of Keys
1-1 [START] : START KEY
1.1 Starting temperature control
By depressing this key before starting temperature control, six zone including the column
oven, injector, detector, TCD, AUX1 and AUX2 start to be heated and their temperatures are
controlled to their preset values.
1.2 Starting measurement
By depressing this key during temperature control, the execution of the temperature pro-
gram and counting of retention time begin.
1.3 Starting auto sampler
When temperature is controlled and the auto sampler is connected, depressing this key
starts the auto sampler.
1.4 Cancellation of hold
In the hold state, depressing the
1.5 Start with shift down mode
HOLDHOLD. T
key or 1 START 1 key cancels the hold.
When temperature is not controlled, depressing keys [SHIFT. D[ and |START| in this
order starts temperature control after elapes of the preset start time.
1-2 [STOP] : STOP KEY
1.2 Completion of analysis
During analysis, depressing this key completes counting of retention time and stops the
execution of the temperature program. Temperature returns to the initial preset value re-
covering the READY state. The auto sampler stops its sample injection operation.
2.2 Stop with shift down mode
During temperature control, by operating keys in the sequence [SHIFT. D[ [STOP| ,
the temperature control is stopped after the elapse of the preset stop time on completion of
program execution. After preset sleep time has passed, temperature control is restarted.
1-3 COLAUX.l COLUMN, AUX1 KEY
This is for selecting either the column oven or satellite oven. Operating COLAUX.l selects the
column oven ; operation [SHIFT.DJand COLAUX.l
in that order selects satellite oven.
(However, this key operation has no meaning by itself. After the key operation, enter the
preset value and depress the |ENT[ key, or depress only the [ENT] key.)
When making up temperature program for the column oven or satellite oven, depressing
- 2 -
this key first starts the setting temperature from programmer step 1.
When monitoring temperatures in the column and the satellite oven, operate |MONI| COLAUX.l
or MONI SHIFT.DCOL
AUX.1 , in that order.
1-4 INJAUX.2 : INJECTOR, AUX2 KEY
This is for selecting either the injector temperature or the temperature of sub-oven
Operating I N JAUX.2
or | SHIFT.D | I N JAUX.2
selects the injector or the sub-oven
respectively.
For setting their temperatures, operate the keys in the following sequence.
INJAUX.2 2 0 0 ENT or SHIFT.D INJ
AUX.2 5 0 ENT .
For monitoring their temperatures, their present temperatures can be displayed by operating
keys in the sequence | MONI I N JAUX.2
or 1 MONI | 1 SHIFT.D r INJ1 AUX.2
1-5TCD
DET: TCD, DETECTOR KEY
This is for selecting either the TCD temperature or the detector temperature ; operating
TCD
DET or SHIFT. DTCD
DETin that order selects the TCD or the detector, respectively.
Operations for setting and monitoring are the same as for the INJAUX.2
key.
1-6 I. TEMP : INITIAL TEMP KEY
This is for setting the initial temperatures of the column oven and satellite oven 1.
For setting the temperatures, operate keys in the sequence COLAUX.l I. TEMP 0 0
ENT or SHIFT.DCOL
AUX.l I. TEMP 1 0 0 ENT . if either the column oven
or the AUX1 is already selected, operate |l . TEMPI \l\ \0\ \0\ |ENT[ , in that order. If
the preset value should be displayed, operate keys in the sequence COLAUX.l I. TEMP ENT
or [SHIFT. D COLAUX.l I. TEMP lENTl . If either the column oven or AUX1 has been
selected, the preset initial temperature is displayed by operating [ I. TEMP |ENTJ , in that
order.
1-7 I. TIME : INITIAL TIME KEY
This is for setting the time of retaining initial temperature for the column oven and AUX 1.
The operating procedure is the same as for the I. TEMP] key.
- 3 -
1-8 P. RATE PROGRAM RATE KEY
This is for setting the temperature program rate. Temperature program rates of the column
oven and AUX1 are set in five steps.
By operating keys [P. RATE| [T| Q ] D[] lENTl , in that order, 5.5 °C/min. is set as the
temperature program rate of the step subsequent to the rate stored. To set the temperature
program rate from the first step, operate keys in the sequence COLAUX.l (or [SHIFT. D
COLAUX.l P. RATE] [5] E] [T Note that this operation leads settings of
other final temperatures of program steps and time of retaining final temperature to the
first step of the temperature program. With this key, unlike FINAL TEMP KEY and FINAL
TIME KEY, by setting a certain step of temperature program rate, the setting automatically
returns to "0" at the subsequent step ; i.e., the preset temperature program enters its final step.
(When "0" is input in the rate, the temperature program is considered to be completed regardless
of the other settings.) Therefore, be careful when changing part of the settings.
When desiring to see the preset program rate, operate keys in the sequence COLAUX.l
P. RATEj^NTi or 1 SHIFT. D| COLAUX.l
P. RATE] |ENT| , and program rate of the first step
is displayed. Each time the [ENT| key is depressed, the second, third steps and so on, are
displayed in sequence.
1-9 IF. TEMPI : FINAL TEMP KEY
For setting the final temperatures of each program steps. The final temperatures in the
column oven and AUX1 can be set within five steps. Operating procedure is the same as for the
PROGRAM RATE KEY.
1-10 | F. TIME) : FINAL TIME KEY
For setting the time of retaining final temperatures. The time of retaining final temperature
of the column oven and the AUX1 can be set within five steps.
Operating procedure is the same as for the PROGRAM RATE KEY.
1-11 | PET | : DETECTOR KEY
For selecting detector.
Four kinds of detectors can be connected simultaneously. (DET1 ~ DET4) Detector 1 is
selected by operating keys in the sequence |DET| [Y\ |ENT| . When the detector number
presently selected is desired, the number is displayed by operating the keys |DET| JENT| , in
that order.
When the type of detector corresponding to the number is desired, operate keys in the
sequence |MONI| |DET| [Y\ |ENT| ; the type is then displayed.
-A-
1-12
For setting the range of a detector. The range of the detector presently selected is set from
0 ^ 4 . Proceed as follows : | RANG] [ 3 | |ENT| . When the range set presently is desired
the range is displayed by operating keys in the sequence of 1 RANG | |ENT|
1-13 IPOLl : POLARITY KEY
For setting the polarity of a detector. Operation is the same as for the 1 RANG | key.
1-14 ICURRl : CURRENT KEY
1-15
For setting the current of a detector. Operation is the same as for the | RANG key.
: FILE, FUNCTION KEYFILEFUNC
For setting a file and dialogue with the auxiliary function.
15.1 Files
File 5 is set by operating the keysFILEFUNC
[ | ] [ENTl , in that order. If file 5 exists,
the file is read ; otherwise, a new area of the file is secured.
To know the file set presently, operate keys in the sequence | MONlJ
I 1
F I L E - [ENTl •[FUNCJ
FILEFUNC or
15.2 Dialogue with FUNC key
Operating keys in the sequence [SHIFT. D
FUNC.
Content of FUNC key
FILEFUNC
ENT[ begins dialogue with
1
13
14
15
Setting of AOC parameter beginning from STRK.
Listing of TIME PROGRAM.
Listing of AOC parameter.
Listing of GC parameter.
Setting of maximum temperature of detector.
Setting of maximum temperature in AUX1.
Setting of maximum temperature in column oven.
Setting of link device.
Self-diagnostic function.
Setting of value "K" of flow-measurement
Listing of temperature program.
1-16 FLOWFLOW. M FLOW, FLOW MEASURE KEY
For setting and measurement of flow. Flows of carrier gas 1 and 2, hydrogen 1 and 2 and
air are set.
- 5 -
FLOW 1 : Carrier gas 1
FLOW 2 : Carrier gas 2
FLOW 3 : Hydrogen 1
FLOW 4 : Hydrogen 2
FLOW 5 : Air
Operating keys in the sequence
to be set on FLOW1.
To learn the setting, operate keys in the sequence
FLOW1 is then displayed.
In measuring FLOW 1, set FLOW 1 by operating keys in the sequence
FLOWFLOW.M
ENTl [41 \0\ lENTi Causes 40.0 mtymin
FLOWFLOW.M
I ENTl ; the set value of
FLOWFLOW.M
ENTl ; then operate the keys 1 SHIFT. D FLOWFLOW.M
, in that order. Measurement is started
and taken four times successively. (See the section "Option")
To cancel the measurement, operate keys again in the sequence | SHIFT. D FLOWFLOW.M
The final measurement value is stored as the actual flow value.
To learn the measurement value, operating keys in the sequence of 1MONI1
[ENTl causes the actual value of the FLOW1 to be displayed.
FLOWFLOW.M
1-17STOP-W
RET. T: STOP WATCH, RETENTION TIME KEY
For monitoring function of stop watch and count of retention time.
On depressing theSTOP-W
RET. Tunit : second).
If theSTOP-W
RET. Tcey is dep
key, display starts to count the time to one decimal place
key is depressed again, the count at the time is displayed and stops.
During counting, other operations can be performed, while only the display continues to
count the time.
The [CEl key can not erase the display.
To learn the retention time during analysis, operate keys in the sequence | MONI |
SHIFT. DSTOP-WRET. T
; the retention time is displayed.
1-18HOLD
HOLD. T
By depressing the
HOLD, HOLD TEMP KEY
key during analysis, the count of the retention time stopsHOLD
HOLD. T
and the temperature remains constant until the HOLD is cancelled, if the temperature is not
rising. If the temperature rises, the temperature continues to rise and remains constant after the
- 6 -
final temperature is reached. This key operates either column oven or Aux 1 which is selected.
By operating keys [SHIFT. DHOLD
HOLD. TJ j [ 0 I |ENT| , in that order, during
analysis, the temperature at the time the |ENT| key is depressed is held for 10 minutes (even
during the temperature elevating). The count of the retention time continues.
1-19 S.NO : SAMPLE NUMBER KEY, (9)
The value "9" is set.
By operating keys in the sequence 1 SHIFT. DS.NO
T] Ho] [ENTl , the sample
number of the auto sampler changes by ones till it reaches 10. When the current sample
number is bigger than 10, it is ignored.
1-20EVNT
: EVENT KEY (8)
The value "8" is set.
Operating keys in the sequence | SHIFT. D
EVNT
EVNTT] [ENT] and | SHIFTTD]
l j [ENTI causes EVENT 1 to be set ON and OFF, respectively.
0] | ENTl , in that
order; they are turned OFF by operating keys | SHIFT. D| [ - 1 1 0 [ , in that order.
All EVENTs are reversed by operating keys) SHIFT. ,DEVNT
1-217
PRG: PROGRAM KEY, (7)
The value "7" is set.
Operating keys in the sequence SHIFT. DPRG
actuates the dialogue mode to
generate the TIME PROGRAM. To escape from the mode, operate keys in the seuqence
SHIFT. D
1-22COPY
ESCAPE
: COPY KEY, (6)
The value "6" is set.
By operating keys in the sequence SHIFT. D
of the file is copied to file No. 3.COPY
, the current contents
1-23RETRN
: RETURN KEY, (5) The value U 5 " is set.
By operating keys in the sequence SHIFT. DRETRN
T] [][] fENT] , the repeated
number (3 times) of the time program and the subsequent file to be executed (5) are set.
- 7 -
1-24DEL
: DELETE KEY (4)
The value "4" is set.
By operating keys in the sequence | SHIFT. D
1-25
DEL
SLEEP. T
T ] lENT[ , file No. 3 is cleared.
: SLEEP TIME KEY, (3)
The value "3" is set.
By operating keys in the sequence | SHIFT. DSLEEP. T
6] KM [0] |ENT| , ten
hours is set for sleep time. (Unit: minj
Operating the keys [SHIFT. D
stored to be displayed.SLEEP. T
[ENT | in this order causes the sleep time
Counts of sleep time and stop time are displayed by operating 1 MONI | 1 SHIFT. D
in the sleep and wait modes, respectively.SLEEP. T
1-26STOP. T
: STOP TIME KEY, (2)
The value "2" is set.
By operating keys in the sequence | SHIFT. DSTOP.T
hours is set for stop time. (Unit: min.)
Operating keys in.the sequence SHIFT. DSTOP. T
~0] [ENTl , three
! ENT I causes the set value of the
1-27
stop time to be displayed.
: START TIME KEY, (1)START. T
The value " 1 " is set.
By operating keys in the sequence | SHIFT. D
hours is set for start time. (Unit: min.)START. T
T\ [ENT|, 8
Operating keys [SHIFT. DSTART. T
1-28
start time to be displayed.
: LOCK KEY, (0)
I ENT | , in that order, causes the set value of the
0
LOCK
The value "0" is set.
By operating keys in the sequence SHIFT. DLOCK
, all keys other than [SHIFT. D
START STOP andLOCK
keys are locked. To cancel the lock, operate keys in
the sequence [SHIFT. D0
LOCK
1-29SCAN
: SCAN KEY, ( • )
A decimal point is set.
By operating keys in the sequence [ SHIFT. DSCAN
, the current temperatures of
the column oven, satellite oven, AUX1 or sub-oven, AUX2, injector, detector and TCD are
displayed cyclically.
1-30ESCAPE
ESCAPE KEY
Operating keys in the sequence | SHIFT. DESCAPE
leads to escape from the dialogue
mode. (The DIALOG lamp is turned off.)
1-31 [CE] : CLEAR ENTRY KEY
Displays are cleared. And when "OVER" is occurred, it's state is cleared.
1-32 [MONll : MONITOR KEY
Press this key when all present values of all sorts are desired to be displayed.
SHIFT DOWN KEY1-33 SHIFT. D
Shift down the key. Shift down is cancelled by depressing once when it has already been
depressed (when the SHIFT. D lamp is lit).
1-34 |ENTl : ENTER KEY
Input values are entered as set values by depressing the | ENT[ key.
- 9 -
2. Setting of Temperature
Item
2-1
2-2
2-3
2-4
2-5
2-6
2-7
Description
Temperature Setting Method
(I) Column oven
(2) Injector
(3) TCD
© AUXl
(5) AUX2
(6) Detector
To learn the set temperature
Procedure for making up the temperature program
(T) Column oven
(2) AUXl
(3) General caution
To learn the set program
To alter part of the program.
Setting the maximum temperature
2-1 Description
The GC-9A/9AM is capable of controlling temperatures at 6 zone in total, and especially in the
cases of the column oven and satellite oven AUXl, the temperature program can be made up.
This paragraph contains the temperature setting method and the procedure for making up the
program.
- 1 0 -
2-2 Temperature setting method
(T) Column oven
Setting method
For example, when the column temperature is to be set to 300°C.
Operation Display
COLAUX. 1
INJT 200 Display content remains intact. In this case, theinjector temperature is displayed.
1. TEMPI
30
300
CITP 300 The input value is not entered without depressing the[ENTi key.
To set a minus temperature, operate keys, for example, much as " | - [ | 5 | [~0~| ".
Injector
Effective range of injector temperature : 0 to 399°C.
(As initial value, 200°C is set.)
(1) Setting method
To set the injector temperature to 350°C.
1
2
3
4
5
Operation
INJAUX. 2
aEJ
[ENTi
Display
CITP 300
3
35
350
INJT 350
Display content remains intact. In this case, theinitial temperature of the column oven is displayed.
The injector tempeature is now set to 350 C.
TCD
Effective range of the TCD temperature : 0 to 399°C (initial value 30°C).
Setting method
- 1 1 -
To set the TCD temperature to 100°C.
Operation Display
TCDDET.T
INJT 200 Display content remains intact. In this case, the injectortemperature is displayed.
10
100
TCDT 100 TCD temperature is set to 100°C.
© AUX1
The GC-9A/9AM is capable of controlling temperature in addition to those of the column
oven, detector, injector and TCD at two places maximum. (AUX1,AUX2). For AUX1, the
temperature program can be made up, as in the column oven temperature.
Effective range of the AUX1 temperature -99°C to 399°C*
Initial value 100°C
Setting method
To set the AUX1 temperature to 150°C.
Operation Display
[SHIFT. D| CITP 200 Display content remains intact. In this case, the initialtemperature of the column oven is displayed. By de-pressing the [SHIFT. D| key, the SHIFT. Dlamp isturned on.
"CUT7AUX. 1 CITP 200 The SHIFT. D lamp is turned off.
I. TEMP CITP 200
15
150
AITP 150 AUX1 temperature (initial temperature) is set to 150°C.
* Note: Cryogenic attachment cannot be used with auxiliary oven, so that the practical
range of the temperature is room temp, to 399°C.
- 1 2 -
AUX2
AUX2 can be adjusted to a constant temperature, but the temperature cannot be programmed.
AUX2 Effective range of temperature 0 to 399°C
Initial value 200 C
Setting method
To set 150°C as the AUX2 temperature.
1
2
3
4
5
6
Operation
SHIFT. D I
INJAUX.2
ms
[ENT|
Display
INJT 200
1
15
150
AUXT 150
Display content remains intact. In this case, theinjector temperature is displayed. The SHIFT. D lampis turned on.
The SHIFT. D lamp is turned off.
AUX2 temperature is now set to 150 C.
Detector
Effective range of the detector temperature 0 to 399°C.
Initial value 200°C
Setting method
To set the detector temperature to 150°C.
Operation Display
[SHIFT. D| INJT 200 Display content remains intact. In this case, the injectortemperature is displayed. The SHIFT. D lamp is turnedon.
The SHIFT. D lamp is turned off.
15
150
DETT 150 The detector temperature is now set to 150 C.
-13-
2-3 To learn the set temperature
To learn the temperature which is set at the time, the set temperature is displayed by operating
as follows. (Listing is another method.)
CD Column oven
1
2
3
Operation
COLAUX. 1
11. TEMPI
lENTl
Display
INJT 200
CITP 300
Display content remains intact. In this case, the injectortemperature is displayed.
The set value of the temperature in the column oven isdisplayed. In this case, the temperature is 300 C.
Injector
Operation Display
iAUX.2CITP 300 Display content remains intact. In this case, the column
oven temperature is displayed.
INJT 200 The set value of the injector temperature is displayed.In this case, 200°C.
TCD
1
2
Operation
TCDDET. T
[ENTl
Display
INJT 200
TCDT 30
Display content remains intact. In this case, the injectortemperature is displayed.
The set value of the TCD temperature is displayed.In this case, 30 C.
AUX1
1
2
3
4
Operation
| SHIFT. Dl
COLAUX. 1
I. TEMP|
|ENTl
Display
TCDT 30
AITP 150
Display content remains intact. In this case, the TCDtemperature is displayed. The SHIFT. D lamp is turned on.
The SHIFT.D. lamp is turned off.
The set value of the AUX1 temperature is displayed.In this case, 150°C.
- 1 4 -
AUX2
1
2
3
Operation
SHIFT. D
INJAUX.2
|ENT|
Dis Display
AITP 150
AUXT 250
Display content remains intact. In this case, the tem-perature of the AUX1 is displayed.
The set value of the AUX1 temperature is displayed.In this case, 250°C.
Detector
1.
2.
3.
Operation
| SHIFT. D
TCDDET.T
[ENT|
Display
AUXT 250
DETT 200
Display content remains intact. In this case, the tem-perature of AUX2 is displayed.
The set value of the detector temperature is displayed.In this case, 200°C.
2-4 Procedure for making up the temperature program
The GC-9A/9AM is capable of making up temperature programs which can elevate temperatures
in the column oven and AUX1 in five steps.
Final Temperature 5
Final Temperature 1
a
Program rate 1
STARTInitialtemperature
Time ofretaininginitialtemperature
Final Temperature 2* Time of
Final Temperature 4
Final Temperature 3Time of retain-ining final tem-̂
Time ofretainingfinal tem-
retainingfinal tem-
perature 2
Time ofretainingfinal tem-erature Program rate
Time
- 1 5 -
(T) Column oven
(1) Setting the initial temperature
The initial temperature is the value which was set in paragraph 2-2 of this section
(Column oven).
(2) Setting time of retaining initial temperature
Time of retaining initial temperature (time from START till the first temperature
program begins).
Effective range 0 to 655 min
Initial value 0.0 min
Setting method
To set the time of retaining initial temperature of column oven to 20 minutes.
1
2
3
4
Operation
COLAUX. 1
I. TIME
[o]
|ENT|
Display
CITP 100
2
20
CITM 20.0
Display content remains intact. In this case, the initialtemperature of the column oven is displayed.
The time of retaining initial temperature of the columnoven is now set to 20 minutes.
(3) Setting of the temperature program rate
The temperature program rate is set to each program step.
Effective range 0 to 40.0°C/min
Initial values 0.0°C/min
Setting method
Ex.) Column temperature program rate 1 .
2.
3.
4.
5.
5 C/min
20°C/min
5°C/min
10°C/min
20 C/min
- 1 6 -
Operation
COLAUX. 1
P. RATE
Display
CITM 20.5 Display content remains intact. In this case, the time ofretaining initial temperature of the column oven is dis-played.
CPR1 5.0 Program rate 1 of the column oven is now set to 5.0C/min.
20
CPR2 20.0 Program rate 2 of the column oven is now set to 20.0C/min.
CPR3 5.0 Program rate 3 of the column oven is set to 5.0 C/min,
10
10 CPR4 10.0 Program rate 4 of the column oven is now set to 10.0C/min.
11
20
12 CPR5 20.0 Program rate 5 of the column oven is now set to 20.0C/min.
Note : Even if a numerical value is input and the |ENT| key pressed after
above operations, display does not change.
(4) Programmed final temperature
The final temperature of each programmed step is set. The final temperature will be the
starting temperature of the subsequent temperature program.
Effective range
Initial value
Setting method
-99 to 399°C
200 C only for final temperature 1, 0 C for others
- 1 7 -
Ex.) Final temperature of column 1
2
3
4
5
200
300
100
250
350
°c
°c
°c
°c
Operation Display
COLAUX. 1
[F. TEMP
CPR5 5.0 Display content remains intact. In this case elevationrate 5 of the column oven.
20
200
CFP1 200 Final temperature 1 of the column oven is now set to200°C.
30
300
CFP2 300 Final temperature 2 of the column oven is now set to300°C.
10
100
CFP3 100 Final temperature 3 of the column oven is now set to100°C.
25
250
10 CFP4 250 Final temperature 4 of the column oven is now set to250°C.
11
35
350
12 CFP5 350 Final temperature 5 of the column oven is now set to350°C.
- 1 8 -
(5) Time of retaining final temperature
All time of retaining final temperature at all programmed steps are set.
Effective range 0 to 655 min
Initial value 0.0 min for all steps
Setting method
Ex.) 1
2
3
4
5
30 min
0 min
20 min
0 min
60 min
O peration Display
COLAUX.. 1
[F. TIME I
CFP5 350 Display content remain intact. In this case final temperature5 of column oven is displayed.
30
CFM1 30.0 Time of retaining final temperature 1 of the column oven isnow set to 30.0 min.
CFM2 0.0 Time of retaining final temperature 2 of the column oven isnow set to 0.0 min.
20
CFM3 20.0 Time of retaining final temperature 3 of the column oven isnow set to 20.0 min.
10
11 CMF4 0.0 Time of retaining final temperature 4 of the column oven isnow set to 0.0 min.
12
60
13 _ENT] CFM5 60.0Time of retaining final temperature 5 of the column oven isnow set to 60.0 min.
- 1 9 -
AIX1
(1) Setting of the initial temperature
Initial temperature is the value set in paragraph 2-2 (AUXl) of this section
(2) Setting of time of retaining initial temperature
Effective range 0 ~ 655 min
Initial value 0.0 min
Setting method
To set 30 minutes for the time of retaining initial temperature of AUXl.
Operation Display
[SHIFT. D | CITP 100
COLAUX.I. TIME
Display content remains intact.In this case the initial tem-perature of the column ovenis displayed.
The SHIFT. D lampis turned on.
The SHIFT. D lampis turned off.
30
AITM 30.0 The time of retaining initial temperature of AUXl is nowset to 30 minutes.
(3) Setting of program rate
Effective range
Initial value
Setting method
Ex.) : Program rate 1
2
3
4
5
0 ~
0.0°
10°
20°
5°
2.5°
10°
40.0 C/min
C/min
C
C
ccc
- 2 0 -
Operation
1 SHIFT. D
_COL_AUX..1
PTRATEI
Display
AITP 100 Display content remains intact.In this case, the initial tem-perature of AUXl is displayed.
The SIFT. D lampis turned on.
The SHIFT.D lampis turned off.
10
APR1 10.0 Program rate 1 of AUXl is now set to 10.0°C/min.
20
APR2 20.0 Program rate 2 of AUXl is now set to 20.0°C/min.
APR3 5.0 Program rate 3 of AUXl is now set to 5.0°C/min.
10
2.5
11 APR4 2.5 Program rate 4 of AUXl is now set to 2.5°C/min.
12
10
APR5 10.0 Program rate 5 of AUXl is now set to 10.0 C/min.
- 2 1 -
(4) Setting of Final temperature
Effective range - 99 ~ 399° C
Initial value 200°C for final temperature 1, 0°C for others
Setting method
Ex.) : Final temperature
Operation Display
|SHIFT. D| APR5 10.0
AUX.. 1
Display content remains intact.In this case, elevation rate 5of AUXl is displayed.
The SHIFT. D lamp isturned on.
F. TEMP
20
200
AFP1 200 Final temperature 1 of AUXl is now set to 200°C.
30
300
AFP2 300 Final temperature 2 of AUXl is now set to 300°C.
10
100
AFP3 100 Final temperature 3 of AUXl is now set to 100°C.
10
15
150
11 AFP4 150 Final temperature 4 of AUXl is now set to 150°C.
12
30
300
13 AFP5 300 Final temperature 5 of AUXl is now set to 300°C.
- 2 2 -
(5) Setting of time of retaining final temperature
Effective range 0 ~ 655 min
Initial value 0.0 min
Setting method
Ex.) : Time of retaining final temperature. 1
2
3
4
5
10
0
30
20
20
mm
min
min
min
min
Operation Display
SHIFT. D AFP5 300
COLAUX. 1
F. TIME
Display content remainsintact.
The SHIFT. D lampis turned on.
The SHIFT. D lamp isturned off.
10
AFM1 10.0 Time of retaining final temperature 1 of AUXl is now set to10 minutes.
AFM2 0.0 Time of retaining final temperature 2 of AUXl is now set to0 minute.
30
AFM3 30.0 Time of retaining final temperature 3 of AUXl is now set to30 minutes.
10
20
11 AFM4 20.0 Time of retaining final temperature 4 of AUXl is now set to20 minutes.
12
20
13 AFM5 20.0 Time of retaining final temperature 5 of AUXl is now set to20 minutes.
- 2 3 -
General caution
[COLj and |AUX1|
In setting the temperature program, either the [COL! key or the [AUXll key
SHIFT. D COLAUX.l
must be depressed first to show the setting of the column oven
or the AUXl. (Refer to the sections on Column oven temperature and AUXl temperature.)
Once one of these keys has been depressed, that setting is stored till the other is depressed.
Therefore, in case of the setting for the column oven, the [COL] key may not be depressed
every time the program rate or the final temperature has been set. First depress the P. RATE
key or the|F. TEMP| key.
Operation Display
COLAUX. 1
AITP 100 Display content remains intact. In this case, the tem-perature of AUXl is displayed. This operation is storedtill keys are operated in the sequence | SHIFT. D COL
(Or till setting for (AUXl) is completed.JAUX.l
I. TIME
10
CITM 10.0 Setting of time of retaining initial temperature of thecolumn.
P. RATE!
CPR1 5.0 Setting of column oven temperature program rate.
F. TEMP
10
11 20
12 200
13 CFP1 200 Setting of column oven program final temperature.
- 2 4 -
Once either the column oven or the AUX1 is selected, it is not altered till the other is
selected.
1
2
3
4
5
6
7
8
9
10
11
Operating
COLAQX. 1
CENT]
I. TEMP 1TENT]
I. TIME
[ENT]
1 MONI [
[SHIFT. E
COLAUX . 1
P. RATE
)]
jENTl
Display
CITP. 100
CITP 100
CITM 5.0
AITP. 150
CPR1 3.0
Display content remains intact. In this case, thetemperature of the column oven is displayed.
This will cause the column oven to be selected.
The setting value of the initial temperature of the columnoven is displayed.
The initial temperature retention time of the column ovenis displayed.
The SHIFT. D lamp is turned on.
The AUX1 temperature is monitored. This operationwill not cause AUX1 to be selected.
The elevation rate of the column oven is displayed.
° Cautions in making up the temperature program
In making up the temperature program, for example, in the case of the program of the
column oven, the initial temperature, the time of retaining initial temperature, the temperature
program rate, the final temperature and the time of retaining final temperature can be set
in any order.
Operation Displayed
COLAUX. 1
INITIAL Display content remains intact. In this case, the initialstate is displayed.
I. TEMPI
1
10
100
CITP
I. TIME I
100
1
10
Initial temperature 100°C
- 2 5 -
Operation Display
CITM 10.0 Time of retaining initial temperature 10 min
|P. RATE]
10 CPR1 5.0 Temperature program rate 1 5°C/min
11 1
10
12 CPR2 10.0 Temperature program rate 2 10°C/min
13 F. TEMP
14 1
15
150
15 CFP1 150 Final temperature 1 150°C/min
16 2
20
200
17 CFP2 200 Final temperature 2 200°C/min
18 F. TIME I
19 1
10
20 CFM1 10.0 Time of retaining final temperature 1 10.0 min
21
22 CFM2 0.0 Time of retaining final temperature 2 0.0 min
23 3
30
24 CFM3 30.0 Time of retaining final temperature 3 30 min
25 |P. RATE |
26
27 CPR3 5.0 Temperature program rate 3 5.0°C/min
28 [F. TEMPI
29 1
15
150
30 CFP3 150 Final temperature 3 150.0 C
- 2 6 -
Even if other operations, such as setting of the INJ temperature, are done during this
operation, the value can be programmed in the subsequent step of the set program by de-
pressing a key, for example [F. TEMP
However, when the COLAUX. 1
key is depressed again, like COLAUX.l
ENT or COLAUX.l
P. RATE] fTl \~0~\ [ENT| , subsequent settings are stored from step 1. (In previous
example, as the COLAUX.l
key is depressed first, the settings are stored from step 1.]
During the setting, the display "LIMIT" shows that the setting has already exceeded five
steps. For example, when CFP5 has already been set, if keys are operated in the sequence
1 S E ] [ENTi , "LIMIT" is displayed.F. TEMP
However, when a try is made to set the final temperature immediately after final temper-
ature 5 is set by depressing |ENT] key only, "LIMIT" is not displayed.
Operation Display
F. TEMP CPR5 10.0 Display content remains intact.
3
30
300
CFP5 300 Shows setting of the final temperature 5
3
35
350
350 Display does not change and nothing is set.Shows the setting exceeding for the five and subsequentsteps.
- 2 7 -
2-5 To learn the set program
To learn the content of the set program, operate in the following manner.
Column oven temperature program
(1) Initial temperature program
1
2
3
Operation
COLAUX..1
I. TEMP
PENT]
Display
INJT 200
CITP 100
Display content remains intact.In this case, the INJ temperature is displayed.
The setting initial temperature of the column oven isdisplayed.
(2) Time of retaining initial temperature
1
2
3
Operation
COLAUX. 1
I. TIME
[ENT|
Display
INJT 200
CITM 10.0
Display content remains intact.In this case, the INJ temperature is displayed.
The setting initial temperature of the column oven isdisplayed.In this case, 10 minutes.
(3) Temperature program rate
Operation Display
COLAUX. 1
CITM 10.0 Display content remains intact.In this case, time of retaining initial temperature isdisplayed.
P. RATE
CPR1 5.0 Temperature program rate 1 is displayed.In this case, 5.0 C/min.
CPR2 10.0 Temperature program rate 2 is displayed.
CPR3 5.0 Temperature program rate 3 is displayed.
CPR4 2.5 Temperature program rate 4 is displayed.
CPR5 0.0 Temperature program rate 5 is displayed.
When the rate is not set, the value 0.0 is displayed.
- 2 8 -
(4) Final temperature
Operation Display
COLAUX.l
CPR5 0.0 Display content remains intact.In this case, temperature rate 5 in displayed.
F. TEMP
CFP1 200 Final temperature 1 is displayed.In this case, 200°C.
CFP2 250 Final temperature 2 is displayed.
CFP3 150 Final temperature 3 is displayed.
CFP4 250 Final temperature 4 is displayed.
CFP5 Final temperature 5 is displayed.
(5) Time of retaining final temperature
Operation Display
COLAUX . 1
CFP5 Display content remains intact.In this case, final temperature 5 is displayed.
F. TIME
CFM1 0.0 Time of retaining final temperature 1 is displayed.In this case, 0.0 minutes.
CFM2 10.0 Time of retaining final temperature 2 is displayed.
CFM3 30.0 Time of retaining final temperature 3 is displayed.
CFM4 0.0 Time of retaining find temperature 4 is displayed.
CFM5 0.0 Time of retaining find temperature 5 is displayed.
Temperature program of AUX. 1 oven.
In case of AUX. 1, the program can be known in the same manner. In this case, operate
keys in the sequence [SHIFT. D~] COLAUX.l
, instead of the COLAUX.l key. The display
characters of the initial temperature and others are as follows.
AUX. 1 Initial temperature
Time of retaining initial temperature
Temperature program rate 1 to 4
Program final temperature 1 to 5
Time of retaining final temperature1 to 5
AITP
AITM
APR 1 to 5
AFP 1 to 5
AFM 1 to 5
- 2 9 -
Note :COL
AUX.l key
By operating keys in the sequence COLAUX.l
LENTM or COLAUX.l
I. TEMP
lENTl , and COLAUX.l
P. RATEl [ENTJ , their displays turn to the ones in the
first step of temperature program as described in the paragraph.
For example, the following procedure can be followed.
Operation Display
COL Display is cleared. (Nothing is displayed.)
I. TEMP 1
CITP 100 Initial temperature.
I. TIME
CITM 10.0 Time of retaining initial temperature.
P. RATE
CPR1 5.0 Temperature program rate 1.
F. TEMPI
CFP1 150 Final temperature 1.
10 F. TIME |
11 CFM1 0.0 Time of retaining final temperature 1.
12 P. RATE
13 CPR2 10.0 Temperature program rate 2.
14 CPR3 5.0 Temperature program rate 3.
15 F. TEMP
16 CFP2 250 Final temperature 2.
17 CFP3 150 Final temperature 3.
Then, by pressing the COLAUX.l
key, the display returns to the first step.
1 Ql o
19
20
21
22
23
COLAUX. 1
P. RATE
[ENTl
F. TEMP
|ENTl
1ENT|
CPR1 5.0
CFP1 150
CFP2 250
Temperature program rate 1.
Final temperature 1.
Final temperature 2.
-30-
2-6 To alter part of the program
To alter some of the set values in the temperature program, proceed as follows.
Ex. : Change column oven final temperature 3 and time of retaining final temperature 2 to
150°C and 20 minutes, respectively.
Operation Display
COLAUX. 1 CITP 100 Final temperature 1 is displayed.
CFP1 150 Final temperature 1 is displayed.
CFP2 250 Final temperature 2 is displayed.When the item preeding item to be altered is displayed,set the value.
15
150
CFP3 150 Final temperature 3 is now 150 C.
F. TIME
10 CFM1 0.0 Set the value to be altered in the same manner as in No. 4.
11
12 20
13 CFM2 20.0 Time of retaining final temperature 2 is now set to 20minutes.
Note : By setting a temperature program rate, 0°C/min is automatically set to the
temperature program rate of the subsequent step.
This is because, when a new program is smaller than the old program, the old
program is not cleared and undesirable temperature rise will occur. (When the
temperature elevating rate of the step is 0°C/min, the temperature does not rise.)
Therefore, when altering a part of temperature program rates, all of the altered
and subsequent rates must be set again.
- 3 1 -
2-7 Setting maximum temperature
Maximum temperatures of the column oven and the AUX. 1 oven can be set. When each
temperature exceeds the set maximum, temperature control is stopped.
(1) Maximum temperature in the column oven
The maximum of the column oven can be set between - 99°C and 400°C. (Initial value is
400°C.) When the temperature in the column oven exceeds this set value, "OVER COL" is
displayed, a buzzer continues to sound and the oven heater stops heating. To cancel this
alarm, depress the ICEI key when the column oven temperature is falling, or when
the maximum temperature in the column is set to a higher value than the current temperature.
Setting method (Setting at 350°C)
Operation Display
SHIFT. D CITP 300 Display content remains intact.In this case, the column oven temperature is displayed.The SHIFT. D lamp is turned on.
FILEFUNC The SHIFT. D lamp is turned off.
CMAX 250 The present maximum of the column oven temperatureis displayed.The DIALOG lamp is turned on.
35
350
LDVC 11 The maximum temperature in the column oven is nowset to 350 C and display content differs.
SHIFT. D The SHIFT. D lamp is turned on.
10 E SCAPE Display content remains intact. The DIALOG lamp isturned off.
Note : Note that if operations 9 and 10 are not performed, the GC-9A/9AM remains in a
state of dialogue and only the setting of a display value can be operated. When
the DIALOG lamp is turned on, the GC-9A/9AM is always in the dialogue state.
Therefore, to escape from the state, perform operations 9 and 10.
-32-
(2) Maximum temperature in the AUX. 1 oven
The maximum temperature in the AUX. 1 oven can be set between -99°C and 400°C.
The initial value is 400°C.
When the temperature in the AUX. 1 oven exceeds this setting, "OVER AUX" is displayed
and a buzzer continues to sound. The heater stops heating. To cancel this, depress the |CE
key when the AUX temperature is falling or when the maximum temperature is set to a
higher value than the current temperature.
Ex. : Set the maximum temperature of the AUX to 350°C.
Operation Display
SHIFT. D AITP 150 Display content remains intact.In this case, the initial temperature of AUX. 1.The SHIFT. D lamp is turned on.
FILEFUNC
The SHIFT. D lamp is turned off.
AMAX 200 The setting maximum temperature of the AUX. 1 isdisplayed.The DIALOG lamp is turned on.If this value is not altered, go to operation 9.
35
350
CMAX 400 The maximum temperature in the AUX is now set to 350 C."CMAX 400" is displayed.
SHIFT. D The SHIFT. D lamp is turned on.
10 ESCAPE The DIALOG and the SHIFT. D lamps are turned off.
Operations 9, 10 cause the GC-9A/9AM to escape from the dialogue state. Therefore, to
perform other operations, these operations must be performed.
-33-
3. Detector
Item 3-1
3-2
3-3
3-4
Introduction
Setting of detector
To learn the set detector
a. The number of the detector presently selected.
b. The type of detector corresponding to its number.
RANG. POL. CURR
3-1 Introduction
The GC-9A/9AM can be connected with 6 types of detectors (FID. TCD. PID. FTD. FPD. ECD)
and four of them can be incorporated in a GC-9A/9AM.
The correspondece of each detector to any of DETECTOR 1 to 4 is either designed on the
detector print board, or at the time of shipment from the factory or upon installation.
3-2 Setting of detector
One of the four detectors furnished with the GC-9A/9AM must be selected to be used.
1
2
3
Operation
|DET |
JENTl
Display
CITP 100
4
DET 4
Display content remains intact.In this case, the temperature in the column oven isdisplayed.
Detector 4 is now selected. For example, when TCD isconnected with the GC-9A as DETECTOR 4, TCD willbe selected as the detector.
3-3 To learn the set detector
a. To learn the number of the set DETECTOR.
1
2
Operation
|DETJ
[ENTl
Display
INJT 200
DET 4
Display content remains intact.In this case, the injector temperature is displayed.
The number of the set DETECTOR is displayed.In this case, DETECTOR 4.
-34 -
Note : In this operation, if a numerical value only has been displayed, the value is set as
a DETECTOR number. To avoid this, clear the display by depressing the |CE |
key.
1
2
Operation
PET]
IENT)
Display
2
DET 2
The numeric key has been depressed before this operation,and the numericc value is displayed :In this case, 2.
DETECTOR 2has been set.
b. To learn the type of DETECTOR, number 1 to 4.
3-4
a.
1
2
3
4
Operation
MQNI1
pDET]
|~2~|
lENT|
Display
INJT 200
2
FID
Enter 2 as a DETECTOR number.
Shows that the DETECTOR 2 is a FID.
RANGE, POLARITY, CURRENT
Setting method
After setting a detector, its RANGE. POLARITY and CURRENT are set.
Ex.: Setting of POLARITY
1
2
3
Operation
POL
H|ENT|
Display
DET 4
1
D4PL 1
Display content remains intact.In this case, DETECTOR number is displayed.
The polarity of DETECTOR 4 is now 1.(When a sample is injected into the injection port in theside of 1, a signal is output positively.)
Note : In setting RANGE and CURRENT, depress the [RANG) and the ICURRJ keys
respectively, instead of the [POL[ key.
If the input numerical value only is displayed in the final display of this opera-
tion, set a detector number and operate again.
- 3 5 -
When the setting of a value beyond the range of the detector is attempted
(Refer to the paragraph - Explanation of detector), "ERROR 4" is displayed and
the setting value remains as it is.
When setting the RANGE, POLARITY and CURRENT on a DETECTOR number
which is not connected with a detector, or when setting an item that can not be
set on a detector (Refer to the paragraph - Detector), "NON" is displayed and
this shows that the item can not be set.
- 3 6 -
4. Starting and Ending Temperature Control
Item 4-1 Description
4-2 Starting and Ending temperature control
4-3 Function as timer
(1) Start with shift down mode
(a) Setting
(b) Execution
(2) Stop with shift down mode
4-4 Monitoring of sleep time
4-1 Description
On completion of the temperature setting, start temperature control. At this time, the start
and stop times can be set.
4-2 Starting and ending of temperature control
Refer for details to the paragraph-analysis.
By first depression of the [ST ART | key, each temperature at all point begin to be raised to its
set value. Temperatures in column oven and AUX.l oven is raised to their initial temperatures.
When the temperature in column oven is within the set value ± 1 C, the READY lamp is turned on.
4-3 Function of timer
Temperature control can automatically be started and ended.
(1) Start with shift down mode
When not controling temperature, to start the temperature controle in a fixed time, perform
this operation.
(a) Setting
First set the time necessary to start temperature control (START TIME). When the
power source switch is turned on, the initial value is 10 minutes. The effective range is
between 0.1 and 3000.0 minutes. The value, rounded off to the nearest minute, is
displayed. For instance, when the set value is 0.1 minutes, 0 is displayed as the START
TIME. However, the START TIME is actually set to 0.1 minutes (6 seconds).
- 3 7 -
(Example : To set 10 hours for the START TIME.)
Operation Display
SHIFT. D CPR4 5.0 Display content remains intact :in this case, column temperature elevation rate 4.The SHIFT. D lamp is turned on.
1START. T CPR4 5.0 The SHIFT. D lamp is turned off.
60
600
STAT 600 SLEEP TIME is now 600 minutes (10 hours).
If a value smaller than 0.1 minutes or larger than 3000 minutes is set for the SLEEP
TIME, "ERROR 4" is displayed and the value originally set remains in effect.
(b) Execution
To start temperature control after lapse of the START TIME, perform the following
operation.
1
2
Operation
| SHIFT. D |
| START
Display
CITP 100
SLEEP
* *
Display content remains intact :in this case, 100 C for the set value of the column oveninitial temperature.The SHIFT. D lamp is turned on.
"SLEEP" is displayed and operation is not started untilthe START TIME has passed.
Temperature adjustment starts after time has elapsed.
On performing this operation during temperature control, the READY lamp is turned off
and "SLEEP" is displayed. Temperature control is then immediately restarted and " * * "
is displayed.
If this operation is performed during execution of the temperature program, the GC-9A
enters the hold state and count of retention time stops. To escape from this state, press
the 1 HOLD 1 key or the 1 START [ key. After the execution of the program, " * * " is
displayed.
- 3 8 -
(2) Stop with shift down mode
At the time of temperature control, the control can be ended after a fixed time, and can
then be restarted.
(a) Setting
First, set the time it takes to end temperature control (STOP TIME). The initial value
is 10 minutes when the power source switch is turned on. Setting range is between 0.1 and
3000 minutes. Values can be set to within one decimal place, but display is only of whole
integers.
Ex : To set STOP TIME to five hours.
Operation Display
SHIFT. D CITP 100 Display content remains intact : in this case, the initialtemperature in the column oven.The SHIFT' D lamp is turned on.
2STOP. T
CITP 100 The SHIFT. D lamp is turned off.
30
300
STP.T 300 The STOP time is now set to 5 hours (300 minutes).
Next, set the period during which when temperature control halts (SLEEP TIME).
The initial value of the SLEEP TIME is also 10 minutes when the power source switch is
turned on.
The setting range is from 0.1 to 3000 minutes. Value can be set to within one decimal
place but only whole integers are displayed.
Ex. : To set SLEEP TIME to 12 hours.
Operation Display
SHIFT. D INJT 200 Display content remains intact : in this case, theinjector temperature.The SHIFT' D lamp is turned on.
3SLEEP.T INJT 200 The SHIFT. D lamp is turned off.
72
720
SLPT 720 SLEEP TIME is now set to 12 hours (720 minutes).
- 3 9 -
If values beyond the limits are set for these values, "ERROR 4" is displayed and the set
value remains unchanged,
(b) Execution
To stop and start a temperature control, perform the following operation.
1
Operation
SHIFT. D|
I STOP!
Display
CITP 100
WAIT
SLEEP
* *
Display content remains intact : in this case, the columninitial temperature.The SHIFT. D lamp is turned on.
"WAIT" is displayed. Temperature control continuestill the STOP TIME has passed.
"SLEEP" is displayed after lapse of stop time ; temperaturecontrol is stopped. Wait till sleep time has passed.
Temperature control is started after lapse of sleep time.
When temperature control has not been made, this operation causes no change.
When "WAIT" is displayed, if execution of the program is desired during temperature
control, the execution is started by pressing the | START] key. Even if the stop time
comes on before the program is completed, the program can be executed to the final
step.
When stop with shift down mode is performed during execution of the temperature
program, a count of the stop time starts after completion of program execution. There-
fore, temperature control will be stopped after lapse of the stop time on completion of
program execution.
4-4 Monitoring of sleep time
In a sleep state, the current sleep time can be monitored.
1
2
3
Operation
1 MONI 1
| SHIFT. D
1 31 SLEEP. T
1
Display
INJT
SLPT
200
27
Display content remains intact : invalue of the injector temperature.
The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.The current sleep time is displayed.
this case, the set
(Unit Minute)
Temperature control is started when the current sleep time reaches the set value, and the
time remains displayed.
-40-
If this operation is performed in a waiting state, current stop time is displayed. (Be care
that "SLPT." is displayed.) When the current stop time reaches the set stop time, tem-
perature control is stopped ; the value "0" is displayed and sleep time control starts.
- 4 1 -
5. Analysis
Item 5-1
5-2
(1)
(2)
•(3)
5-3
(1)
(2)
(3)
(4)
(5)
Description
Analysis starting
START (1)
START (2)
In case of AUX. 1 temperature programmer
Operation during analysis
Temperature monitor at the points of control
Hold
a. Temperature hold
b. Retention time hold
c. AUX. 1 hold
Monitoring of retention time
Monitoring of the program
Others
5-1 Description
After completion of all settings necessary to analysis such as column oven temperature,
temperature program, and setting of detector, actual analysis is started. Various operations
can be performed during analysis.
5-2 Starting of analysis
(1) START (1)
By depressing the [START] key, temperature control is started.
Operation Display
Temperature control starts
Note : When a display operates as a stop watch, it continues to display the current time,
and temperature control is started. When the GC-9A/9AM is in a dialog with
program, list and others (the DIALOG lamp is turned on), temperature control
is not started by this operation.
By depressing the | START| key, temperatures in the column oven (and AUX. 1, if
connected) are heated to the set initial temperature. Temperatures of the injector and a
- 4 2 -
detector (and TCD, AUX 2, if they are connected) are also heated to their set temperatures.
When the temperature in the column oven is ± 1°C within the set temperature, the READY
lamp is turned on. However, since there is slight fluctuation of the temperature in the
column oven before the temperature reaches the set value, the READY lamp will go off a few
times but soon will remain on.
(2) START (2)
When the [START] key is pressed again, the temperature program is executed and
analysis is started.
Operation Display
RT 0.00 Retention time is displayed. Unit : minute
° Temperature program in the column oven
if this operation is performed before the column oven temperature rises to the initial
temperature, "NOT RDY 1" is displayed and analysis is not started.
Display of "NOT RDY 3" when | START] key is pressed indicates that the detector
temperature has not risen to the set value. Therefore, check the detector temperature
and start analysis when the temperature does reach the set value.
The process of temperature program execution can be observed by lamps on the control
panel.
In a step where the column oven initial temperature is retained, the READY lamp is turned
off and the INITIAL lamp is turned on. In a temperature program step, the RAISE lamp is
lit, in the step of the final temperature retention, the FINAL lamp is turned on. In the
following temperature program , the RAISE lamp is again turned on ; when the final tem-
perature retention step is reached, the FINAL lamp is lit.
Repeat this process the number of times specified. If the final temperature is lower
than the starting temperature in a temperature programmed process, the RAISE lamp is
instantly turned on and off, and the FINAL lamp is lit. Temperature starts to fall at this
time. (At this time, the GC-9A/9AM enters a state of the final temperature retention as
described in the section on Temperature Program. Thus, sufficient time of retaining final
temperature is required stabilize temperature.)
On completion of execution of the temperature program, (Setting the subsequent tem-
perature program rate to 0.0°C/min is considered to be the completion of the temperature
program.), the COOL lamp is turned on and the column oven temperature falls to the
-43-
initial temperature value setting. The count of the retention time is ended. If the tem-
perature reaches the initial temperature, the READY lamp is turned on.
When the final temperature of the last temperature program is higher then the initial
temperature, the COOL lamp is also turned on after completion of program execution. In
this case, the column temperature continues to rise to the initial temperature.
(3) Temperature program in AUX. 1
Same as in the column oven.
Lamps are not lit.
5-3 Operation during analysis
(1) Temperature monitor
All current temperatures can be monitored at all temperature controling points during
analysis.
1
2
Operation
1 MQNI |
COLAUX.l
Display
RT. 5.36
CITP. 122
Display content remains intact.In this case, retention time.
The current temperature in the column oven is displayed.Display "CITP" does not show the set value of the columninitial temperature. This can be determined by theflickering of the period between the value and "CITP".
1
2
Operation
[ MQNI 1
INJAUX. 2
Display
CITP. 122
INJT. 199
Display content remains intact : in this case, the tem-perature in the column oven.
Current temperature in the injector.
1
2
Operation
1 MONI1
TCDDET. T
Display
INJT. 199
TCDT. 50
Display content remains intact : in this case, the tem-perature in the injector.
Current TCD temperature.
1
2
3
Operation
| MONI |
I SHIFT. D |
COLAUX. 1
Display
TCDT. 50
AITP. 100
Display content remains intact : in this case, the TCDtemperature.
The SHIFT. D lamp is turned on.
Current AUX 1 temperature.The SHIFT. D lamp is turned off.
- 4 4 -
1
2
3
Operation
1 MONI 1
SHIFT. D 1
INJAUX. 2
Display
AITP. 100
AUXT. 150
Display content remains intact : in this case, the AUX 1temperature.
The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.Current AUX 2 temperature.
1
2
3
Operation
1 MONI |
SHIFT. D
TCDDET
Display
AUXT. 150
DETT. 200
Display content remains intact :In this case, the AUX 2 temperature.
The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.The current detector temperature.
The display momentarily changes with these operations. The temperature remains to be
displayed until the following operation is performed.
Note : In order to distinguish these displays from set values, when the current temper-
ature is displayed, the period " • " flickers.
Use the |SCAN 1 key to monitor temperatures at six places every about two seconds.
1
2
Operation
| SHIFT. D |
SCAN
Display
CPR1 0.0
CITP- 100
AITP. 100
INJT. 200
DETT. 200
AUXT. 150
TCDT. 40
CITP. 100
Display content remains intact : in this case, column oventemperature program rate 1.The SHIFT. D lamp is turned off.
The current column oven temperature.The SHIFT. D lamp is turned off.
The current AUX 1 temperature.
The current injector temperature.
The current detector temperature.
The current AUX 2 temperature.
The current TCD temperature.
The current column temperature
-45-
Note : When the |SCAN[ key is depressed, it is uncertain which temperature is
displayed first.
The sequence of display is as shown above. Each temperature is successively
displayed until the following operation is performed. To end the display,
depress the |CE| key or perform other operations.
These temperatures can be monitored, whether AUX, TCD and others are
connected or not. If they are not connected, "AITP. -105", "AUXT. - 5",
"TCDT. - 5 " are displayed.
(2) HOLD. T
a. Temperature hold
Interrupts the temperature elevation temporarily. During the interruption, the counting
of the retention time continues.
Operation Display
COLAUX.l
CITP 100 Display content remains intact : in this case, the tem-perature in the column oven.
SHIFT. D CITP 100 The SHIFT. D lamp is turned on.
HOLDHOLD. T CITP 100 The SHIFT. D lamp is turned off.
The temperature at the time the | ENTj key is de-pressed holds for 10 minutes.
10
HLDC 10.0
Note : If this operation (step [j6j ) is performed during the temperature elevation
(when the RAISE lamp is turned on), the current temperature is held for a
fixed time (in this case, 10 minutes) and then rises. During that period, counting
of retention time continues.
In this operation is performed before elevating temperature (when the INIT lamp
or READY lamp is turned on), the initial temperature is held for a fixed time
before the temperature rises. During the time of retaining final temperature,
the temperature holds for a fixed time before the following program starts.
Take notice that the following operation will cause the preset hold time to be
reset.
- 4 6 -
1
2
3
4
Operation
COLAUX. 1
I SHIFT. D|
HOLDHOLD. T
[ENT|
Display
RT. 0.00
HLDC 2.00
Display content remains intact : in this case, the reten-tion time.
The SHIFT. D lamp it turned on.
The SHIFT. D lamp it turned off.
The previously set value is displayed and the newlydisplayed value is in turn.
b. Retention time hold
The retention time can momentarily be held during analysis. By depressing the [HOLD!
key, the counting of retention time is stopped. By depressing the key again, the count is
started from the halting value.
1
Operation
HOLDHOLD. T
Display
HOLD The counting of retention time is stopped.
1
Operation
* HOLDHOLD. T
Display
RT. 3.67 The count is restarted from the halting value.
* The START key can be depressed.
If this operation is performed when the temperature in the column oven is the initial or
final temperature, the temperature, as well as the retention time remains constant till the
HOLD operation is completed.
If this operation is performed when the column temperature is rising, the temperature
rises to the final temperature of this step, where it remains unchanged. On cancellation
of HOLD, the program is executed from the time of the end of rising temperature of the
step. In other words, after cancellation, the temperature is held till the time of retaining
final temperature has passed, when the subsequent temperature program starts.
Even in a Hold state before the execution of the program, depressing the [START 1 key
will result in escape from that state.
If, during the execution of the program, other operations are performed after hold
operation and then the display changes, monitor the retention time in the operation as
described in the following and determine whether the value has stopped or not.
-47-
c. Hold of AUX 1 temperature
In the case of AUX 1, as with the column, the temperature hold operation can be
performed. The AUX temperature can be held constant for a fixed time when program
execution is temporarily interrupted, and the program execution can be resumed.
1
2
3
4
5
6
7
Operation
| SHIFT. D
COLAUX. 1
SHIFT. D
HOLDHOLD.T
B
|ENT|
Display
AITP. 220
AITP. 221
1
10
HLDA 10.0
Display content remains intact : in this case, AUX 1temperature.The SHIFT. D lamp is turned on.
The SHIFTtD lamp is turned off.
The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
In this case, AUX 1 holds the temperature in performingoperation 7 for 10 minutes and then returns to theprogram.
Note that the HOLD lamp is not lit up even in a Hold state of AUX 1 temperature.
(3) Monitoring of retention time
On depressing the | START 1 key, the retention time count is displayed. To display the
current retention time count after the display has been cleared by such operations as monitor-
ing of temperature, operate as follows.
1
2
3
Operation
1 MONI [
| SHIFT. D|
STOP-WRET.T
Display
CITP. 100
RT. 5.37
Display content remains intact : in this case, the columnoven temperature.
The SHIFT. D lamp is turned on.
Count of the retention time is displayed.The SHIFT. D lamp is turned off.
By performing this operation before the execution of the program, "RT. 0.00" is displayed.
When the retention time is in. a hold state, the retention time at the time of the hold remains
on display.
(4) Monitoring of TIME program
The subsequent program number to be executed can be monitored. By the following
operation, the program number showing the execution order of the program (the order dis-
played on a printer or CRT when monitoring the TIME program), is displayed.
- 4 8 -
1
2
3
Operation
| MQNI1
SHIFT. D|
7PRG
Display
CITP. 100
CITP. 100
PROG 5
Display content remains intact : in this case, the columnoven temperature.
The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.The number of the subsequent program to be executedis displayed. In this case, program 4 has been executed,and the next is 5.
During monitoring, the display changes following the execution of the program at the
displayed number.
If this operation is performed when the time program has not yet been made up, "PROG 0"
is displayed, showing the nonexistence of a Time program.
If this operation is performed when temperature is not controled, "PROG XX" is displayed.
(5) Direct operation of event by keys
Event is output at any time by using keys, disregarding the Time program.
'EVENT 0 Reversing
EVENT-0 All OFF
EVENT 1 to 8 Set transistor output ON.
EVENT 9 to 16 .... Set relay output ON.
EVENT 91 and 92 . Set the relay output (the sockets furnished with the GC-
9A) ON.
Operation Display
SHIFT. D CITP. 150 Display content remains intact : in this case, the columnoven temperature.The SHIFT. D lamp is turned on.
EVENT The SHIFT. D lamp is turned off.
12
EVNT 12 In step [_5j , the output corresponding to EVENT 12is set ON.
When the operation for setting the event ON is added state, the same content is displayed
but the input situation does not change.
To set an event OFF, perform the following operation.
-49-
1
2
3
4
5
6
Operation
SHIFT. D
8EVENT
B0@
|ENT|
Display
CITP 100
-
1
12
EVNT -12
In this case, indicates the column oven temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
Output of Event 12 is now off.
When the operation for setting the event OFF is added to the event in the OFF state, the
same content is displayed and the event remains OFF.
EVENT 0 changes outputs of transistor and relay from on (/off) to off (/on). EVENT -0
turns all outputs of transistors and relays OFF.
In an Event number, figures below a decimal point are omitted and only integrals are
accepted. If an impossible value is set as an Event number (less than -255 or larger than
255), "ERROR 4" is displayed, with no change.
Note that the following operations cause an unintended Event number to be accepted.
1
2
3
Operation
I SHIFT. D
8EVENT
|ENT|
Display
CITP. 40
EVNT 40.1
Display content remains intact : in this case, the columnoven temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
If the IENT) key is depressed before setting of theEVENT number, the current 4 digit display value will beset as the number. In this case, the situation is identifiedas " Event 40".
In event operation, unlike other operations, the current state of ON or OFF can not be
monitored by operating keys.
(5) Others
In case of an analysis using auto-sampler, the current sample number can be monitored.
(Refer to the section on Auto Sampler.)
- 5 0 -
6. Time Program
Item 6-1 Description
6-2 Items that can be programmed
6-3 Procedure for making up the Time Program
6-4 To see the Time Program
6-5 Alteration of the Time Program
6-6 When the Time Program is larger than memory
6-7 Starting and Ending of the Time Program
6-1 Description
The GC-9A/9AM has the function of the time program. In the time program, time lapse after
the program is started and the parameters to be varied during that time are programmed.
Different program can be made by using file.
6-2 Items that can be programmed
(a) RANGE, POL, CURR.
Range, polarity and current of a detector can be freely altered.
Example : "D1RG 2" : Range 102
(b) EVENT91, EVENT92
Two relays can be furnished in case of a standard configuration and the ON and OFF can be
operated, (optional relay, P/N 065-61564)
Example : "EVNT - 91" : EVENT 91 OFF
(c) Other EVENTs
With an option printing board (PRG board), eight transistor outputs and eight lead relay
outputs can be made available.
Example : "EVNT 1": EVENT 1 ON
(d) RETRN
The program can be executed repeatedly.
The file can be altered after the repeated execution of the program and the altered file
can be executed.
Example: "RETN 102" File 2 is selected after the program on the file of just now
is executed 10 times, then the file 2 is executed.
(e) INJ1
Alteration of the number of injections into injection port 1 with AOC.
Example: "IJ1T 2" Two times injection into injection port 1.
- 5 1 -
(f) INJ2
Alteration of the number of injections into injection port 2, with AOC.
(g) STRK
In AOC, alteration of the syringe stroke.
Example : "STRK 60" Stroke 60 %.
(h) REPT
Alters the repeated number of AOC.
Example : "REPT 5" Repeat five times
(i) DET (With this operation alone nothing is made.)
Example : Designate a detector before setting RANG, POL and CURPv.
[DETl \T\ |ENT| (RANGE 1 \Y\ (ENT(
(j) STOP
The Time program can be stopped in the execution of a program.
6-3 Procedure for making up the time program (expressed in minute down to second decimal
place)
Operation Display
SHIFT. D CITP 100 Display content remains intact : in this case, the columnoven temperature.The SHIFT D lamp is turned on.
PRG TIME ? The DIALOG lamp is turned on.In the state of dialogue.When is the program started ?
The SHIFT. D lamp is turned off.
10 The program will begin execution 10 minutes afterstarting.
FUNC VL? What item is programmed ?
SHIFT. D
EVENT
TIME? EVENT 1 was set to ON.When is the next program started ?
- 5 2 -
10
11
12
Operation Display
15
FUNCVL? This was set 15 minutes after starting.
13 [SHIFT. D
14 EVENT
15
16 - 1
17 TIME? EVENT 1 was set to OFF.When is the next program started?
18
19 15 Two or more programs can be set at the same time-
20 FUNC VL?
21
22
23 TIME? RANGE 1 is set.The time may be random.
24
25 FUNC VL?
26
27 RANGE 2 is set.
28 TIME?
29
30 30
31 FUNCVL?
32 SHIFT. D
33 RETRN
34
35 50
36 TIME? Repeat this program (as well as the temperature program)five times and return to file 0.
37
38
i SHIFT. Dl
[ESCAPE |
The SHIFT. D lamp is turned on.The SHIFT. D lamp and DIALOG lamp are turned off.The GC-9A/9AM is not in the dialogue state.
- 5 3 -
6-4 To see the time program
Set the file of the desired Time Program.
Note that by altering a file during temperature control, all controled temperatures are changed,
from those of the previous file to those of the new file.
Operation Display
SHIFT. D INJT 200 Display content remains intact : in this case, the INJtemperature.The SHIFT. D lamp is turned on.
PRG TIME 5.00 Time for the first program to be executed is displayed.
D1RG Item of the time.
TIME 10.00 And so on.
EVNT
TIME 15.00
EVNT - 1
TIME 15.00
D1RG
10 TIME 30.00
11 REPT 50
12 TIME ? Time program ends. To add new steps, continue here.Any time value may be input. Later, the program willbe arranged (in time order) by the GC-9A/9AM.
13 SHIFT. D The SHIFT. D lamp is turned on.
14 ESCAPE The SHIFT. D lamp and DIALOG lamp are turned off.
6-5 Alteration of the time program
To partially change the time program, input new settings while "TIME? " or "TIME XX"
(XX is a given value) is being displayed.
To partially cancel the time program, operate as follow.
- 5 4 -
1
2
3
4
5
6
7
8
Operation
SHIFT. D
PRG
[ENT]
IENT]
SHIFT. D j
4DEL
[SHIFT. D
| ESCAPE |
Display
CITP 100
TIME 5.00
D1RG 2
TIME 15.00
TIME 30.00
Display content remains intact : in this case, the columnoven temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off. The DIALOG lamp isturned on.
Repreat depressing the [ENT| key until the time atwhich the program to be cancelled is displayed.
The SHIFT. D lamp is turned on.
The program is cancelled and the subsequent program timeis displayed. The SHIFT. D lamp is turned off.
The SHIFT. D lamp is turned on.
The SHIFT. D and DIALOG lamps are turned off.The GC-9A/9AM is no longer in the dialogue state.
6-6 When the time program is beyond capacity of memory
If not "TIME?" but "TIME 0.00" is displayed when the time program is made up, this shows
that memory is already full and more program can not be entered.
If further programming is desired, cancel unnecessary files to secure memory areas.
6-7 Starting and ending of the time program
As in the temperature program, the time program is started by START. (Refer to the section
on Starting the Temperature Program.)
For interruption of the program, stop by STOP. Stopping execution of the time program
also stops the temperature program.
- 5 5 -
7. Files
Item 7-1 Description
7-2 Setting
7-3 To learn the number of the current file
7-4 Copy
7-5 Cancellation of files
7-6 When there is no memory area for extending files
7-1 Description
The GC-9A/9AM has a maximum capacity of ten files. Each can contain a time program, GC
parameter, temperature program and AOC parameter. For AOC parameter, all items except
IJ1T, IJ2T, STRK, and REPT are common to all files.
Each file is variable-length. Variable-length means that the file area is not memory-seeured
until the file is set. Therefore, if the file is short, many files can be made (max. 10) and if long,
accordingly fewer.
When the power source switch is turned on (when files have not yet been set), "File 0" is
opened. If a program is made up without setting a file, the program will be incorporated into
"File 0".
7-2 Setting files
Before a time program, GC parameter and a temperature program are made up, set the file
by keying as follows. (If the file is not set, the file number will be 0.)
Programs to be executed are those which are incorporated into the file number set at the
time.
Example : Set the file number 4.
1
2
3
Operation
FILEFUNC
a|ENT|
Display
CITP 200
4
FILE 4
Display content remains intact : in this case, the currentcolumn oven temperature.
File 4 is now set. Both setting and execution mustfollow the file 4.
- 5 6 -
7-3 To know the current file number
1
2
Operation
MONIJ
1 FILE 1LFUNCJ
Display
CITP
FILE
100
4
Display content remains intact : in this caseoven temperature.
The file number now in use is displayed : inFILE 4.
, the
this
column
case,
7-4 Copy
The entire contents of the file now in use can be transferred to another file. This operation
causes the entire contents of the file now in use to be copied into a specified file, while the
original file continues to be used. Delete the distination file which is already opened, before
copying.
1
2
3
4
Operation
SHIFT. D
_ ^ _COPY |
slENT|
Display
INJT
COPY
200
3
3
Display content remains intact. The SHIFT.on.
The SHIFT. D lamp is turned off.
The contents of the file are now copied to the
D is turned
File 3.
7-5 Cancellation of files
Contents of files can be cancelled except those of the file now in use.
Operation method
Cancel File 3.
1
2
3
4
Operation
SHIFT. D
4DEL
0[ENT]
Display
TCDT 30
3
DELT 3
Display content remains intact: in this case, the TCDtemperature. The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
Contents of File 3 are now initial values.
-57-
7-6 When there is insufficient storage area for file extention
If a long time program is made up or many long files are set, new files cannot be set.
For example, the message "LIMIT", displayed when copying files or setting a new file, indi-
cates that there is insufficient storage for file extension. At this time, cancel unnecessary files
to secure file areas.
Even if there is not enough storage area to extend a new file, there will generally remain
sufficient memory capacity to make up some time programs and temperature programs.
- 5 8 -
8. Other Operations
Item 8-1
8-2
8-3
8-4
8-1 LOCK
Keystrokes on the keyboard can be locked.
LOCK
Stopwatch
Self-diagnostic function
List
1
2
Operation
SHIFT. D
0LOCK
Display
CITP 100 Display content remains intact : in this case, the columnoven temperature.The SHIFT. D lamp is turned on.
Display content remains intact.The SHIFT. D lamp is turned off.The LOCK lamp is turned on.
By depressing the [LOCK] key, all keys except 1 START SHIFT. Dl ,and
1 LOCK 1 keys are locked and can no longer be operated.
Whether or not keys are locked can be determined by observing the |LOCK] lamp.
To escape from this state, depress the 1 LOCK) key once again.
1
2
Operation
SHIFT. D |
1 LOCK 1
Display
CITP 100 The LOCK lamp is now turned on.Display content remains intact.The SHIFT. D lamp is turned on.
Display content remains unchanged.The SHIFT. D and LOCK almps are turned off.Now, keys are not locked.
-2 Stopwatch
Display can be used as a stopwatch.
1
2
Operation
STOP-WRET. T
STOP-WRET. T
Display
000.0
j
44,3
On depressing this key, time count is started.
Unit : second ; display range : to one decimal place
By depressing this key again, time count is ended.The time from the first keystroke till the second isdisplayed in ten the of a second.
-59-
Other operations can be performed with the stopwatch operation.
Operation Display
STOP-WRET. T
000.0 Stopwatch begins to operate.
I N JAUX.2
40.0 Injection temperature is set.Stopwatch count is displayed.
Stopwatch display is cleared.
20
200
INJT 200 On displaying the message "INJT 200", the stopwatchis displayed.
48.7 The display time is greater than that previous by the timetaken in the setting, because the stopwatch has operatedduring setting.
220.0 Timing is ended.
The stopwatch display is not cleared by pressing the [CE| key.
-3 Self-diagnostic function
(1) Self-diagnostic function
This operation diagnoses whether contents of the RAM are normal or not, and also initializes
them.
(2) Operation
1
2
3
4
5
Operation
SHIFT. D |
FILEFUNC
E
|ENT|
Display
INJT 200
1
13
CITP. X X
Display content remains intact : in this case, the injectortemperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
The AUX function 13 is self-diagnostic.
For a moment, usually nothing is displayed and the buzzercontinues to sound.If there is nothing unusual, the message "CITP. X X" isdisplayed. If there is, address is displayed.
-60-
(3) Caution
Notice that this operation causes the setting values to be initialized. If this operation is
performed during a temperature control, the control will be stopped.
-4 List
(1) Listing
The AOC parameters, temperature programs, Time programs and GC parameters input in
files of the GC-9A/9AM can be printed for each file through external devices (CR2A and others).
(2) Procedure
Determine the number of the output device in accordance with the section on "Link Device".
Set the file number which you intend to print, in accordance with the section on Setting of
Files.
(2-1) Listing of time program
1)
1
2
3
4
5
6
Operation
SHIFT. D
FILEFUNC
a|ENT|
inlENTJ
Display
CITP 100
2
LIST GP
1
LIST GP
Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
Listing of time program is the AUX function 2.
The DIALOG lamp is turned on.The GC-9A/9AM is now in the dialogue state.
When you want to list the program, key in 1.
During a listing, the PRG lamp remains on.After the completion of a listing, the lamp is turned offand the GC-9A/9AM will no longer be in the dialogue state
(2-2) Listing of AOC parameter
1
2
3
4
5
Operation
|SHIFT. D
FILEFUNC
[3]
|ENT[
m
Display
CITP 100
CITP 100
3
LIST A
1
Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
AUX function 3 list, AOC parameter.
The DIALOG lamp is turned on.
To list the parameter, key in 1.Listing is begun. After completion of listing, DIALOGlamp is turned off.
- 6 1 -
(2-3) Listing of GC parameter
Operation Display
SHIFT. D | CITP 100 Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
FILEFUNC
The SHIFT. D lamp is turned off.
AUX function 4 lists GC parameter.
LIST A The DIALOG lamp is turned on.
To list the parameter, key in 1.
LIST GI Listing is begun. After completion of listing, DIALOGlamp is turned off.
(2-4) Listing of temperature program
Operation Display
SHIFT. D CITP 100 Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
15 AUX function 15 lists the temperature program.
LIST GP The DIALOG lamp is turned on.
To list the program, key in 1.
LIST GP Listing is begun. After completion of listing, DIALOGlamp is turned off.
(3) No listing
If no listing, key in 0 instead of 1. At this time, the DIALOG lamp is turned off; the GC-9A
does not then enter the dialogue state.
The operation by which the GC-9A/9AM escapes from the dialogue state - [SHIFT. D
[ESCAPE] - may be performed.
(4) Error message
When requesting a listing, if no setting necessary for listing is input, messages such as shown
below will be displayed. Then these messages are displayed, the GC-9A/9AM escapes from the
dialogue state.
- 6 2 -
"SET LDVC"
This occurs when the GC-9A/9AM cannot determine which external output device to be used
for listing due to lack of designation link device.
At this time, designate an appropriate link device. (Refer to the section on "Setting of Link
Device". (Supplementary volume) .)
"NOT LINK"
External output devices have not been fully linked to the GC-9A/9AM. if this message is
displayed, link the devices.
- 6 3 -
9. Option
Item 9-1 Measurement of flow rate
9-2 Auto sampler
9-3 Connection with exterior data processor
9-1 Measurement of flow rate
(1) Flow rate
Flow rate of five kinds of gases - carrier gas, hydrogen, and air - can be set. (0 to 999.
m#/min.)
FLW1
FLW2
FLW3
FLW4
FLW5
Content
Carrier gas 1
Carrier gas 2
Hydrogen 1
Hydrogen 2
Air
Initial value
40.0
40.0
30.0
30.0
200.0
(1-1) Setting
Example : To set carrier gas 1 to 60 m£/min.
Operation Display
FLOWFLOW. M
CITP 200 Display content remains intact : in this case, the columnoven initial temperature.
FLOW
60
FLW1 60.0 Flow rate of the carrier gas 1 is now 60 m#/min.
Set flow rates of other gases in the same manner.
(1-2) When a setting is made incorrectly
When a numerical value is pressed incorrectly, if the [ENTJ key has not yet been
pressed, press the [CE[ key to clear the value and then enter the correct value. If the
[ENTI key has already been pressed, reset by pressing the parameter key once again.
In correcting the number of the set FLOW after operation 1.1 [JT] , first press the
- 6 4 -
[CEj key, or press the |ENT| key once again, to display the set value and then return
to the first step.
If a numerical value which goes below the decimal point is entered as the FLOW
number, the portion below the decimal point is cut off. If a value less than 1 or greater
than 5 is entered, the message "ERROR 3" is displayed.
If a value less than 0 or greater than 999.8 (unit : m£/min) is set, the message
"ERROR 4" is displayed and the set flow value remains unchanged.
(1-3) To learn the set value
Example : To learn the set value of FLOW 1.
1
2
3
4
Operation
1 FLOW1 FLOW. M
CDlENT[
ENT)
Display
CITP 100
1
FLOW 1
40.0
Display content remains intact : in this case, the columnoven initial temperature.
The set value of the flow rate of the carrier gas 1 isdisplayed. In this case, 40.0 mfi/min.
(1-4) Measurement of flow rate
Use of an optional unit permits measurement of gas flow. By performing the opera-
tion only once, the flow rate can be measured four successive times and can be adjusted
according to the measurement value is stored in the GC-9A as the current flow rate of the
gas.
1) First, set the FLOW to be measured. JJ"ENT"
FLOW
1
2
Operation
[SHIFT. D|
FLOWFLOW. M
Display
CITP 100
0000
FLl 47.3
Display content remains intact : in this case, the columninitial temperature.The SHIFT. D lamp is turned on.
Measurement is started and counting of time is started.The SHIFT. D lamp is turned off.
After the completion of the first measurement, themeasurement value is displayed (unit : mJ2/min). Monitorthe value ; then, adjust the mass-flow knob to the flowdesired.
-65 -
Operation Display
0.0
:
FL1 51.3
0.0
:
FL1 50.1
The second measurement and time count are begun.
The second measurement is completed and the measure-ment value is displayed.
After this procedure is repeated four times, the measure-ment is ended and the final measurement value is stored ;in this case, as flow rate of FLOW 1.
To stop during measurement, follow the same procedure as above.
1
2
Operation
| SHIFT. D
FLOWFLOW. M
Display
13.3
FLM-STOP
During flow rate measurement.Time count or measurement value is displayed.The SHIFT. D lamp is turned on.
On performing this operation, the measurement of theflow ends. The measurement value becomes the valuein effect prior to this operation, or the initial value"0.0", when no measurement has been taken.
When the flow is insafficient for measurement, or when no gas flows, measurement is
continued for a moment ; then the message "ERROR 2" is displayed, resulting in the end
of measurement. When no flow measurement device is connected, the result is the same
as with unsufficient flow.
1
2
3
4
Operation
IMONII
FLOWFLOW M
m|ENT[
Display
CITP
CR1
100
1
45.1
Display content remains intact :oven initial temperature.
Enter the flow number desired.
The measured flow value (In this1) is displayed.
in this case, the column
In this case, FLOW 1.
case, flow of carrier gas
This measured value cannot be altered by pressing keys. The value varies only when
a new value is measured or the value is initialized by turning off the power source switch.
- 6 6 -
9-2 Auto sampler
(1) AOC parameter
STRK
ISNO
FSNO
REPT
WASH
WSHT
TWTE
PROD
IJ1T
: Stroke
: Initial sample number
: Final sample number
: Repeated number
: Types of wash liquid
: Wash number
: Time wait
: Period
: Injecting number ofInjector 1
Setting range
10,
0
0
1
o,1
1
0
0
20,40,80
~ 50
~ 50
~ 10
1
~ 10
~ 10
~ 655 (min)
~ 10
Initial value
1
1
49
1
1
1
5
10
1
IJ2T : Injecting number ofInjector 2
0 ~ 1 0
(2) Setting method
Operation Display
SHIFT. D TCDT 30 Display content remains intact : in this case, the TCDtemperature.The SHIFT. D lamp is turned off.
"FICE"FUNG The SHIFT. D lamp is turned off.
STRK 10 The first AOC parameter is displayed and the DIALOGlamp is turned on. (The GC-9A enters the dialogue state.)
20
ISNO 20 is input in the stroke and the subsequent AOC para-meter is displayed.
FSNO 49 The first sample number becomes 5 and the subsequentAOC parameter is displayed.
10
11 45
12 REPT The final sample number becomes 45, and "REPT 1" isdisplayed.
- 6 7 -
13
Operation Display
WASH The repeated number remains 1 (this value has already beenset). Display content changes.
14
15 WSHT Type of wash liquid is determined and "WSHT 1" isdisplayed.
16 TWTE " 1 " enters the wash number. Display content changes.
17
18 PROD 10 " 3 " is input in time wait and the subsequent parameter,"PROD 10", is displayed.
19
20 20
21 IJ1T 1 Period becomes 20 minutes and "IJIT 1" is displayed.
22
23 IJ2T1 Designate the times of injection 1 as 2 and the subsequentparameter is displayed.
24
25 FLWK 500.0 The times of injection 2 is designated as 2. Setting of allAOC parameter is now completed. From this point on,depressing the |ENT[ key causes AMAX, CMAX andothers cordes to be displayed, which have no relationwith AOC.
26 SHIFT. D FLWK 500.0 Steps [26] and [27] are performed so that the GC-9A/9AM can escape from the dialogue state.The SHIFT. D lamp is turned on.
27 ESCAPE The SHIFT! D and the DIALOG lamps are turned off.The GC-9A/9AM is no longer in the dialogue state. TheAOC parameter cannot he set in this state.
(3) To learn the current set value
1
2
3
4
5
Operation
SHIFT. D
FILEFUNC
0|ENT|
lENTl
Display
CITP 100
CITP 100
1
STRK 20
ISNO 5
Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
The DIALOG lamp is turned on and the set value ofthe stroke is displayed.
The set value of the initial sample number.
-68-
Operation Display
FSNO 45 The set value of the final sample number.
REPT The set value of the repeated number.
WASH The set value of the type of the wash liquid.
WSHT The set value of the wash number.
10 TWTE The set value of the time wait.
11 PROD 20 The set value of the period.
12 IJ1T The set value of the times of injection 1.
13 IJ2T The set value of the times injection 2.
14 ! SHIFT. D All AOC parameters are now displayed. Steps |14| andj~X5j must be performed so that the GC-9A/9AM can escape
from the dialogue state. The SHIFT. D lamp is turned on.
15 ESCAPE The GC-9A/9AM is no longer in the dialogue state. TheSHIFT. D lamp is turned off.
In addition, if the CR2A is connected, the AOC parameters may be listed on the printer
so that the set value may be known. If the CRT is connected, the parameters, can be listed
on the screen. Refer to relevant sections for each procedure.
(4) For partial correction of the setting value
Example : Correct WASH from 1 to 0, PROD from 20 to 15.
Operation Display
| SHIFT. D| TCDT 30 Display content remains intact : in this case, the TCDtemperature.The SHIFT. D lamp is turned on.
FILEFUNG The SHIFT D lamp is turned off.
STRK 20 The DIALOG lamp is turned on. (The GC-9A/9AM is in thedialogue state.)
ISNO
FSNO 45
REPT
WASH The set value to be corrected is displayed.
10 WSHT Now WASH becomes 0 and the subsequent AOC parameteris displayed.
- 6 9 -
11
12
Operation Display
TWTE
PROD 20 The set value to be corrected is displayed.
13
14 15
15 IJ1T Now the PROD becomes 15 and the following AOCparameter is displayed.
16 SHIFT. D | When this key is pressed, the GC-9A escapes from thedialogue state.The SHIFT. D lamp is turned on.
17 ESCAPE The SHIFT. D and DIALOG lamps are turned off.
After the completion of settings or checking of the set values, always press the [ESCAPE
key to cancel the dialogue state of the GC-9A/9AM. Notice that after the parameter to be set
is displayed, the setting value must be entered. (In case of the P. RATE, the setting value
must be entered before the parameter is displayed.)
(5) Analysis with automatic sample injector
1. Start
For the analysis with automatic sample injector, the second start is caused by the sample
injector automatically. The temperature program and the retention time indication start at
the time of sample injection.
2. Temperature programing
For TPGC, please set PROD a little longer than the period of TPGC. Even if the PROD
is shorter than the period of TPGC, the next sample is injected after the temperature of the
column oven becomes READY. The stability of the temperature of the column oven,
however, maynot be good enough in such condition.
3. Terminating
The automatic analysis is terminated after the designated final sample is analysed. When
the automatic sampler is stopped, the sample number will be the next of the designated
final number.
4. Monitoring of the current sample number
The current sample number can be monitored by the following'operations.
1
2
3
Operation
| MONl|
SHIFT. D
jS.NOj
Display
CITP
CITP
SNO.
100
100
5
The formar indication.
SHIFT. D lamp will be lit.
The current sample number is indicated.
-70-
5. Direct appointment of sample number
Arbitrary sample can be injected with automatic sampler by using following operations.
1
2
3
4
Operation
SHIFT. D
1 S.NO|
mlENT|
Display
CITP.
CITP.
S. NO
100
100
5
5
The former indication.SHIFT. D Lamp is on.
SHIFT. D Lamp is off.
The sample number is set.
When this procedure is finished, the designated sample will be injected next time. But
when the designated number is smaller than the current sample number, it is neglected.
The number which is larger than the final sample number cannot be designated.
9-3 Connection with exterior data processor
The GC-9A/9AM can be connected with the C-R2A by furnishing the current loop substrate;
the two operations can be coupled. Further, application of the BASIC function of the C-R2A will
permit a great improvement of the functions of the GC-9A/9AM.
For the method of connection with the C-R2A refer to the relevant manual.
1. Setting of Link Device
(1) Link device
For time program, AOC parameter, GC parameter etc., stored in the GC-9A/9AM, to be
output on an external device, the appropriate device number must be designated.
Setting range 0 to 55 (Device number)
Initial value 0
(2) Setting method
1
2
3
Operation
| SHIFT. D
FILEFUNGlool
Display
CITP 100
8
Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
The link device is designated as the AUX function 8.
- 7 1 -
Operation Display
LDVC The link device set value at the time is displayed.The DIALOG lamp is turned on.The GC-9A/9AM is now in a dialogue state.
Designate link device 11.
11
STRK 10 Link device is designated as 11 and the parameter"STRK 10" is displayed. By pressing the [ENT| key,display content now changes successively, as described inthe section on AOC. and "LVDC" will be displayed again.
[SHIFT. After the completion of settings, the dialogue state mustbe stopped.This operation is performed to escape from the dialoguestate.The SHIFT. D lamp is turned on.
ESCAPE The DIALOG lamp is turned off.The SHIFT. D lamp is turned off.The GC-9A/9AM is now out of the dialogue state.
(3) When setting is made incorrectly
If the |ENT[ key has not yet been pressed, press the [CE| key to clear the display,
then enter the number once again. If the [ENT] key has already been pressed, press the
the lENTl key several times to display the LDVC, or first escape from the dialogue
state by performing the steps 8 and 9 and then restart from step 1.
Take note that after setting, the dialogue state must be escaped. Otherwise, other
operations cannot be performed.
(4) To monitor the value
1
2
3
4
5
6
Operation
SHIFT. E
FILEFUNC
>
DO1ENT|
SHIFT. D
ESCAPE
Display
CITP 100
8
LDVC 11
Display content remains intact : in this case, the columnoven initial temperature.The SHIFT. D lamp is turned on.
The SHIFT. D lamp is turned off.
The link device set at the time is displayed.The DIALOG lamp is turned on.
The SHIFT. D lamp is turned on.For escaping from the dialogue state.
The SHIFT. D lamp is turned off.The DIALOG lamp is turned off.The GC-9A/9AM is no longer in the dialogue state.
-72-
(5) Meaning of LDVC
"LDVC" is an abbreviation for "Link Device Code".
This code sets up the input port number (1 or 2) of the external device (C-R2A) and
determines whether the list of the GC-9A/9AM will be output on the CRT or the plotter of
the C-R2A. Setting is shown as a 2 digit number. The first digit spcifies to which C-R2A
channel the detector signal is to be connected the (if it is to be connected to both channels
1 and 2, set 3 as first digit). The second digit specifies either CRT or Plotter (of the C-R2A).
(For CRT, set 2 ; for plotter, set 1.)
LDVC 22 means that the detector signal is connected with channel 2 and the list is to
be printed on the CRT.
-73-
Appendix 1 Error Display
The following error messages are displayed depending on kind of error (example : mis
operation, and unusual procedure).
"OVER COL"
This occurs when the column oven temperature exceeds the maximum set for the
column oven temperature.
At this time, a buzzer continues to sound and temperature control is stopped.
When the column oven temperature accords with the set value but the set maximum
temperature value is too low, the maximum must be set higher.
If the column temperature is extremely high, turn off the power source switch and
determine and correct the couse. When this message is displayed, press the |CE[ key
after the column temperature becomes lower than the maximum setting. The buzzer
will stop and temperature control will be restarted.
"OVER INJ"
When either the injector temperature exceeds 450°C or the detector temperature
exceeds the maximum setting, this message is displayed and the buzzer sounds. A
temperature such as 450° cannot be set as Injector temperature. Hence, if the Injector
temperature exceeds 450°C, this is clearly abnormal.
Care should be taken that when the detector temperature is greater than the maximum
setting, this message is also displayed.
When this occurs, all temperature adjustments are stopped.
"OVER AUX"
When the AUX 1 temperature exceeds the maximum setting, this message is displayed
and the buzzer sounds.
"ERROR CM"
This occurs when the contents of memory are changed during AC power OFF or the
reliability of the contents is lost because the AC power is OFF during the key-operation.
(This indication will not appear when PROTECT switch is OFF.)
"ERROR CR"
This occurs by some troubles between the data processor and GC. When this message
appears, please shut off the AC power of GC and link the data processor again.
"ERROR 1"
Send error or receive error on current loop transfer interface.
"ERROR 2"
In flow measurement, gas does not flow or flow is too small to be measured.
- 7 4 -
"ERROR 3"
General error. This occurs when the desired function is not input.
"ERROR 4"
General error. The input value is not permissible.
"NON"
In setting a detector, when a number other than 1 to 4 is selected as a detector
number, this message indicates that no detector of that number exists.
"CITP. X X", "INJT. X X", "PROG. X X"
When monitoring the current temperature and program number, if temperature control
has not yet been made, this message is displayed. As soon as the temperature control
is started by pressing the [START] key, the correct value, instead of X X, is dis-
played. •
"SET LDVC"
When listing a program, the number of the output device has not yet been set.
"NOT LINK"
In transmitting to the I/O device (Data Processor), this is displayed when no link
with the external device has been formed yet.
Other messages
This message shows that temperature control is either starting or ongoing.
"LINK OK"
This message is displayed when link with the external device is established ; buzzer
sounds for two seconds.
Error message (Additional)
"LIMIT"
When there is insufficient storage area to extend files or temperature porgram
or more steps are attempted.
"NOTRDY 1"
Start of analysis is attempted before the column oven is in the READY state.
"NOTRDY 2"
Start of analysis is attempted before the C-R2A is in the READY state. (Only when the
C-R2A is connected.)
- 7 5 -
"NOTRDY 3"
Start of analysis is attempted before injector or detector is in the READY state.
"NOTRDY 4"
Start of analysis is attempted when the EXT. RDY is still in the WAIT state.
"INITIAL"
The parameters are initialized when this indication appears.
This occurs when the contents of memory are drastically changed even if PROTECT
switch is ON. All parameters should be set again.
"FAULT"
This occurs when ROM is broken. GC cannot be used under this state. Call for a
service person.
- 7 6 -
Appendix 2 Incorrect Keystroke
Item A. When keys are pressed incorrectly •
A-l Function key
A-2 Numeric key
B. Effective digit of a numerical value
C. Incorrect operation during a dialogue
A. When keys are pressed incorrectly
When keys are pressed incorrectly, proceed as follows.
A-l In case of the function key
Correctly press the function key once again.
Example : INJAUX.2
COLAUX.l
I. TEMP]
If not the COLAUX.l
key but the INJATTX ?
is pressed incorrectly, press the COLAUX.l
key and continue the setting. With the operation shown above, the column initial temper-
ature will become 100 C.
Exception
1. [SHIFT. D| When the SHIFT. D lamp is turned on by pressing this .key, press it again,
2. STOP-W
or press another key once, and the SHIFT. D lamp will be turned off.
When this key is pressed incorrectly, press it again to stop the time
count. If not, the display will remain on a stopwatch.
A-2 In case of the numerical key
1. if the | ENTl key has not yet been pressed.
When the numerical key is pressed incorrectly in setting various numerical values, if the
|ENTl key has not yet been pressed, press the |CE| key to clear the display and then
presjs the correct numerical keys.
Example : COLAUX.l H.TEMPI [E E E FCE"
In this example, in setting the column oven initial temperature to 200°C, the value
300 (°C) was pressed by mis take. Therefore, the [CE| key was pressed to clear the
display. Then, 200 (°C) was entered again. This operation sets 200°C to the column
oven initial temperature.
When pressing a numerical key and the [ENT| key in at order, perform this opera-
tion.
- 7 7 -
2. If the |ENT[ key has already been pressed.
If the incorrect numerical value is entered and the |ENT| key has already been pressed,
the value will be set ; thus, the correct value must be reset.
Example : COLAUX.l
I .TEMPI U f o l f O ] lENT 1 [T.TEMPl
In this example, as the column oven initial temperature was incorrectly set at 300°C,
it was reset to 200°C. During the execution of temperature control the column oven
temperature rises toward 300°C with the first setting, with the next setting, the tem-
perature falls toward 200°C.
B. Effective digit of a numerical value
B-l When only whole integer is effective
For example, in case of setting of file number, detector number polarity and repeated
number, figures below the decimal point in the value are ignored.
| FILE| \T\ Q] [U [ENTl
By pressing keys as shown above "FILE 1" is set.
B-2 Temperature
In case of temperature setting, figures up to the first decimal place can be used as the
value.
[INJ] [ 5 ] [ O ] Q [ O ] 0 [ENTl
Figure below that are ignored.
In case of column oven, up to the second decimal place is effective.
For details refer to the separate manual.
B-3 Time
Time in the time program can be set and displayed up to the second decimal place.
Other programs can be set up to the first decimal place.
- 7 8 -
C. Misoperation during Dialogue
C-l Time program
If setting is made incorrectly during the creation of a Time program, normal error message
is not displayed.
1
2
3
4
5
6
7
Operation
SHIFT. Dj7
LPRG
0
0
1ENT|
Display
TIME ?
9
r 99
999
9999
TIME ?
Although entry of 999 (minutes) was intended, a valuebeyond the setting range, "9999", was entered.
At this time, no time is set ; the final is requested again.
At the time, no time is set ; the final is requested again.
FUNC VL?
INJAUX.;
10
100
FUNC VL ? As the time program cannot affect the injector tem-perature, the function value is requested again.
- 7 9 -