GC 2014en
GC 2014en
GC 2014en
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1 Installation
1.2 Power supply and wiring
6
GC-2014
Q Fuse
The following fuses are used in the GC-2014.
Q Allowing the GC to dry after transport.
Under some transport conditions, condensation may form inside the GC components. To
avoid injection port or detector heater unit short-circuits, allow the unit sufficient time to dry
after transport, and follow the procedure below after installation.
(1) Seal the injection port and detector without attaching a column. (Refer to the figure
below.)
(2) Remove the injection ports (INJ) and detectors (DET) from all configured analytical flow
lines to prevent the heater from turning ON.
(3) Set the column oven temperature to 300 C and start the GC.
(4) Keep the column temperature at 300 C for 2 hours or more.
Fuse, No.
Rated current/voltage
Type *
Classification depending
on IEC127. 115 V model 230 V model
F1, F2 15 A/250 V 10 A/250 V T
F3, F4 5 A/250 V 3.15 A/250 V T
F5, F6 5 A/250 V 5 A/250 V T
CAUTION
GC-2010 may get wet from humidity in some transport conditions. In
such case drying-out is necessary to avoid a short circuit at the
heater in the injection port or the detector.
Thermal
insulation cup
Graphite ferrule
with a wire
Column nut
(or Column nut
of injection port)
When a capillary column connecting
joint is used
2NWI
When a packed column connecting
joint is used
7
1 Installation
1.3 1.
GC-2014
1.3Gas Supply Plumbing
Q Supply gases
The following gases and associated purity values are required to maintain the optimum
performance of the unit.
For detectors other than FID and TCD, refer to the instruction manual corresponding to each detector.
1. Gas types
Carrier gas types
(Packed FID analysis)
Both helium and nitrogen can be used. Nitrogen is more reasonable in terms of price.
(Packed TCD analysis)
Using helium or hydrogen as carrier gas helps analyzing other materials at high
sensitivity. Because hydrogen is flammable, helium is generally used for safety.
However, to analyze helium or hydrogen, use nitrogen or argon as carrier gas. Nitrogen
is convenient to analyze minor components in the air because the nitrogen peak is not
detected when it is used as carrier gas.
(Capillary analysis)
Helium is the most suitable for separation.
Although nitrogen, which is more reasonable than helium, can also be used, the optimum
separation conditions may not be reached.
Makeup gas types
(Capillary FID)
Both helium and nitrogen can be used. Nitrogen has a slightly higher sensitivity.
(Capillary TCD)
The same gas is used as makeup gas and reference gas for capillary TCD.
Select a type of gas by the same method to select carrier gas.
2. Gas purity
Helium (carrier gas, makeup gas) : 99.995 % or higher
Nitrogen (carrier gas, makeup gas) : 99.995 % or higher
Argon (carrier gas, makeup gas) : 99.995 % or higher
Hydrogen (FID detector gas) : 99.995 % or higher
Air (FID detector gas) : Dry air (oil and other organic components eliminated)
Compressed air(must be suppressed by an oil-free
compressor and dehumidified)
CAUTION
1.Gas supply pressure should not exceed the maximum pressure
listed below.
Excessive pressure may break pressure control valve or other parts.
2.When sharing a gas source with other instruments, check
specifications of all instruments to be used including this unit and
supply gas so that requirements of all the instruments can be
satisfied at the same time.
1 Installation
1.3 Gas Supply Plumbing
8
GC-2014
3. Gas supply pressures
Carrier gas 300 - 980 kPa (Hydrogen: 300 - 500 kPa)
Makeup gas 300 - 980 kPa
Hydrogen 300 - 500 kPa
Air 300 - 500 kPa
The relationship of kPa and bar is as follows
100 kPa = 1 bar
Convert units between kPa and kgf/cm
2
as follows.
1 kPa = 1.0
2
10
-2
kgf/cm
2
1 kgf/cm
2
= 98.1 kPa
Convert the units between kPa and psi as follows.
1 kPa = 1.45 10
-1
psi
1 psi = 6.89 kPa
NOTE
1 Installation
1.3 Gas Supply Plumbing
9
GC-2014
Q High pressure gas cylinder precautions
General precautions are provided below.
Consult state and local regulations for specific precautions.
Keep gas cylinders away from the lab, preferably outdoors, but not exposed to direct sun-
light. The area must be well-ventilated. Use tubing to bring the gases to the lab.
The temperature of gas cylinders must not exceed 40 C. Flammable items must be kept at
least 2 m from a gas cylinder.
When using high pressure gases, pay strict attention to ventilation, and perform daily leak
checks. In particular, when using flammable gases (such as hydrogen), never smoke or
allow open flame within 5 m of the equipment. Fire extinguishers must be present.
Secure gas cylinders firmly with cylinder clamps so they cannot fall over. Use oil-free pres-
sure valves only. Never use tubing which has contacted oil. When finished with the gas,
tighten the main valve of the cylinder immediately.
WARNING
HIGH PRESSURE
Gas cylinders are under high pressure. When handling gas cylinders,
instruction and safety measures provided by the gas supplier must be
strictly observed to prevent accidents.
1 Installation
1.3 Gas Supply Plumbing
10
GC-2014
Q Precautions on handling hydrogen gas
WARNING
HYDROGEN GAS PRECAUTIONS
Hydrogen can explode if it is allowed to accumulate in a poorly venti-
lated area.
1.Connect gas lines correctly. Hydrogen is released into the room if
the tubing is accidentally connected to the air inlet.
2.When the unit is not in use, close the main valve of the hydrogen
gas cylinder. Check for leaks at the main valve.
3.Every time the unit is used, check for leaks along the flow line from
gas cylinder to the unit interior.
4.To prevent an explosion due to a hydrogen gas leak, the room in
which the unit is used should be well ventilated. Prohibit the use of
open flame in this room.
5.Close the main valve of the hydrogen cylinder immediately after
completing the analyses. Then, turn OFF the unit and perform
normal shut-down procedures.
WARNING
HYDROGEN GAS HANDLING PRECAUTIONS
The accumulation of hydrogen gas inside the column oven can cause
an explosion.
Close all hydrogen regulator valves not in use and stop gas supply.
(When a manual regulator valve is used, turn its control to make the
pressure zero. For APC, turn off the APC for hydrogen gas.) Seal the
column connection.
When a detector that uses hydrogen gas is not in use
Capillary adapter
Graphite ferrule
with a wire
Column nut
Plug
1 Installation
1.3 Gas Supply Plumbing
11
GC-2014
CAUTION
Hydrogen gas supply precautions
Make sure that the supply pressure to the flow controller does not
exceed 500 kPa.
If the flow controller fails with a hydrogen gas supply pressure over
500 kPa, a dangerous situation exists. Lange amounts of leaking
hydrogen could cause the FID flame to expand out of the detector.
Hydrogen gas is lighter than air. If it leaks, it can accumulate near the
ceiling. Pay strict attention to ventilation so that leaking hydrogen is
vented out of the room and cannot accumulate.
WARNING
Hydrogen carrier gas precautions
If much hydrogen gas is released into the poorly ventilated room, it
may cause the explosion.
1.In order to prevent hydrogen gas accumulate in the room, attach
tubes to split vent, purge vent, TCD vent and ECD vent. Discharge
the gas to open air or a ventilation equipment (such as the draft
chamber).
2.Install the GC in the well ventilated area. (Ex. in the draft chamber)
3.In order to measure hydrogen gas concentration, equip a hydrogen
gas sensor in the room. Keep the hydrogen concentration low.
1 Installation
1.3 Gas Supply Plumbing
12
GC-2014
Q Supply gas tubing
There are two types connections in the Gas Chromatograph: Type M and Type G. Type M
connections are located at the main tubing connections in the instrument interior and exte-
rior. The metal fittings contact directly.
Type G connectors, which are used in high temperature areas, are connected by tightening
three to five aluminum gaskets between the fittings.
Fig. 1.3.1 Joining Type M fittings
Fig. 1.3.2 Joining Type G fittings
Tightening the tubing connections
Tools
2 wrenches 1012 (standard accessory)
Use the 12 mm wrench for Type M connections and the 10 mm wrench for type G
connections.
Fig. 1.3.3 Tightening the joints
MF fitting
MM fitting
GF fitting
Alminum gaskets (3-5 pcs)
GM fitting
1 Installation
1.3 Gas Supply Plumbing
13
GC-2014
Q Tubing between the gas cylinder and gas chromatograph
Fig. 1.3.4 Tubing between the gas cylinder and gas chromatograph
Use tubing with a 3 mm O.D. and 2 mm I.D. between the gas cylinder and gas chromatograph.
The use of a gas filter is highly recommended. Contaminated tubing or poor quality gases
can interfere with baseline stability.
<Option> Gas filter (P/N 221-05619-01)
This absorbs organic compounds and moisture in the supply gas, improving its
purity. The filter can be regenerated by baking in the GC oven at 250 C with
30 mL/min carrier gas purging the filter.
Capacity: Approx. 200 mL
Absorbent: Molecular sieve 5 A
Fig. 1.3.5Gas filter
Gas filter <option>
Gas
cylinder
1 Installation
1.3 Gas Supply Plumbing
14
GC-2014
Q Gas chromatograph tubing connections
Connections are provided on the rear panel of the unit for connecting external tubing.
They are labeled as follows.
Carrier gas ..................... CARRIER
(L and R mean the left and right side of dual INJ.)
Makeup gas ................... MAKE UP
Hydrogen ....................... HYDROGEN
Air .................................. AIR
Fig. 1.3.6 Plumbing (Example of the GC-2014ATF+SPL model)
Flow controller
for the dual FID
Right Left
AFC for SPL AFC for the dual INJ
Supply the carrier gas for the left inlet of the dual INJ to CARRIER L
and the carrier gas for the right inlet of the dual INJ to CARRIER R.
1 Installation
1.3 Gas Supply Plumbing
15
GC-2014
Q Checking for gas leaks
After plumbing the unit, check for gas leaks according to the following guidelines.
(1) Open the main valve of the gas cylinder.
(2) Adjust the gas supply to the specified pressures.
(3) Check for leaks with leak detecting fluid (option) or soapy water on all connections.
Bubbles can be observed if a leak exists.
(4) If a leak is detected:
Further tighten the connection, or retighten it.
Replace the seal material.
(5) Wipe off the leak detecting fluid or soapy water using a wet cloth.
Electronic leak detectors can also be used for hydrogen and helium leaks.
<Option> Snoop Gas leak detecting fluid (P/N 670-11514)
Fig. 1.3.7 Leak detecting fluid
LIQUID LEAK DE
1 Installation
1.3 Gas Supply Plumbing
16
GC-2014
This page is intentionally left blank.
17
2.1 2. 2.
GC-2014
2 Before Use
2.1Setting Analytical Flow Lines
GC-2014 does not operate normally without setting analytical flow lines. Always set
analytical flow lines before using the unit. Refer to Chapter 3. Installing Packed Columns
and Setting Analytical Flow Lines and Chapter 4. Installing Capillary Columns and Setting
Analytical Flow Lines for detailed descriptions.
Setting analytical flow lines creates the following benefits during operation.
1. Conditions of analytical parameters for
each line can be set and monitored.
For example, when the [SET] key of
the gas chromatograph is pressed,
temperatures of columns, injection
ports, and detectors as well as carrier
gas flow rate can be set and monitored
on a single screen.
2. A protective mechanism operates to
foster more stable operation conditions.
For example, when a carrier gas
cylinder becomes empty while TCD is
used, the flow controller detects an
error and automatically lowers the
column temperature and stops
conduction to the TCD filament in order
to prevent damage to the column and
TCD filament.
2 Before Use
2.1 Setting Analytical Flow Lines
18
GC-2014
Q Analytical flow lines
An analytical flow line consists of the flow
controller, injection port, column, detector cell,
and detector amp as shown in Fig. 2.1.1.
During analysis, the flow controller feeds
carrier gas to the injection port, a sample
injected to the injection port goes through the
column to reach to the detector cell, and a
detected signal is amplified by the detector
amp to be outputted.
In order to allow the gas chromatograph to
recognize these units as an analytical flow line,
specification for the connection between them
is necessary.
For regular analysis, specify the combination
between an injection port and detector to
which a column is connected. (Refer to the
following page for setting procedures.)
Connections of the flow controller(s) and injection
port(s) and connections of detector cell(s), and
detector amplifier(s) are specified by a serviceperson
at shipment or installation. They do not need to be
specified for regular analysis.
Fig. 2.1.2 shows a representative example of
the line configuration for packed column FID
analysis using the GC-2014.
In this example, the dual INJ and dual FID are
connected with two columns and the difference
between two FID signals is outputted from the
dual FID amp. Two columns are used because
the dual INJ and dual FID are recognized as a
single unit respectively. However, this is
considered to be a single line.
Outputted Signal
Column
Injection
port
flow
comtrol
Detector
amp
Detector
cell
Fig. 2.1.1 Concept of
analytical flow lines
NOTE
Column(L) Column(R)
L
(L) (R)
Dual INJ R
L R
Dual AFC
Dual FID
amp
Dual FID
Outputted Signal
Fig. 2.1.2 An example of
analytical flow lines
2 Before Use
2.1 Setting Analytical Flow Lines
19
GC-2014
How to set lines
(1) Press the [SET] key then press the
[PF2] key (Line Config).
(2) Move the cursor to the unit to be set in a
line and select a line using [ Y ] [ Z ] keys.
Make sure to specify an injection port
and a detector to which a column is
connected in the same line. Any
number from LINE1 through LINE4 can
be selected.
Precautions for setting analytical flow lines
1. Specify units to be used as part of a line.
Only units specified as part of a line are temperature-regulated.
Gas is controlled only for injection ports (flow controllers) specified as part of a line.
Examples
If an injection port that a column is connected is not specified as part of a line, carrier
gas does not flow. If the column's temperature rises in this condition, the column may be
damaged.
To keep feeding gas to units or maintain their temperature even though they will not be
used for analysis for a while, specify the units as part of a line.
2. Remove the units not in use from a line.
Examples
If a detector without a column stays on a line, it may damage TCD filament or cause an
error such as FID ignition error.
If the setting for the flow controller is turned OFF without removing an injector port
without a column from a line, an error is detected and the protection mechanism works
to lower the column temperature.
If a split/splitless injection port (SPL) without a column is not removed from a line, an
error is detected and the protection mechanism works to lower the column temperature.
CAUTION
Set analytical flow lines correctly.
Incorrectly set analytical flow lines hinder the unit's normal operation
and may also damage columns or detectors at worst.
2 Before Use
2.2 2.
20
GC-2014
2.2Outputting Analog Signals to the Chromatopac
GC-2014 can output analog signals for two channels, and detector signals to be outputted to
each channel can be set using keys. When a detector is changed, output can be changed
using keys without changing the connection on the back of the GC.
Connecting the Chromatopac signal cable
Connect the attached Chromatopac signal cable to the connector (ANALOG OUT1 or 2) on
the back of the GC. (Fig. 2.2.1)
Using this cable, analog signals can be outputted and the Chromatopac can be started when
the GC starts. (Refer to 16.6.9 Setting the link device code)
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Back of the GC
AOC built-in power source
ANALOG OUT 1=Ch1
ANALOG OUT 2=Ch2
Fig. 2.2.1 Connecting the Chromatopac signal cable
2 Before Use
2.2 Outputting Analog Signals to the Chromatopac
21
GC-2014
Setting analog signal output
1. Set a line
(1) Press the [SET] key then press the
[PF2] key (Line Config).
(2) Specify an injection port and detector
to which a column is connected in the
same line.
The screen on the right shows an
example where a column is connected
to the dual INJ and dual FID.
Without specifying a detector in a line, the screen to set analog signal output below does not appear.
2. Set analog signal output.
(1) Press the [DET] key.
(2) The outlined part is a parameter for
analog signal output for all detectors.
Set the parameter following the
description below.
For Background signal save/
compensation and Detector signal
subtraction, refer to Chapter 13
Detector [DET].
Signal Output Port
Specify a connector number to output
analog signals.
(ANALOG OUT 1 = Ch1, ANALOG OUT 2 = Ch2)
Channel number of a detector specified at
the last is effective. (If TCD signal was
outputted to Ch1 formerly and FID signal is
newly specified to be outputted to Ch1 as
shown in the screen on the right, TCD
signal becomes OFF automatically.)
NOTE
2 Before Use
2.2 Outputting Analog Signals to the Chromatopac
22
GC-2014
Signal Attenuation or Signal Range
Names of items automatically change according to types of analog signals as listed below.
Set multiplying power (attenuation rate) of output signals for all types. Change the setting
when the peak obtained by the data processing unit is saturated.
Signal attenuation: When analog signal type is wide
Output signal becomes smaller when the setting is changed from x 1 x 2
-1
x 2
-2
x 2
-3
x 2
-4
Signal range: When analog signal type is linear
Output signal becomes smaller when the setting is changed from x1 x10
-1
x10
-2
x 10
-3
x 10
-4
Analog Signal Type
Set a signal type according to the type of Chromatopac to be connected. If this is set
incorrectly, data cannot be processed correctly.
Wide : C-R8A, C-R7A, C-R7Aplus
Linear: Chromatopacs other than C-R8A, C-R7A, C-R7Aplus
Calibration of analog wide range signal
When the GC is connected to the Chromatopac (C-R8A, C-R7A, C-R7Aplus) with a
chromatopac signal cable and the analog signal type described above is set to Wide,
calibration is necessary in order to match the zero level of the GC and Chromatopac.
Perform calibration in the following cases.
When the GC and Chromatopac are connected for the first time (during installation)
When the GC or Chromatopac is changed with other instrument.
When a connection channel number is changed by switching a connector on the GC side
When a two-channel board is installed on the Chromatopac and a connection channel
number is changed by switching a connector on the Chromatopac side
Calibration is not necessary when a detector is changed (e.g. when signal to be outputted to Ch1 is
changed from TCD to FID).
The following is calibration procedures.
(1) Press the [DET] key on the GC to turn OFF the detector control.
(2) Load the BASIC calibration program.
C-R7A, C-R7Aplus: Type LOAD ZCALIB on the [Win3] key screen.
C-R8A: Type LOAD 8.ZCALIB.BAS when key input is possible.
(3) Press the [RUN] key of the Chromatopac.
(4) Enter the Chromatopac channel number when the following sentence is displayed.
C-R7A, C-R7Aplus: Channel No. (1:CH1 2:CH2) : ?
C-R8A: CH No. (1:CH1 2:CH2) : ?
(5) Enter Y when the sentence below is displayed to save calibration results on the
Chromatopac. If they are not saved on the disk, calibration is required again when
starting the Chromatopac after turning its power off.
C-R7A, C-R7Aplus: Save to disk (Y: Yes N: No) : ?
C-R8A: Save to the disk (Y: Save N: No) : ?
(6) Press the [DET] key of the GC to turn ON the detector control.
NOTE
23
2 Before Use
2.3 2.
GC-2014
2.3Outputting Digital Signals to a Personal
Computer
GC-2014 can be directly connected to a personal computer to output digital signals.
GCsolution software allows a PC to control the unit and take data.
For operation of GCsolution, refer to its instruction manual.
Connecting the RS-232C cable
Connect the RS-232C cable attached to GCsolution workstation to the connector on the
back of the GC. (Fig. 2.3.1)
To connect one PC with more than one GCs, separate RS-232C cables are necessary and
an expanded COM port needs to be attached to the PC.
AOC built-in power source has the same connector. Connect the cables correctly. NOTE
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AOC POWER SUPPLY
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RS-232C
Back of the GC
AOC built-in power source
Fig. 2.3.1 Connection of RS-232C cable
2 Before Use
2.3 Outputting Digital Signals to a Personal Computer
24
GC-2014
Setting transmission parameters
(1) Select 6. GC CONFIGURATION on
the [FUNC] key screen and then select
3. TRANSMISSION PARAMETER.
(2) Set transmission parameters.
Protocol = LEVEL3
Baud rate (bps) = 115200
(3) Press the [PF2] key (Apply).
Turning ON the power of the GC is not
necessary.
NOTE
25
2 Before Use
2.4 2.
GC-2014
2.4Connecting a RS-232C Cable to the
Chromatopac C-R8A
Connecting the GC-2014 and Chromatopac C-R8A with a RS-232C cable allows for various
functions such as printing out parameters of the GC.
For detailed information about C-R8A, refer to its instruction manual.
Connecting RS-232C cable
Connect an optional RS-232C cable to the connector on the back of the GC. (Fig. 2.4.1)
AOC built-in power source has the same connector. Connect the cables correctly. NOTE
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Back of the GC
AOC built-in power source
RS-232C
Fig. 2.4.1 Connection of RS-232C cable
2 Before Use
2.4 Connecting a RS-232C Cable to the Chromatopac C-R8A
26
GC-2014
Setting transmission parameters
Set transmission parameters when performing digital-transmission between the GC and
Chromatopac for the first time. (This is not required for each operation.)
1. Set transmission parameters for the GC
(1) Select 6. GC CONFIGURATION on
the [FUNC] key screen and then select
3. TRANSMISSION PARAMETER.
(2) Set transmission parameters.
Protocol = LEVEL2
Baud rate (bps) = 9600
Stop bit = 1 bit
Parity = EVEN
(3) Press the [PF2] key (Apply).
Turning ON the power of the GC is not
necessary.
2. Set transmission parameters for the C-R8A
(1) Press the [CONFIG] key and then press the [T] key (T:TRS).
(2) Press the [ ] key until the STD2 Port (RS-232C) Setup screen appears.
(3) Set transmission parameters.
MODE = 12917 (Protocol LEVEL2, Stop bit 1 bit, Parity EVEN)
#No. = 8 (logical port number)
BPS = 9600 (baud rate)
(4) After completing setting, press the [EXIT] key and then press the [Y] key to save the
settings.
(5) After changing transmission parameters, reboot the C-R8A to enable the new settings.
Procedures to start digital transmission
After setting transmission parameters, start digital transmission.
1. Start digital transmission.
(1) Type OPEN TRS 8 using the C-R8A keyboard and press the [Enter] key.
(2) The transmission port will open and transmission between the GC and C-R8A will start.
To turn OFF the power of the GC or Chromatopac after opening the transmission port, type CLOSE
TRS 8 using the C-R8A keyboard and press the [Enter] key.
PORT | MODE | #No. | BPS
STD2 | 12917 | 8 | 9600
NOTE
NOTE
27
2 Before Use
2.5 2.
GC-2014
2.5Connecting Auto Injector/Auto Sampler
AOC-20 Series
Connecting the GC-2014 and the auto injector/auto sampler power source unit using an
AOC RS-232C cable allows AOC parameters to be set using the GCs keyboard.
Refer to AOC-20 users manual for details about AOC-20.
Cable connections
Connect the READY/START cable attached to the AOC built-in power source and the AOC
RS-232C cable to the connectors on the back of the GC. (Fig. 2.5.1)
Connect the AOC power cable to the connector on the back of the GC and the auto injector
or auto sampler.
There are two identical RS-232C connectors. Make sure to make the correct connections. NOTE
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3
2
C
O
P
1
L
IN
K
S
T
A
R
T
O
U
T
/R
E
A
D
Y
IN
START I N
READY OUT
AOC POWER SUPPLY
START OUT
Back of the GC
AOC built-in power source
SMAPLER=auto sampler
INJECTOR1=auto injector
AOC power cable
READY/START cable
Wire the cables according to the
numbers on them. Press the
buttons on the terminal when
inserting or removing cables.
Connect the cable to the "AOC"
connector and "RS-232C"
connector on the AOC built-in
power source.
AOC RS-232C cable
Button Cable inlet
1
2
3
4
5
6
Fig. 2.5.1 Connection of the AOC-20 series
2 Before Use
2.5 Connecting Auto Injector/Auto Sampler AOC-20 Series
28
GC-2014
Setting AOC parameters
1. Set a line.
(1) Press the [SET] key and then press the
[PF2] key (Line Config).
(2) Specify AOC1 on the line with the
injection port that the auto injector has
been attached to.
(3) The GC and AOC built-in power source
will be automatically linked.
2. Set AOC parameters.
(1) Press the [OPTION] key. If other option
screens appear, press the [OPTION]
key repeatedly until the AOC
Parameter screen appears.
(2) Set AOC parameters.
Parameters will be transmitted to the
AOC as soon as they are set.
For detailed information about setting AOC
parameters, refer to 15.1 Auto Injector
Parameters or AOC-20 users manual.
If the AOC Parameter screen is not
displayed, check the connection of RS-
232C cable and settings for line
configuration.
NOTE
29
2 Before Use
2.6 2.
GC-2014
2.6Connecting the Relay Terminals
By using the optional relay cable (P/N221-48568-91), relay that operates according to event
commands can be used.
For detailed information about setting events, refer to 16.3 Time Program or 16.5 Direct
Operation.
For example, if the cable is connected to COM and NO found in Fig. 2.6.1, they are
connected by EVENT91 and disconnected by EVENT-91. If it is connected to COM and
NC, they will be connected by EVENT-91 and disconnected by EVENT91.
1 3
1
2
A
N
A
L
O
G
O
U
T
2
A
N
A
L
O
G
O
U
T
1
A
O
C
I
N
J
E
C
I
O
R
1
I
N
J
E
C
I
O
R
2
S
A
M
P
L
E
R
E
V
E
N
T
O
P
T
I
O
N
1
2
3
4
5
6
R
S
-
2
3
2
C
R
S
-
2
3
2
C
O
P
1
L
IN
K
S
T
A
R
T
O
U
T
/R
E
A
D
Y
IN
START I N
READY OUT
AOC POWER SUPPLY
START OUT
Back of the GC
AOC built-in power source
COM
NC
NO
COM
NC
NO
EVENT91
EVENT92
(Red)
(White)
(Black)
(Yellow)
(Blue)
(Green)
Fig. 2.6.1 Connecting a relay cable
2 Before Use
2.6 Connecting the Relay Terminals
30
GC-2014
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31
3.1 3. 3.
GC-2014
3 Installing Packed Columns and Setting Analytical Flow Lines
3.1Installation Location for Packed Columns
Injection ports and detectors for packed columns can be installed in positions described in
Table 3.1.1 and Fig. 3.1.1.
Table 3.1.1 Installation location for injection ports/detectors for packed columns
Installation location numbers indicate the positions of column connecting joints.
Name Possible installation location
Injection ports
Dual INJ 1-2, 2-3, 3-4
Single INJ 1, 4
Detectors
Dual FID 6-7
TCD 9-10
Single DET 5, 6, 7, 8
Fig. 3.1.1Fig. 3.1.1 Installation location for injection ports/detectors for packed
columns (layout viewed from the top of the unit)
3 Installing Packed Columns and Setting Analytical Flow Lines
3.1 Installation Location for Packed Columns
32
GC-2014
Check which units the joints found on the column oven correspond to.
Fig. 3.1.2 shows the layout for the GC-2014ATF+SPL model.
Left and right sides viewed from the front of the unit are indicated as L (left) and R (right)
respectively.
Fig. 3.1.2 Column connecting joints (GC-2014ATF+SPL model)
SPL
Dual INJ
Dual FID
. 4
L R
TCD
. 4
33
3 Installing Packed Columns and Setting Analytical Flow Lines
3.2 3.
GC-2014
3.2Dual-Column Packed FID Analysis
Connecting the left (L) sides and right (R) sides of the dual INJ and dual FID with columns
respectively allows for analysis with the dual-column configuration.
Dual-column configuration is used in following cases.
1. Same type of columns are connected to the left and right sides in order to background-
compensate the increase of the baseline during programmed temperature analysis.
2. Different types of columns are connected to the left and right sides in order to obtain a
different chromatogram when a sample is injected to the left (L) side and right (R) side
of the dual INJ.
Do not cross the columns (L/R). It hinders correct analysis.
Fig. 3.2.1 Dual-column configuration
NOTE
Column (L) Column (R)
Dual FID
L
(L) (R)
Dual INJ
R
L R
Dual AFC
3 Installing Packed Columns and Setting Analytical Flow Lines
3.2 Dual-Column Packed FID Analysis
34
GC-2014
Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install columns and input analytical conditions, refer to the operation
manual.
1. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the dual INJ (DINJ) and dual FID (DFID) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
2. Set the dual AFC.
(1) Press the [FLOW] key.
(2) Set Control mode to Dual.
3 Installing Packed Columns and Setting Analytical Flow Lines
3.2 Dual-Column Packed FID Analysis
35
GC-2014
3. Set the dual FID.
(1) Press the [DET] key.
(2) Set Control mode to Dual.
(3) Set Signal polarity as described below.
: The FID (L) - FID (R) signal is outputted.
(When a sample is injected into the dual INJ (L))
: The FID (R) - FID (L) signal is outputted.
(When a sample is injected into the dual INJ (R))
+
-
3 Installing Packed Columns and Setting Analytical Flow Lines
3.3 3.
36
GC-2014
3.3Single-Column Packed FID Analysis
Connecting either of the left (L) sides or right (R) sides of the dual INJ and dual FID with a
column allows for analysis with the single-column configuration.
Single-column configuration is used in following cases.
1. Background-compensation is unnecessary because the baseline level does not
increase during isothermal analysis.
2. Background-compensation is unnecessary because the baseline level does not
increase so much even during programmed temperature analysis.
1. When single-column configuration is set, unspecified flow controller does not supply gases. Make
sure to remove unspecified column to prevent deterioration.
2. Make sure to stop the FID detector gas supply (hydrogen and air) on unspecified side. (Turn the
control of the flow controller to set the pressure to zero.)
3. Do not cross the columns (L/R). It hinders correct analysis.
Fig. 3.3.1Single-column configuration (FID)
(A column is connected to the left (L) sides.)
NOTE
Column (L)
Dual FID
L
(L) (R)
Dual INJ R
L R
Dual AFC
3 Installing Packed Columns and Setting Analytical Flow Lines
3.3 Single-Column Packed FID Analysis
37
GC-2014
Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install columns and input analytical conditions, refer to the operation
manual.
1. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the dual INJ (DINJ) and dual FID (DFID) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
2. Set the dual AFC.
(1) Press the [FLOW] key.
(2) Set Control mode as described below.
Set to Single L when the column is connected to the left (L) side of the dual INJ and Single
R when it is connected to the right (R) side.
3 Installing Packed Columns and Setting Analytical Flow Lines
3.3 Single-Column Packed FID Analysis
38
GC-2014
3. Set the dual FID.
(1) Press the [DET] key.
(2) Set Control mode as described below.
Set to Single L when the column is connected to the left (L) side of the dual FID and Single
R when it is connected to the right (R) side.
39
3 Installing Packed Columns and Setting Analytical Flow Lines
3.4 3.
GC-2014
3.4Packed TCD Analysis
Connecting the left (L) sides and right (R) sides of the dual INJ and TCD with columns
respectively allows for analysis with the dual-column configuration.
Dual-column configuration is used in following cases.
1. Almost equal columns are connected on the left and right sides to balance TCD's zero
point for analysis.
2. Different types of columns are connected to the left and right sides in order to obtain a
different chromatogram when a sample is injected to the L and R of the dual INJ.
1. Do not cross the columns (L/R). It hinders correct analysis.
2. If left and right columns are extremely different (e.g. liquid quantity, flow rate), zero point may not be
achieved by turning the control on the right side of the GC unit. In this case, adjust the column flow
rate on the side that a sample is not analyzed (reference side).
Fig. 3.4.1 Dual-column configuration (TCD)
CAUTION
1.Carrier gas has to be fed to both of left and right (L/R) sides of the
TCD. Using the TCD without carrier gas will damage the filament.
2.During analysis with a single column, connect a pipe to the other
flow path instead of a column and feed carrier gas.
Column (L) Column (R)
L
(L) (R)
Dual INJ R
Dual AFC
TCD
L R
NOTE
3 Installing Packed Columns and Setting Analytical Flow Lines
3.4 Packed TCD Analysis
40
GC-2014
Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install columns and input analytical conditions, refer to the operation
manual.
1. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the dual INJ (DINJ) and TCD (DTCD) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
2. Set the dual AFC.
(1) Press the [FLOW] key.
(2) Set Control mode to Dual.
3 Installing Packed Columns and Setting Analytical Flow Lines
3.4 Packed TCD Analysis
41
GC-2014
3. Set the TCD.
(1) Press the [DET] key.
(2) Set Signal polarity as described below.
: The TCD (L) - TCD (R) signal is outputted.
(When a sample, which a plus peak is detected, is injected into the dual INJ (L))
: The TCD (R) - TCD (L) signal is outputted.
(When a sample, which a plus peak is detected, is injected into the dual INJ (R))
TCD signals do not necessarily have a plus peak because they are determined by relationship of heat
conduction between a substance to be analyzed and carrier gas. However, the data processing unit
normally calculates the area of a plus peak. When a minus peak is detected, signal polarity needs to
be inverted into a plus peak. In this case, inject a sample into the opposite inlet of the one instructed on
the popup screen shown below.
Signal polarity can be changed using the time program during analysis. (For detailed descriptions
about setting the time program, refer to 16.3 Time Program)
+
-
NOTE
3 Installing Packed Columns and Setting Analytical Flow Lines
3.5 3.
42
GC-2014
3.5Packed Analysis Using the Single DET
To perform glass packed column analysis using the unit with the single DET (single FID,
ECD, FPD, and FTD for packed analysis), move the dual INJ to the front of the single DET
prior to connecting a column.
1. When a SUS column is used, the dual INJ does not need to be moved.
2. If the single packed INJ is installed in front of the single DET, analysis can be performed without
moving the dual INJ. For detailed descriptions, refer to instruction manual of the single packed INJ.
Fig. 3.5.1 Single DET configuration
CAUTION
Dual INJ is set on the single mode so carrier gas is not fed to the
unspecified port (L on the figure above). Do not connect a column to
the port.
L
(L) (R)
Dual INJ R
Dual AFC
Dual FID/TCD
Column
L R
Single DET
NOTE
3 Installing Packed Columns and Setting Analytical Flow Lines
3.5 Packed Analysis Using the Single DET
43
GC-2014
Procedures to move the dual INJ
Move the dual INJ following the procedures below. Perform backward processes to return it
to its original position.
(1) Set the dual INJ temperature at room temperature or lower and wait until it becomes
40 C or less.
(2) Turn OFF the power of the GC unit.
(3) Remove the column connected to the dual INJ.
(4) Detach wiring connected to the dual INJ in order to improve workability.
(5) Unfasten the three screws that fasten the dual INJ (Fig. 3.5.2 (a)) and pull the dual INJ
upward.
(Sems screws with a flat washer are used. Be careful not to drop flat washers.)
(6) Take out the heat insulator laid on the bottom of the dual INJ using tweezers or other
similar tools.)
WARNING
Carry out the procedures after the injection port becomes 40 C or
less to prevent burns.
CAUTION
Some insulation materials include ceramic fibers.
Refer to When Handling Insulation of Introduction in the GC-2014
Operation manual before you handle these materials.
CAUTION
When cutting a heat insulator, handle a cutting knife, etc. with care.
Fig.3.5.2 (a)
Screws (sems screws + flat washers)
Single DET
Dual INJ
3 Installing Packed Columns and Setting Analytical Flow Lines
3.5 Packed Analysis Using the Single DET
44
GC-2014
(7) Cut out the heat insulator using a cutting knife, etc. as shown in Fig. 3.5.2 (a).
(The heat insulator is approximately 3 cm thick. Cut the sheet metal on the bottom of the
heat insulator as well.)
(8) Move the cut heat insulator to the left.
(9) Insert the dual INJ on top of the heat insulator that has been taken out in step (6) and
fasten it with three screws. (Refer to Fig. 3.5.2 (c)).
(10) Connect the wiring that has been removed in step (4) to the dual INJ as it was originally.
Fig.3.5.2 (b)
Fig.3.5.2 (c)
50mm
Screws (sems screws + flat washers)
3 Installing Packed Columns and Setting Analytical Flow Lines
3.5 Packed Analysis Using the Single DET
45
GC-2014
Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install columns and input analytical conditions, refer to the operation
manual.
1. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the dual INJ (DINJ) and single DET (PECD in the screen below) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
2. Set the dual AFC.
(1) Press the [FLOW] key.
(2) Set Control mode as described below.
Set to Single L when the column is connected to the left (L) side of the dual INJ and Single
R when it is connected to the right (R) side.
3 Installing Packed Columns and Setting Analytical Flow Lines
3.5 Packed Analysis Using the Single DET
46
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47
4.1 4. 4.
GC-2014
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.1Installation Location for Capillary Columns
Injection ports and detectors for capillary columns can be installed in positions described in
Table 4.1.1 and Fig. 4.1.1.
(Injection ports and detectors that can be used for packed columns are included.)
Table 4.1 Installation location for injection ports/detectors for capillary columns
Installation location numbers indicate the positions of column connecting joints.
Name Possible installation location
Injection ports
SPL 1, 4
WBI 1, 4
Dual INJ 1-2, 2-3, 3-4
Single INJ 1, 4
Detectors
Dual FID 6-7
Single DET 5, 6, 7, 8
FTD-2014c 11, 12
TCD 9-10
Fig. 4.1.1 Installation location for injection ports/detectors for capillary columns
(layout viewed from the top of the unit)
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.1 Installation Location for Capillary Columns
48
GC-2014
Check which units the joints found on the column oven correspond to.
Fig. 4.1.2 (a) and (b) show the layout for the GC-2014ATF+SPL model and GC-2014AFsc
model. Left and right sides viewed from the front of the unit are indicated as L (left) and R
(right) respectively.
Fig.4.1.2 (a) Column connecting joints (GC-2014ATF+SPL model)
Fig.4.1.2 (b) Column connecting joints (GC-2014AFSC model)
SPL
Dual INJ
Dual FID
. 4
. 4
Dual TCD
. 4
52.
Single FID
49
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.2 4.
GC-2014
4.2Capillary Analysis Using the Dual FID
(When a detector adapter with purge is used)
To perform capillary analysis using a unit with the dual FID, makeup gas needs to be
supplied to the FID that a column is connected to.
In order to supply makeup gas, attach a detector adapter with purge (P/N 221-34012-91) to
the joint of the dual FID. Connect the purge piping of the adapter to the dual INJ so that
makeup gas is supplied from the dual AFC through the dual INJ.
(The dual AFC is off the line and operates as an independent mass flow controller.)
Although an adapter and column are connected to the right (R) sides of the dual INJ and
dual FID in the figure below, they can be connected to either side (L/R).
Fig. 4.2.1 Dual FID (detector adapter)
Column Detector
adapter
with purge
Dual FID
L
(L) (R)
Dual INJ R
L
R
Dual AFC
SPL
AFC
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.2 Capillary Analysis Using the Dual FID (When a detector adapter with purge is used)
50
GC-2014
Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install an adopter and columns and input analytical conditions, refer to the
operation manual.
1. Change the dual AFC configuration.
(1) Select 6. GC CONFIGURATION on the [FUNC] key screen and then select 9. Other
configuration.
(2) Specify AMC.LR at DAFC unit.
2. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the SPL and dual FID (DFID) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
If the dual AFC is specified for AMC.LR, the indication of DINJ disappears. NOTE
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.2 Capillary Analysis Using the Dual FID (When a detector adapter with purge is used)
51
GC-2014
3. Set the makeup gas flow rate.
(1) Press the [OPTION] key.
(2) Set AMC.L when the detector adopter is connected to the left (L) side of the dual INJ
and set AMC.R when it is connected to the right (R) side.
Start control and set the makeup gas flow rate and gas type.
4. Set the dual FID.
(1) Press the [DET] key.
(2) Set Control mode as described below.
Set to Single L when the column is connected to the left (L) side of the dual FID and Single
R when it is connected to the right (R) side.
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.3 4.
52
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4.3Capillary Analysis Using the Dual FID
(When a makeup gas flow controller is used)
To perform capillary analysis using a unit with the dual FID, makeup gas needs to be
supplied to the FID that a column is connected to.
In order to supply makeup gas, the optional makeup gas flow controller (P/N 221-70877-91:
1 flow path, 221-70877-92: 2 flow paths) are used.
Prior to installing a column, install the detector adapter (P/N 221-33193-91) to the detector's
joint.
Although an adapter and column are connected to the right (R) side of the dual FID in the
figure below, they can be connected to either side (L/R).
Fig. 4.3.1 Dual FID (flow controller)
Column
Dual FID
L
(L) (R)
Dual INJ R
L
R
Dual AFC
SPL
AFC
Detector
adapter
Hydrogen
Makeup gas
Flow controller
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.3 Capillary Analysis Using the Dual FID (When a makeup gas flow controller is used)
53
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Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install an adopter and columns and input analytical conditions, refer to the
operation manual.
1. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the SPL and dual FID (DFID) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
2. Set the dual FID.
(1) Press the [DET] key.
(2) Set Control mode as described below.
Set to Single L when the column is connected to the left (L) side of the dual FID and Single
R when it is connected to the right (R) side.
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.4 4.
54
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4.4Capillary TCD Analysis
To perform capillary analysis using a unit with the TCD, makeup gas needs to be supplied to
the TCD joint that a column is connected to and carrier gas (called reference gas) also
needs to be supplied to the TCD joint that a column is not connected.
In order to supply makeup gas, install the detector adapter with purge (P/N 221-34012-91) to
the TCD joint. Connect the purge piping of the adapter to the dual INJ so that makeup gas is
supplied from the dual AFC through the dual INJ.
(The dual AFC is off the line and operates as an independent mass flow controller.)
Reference gas is supplied from the dual AFC when the dual INJ and TCD are connected
with a MF-MF joint.
The figure above shows an example where makeup gas and reference gas are connected to
the left (L) and right (R) sides of the dual INJ respectively and a column and reference gas
piping are connected to the left (L) and right (R) sides of the TCD respectively. They can be
connected to either side (L/R).
Fig. 4.4.1Capillary TCD
CAUTION
1.Carrier gas (makeup gas and reference gas) has to be fed to both
of left and right (L/R) sides of the TCD. Using the TCD without
carrier gas will damage the filament.
2.When makeup gas and reference gas are supplied from the dual
AFC, TCD filament's protection mechanism does not work even if
an error occurs.
MF-MF
piping
L R
Column
Detector
adapter
with purge
TCD
L
(L) (R)
Dual INJ
R
Dual AFC
SPL
AFC
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.4 Capillary TCD Analysis
55
GC-2014
Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install columns and input analytical conditions, refer to the operation
manual.
1. Change the dual AFC configuration.
(1) Select 6. GC CONFIGURATION on the [FUNC] key screen and then select 9. Other
configuration.
(2) Specify AMC.LR at DAFC unit.
2. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the SPL and dual TCD (DTCD) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
If the dual AFC is specified for AMC.LR, the indication of DINJ disappears. NOTE
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.4 Capillary TCD Analysis
56
GC-2014
3. Set the makeup gas/reference gas flow rates.
(1) Press the [OPTION] key.
(2) The left (L) side of the dual INJ corresponds to AMC.L and the right (R) side
corresponds to AMC.R. Start controlling both AMC.L and AMC.R and set the flow rates
and gas types according to the connection of detector adopter and reference gas
piping.
4. Set the TCD.
(1) Press the [DET] key.
(2) Set Signal polarity as described below.
: The TCD (L) - TCD (R) signal is outputted.
(When a column is connected to TCD (L) and a sample that a plus peak is
detected is injected)
: The TCD (R) - TCD (L) signal is outputted.
(When a column is connected to TCD (R) and a sample that a plus peak is
detected is injected)
+
-
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.4 Capillary TCD Analysis
57
GC-2014
TCD signals do not necessarily have a plus peak because they are determined by relationship of heat
conduction between a substance to be analyzed and carrier gas. However, the data processing unit
normally calculates the area of a plus peak. When a minus peak is detected, signal polarity needs to
be inverted into a plus peak.
Signal polarity can be changed using the time program during analysis. (For detailed descriptions
about setting the time program, refer to 16.3 Time Program.)
NOTE
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.5 4.
58
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4.5Single DET
To perform capillary analysis using a unit with the single DET (single FID, ECD, FPD, and
capillary FTD), makeup gas is used as described below.
Install the detector adapter to the detector joint then install a column. Detector adapter
comes with all single DET units listed above.
A makeup gas flow controller comes with them.
Makeup gas is unnecessary.
Fig. 4.5.1Single DET (In case of FID)
Single FID, ECD, and capillary FTD
FPD
Column
Detector
adapter
Single DET
SPL
AFC
Hydrogen
Makeup gas
Flow controller
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.5 Single DET
59
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Setting analytical flow lines
Setting analytical flow lines is described below.
For procedures to install columns and input analytical conditions, refer to the operation
manual.
1. Set a line.
(1) Press the [SET] key and then press the [PF2] key (Line Config).
(2) Set the SPL and single DET (SFID in the screen below) on a same line.
LINE1 is specified in the example below. Lines 1 through 4 can be selected.
4 Installing Capillary Columns and Setting Analytical Flow Lines
4.5 Single DET
60
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61
5.1 5. 5.
GC-2014
5 Analysis
5.1Analysis Flow Chart
For detailed descriptions about analysis procedures, refer to the operation manual.
5.1.1 Preparation
Injection port preparation Select an injection port suitable to the sample injection method.
Confirm that the septum and insert are properly attached.
Check dirt on the septum and the number of injections and replace it
when necessary (after approximately 100 injections).
Column preparation Attach the column to the injection port and detector correctly.
When the above preparations are complete, turn ON the GC (power switch on the lower
right side of the GC).
5.1.2 Setting Parameters
Set the column information Set parameters on the [FLOW] key screen. Set the column inner diameter,
and the flow rates column length, and the film thickness on [Column] (PF menu). For
the SPL and WBL, set the purge flow rate on [Purge] as well.
(When the column flow rate is set by the AFC, changing the column
temperature changes the column flow rate.)
Set the temperature of the Set the temperatures on the [INJ] and [DET] key screens. (If the detector
detector and the injection port is set to Off, turn it On.) When the APC is used, set hydrogen, air,
makeup gas, etc. from [DET Gas] (PF menu).
Set the COL temperature and From the screen of the [COL] key, set the column initial temperature
the temperature program and the temperature program. Temperature settings must be within
the allowable column and detector ranges.
Start GC control Press the [SYSTEM] key to display the main screen.
Press [Start GC] (PF menu) to start GC control.
Press the [MONIT] key, and ensure that the temperature of each
zone, the gas flow rate, the gas pressure, etc. are correct.
Set the detector From the screen of the [DET] key, set the range and the time filter
constant.
Ensure that the temperature of the detector is rising, then ignite the
FID or set the TCD current value.
When all parameters reach their respective setup values, the STATUS indicator light
becomes green and the system is ready for analysis.
When the dual packed INJ is used, a monitor injection screen to show the inlet to be used
appears.
The default zero parameter, Zero at Ready zeroes the detector sig-
nal when the GC is ready.
5 Analysis
5.1 Analysis Flow Chart
62
GC-2014
5.1.3 Analysis
Set the data processing Perform the required settings for the data processing unit, such as
unit specifying the processing parameters.
Check the baseline Press the [MONIT] key, and ensure that the baseline is stable.
When the baseline is stable, you can start analysis. Press [Zero
Adg] (PF menu) to zero the detector output if necessary.
Inject the sample Aspirate the sample in the syringe, inject it into the GC injection port,
and press [START] to analyze it.
WARNING
Wear protective goggles when using a
syringe to inject samples.
The syringe plunger could be expelled
due to injection port back pressure.
Sample could get into the eyes.
By holding and supporting the plunger
from the side with your middle finger,
you can smoothly inject the sample and
keep the plunger in the syringe.
Do not bend the plunger when holding
the syringe in this position.
Hold here
(Example)
How to hold a syringe
when injection
63
5 Analysis
5.2 5.
GC-2014
5.2Notes for Analysis
Q Analytical column
Make sure that carrier gas is flowing through the column before increasing the column
oven temperature because the column cannot separate compounds properly when its
liquid phase is oxidized. This is especially important for polar columns. Press the
[SYSTEM] key and set a start time so that carrier gas flows for the set time prior to
temperature control of the heated zones.
Selection of the analysis column is very important in GC analysis. In general, select a
liquid phase whose polarity and chemical characteristics are similar to those of the
analysis target compound to obtain good peak shape. However, highly polar columns
require low temperatures and do not last long.
Therefore, when analyzing an unknown sample, begin by analyzing it on a neutral column
with a higher allowable temperature limit. Switch to a more polar column if necessary.
Q Sample injection modes(Capillary column analysis)
[Split injection]
In capillary columns, the inner diameter is small and the sample load capacity is low. Unlike
packed columns, only a small (1-2 L) amount of sample can be injected at onetime. The
split injection mode only allows part of the injected sample to enter the column. This method
is useful for samples of high consentration or about which nothing is known.
Try to perform a split injection method first. Set the split ratio to approximately 1:50. If the
target peak is too large, increase the split ratio. If the target peak is too small or cannot be
detected, decrease the split ratio. Select a proper split ratio in this way.
If the peak is still small with a split ratio set to 1:10 or less, try the splitless injection method.
[Splitless injection]
In the splitless injection method, almost all of the sample amount injected is introduced in the
column by temporarily suspending the split flow.
This method is effective for analyzing a low concentration sample which cannot be easily
analyzed by the split injection method.
To reduce band broadening and sharpen peaks, create a temperature ramp program. The
column initial temperature is set to a temperature lower than the boiling point of the sample
solvent.
[Direct injection]
In the direct injection method, almost the entire amount of injected sample is introduced into
a wide bore column. Because the inner diameter of the wide bore column is 0.53 mm or
more, separation is not as good as that of a column with smaller inner diameter. Because
the peak shape is broad, sensitivity may not be good enough.
For the direct injection method, the WBI (Wide Bore Injection) injection port is required.
5 Analysis
5.2 Notes for Analysis
64
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Q Setting the heated zone temperatures
The temperature of the injection port, the column oven and the detector are set individually.
Usually, the injection port and the detector are set to a temperature 20 C higher than the
column.
Never set the column temperature higher than the detector because the detector could
become contaminated.
When creating a temperature program, be careful not to set the final oven temperature
higher than that of the detector.
Q Column temperature program
Use a temperature program mainly to analyze samples with a wide boiling point range.
When developing analytical conditions for an unknown sample or a sample which will gener-
ate an unpredictable elution attend, use an initial program with a temperature increase rate
of approximately 10 C/min. Based on the results, check the temperature range in which the
peaks appear, then examine the analytical conditions. This procedure facilitates time pro-
gram development.
Q Injection counter
The injection port septum and the glass insert are required to be inspected and replaced
periodically. The GC-2014 probides a function which counts the number of injections. When
the number of injections exceeds the limit, you are prompted to perform maintenance. (What
is actually counted is the number of START times.)
Select the analysis counter on the [DIAG] key screen to set and reset the counter limit. Set
the limit to perform maintenance on a regular basis.
The septum/glass insert replacement cycle varies, depending on the analytical conditions
and samples. If the glass insert is easily contaminated (when analyzing non-volatile com-
punds for example), set a low counter limit. On the other hand, when analyzing cleaner sam-
ples, the limit can be increased.
Q Starting up the GC
Turn on the power and/or press the [SYSTEM] key to display the GC starup screen. On this
screen, specify the files used for instrument startup and instrument cleaning (column bake -
out).
Press [Start GC] (PF menu) to start temperature control of each heated zone accoding to the
parameters set in the file.
A start up method should be used to initialize the system once it has been turned on. Set the
start up method to auto to start the file as soon as the power is on; this helps with instru-
ment recovery after a power failure.
The initial step in the startup method should be turning on the carrier gas flow. After a set
time, increase the injection port and detector temperatures. The column oven temperature
can then be set to increase. The oven temperature increases last to protect the column from
damate and the detctor from contamination. The GC-2014 is designed to control the temper-
atures so that the column temperature never exceeds the detector temperature, even if all
temperatures are set to increase at the same time.
A clean up method uses higher oven temperatures than those used for the analysis. After
set bake-out time, return the temperatures to their normal analytical parameter.
5 Analysis
5.2 Notes for Analysis
65
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Q Shutting down the GC
To shut down the system, select [Stop GC] (PF menu) on the [SYSTEM] key screen. Then,
the system stops temperature control after the period of time set as the stop time, flows the
carrier gas for the period of time set as the flow-off time, then stops.
When shutting down the GC, the temperature of each part should be decreased at first, then
the carrier gas should be stopped so that the column can be protected. It is convenient to
use the stop time and the flow-off time.
Do not turn off the power, before select [Stop GC] (PF menu).
When shutting down the GC, the heated zones are cooled, and then the carrier gas flow is
turned off. To accomplish these in the correct sequence automatically, use a stop time (this
stops temperature control at the set time) and flow off time (turns off carrier gas flow at the
set time). Do not turn off the GC without first selecting [Stop GC] (PF menu).
Q Obtaining reproducible analysis results
Follow these suggestions to obtain reproducible results:
Using an AOC-20i auto injector is suggested in order to inject a sample to obtain highly
reproducible results.
Do not increase the temperatures of unused injection ports.
The GC is designed to perform optimally at room temperatures of 18-28 C. Room tem-
peratures above 28 C will negatively inpact reproducibility.
5 Analysis
5.2 Notes for Analysis
66
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This page is intentionally left blank.
67
6.1 6. 6.
GC-2014
6 Basic Key Operation
6.1Keypad Description and Operation
The keypad functions control the unit, and displays the operational status.
START STOP DIAG SYSTEM
STATUS TEMP FLOW
PF1 PF2 PF3
MONIT SET
COL FUNC
FLOW 7 8 9
INJ 4 5 6
DET 1 2 3
OPTION 0
HELP CE ENTER
ON
OFF
START/
STOP key
Starts/stops analysis.
Screen Displays 16 lines of
information at a time on
the large display area.
Displays the list of
frequently accessed
items.
Monitors the GC status
and the chromatogram.
MONIT key
SYSTEM
key
Starts/stops the GC.
DIAG key Executes and allows
diagnosis settings.
PF key Selects PF (programmable
functions) displayed at the
bottom of the screen.
Toggle key Toggles among PF items
displayed.
Toggle key
+
Cursor
keys
Sets On/Off of backlight
and adjustment of
contrast.
Cursor
keys
Moves the cursor up,
down, left and
right respectively.
Numeric
keys
Inputs numeric values.
ENTER
key
Validates input or
selection.
CE key Clears a numeric input
or error.
HELP key Explains currently
displayed items.
UNIT keys Displays the setup
screen for the zone
indicated on the key.
FUNC key Displays items
which are not
frequenty used.
SET key
STATUS/
TEMP/
FLOW lamp
Indicates the status of
the entire GC, the
heater and the flow
controller, respectively.
S T A T U S
lamp
TEMP lamp
Flow lamp
S Y S T E M
key
DIAG key
PF key
Toggle key
Cursor keys
ENTER
CE key
START key
STOP key
Screen
MONIT key
FUNC key
UNIT key
HELP key
+
6 Basic Key Operation
6.1 Keypad Description and Operation
68
GC-2014
6.1.1 Keypad operation
The keypad is used to operate the system and make parameter settings. The table below
shows the function of each key.
Name Function
START key Starts the temperature program, pressure/flow rate program and time program.
If a Pre-Run program is set, the Pre-Run program starts.
STOP key Stops the program.
DIAG key Performs unit self-diagnosis.
Also, used for maintenance functions such as confirmation of various logs, part
replacement status, and standard signal out put.
SYSTEM key Starts/stops GC.
Manages the analytical condition file.
PF key Selects the PF menu displayed at bottom of the screen.
(PF = programmable function)
Toggle key Toggles through the PF menu displayed at bottom of the screen.
MONIT key Monitors the GC status and analysis status.
Displays the GC temperature, pressure and flow rate status for each heated zone,
as well as chromatograms.
SET key Accesses commonly-used items, such as temperature, pressure and flow rate for
each component on one screen.
Manages the analytical condition file like the [SYSTEM] key.
FUNC key Accesses less frequently used items.
COL key Sets the oven temperature program.
FLOW key Sets the carrier gas flow rate parameters, such as pressure, flow rate and split
ratio.
INJ key Sets the temperature of injection port (or temperature program for an OCI/PTV).
DET key Sets the detector temperature, range and current or other detector-related param-
eters.
OPTION key Sets the parameters for auto injector, AUX temperature controller, AUX APC, AUX
AMC, and CRG.
HELP key Describes the procedure and sugggests valid parameter ranges.
Jumps to a desired item using an index function.
Cursor key
[ ], [ ], [ ] and [ ]
Moves cursor up, down, left and right.
A blinking cursor indicates the location of parameter value entry.
[ ] and [ ] keys may be used to change the selection.
Numeric keys
[0] ~ [9]
Enter numeric values.
Clear key
[CE] key
Clears the current numeric value.
Clears display and alarm during an error.
ENTER key Validates parameter input or item selection.
+
-
6 Basic Key Operation
6.1 Keypad Description and Operation
69
GC-2014
6.1.2 Screen
The areas of the 16-line screen display a variety of items. These items are divided by lines
on the screen.
If all items cannot be displayed on one screen, and are displayed in the message
line. Scroll through the screen by moving the cursors.
Q [Return] (PF menu)
[Return] (PF menu) displayed in the PF menu line returns the display to the previous screen.
[Return] (PF menu) is displayed in PF1.
Q Actual and set values
Actual (current) values are highlighted, while set values are underlined. The actual value
blinks when it is NOT READY (the actual value has not reached the set value). When the
values are equal (READY status), the actual value stops blinking.
When the DINJ is used When the SPL is used
Fig. 6.1.1
When the DINJ is used When the SPL is used
Fig. 6.1.2
Displays the screen
title and the GC
status (READY,
NOT READY or
RUN etc.).
Displays a message
or error about the
operating procedure.
Displays the menu
selected by the [PF]
key.
Actual values Set values
Actual values Set values
6 Basic Key Operation
6.1 Keypad Description and Operation
70
GC-2014
6.1.3 Status indicators
Three status lights indicate the GC status regardless of the screen display. The STATUS,
TEMP and FLOW lights indicate the GC status, the temperature control status and the gas
control status, respectively. Light color and illumination are also used to indicate instrument
parameter status.
Q STATUS indicator
Q TEMP indicator
Q FLOW indicator
Color Status Meaning
Off Power is OFF.
Green
On System is ready.
Blinking Program, like the temperature program, are executing.
Yellow
On System is OFF. Alternatively, the system is ON, but is not ready.
Blinking Diagnosis, baking or flow controller calibration is being executed.
Red On An error has occurred in system.
Color Status Meaning
Off Temperature control is not performed.
Green
On All temperature controlled zones are ready.
Blinking Temperature program is running.
Yellow
On One of the temperature controlled zones is not ready.
Blinking Temperature program is finished, and system is being cooled.
Red On An error related to temperature control has occurred.
Color Status Meaning
Off Gas control is not performed.
Green
On All gas control lines are ready.
Blinking
Pressure/flow rate program is running, it is sampling time, or
high pressure injection is occurring.
Yellow
On One of the gas control lines is not ready.
Blinking
Pressure/flow rate program is finished, and default values are
being set.
Red On An error related to gas control has occurred.
71
6 Basic Key Operation
6.2 6.
GC-2014
6.2Adjusting The Display
In the following procedure, [Toggle] + [ ] key indicates that [ ] key is pressed while pressing and
holding the [Toggle] key.
Turn the backlit LCD display on and off by pressing [Toggle] + [ ] to turn it off and [Toggle]
+ [ ] to turn it on.
When the keypad is not in use, turning the backlit LCD display off is recommended, to pro-
long the life of the display.
The display turns off automatically with the backlit display saver (See 16.6.11 Other
Settings). When the display turns itself off, turn it back on by pressing any key.
To adjust the contrast the contrast, stand in front of the screen and press the [Toggle] + [ ]
or [ ] keys.
Fig. 6.2.1
NOTE
NOTE
Change the selection by
pressing the [ ] and [ ] key.
In this example, the selection
changes in this order:
On Off On ...
Press the [ENTER] key to
validate the selection.
File
Displays the file list to change to another method file.
On this sub screen, select files to load, edit, copy, initialize and rename.
8.2
Clean Up
Sets clean up parameters.
In system ON status, select direct operation (PF menu) to run the clean up.
7.2
Start Seq
Sets the parameters for the next GC start up.
Start time, detector and clean up parameters on this sub screen are
immediately reflected on the [SYSTEM] key main screen.
7.3
Stop Seq
Sets the stop procedures.
This item is not displayed in system ON status.
7.4
Maint INJ
Prepares the GC for maintenance of the injection port (replacement of
septum, glass insert, etc.) .
When GC is ready for maintenance, the message GC is ready for maintenance
appears.
4.3 General
maintenance
procedures
in the operation
manual
Anal.
Restores the GC for analysis after performing injection port maintenance.
When pressed after maintenance of injection port is completed.
7 Starting and Stopping the GC [SYSTEM]
7.2 7.
82
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7.2Specifying Clean Up Parameters
7.2.1 Screen Description
Select [Clean Up] (PF menu) from the [SYSTEM] key main screen to display the clean up
parameter setup screen shown in Fig. 7.2.1. The parameters set for the clean up program
are set by including Clean Up Para as part of the GC start procedure.
Clean up should be performed to eliminate contamination before analysis.
Reform the clean up when the gas chromatograph has not been used for a while or if a new
column has been installed.
(a) DINJ (b) SPL
Fig. 7.2.1 Setting the clean up parameters
7 Starting and Stopping the GC [SYSTEM]
7.2 Specifying Clean Up Parameters
83
GC-2014
7.2.2 Parameter list
Q Main screen of clean up
COLUMN OVEN
TEMP
Range: 0.0400.0 C, Default: 25.0 C
Sets the default value of the column oven temperature for the clean up method.
The clean up oven temperature should be 20 to 30 C higher than the temperature
program used for actual analysis. (Neither temperature should exceed the maximum
temperature indicated on the column).
If the clean up oven temperature exceeds the maximum column temperature, indicate
that the regular analysis parameters should be used for clean up by setting Analysis
Para for the start procedure.
FLOW
Dual packed INJ (DAFC is used)
L column flow rate, R column flow rate
Range: 0.0100.0 ml/min, Default: 50.0 ml/min
Sets the initial pressure for the clean up column flow rate.
SPL(AFC is used)
INLET PRESS
Range: 0.0970.0 kPa (Refer to Fig. 12.2.5.), Default: 100.0 kPa
Sets the default value of the column inlet pressure for the clean up method.
PURGE FLOW RATE
Range: Refer to Fig. 12.2.15, Default: 3.0 ml/min
Sets the septum purge flow rate for the clean up method. The septum purge removes
contamination in the injection port near the septum. If the split ratio is set to -1.0, the
total flow rate remains fixed regardless of to the oven temperature.
SPLIT RATIO
Range: -1.0/0.09999.9, Default: -1.0
Sets the split ratio for the clean up method.
Set the split ratio to -1.0 for the total flow rate to remain fixed regardless of the oven
temperature.
INJECTION PORT
Temperature
Range: 0.0400.0 C, Default: 250.0 C
Sets the injection port temperature for the clean up method.
DETECTOR
Temperature
Range: 0.0400.0 C (FID), Default: 250.0 C
Sets the detector temperature for the clean up method.
For any detector other than an FID, its set temperature must be within the valid range of
the detector.
Makeup flow rate
The range and default value depends upon the kind of detector. Refer to the values
given for each detector.
This sets the flow rate of an inert gas supplied to the detector side during clean up.
AMC.L, AMC.R
Flow rate
Range: 0.0100.0 ml/min, Default: 50.0 ml/min
Sets the AMC.L, R flow rate for the clean up method. (Usually equivalent to the flow rate
of the inert gas supplied to the detector.)
7 Starting and Stopping the GC [SYSTEM]
7.2 Specifying Clean Up Parameters
84
GC-2014
This item is only valid when DAFC is set to AMC.LR.
AUXAPC
Pressure
Range: 0.0970.0 kPa, Default: 100.0 kPa
Sets the AUX APC pressure for the clean up method.
This item is only valid when an AUX APC has been installed.
AUXAMC
Flow rate
Range: 0.0100.0 ml/min, Default: 50.0 ml/min
Sets the AUXAMC flow rate for the clean up method. This item is only valid when an
AUX AMC has been installed.
When a manual flow controller is used, turn the control of the pressure regulator to set a pressure.
Q Clean up column oven temperature program
(The clean up temperature program consists of a single program ramp.)
CLEAN UP RATE
Range: END/-250.00250.00 C/min, Default: END
Sets the rate of column temperature increase for the clean up program.
CLEAN UP TEMP
Range: 0.0450.0 C, Default: 25.0 C
Sets the final temperature for the column oven temperature clean up program.
Do not exceed the maximum column temperature.
CLEAN UP TIME
Range: 0.009999.99 min, Default: 0.00 min
Sets the final temperature hold time for the clean up program.
Q Clean up column Inlet pressure program (when the AFC control mode is pressure)
(The clean up pressure program consits of a single program ramp.)
CLEAN UP RATE
Range: END/-400.00400.00 kPa, Default: END
Sets the rate of column inlet pressure for the clean up program.
CLEAN UP PRESS
Range: 0.0970.0 kPa (Refer to Fig. 12.2.5.) , Default: 0.0 kPa
Sets the final pressure for the column inlet pressure clean up program.
CLEAN UP TIME
Range: 0.009999.99 min, Default: 0.00 min
Sets the final pressure hold time for the clean up program.
Q Clean up flow rate program (when the DAFC and AFC control mode is flow rate)
(The clean up total flow rate program consists of a single program ramp.)
CLEAN UP RATE
Range: END/-400.00400.00 ml/min
2
, Default: END
Sets the rate of total flow increase for the clean up program.
CLEAN UP FLOW RATE
Range: 0.0100.0 ml/min (DAFC), 0.01,200.0 ml/min (AFC)
(refer to Fig. 12.2.5), Default: 50.0 ml/min
Set the final flow rate for the total flow rate clean up program.
NOTE
7 Starting and Stopping the GC [SYSTEM]
7.2 Specifying Clean Up Parameters
85
GC-2014
CLEAN UP TIME
Range: 0.009999.99 min, Default: 0.00 min
Sets the final flow rate hold time for the clean up program.
7.2.3 PF menu
PF menu Description
Reference
section
Temp Prog Sets the column oven temperature for the clean up program. 11.2
Press Prog
Sets the column inlet pressure for the clean up program.
It is displayed when the control mode is pressure on the [FLOW] key
screen of the AFC.
12.5.5
Flow Prog
Sets the flow rate for the clean up program.
Sets the column flow rate program for the DAFC and the total flow rate
program for the AFC.
Display is possible for the DAFC and when the control mode is set at flow
rate on the [FLOW] key screen of the AFC.
12.5.6
Run
Displayed only while GC is in system ON status. Immediately runs the clean
up program.
Stop
Stops clean up.
This item is displayed only when the clean up program is in progress.
Next Line Displays the clean up program set up screen for another analytical flow line.
7 Starting and Stopping the GC [SYSTEM]
7.3 7.
86
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7.3Specifying Start Procedures
7.3.1 Screen description
Select [Start Seq] (PF menu) from the [SYSTEM] key main screen to display the start
procedure setup screen shown in Fig. 7.3.1.
On this screen, set whether the system automatically starts (Auto Start) when the power is
next turned on, or whether the system does not start until [Start GC] (PF menu) is pressed
(Manual Start). Alternatively, only carrier gas flow is turned on the next time the power is
turned on. To start the system, select [Start GC] (PF menu) as for a manual start. This is
known as a semi-auto start. Finally, an analysis file can be set to begin the next time the
power is turned on or the GC is restarted. Any settings changed on this screen are reflected
in the [SYSTEM] key main screen.
Fig. 7.3.1 Setting the start procedures for the next GC restart
7 Starting and Stopping the GC [SYSTEM]
7.3 Specifying Start Procedures
87
GC-2014
7.3.2 Parameter list
FILE LOAD
Selection: File No. 09, Default: Current file
Selects a file to be loaded the next time the power is turned on or the GC restarted.
START GC
Selection: Auto Start/ Manual Start/Semi-Auto, Default: Manual Start
Sets the start method for the next time the power is turned on:
Select Auto Start to automatically start the GC.
Select Manual Start to start the GC by presssing [Start GC] (PF menu) from the [SYSTEM]
key main screen.
Select Semi-Auto to start carrier gas flow only. The GC must still be started by pressing
[Start GC] (PF menu) from the the [SYSTEM] key main screen.
START TIME
Range: 0.06000.0 min, Default: 0.0 min
Sets the period of time after gas control starts until temperature/detector control starts.
The Start Time value on the [SYSTEM] key main screen is set here.
The start time set here can be overridden by entering another start time in the [Start GC] (PF menu)
screen.
This function is useful if the preset start time is too long.
START TEMP/DET
Selection: Yes/No, Default: Yes
Select Yes to start temperature/detector control after the start time is elapses.
Select No to continue carrier gas flow only without starting temperature/detector control.
DETECTOR
Selection: On/Off, Default: On
Prepares the configured detector for analysis, but does not ignite the FID or FPD.
The DETECTOR setting on the [SYSTEM] key main screen is set here.
AUTO IGNITE
Selection: On/Off, Default: On
Establishes FID/FPD ignition conditions.
Select On for the FID/FPD detector to stand by in the ignited status. Select Off for it stand
by without igniting.
The AUTO IGNIT setting on the [SYSTEM] key main screen is set here.
CLEAN UP
Selection: Off/Analysis Para/Clean Up Para, Default: Off
When performing clean up, select whether to use an analysis method or the program set in
[Clean Up] (PF menu).
The CLEAN UP setting on the [SYSTEM] key main screen is set here.
7.3.3 Example: starting the system with carrier gas flow
In this example, carrier gas flows for a certain period of time before temperature control
begins. The length of time the carrier gas should flow depends on how long the carrier gas
flow was shut off.
If the same column is used in the same analytical flow line as the day before:
set a START TIME of approx. 10 minutes.
If a different column is installed on the same flow line that has been in use:
set a START TIME of approx.10 minutes.
If the system has been out of use for a time with no column connected:
set a START TIME of 1 to several hours.
NOTE
7 Starting and Stopping the GC [SYSTEM]
7.4 7.
88
GC-2014
7.4Specifying the Stop Procedures
7.4.1 Screen
Select [Stop Seq] (PF menu) from the [SYSTEM] key main screen to display the stop
procedure setup screen shown in Fig. 7.4.1. Stop Seq is displayed only when the system is
in OFF status.
The stop procedure setup screen consists of parameters equivalent to those on the
[SYSTEM] key main screen when the GC is in system ON status, except that the current file
cannot be changed.
Parameter changes on the stop procedure setup screen are reflected on the [SYSTEM] key
main screen.
7.4.2 Parameter list
STOP TIME
Range: 0.06000.0 min, Default: 0.0 min
Sets the period of time after [Stop GC] (PF menu) is pressed (or after a program finishes if
the program was running) to stop temperature/detector control.
The STOP TIME value on the [SYSTEM] key main screen is set here.
FLOW OFF TIME
Range: 0.06000.0 min, Default: --- (because the gas control is set to Cont.)
Sets the period of time between the end of temperature/detector control and the end of gas
control.
This item cannot be set if Flow Control is Cont (that is, if carrier gas is kept flowing).
The [FLOW OFF TIME] setting on the [SYSTEM] key main screen is set here.
Fig. 7.4.1 Setting the stop procedures
7 Starting and Stopping the GC [SYSTEM]
7.4 Specifying the Stop Procedures
89
GC-2014
FLOW CONTROL
Selection: End/Cont, Default: Cont
Select End to end gas control after the flow off time elapses.
Select Cont to continue the carrier gas flow.
The GAS CONTROL setting on the [SYSTEM] key main screen is set here.
SLEEP TIME
Range: 0.16000.0 min, Default: --- (because the RESTART GC could be set to Off.)
Sets the period of time after temperature/detector control ends until the GC restarts.
This item cannot be set if the GC is not set to restart automatically.
The SLEEP TIME setting on the [SYSTEM] key main screen is set here.
RESTART GC
Selection: On/Off, Default: Off
Select On to restart the GC once the sleep time has elapsed.
Select Off to not restart the GC automatically.
The Restart GC setting on the [SYSTEM] key main screen is set here.
7.4.3 System shut down examples
The following examples show various situations where STOP TIME and FLOW OFF TIME
can be used effectively.
After the end of an analysis, each heated zone is cooled. Once the column over is
cool, carrier gas flow is shut off.
STOP TIME = 0 minutes
FLOW CONTROL = End
FLOW OFF TIME = Approx. 20 minutes
A column is conditioned, then the column over is cooled. Carrier gas flow is then
shut down.
STOP TIME = Column conditioning time
FLOW CONTROL = End
FLOW OFF TIME = Approx. 20 minutes
At the end of an analysis, each heated zone is cooled, but carrier gas is kept flowing
for rapid equilibration for the next days analysis. The next day, the system is automati-
cally restarted (15 hours = 900 minutes later), and temperature control resumes.
START TIME = 0 minutes (because the carrier gas continued to flow)
STOP TIME = 0 minutes
FLOW CONTROL = Cont (to keep carrier gas flow on)
RESTART GC = On
SLEEP TIME = 900 minutes (at the end of the SLEEP TIME, the GC
restarts)
At the end of an analysis, each heated zone is cooled, and the carrier gas flow is
stopped once the column oven is cool. The following day (15 hours = 900 minutes
later), carrierr gas flow is turned back on and temperature control begins.
START TIME = 10 minutes (because carrier gas flow was off)
STOP TIME = 0 minute
FLOW CONTROL = End
FLOW OFF TIME = Approx. 20 minutes
RESTART GC = On
SLEEP TIME = 900 minutes (at the end of the SLEEP TIME, the GC
restarts)
7 Starting and Stopping the GC [SYSTEM]
7.4 Specifying the Stop Procedures
90
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This page is intentionally left blank.
91
8.1 8. 8.
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8 Setting the Analytical Parameters and File Management
8.1[SET] Key Main Screen
8.1.1 Main screen
Press the [SET] key to display the main screen shown in Fig. 8.1.1 and to make frequently
used parameter settings.
To make changes to the [COL], [FLOW], [INJ], and [DET] parameters, the [customiz] (PF
menu) key is pressed. Changes to these parameters are reflected in the [SET] key main
screen.
The screen shows parameters of a line that consists of an injection port, detectors, and
options connected to a column (two columns for the dual packed column INJ). The combina-
tion can be changed on the [Line Config] (PF menu) sub screen.
When the system is turned on, the temperatures are controlled for the components in the
flow line. If the AFC is present, carrier gas is supplied to the injection port specified. If APC is
present, detector gases are supplied to the detector specified.Temperatures are not con-
trolled, and gases are not supplied, to components which are not part of the analytical flow
line. Although two or more detectors can be set for a line, only one injection port can be set.
(a) When the DINJ is used (b) When the SPL is used
Fig. 8.1.1 [SET] key main screen
8 Setting the Analytical Parameters and File Management
8.1 [SET] Key Main Screen
92
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8.1.2 Parameter list
COLUMN OVEN
Range: 0.0400.0 C, Default: 25.0 C
Sets the default temperature in the oven temperature program.
Flow
When the packed INJ (DAFC) is used
L. inlet pressure, R. inlet pressure
Column inlet pressures are indicated. (L: left side, R: right side)
L. column flow rate, R. column flow rate
Range: 0.0100.0 ml/min, Default: 50 ml/min
Enter the column flow rate. Set the initial flow rate to set a flow rate program. When the
control mode is set to Single L or Single R, only the specified side is displayed.
When the SPL, etc. (AFC) is used
INLET PRESS
Range: 0.0970.0 kPa (Refer to Fig. 12.2.5.), Default: 100.0 kPa
Sets the column inlet pressure.
The initial pressure must be set in order to create a pressure program.
When the control mode is set to pressure, the system keeps the column inlet pressure at a
constant value while the oven temperature program is running.
COLUMN FLOW RATE
Default:
1
1.00 ml/min
Sets the carrier gas flow rate at the capillary column exit (atmospheric pressure at 25 C).
When you set the carrier gas flow rate, the system calculates the column inlet pressure
based on the inner diameter and the length of the column. The column flow rate is set
separately so that the carrier gas flow rate desired occures at the initial temperature in the
oven temperature program.
LINEAR VELOCITY
Default:
2
30.0 cm/s
Sets the average linear velocity of the carrier gas flowing in the capillary column.
When you set the linear velocity, the system calculates the column inlet pressure based on
the inner diameter and the length of the column. The linear velocity is set separately so that
the linear velocity desired occures at the initial temperature in the oven temperature
program.
When the control mode is set to linear velocity, the column inlet pressure automatically
changes so that the linear velocity remains constant even while the oven temperature
program is running.
TOTAL FLOW RATE
Range: 0.01200.0 ml/min (Refer to Fig. 12.2.5.), Default: 500.0 ml/min
The total flow rate varies depending on the injection mode as follows:
In split or splitless mode, the total flow rate is equivalent to column flow rate + split flow rate
+ septum purge flow rate.
In direct mode, the total flow rate is equivalent to column flow rate + septum purge flow rate.
SPLIT RATIO
Range: -1.0/0.09999.9, Default: -1.0
The split ratio is split flow rate / column flow rate.
When you set a split ratio, the system sets the total flow rate based on the calculated carrier
gas flow rate and split flow rate, so that the desired split ratio occurs at the oven
temperature.
Set the split ratio to -1.0 to fix the total flow rate regardless of the oven temperature.
8 Setting the Analytical Parameters and File Management
8.1 [SET] Key Main Screen
93
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PURGE FLOW RATE
Range: Refer to Fig. 12.2.15, Default: 3.0 ml/min
Set the septum purge flow rate.
SAMPLING TIME
Range: 0.009999.99 min, Default: 1.00 min
Sets the sampling time for splitless analysis.
The sampling time indicates the period of time after analysis starts until the split flow line is
opened.
SPLIT MODE
Selection: SPLIT/SPLITLESS/DIRECT, Default: SPLIT
SPLIT: Controls the column inlet pressure and the total flow rate so that the column
inlet pressure and split ratio occur as specified.
SPLITLESS: Closes the split flow line during the sampling time so that the set column inlet
pressure is controlled by the Total Flow Controller.
Opens the split flow line and controls the Electronid Split Controller so that the
preset column inlet pressure occurs (Refer to Fig. 12.2.2.) after the sampling
time elapses.
DIRECT: Closes the split flow line and the set column inlet pressure (in pressure mode)
or the set total flow rate (in flow mode) occurs. When making direct injection
analyses, select WBI in the setup screen so that SPLIT mode is not available.
CONTROL MODE
Selection: PRESS/VELOCITY/FLOW (for direct injection mode), Default: PRESS
When the injection mode is set to SPLIT or SPLITLESS
PRESS: Controls the system so that the column inlet pressure remains constant.
VELOCITY: Controls the system so that the linear velocity remains constant.
When the injection mode is set to DIRECT
PRESS: Controls the system so that the column inlet pressure remains constant.
VELOCITY: Controls the system so that the linear velocity remains constant.
FLOW: Controls the system so that the flow rate remains constant.
INJECTION PORT TEMP
Range: 0.0400.0 C, Default: 25.0 C
Set the injection port temperature (the default temperature for a programmable injection
port).
DETECTOR TEMP
Range: 0.0400.0 C (in FID), Default: 25.0 C
Set the detector temperature.
Allowable temperature ranges vary for each detector. Refer to range specified for the detec-
tor(s) in use.
1 The column flow rate ranges from 0 to the value at which the calculated column inlet pressure is
970 kPa or less and the calculated total flow rate is 1,200 ml/min.
2 The linear velocity ranges from 0 to the value at which the calculated column inlet pressure is 970 kPa
or less.
3 The purge flow rate ranges from 0 to the total flow rate subtracted by the column flow rate and the split
flow rate.
8 Setting the Analytical Parameters and File Management
8.1 [SET] Key Main Screen
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8.1.3 PF menu
PF menu Description
Reference
section
File
Displays file list to change the current file.
On this sub screen, you can select files to load, copy, initialize and rename.
8.2
Line Confg
Specifies the injection port, detectors and options which make up the ana-
lytical flow line.
Units set on this sub screen are displayed on the [SET] key main screen.
8.3
Customiz Set the parameters displayed on the [SET] key main screen. 8.4
Print Prints temperature, pressure and total flow rate on a Chromatopac.
Next Line
Switches through each of the parameter screens in turn. Press the [SET]
key from the [SET] key main screen to switch to the next screen.
95
8 Setting the Analytical Parameters and File Management
8.2 8.
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8.2File Management
8.2.1 Screen description
Select [File] (PF menu) from the [SYSTEM] key main screen to display the file list shown in
Fig. 8.2.1.
To change the current file, enter a file No. or move the cursor using the [ ] and [ ] key;
then press the [Load] (PF menu) key.
8.2.2 PF menu
Fig. 8.2.1 File list screen
PF menu Description
Reference
section
Load Selects the current file.
Copy Copies file name and file contents from the source file to a destination file. 8.2.3
File Init
Initializes file name and file contents.
The current file cannot be initialized.
8.2.5
Rename Changes the file name. 8.2.4
8 Setting the Analytical Parameters and File Management
8.2 File Management
96
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8.2.3 Copying a file
Select [Copy] (PF menu) on the file list screen to display the file copy screen shown in Fig. 8.2.2.
Enter the source file number (Src. File) and the destination File number (Dst. File), then press
[Copy] (PF menu). The name and contents of the source file are copied to the destination file.
8.2.4 Renaming a file
Select [Rename] (PF menu) on the file list screen to display the file rename screen shown in
Fig. 8.2.3. Move the cursor using the [ ] and [ ] keys to select the file to be renamed.
Enter the new file name using the numeric keys and the [ ] and [ ] keys. Refer to 6.3.5
Changing item names for more information..
Fig. 8.2.2 Copying File
Fig. 8.2.3 Renaming a file
NOTE
8 Setting the Analytical Parameters and File Management
8.3 Specifying the Analytical Flow Line Components ([Line Config])
99
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Q Line configuration examples
SPL (split/splitless injection port) and DINJ (dual packed INJ) are installed as the injection
port. DFID (dual hydrogen flame ionization detector) and DTCD (thermal conductivity
detector) are installed as the detector.
(1) To use only a SPL and FID
Select the SPL and DFID for Line 1. In this case, only the temperature of the SPL and
DFID will be controlled. Carrier gas (including detector gas if APC is used for detector
gas) will be supplied.
(2) To use only a DINJ and DFID
Select the DINJ and DFID for Line 1. Two columns will make one line.
Fig. 8.3.2 Line configuration (Example 1)
Fig. 8.3.3 Line configuration (Example 2)
INJ
DET
COL
8 Setting the Analytical Parameters and File Management
8.3 Specifying the Analytical Flow Line Components ([Line Config])
100
GC-2014
In the following examples, the PFPD (packed column flame photometric detector) is installed
as an additional detector.
(3) To use a SPL and FPD for one line and a DINJ and DFID for another line
Select the SPL and FID for Line 1 and the DINJ and DFID for Line 2.
(4) When using a single column connected to two detectors:
Fig. 8.3.4 Line configuration (Example 3)
Fig. 8.3.5 Line configuration (Example 4)
INJ
DET DET
COL
101
8 Setting the Analytical Parameters and File Management
8.4 8.
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8.4Changing Items Displayed with [Customiz]
8.4.1 Screen description
Select [Customiz] (PF menu) from the [SET] key main screen to display the Display Custom-
ization screen shown in Fig. 8.4.1.
On this screen, set the items which will be displayed on the [SET] key main screen. Set an
item to On to display it on the main screen. Set the item to Off to wide its display.
Settings are the same for all lines. However, for the dual AFC, only column inlet pressure,
column flow rate, and control mode are displayed. For the AFC, when the sampling time is
set to On, the sampling time is only displayed on the SPLITLESS injection mode.
Move the cursor using the [ ] and [ ] keys to select an item to be changed; select On
or Off using the [ ] and [ ] keys, then press the [ENTER] key to validate the selection.
The default it setting displays the column inlet pressures, column flow rate, split ratio,
sampling time and the split mode.
Fig. 8.4.1Customizing the [Set] key main screen
ELP CE ENTER
ON
OFF
Temperature axis
Time axis
Signal axis
4
6
2
8
5
9 Monitoring the GC
9.1 [MONIT] key Main Screen
105
GC-2014
9.1.2 Parameter list
RETENTION TIME (Rt)
Retention time is the length of time from compound injectio to detection.
The retention time is specific to each compound. Compounds are identified based on match-
ing the retention time to a standard compound retention time.
REMAIN TIME
The longest program time subtracted by the current retention time is displayed.
LONGEST PROGRAM TIME
The longest program time indicates the total time of the longest program when comparing
the temperature program, the pressure program, the flow rate program and the time
program.
9.1.3 PF menu
PF menu Description
Reference
section
Temp Mon
Displays the current and set temperatures of column, injection port and
detector.
9.2
Flow Mon
Displays inlet pressure, total flow rate and purge flow rate for injection port,
and hydrogen flow rate, air flow rate and makeup gas flow rate for detector.
The display format depends on the typeof flow controller installed.
9.3
Zero Adj Automatically moves the baseline to zero point. 9.4
Zero Free Returns to the baseline level before zero point adjustment. 9.4
Up Moves the baseline up by 100 V from current level. 9.4
Down Moves the baseline down by 100 V from current level. 9.4
Chng Graph
Switches the graph display from chromatogram and column oven tempera-
ture program to chromatogram and pressure program. For direct injection
mode with flow control, the flow rate program is displayed instead of the
pressure program.
Chng Line
Displays the monitor screen for another configured analytical line. Switch
between monitored lines by pressing [MONIT] key from the monitor screen.
9 Monitoring the GC
9.2 9.
106
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9.2Monitoring the Temperature with [Temp Mon]
9.2.1 Screen description
Press [Temp Mon] (PF menu) from the [MONIT] key main screen to display the Temp Moni-
tor screen shown in Fig. 9.2.1.
Monitor the temperature of all installed column ovens, injection ports and detectors from this
screen.
Heated zones without installed components are not displayed on the screen.
9.2.2 PF menu
Fig. 9.2.1Temperature monitor
PF menu Description
Reference
section
Flow Mon Monitor pressure and flow rate for the injection ports and detectors. 9.3
NOTE
The components that are
included in the current ana-
lytical line are underlined.
107
9 Monitoring the GC
9.3 9.
GC-2014
9.3Monitoring the Flow Rate with [Flow Mon]
9.3.1 Screen description
Press [Flow Mon] (PF menu) from the [MONIT] key main screen to display the Flow Monitor
screen shown in Fig. 9.3.1.
Monitor the flow rate and the pressure of the injection ports, and the detector gas flow rates
of the detectors.
Flow controllers that have hot been installed are not displayed on the screen.
9.3.2 PF menu
Fig. 9.3.1Flow rate monitor
PF menu Description
Reference
section
Temp Mon Monitor temperature of the column oven, injection ports and detectors. 9.2
NOTE
The name of injection port
and detectors constructing
the current line are under
lined.
Displayed items depend on
the type of injection ports,
detectors and flow controllers.
9 Monitoring the GC
9.4 9.
108
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9.4Zero Point Adjustment
Zero point adjustment should be executed when the baseline is off-scale. If the baseline cannot
be seen on the screen, execute zero point adjustment so that the baseline returns to the zero
point. The baseline level can also be manually adjusted.
9.4.1 Screen description
Press [Zero Adj] or [Zero Free] (PF menu) from the [Monit] key main screen, the chromatogram
displayed on the monitor screen changes as shown in Fig. 9.4.1 or Fig. 9.4.2.
Press [Up] or [Down] (PF menu) to adjust the baseline level manually.
Zero point adjustments are effective not only for the GC monitor screen, but also a con-
nected pc or Chromatopac. However, zero point adjustments made on the Chromatopac do
not adjust the monitor screen baseline level.
Zero point adjustments are only valid for the currently displayed detector. To adjusts the zero point for
another detector, first switch to its display by pressing [Chng Line] (PF menu), then execute the adjust-
ment.
For the TCD, press [Zero Free] first, turn the TCD zero point rough adjuster on the right side of the unit
to set the baseline close to 0V, and then press [Zero Adj].
Fig. 9.4.1Zero point adjustment Fig. 9.4.2 Zero free adjustment
Since the [Down] has been held down too long,
the zero point has deviated into the negative zone.
[Down]
(Held down)
[Up]
(Held down) [Zero Adj]
[Zero Adj]
[Zero Free]
NOTE
109
10.1 10. 10.
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10 Starting and Stopping Analysis
10.1Making an Injecting and Starting an Analysis
10.1.1 Verifying the gas chromatograph status
(1) Ensure that the STATUS indicator light is green.
(2) When the STATUS light is green, perform a zero-cause-adjustment control if necessary.
(For a description of the items which determine the Ready Status, refer to 16.6.6
Setting the Ready Check Parameters.)
For the dual packed INJ, the STATUS light becomes green and also the monitor injection
screen appears. Inject a sample following the directions displayed on the screen.
Instructions on the monitor injection screen are based on the polarity settings of the detector. When
settings are opposite from polarity in order to invert the peak, for example to analyze hydrogen using
nitrogen carrier gas on the TCD, inject a sample into the opposite inlet of the one instructed on the
screen.
Regular key operation is possible when the monitor injection screen is displayed. If there is
no key operation for a minute, the screen display automatically returns to the monitor
injection screen.
Fig. 10.1.1Monitor injection screen
NOTE
10 Starting and Stopping Analysis
10.1 Making an Injecting and Starting an Analysis
110
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10.1.2 Making manual injection
Q Aspiration
1. Preparation
10 L Syringe
Sample
Rinse solvent
Liquid waste container
2. Syringe handling precautions
Fig. 10.1.2Typical syringe
The plunger keeps the sample from becoming contaminated. Do not bend it or touch
it. Keep it clean.
Never bend the needle.
3. Solvent pre-wash
Clean the syringe with solvent 3 to 5 times using the following procedure.
(1) Place the syringe into the rinse solvent. Pull the plunger to aspirate approximately 10
l of Solvent.
(2) Expel the solvent into the liquid waste container.
4. Sample pre-wash
Flush the syringe with sample 3 to 5 times using the following procedure.
(1) Place the syringe into the sample. Pull the plunger to aspirate approsimately 10 l of
sample.
(2) Expel the sample into the liquid waste container.
5. Preparing to inject
(1) With the needle in the sample vial, pump the plunger to eliminate air bubbles inside
the syringe.
(2) When air bubbles are eliminated, aspirate exactly 1 l of sample.
(3) Gently wipe the syringe needle with a lint-free wipe.
(4) Aspirate an additional 0.5 l of air.
Fig. 10.1.3
10 Starting and Stopping Analysis
10.1 Making an Injecting and Starting an Analysis
111
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Q Injection
10.1.3 Starting the analysis
Start an analysis program when the STATUS light is green.
Press the [START] key to start the temperature program, the time program, the pressure
program and the flow rate program.
Any pre-set programs execute prior to the start of the analysis programs.
Aspirate sample. Insert syringe until it
touches needle guide.
Push plunger to inject
sample.
At same time, press
[START] key of gas
chromatograph.
Promptly pull out
syringe.
WARNING
Wear protective goggles when handling samples.
10 Starting and Stopping Analysis
10.2 10.
112
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10.2Terminating the Analysis
10.2.1 Terminating the analysis
When the various programs (temperature, time, pressure, and flow rate) are finished, the
gas chromatograph automatically returns to the initial status and becomes ready.
To stop the programs before their completion, press the [STOP] key. The chromatograph
automatically returns to the ready status.
10.2.2 External devices
Q When the gas chromatograph is connected to a Chromatopac
Key operation of the gas Chromatograph
Press the [START] key of the gas chromatograph to start the Chromatopac automatically.
Pressing the GC [STOP] key, however, does not stop the Chromatopac.
The [STOP] key of the Chromatopac needs to be pressed as well.
To prevent automatic start of Chromatopac, refer to 16.6.9 Setting the link device code
Key operation from the Chromatopac
The gas chromatograph is not controlled by the Chromatopac. Pressing the Chromatopac
[START] or [STOP] key does not start or stop a GC analysis.
Q When the gas chromatograph is linked to a personal computer (pc).
Start analysis using the computer. Control for both the gas chromatograph and computer is
automatically stopped after a series of process is complete.
To inject a sample manually, start analysis using the computer so that data can be taken in,
inject the sample, and press the [START] key of the gas chromatograph.
To pause analysis, use the computer to stop it.
NOTE
113
11.1 11. 11.
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11 Creating an Oven Temperature Program
11.1[COL] Key Main Screen
11.1.1 Screen description
Press the [COL] key to display the column screen shown in Fig. 11.1.1. The oven temperature
program is set from this screen.
Enter a value other than 0 in the rate field displayed with END. Once a valid rate has been
entered, set the temperature (final temp) and time (hold time) for the line.
In addition to the oven temperature program, the equilibration time is set from this screen.
Equilibration time is the length of time allowed for the oven temperature to properly equili-
brate before the system is Ready.
Press the [COL] key, to move the cursor directly to the temperature portion of the ramp.
This facilitates program edits when only the temperature needs to be changed.
Fig. 11.1.1 [COL] key main screen
NOTE
Up to 20 temperatue increase/
decrease ramps can be set.
11 Creating an Oven Temperature Program
11.1 [COL] Key Main Screen
114
GC-2014
11.1.2 Parameter list
TEMP
Range: 0.0400.0 C, Default: 25.0 C
Set the initial and the final temperature for each ramp of in the oven temperature program.
The column oven temperature should never exceed the maximum operating temperature of
the column. Keep the column temperature as low as possible to prolong the column life and
reduce detector noise. To set the maximum over temperature, refer to 16.6.4 Setting the
maximum temperature limits
TIME
Range: 0.009999.99 min, Default: 0.00 min
Set the hold time for the initial temperature and the final temperature for each stage of the
oven temperature program.
RATE
Range: END/-250.0250.0 C/min, Default: END
Set the program rate for the oven temperature program.
Set the rate to 0; END appears and the program finishes at the previous ramp.
Move the cursor to END and set any numeric value other than 0 to complete the
temperature and the time for that ramp.
EQUILIBRATION TIME
Range: 0.009999.99 min, Default: 3.00 min
After the programs finish and the oven temperature returns to the initial value, the
equilibration time must elapse befor the system is considered Ready. This allows for even
temperature distribution.
11.1.3 PF menu
Fan Off cannot be operated when the column oven temperature setting value is 40C or higher or a
program is running.
CAUTION
Never increase the column oven temperature while air (oxygen) is
mixed with the carrier gas. This can damage the column (especially
for polar columns).
PF menu Description
Reference
section
Del Line Deletes the current line.
Ins Line Inserts a line in line at the current cursor position.
Fan Off Stops the fan operation.
Fan On Restarts the fan operation.
Print Prints the column oven program from a Chromatopac.
NOTE
115
11 Creating an Oven Temperature Program
11.2 11.
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11.2Temperature Programs
11.2.1 Isothermal analysis
The isothermal analysis technique keeps the column oven temperature at a constant value.
This method is useful for separating compounds within a narrow boiling point range.
11.2.2 Programmed analysis
When the sample contains compounds over a wide boiling point range, isothermal analysis
is irsufficient for separating all the compounds. At lower temperatures, the high boiling point
compounds will co-elute with wide peaks. Low concentrations of high boiling point com-
pounds may never be detected. On the other hand, at a higher temperatures, the com-
pounds with a low boiling point will co-elute too rapidly.
There is an optimal temperature for separating various compounds. Using an oven tempera-
ture that increases gradually controls the elution, and improves the separation, of all the
compounds.
11.2.3 Creating a temperature program
Q Screen terminology
1-ramp temperature program
Initial setting (TEMP).... T1
Initial setting hold time (TIME)..... a
Program rate (RATE)....
Final temperature (TMP)...... T2
Final temperature hold time (TIM)....... c
Equilibration time (ETIM)..... d
Column oven
temperature
Time
T2
T1
a
c
d
b
Program
starts.
Program
finishes.
T 2 -T 1
b
11 Creating an Oven Temperature Program
11.2 Temperature Programs
116
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Q Program creation
1-ramp temperature program
2-ramp temperature program
Fig. 11.2.1 Temperature program (Example 1)
Fig. 11.2.2 Temperature program (Example 2)
220 (2 min)
60 (2 min)
Initial
temperature
1st stage
10 /min
5 min
160 (5 min)
120 (2 min)
60 (2 min)
5 /min
10 /min
3 min
Initial
temperature
1st stage 2nd stage
11 Creating an Oven Temperature Program
11.2 Temperature Programs
117
GC-2014
Multiple-ramp temperature program (with temp increase /decrease)
Q Allowable temperature settings and ranges for temperature programs
Fig. 11.2.4Example of column oven temperature increase/decrease curve (115 V model)
Fig. 11.2.3 Temperature program (Example 3)
Item Set Range Control Range
Default
value
Program rate
Heating
115 V model
Up to 150 C
0250
C/min
030 C/min
0 C/min
Up to 250 C 020 C/min
Up to 380 C 010 C/min
Up to 400 C 07 C/min
Heating
230 V model
Up to150 C
0250
C/min
060 C/min
Up to 250 C 040 C/min
Up to 380 C 020 C/min
Up to 400 C 015 C/min
Cooling
2500
C/min
Differ from the room
temperature or the
oven temperature.
Initial
temperature
1st
stage
2nd
stage
3rd
stage
70 (1 min) 70 (3 min)
200 (5 min)
120 (0 min)
-5 /min
10 /min
5 /min
250
380
400
150
20 /min
7 /min
10 /min
30 /min
50
11 Creating an Oven Temperature Program
11.2 Temperature Programs
118
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119
12.1 12. 12.
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12 Injection Port
12.1Packed Column Injection Port (Dual INJ)
During analysis using packed columns, a sample is injected into an injection port and the entire
evaporated sample is injected to the columns. A mass flow controller is used to control the
column flow rate so gas is supplied at a specified flow rate even when the column flow path
resistance and temperature change.
The GC-2014 packed model has an injection port that two packed columns can be attached to
(dual INJ) as standard. An injection port that only one column is attached to (single INJ) is
available as an option. For the single INJ, refer to its instruction manual.
Fig. 12.1.1 Dual-column packed analysis
Control
Control
Dual AFC Dual INJ
Packed column
12 Injection Port
12.1 Packed Column Injection Port (Dual INJ)
120
GC-2014
12.1.1 Setting the temperature with [INJ] key
12.1.1.1 Screen description
Press the [INJ] key to display the main screen shown in Fig. 12.1.2 and to set the
temperature of the injection port.
Fig. 12.1.2[INJ] key main screen
12 Injection Port
12.1 Packed Column Injection Port (Dual INJ)
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12.1.1.2 Parameter list
TEMP
Range: 0.0400.0 C, Default: 25.0 C
Set the temperature of the injection port.
Keep the injection port temperature as low as is practical to increase the service life of
the temperature sensor. In order to instantly vaporize samples inside the injection port,
set the injection port temperature approximately 30 C above the column oven
temperature (final temp). Due to the minute quantity of sample injected, the sample
vaporizes at temperatures lower than the boiling point of sample elements. To set the
injection port maximum temperature limit, refer to 16.6.4 Setting the maximum
temperature limits in 16.6 GC Configuration.
12.1.1.3 PF menu
PF menu Description
Reference
section
Print Prints the injection port temperature on Chromatopac.
Next Inj
Toggles among the setup screeens if two or more injection ports are
installed in this system.
The [INJ] key can also be used to switch screens.
12 Injection Port
12.1 Packed Column Injection Port (Dual INJ)
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12.1.2 Setting the Flow Rate
12.1.2.1 Screen description
Press the [FLOW] key to display the screen shown in Fig. 12.1.3 and to set parameters
for the dual AFC (Advanced Flow Controller) that controls carrier gas flow rate.
1. When the control mode is set to Single L or Single R, parameters of only specified side are
displayed.
2. Inlet pressures can be monitored but cannot be set.
12.1.2.2 Parameter list
CONTROL MODE
Selection: Dual/Single L/Single R, Default: Dual
When the control mode is set to Dual, flow controllers on both left and right inlets are
controlled. When it is set to Single L or Single R, a flow controller on either left or
right inlet is controlled.
COLUMN FLOW RATE
Range: 0.0100.0 ml/min, Default 50.0 ml/min
Set the flow rate of gas to be supplied to columns connected to left and right inlets. A
mass flow controller is used to control the column flow rate so gas is supplied at a
specified flow rate even when the column resistance changes due to a column
replacement or the column temperature changes.
CARRIER GAS TYPE
Selection: He/N2/H2/Ar, Default: He
Specify the type of carrier gas supplied to the AFC. This parameter is used for the
measurement/control of the flow rate. If this parameter is not set correctly, calculations
may not be performed correctly.
Fig. 12.1.3 FLOW key main screen
NOTE
Flow rate of the column
connected to the left inlet
Flow rate of the column
connected to the right inlet
12 Injection Port
12.1 Packed Column Injection Port (Dual INJ)
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12.1.2.3 PF menu
PF menu Description
Reference
section
Column
Sets inner diameter, length, and film thickness of a column used.
Values entered here are simply for notes and they are not used for flow
rate calculations.
12.1.3
On/Off
Set the flow controller to be used to On.
When the GC starts, the AFC in the current analytical line which is set to be
On is controlled.
L Flow prog. Sets the flow rate program for the flow controller on the left inlet.
12.1.4
R Flow prog. Sets the flow rate program for the flow controller on the right inlet.
Offset
Performs offset calibration of the AFC sensor. This calibration contributes
to good reproducibility of results.
12.4
Next Flow
Toggles among the AFC set up screens when two or more AFCs are
installed in the system. The [FLOW] key can also be used to switch
screens.
12 Injection Port
12.1 Packed Column Injection Port (Dual INJ)
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12.1.3 Entering Columns Parameters
Set values for column dimensions are not used for calculation for controlling the dual AFC.
Values entered here are simply for notes.
12.1.3.1 Screen description
Select [Column] (PF menu) on the [FLOW] key main screen to display the screen
shown in Fig. 12.1.4.
12.1.3.2 Parameter list
COLUMN I.D. (internal diameter)
Range: 0.016.00 mm, Default: 0.32 mm
COLUMN LENGTH
Range: 0.1250.0 m, Default: 25.0 m
FILM THICKNESS
Range: 0.00300.00 m, Default: 0.50 m
Fig. 12.1.4 Column parameters entering screen
Dimensions of a column
connected to the left inlet
Dimensions of a column
connected to the right inlet
12 Injection Port
12.1 Packed Column Injection Port (Dual INJ)
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12.1.4 Creating a Flow Rate Program
Column flow rate can be increased or decreased during analysis by making a flow rate
program.
12.1.4.1 Screen description
Select [L. Flow Prog] or [R Flow Prog] (PF menu) on the [FLOW] key main screen to
display the screen shown in Fig. 12.1.5.
12.1.4.2 Parameter list
FLOW RATE
Range: 0.00100.0 ml/min, Default: 50 ml/min
Set the initial flow rate and the final flow rate for each stage of the flow rate program.
TIME
Range: 0.009999.99 min, Default: 0.00 min
Set the hold time for the initial flow rate and final flow rate for each stage of the flow rate
program.
RATE
Range: END/-400.00 +400.00 ml/min
2
, Default: END
Set the flow rate program rate. If you set the rate to 0, END appears and the program
finishes at the previous ramp. If you move the cursor to END and set any numeric
value other than 0, the final flow rate and time for that ramp can be entered.
12.1.4.3 PF menu
Fig. 12.1.5 Flow rate program setup screen (e.g. L flow rate program)
PF menu Description
Reference
section
Del Line Deletes a line at the current cursor position.
Ins Line Inserts a line above the line that the cursor is positioned.
Print Prints the flow rate program through a Chromatopac.
Up to 7 ramps of flow rate
increase/decrease can be set.
12 Injection Port
12.2 12.
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12.2Split/Splitless Injection System
Q Split injection system
In a split injection system, only a portion of the sample injected into the injection port is
introduced into the capillary column. The remaining sample is sent to the split line due to
high sample volume or concentration.
Fig. 12.2.1
Q Splitless injection system
The splitless injection system is used to analyze samples of low concentration.
In a splitless injection system, the split vent is closed and the initial temperature of the column
oven is low. Then, after injection, and once the vaporized sample has moved to the column,
the split vent is open and the column temperature increased so that the condensed sample
inside the column is vaporized again and separated.
Fig. 12.2.2
Control
TFC
CARRIER
PURGE
PURGE VENT
SPLIT VENT Control
Control
ESC
SPLIT
Capillary column
Control
TFC
CARRIER
PURGE
PURGE VENT
SPLIT VENT Close
SPLIT
Capillary column
(a) During sampling time
Control
Control
TFC
CARRIER
PURGE
PURGE VENT
SPLIT VENT Control
ESC
SPLIT
Capillary column
(b) After sampling time
Control
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.1 Setting the temperature with [INJ] key
12.2.1.1 Screen description
Press the [INJ] key to display the main screen shown in Fig. 12.2.3 and to set the
temperature of the injection port.
Fig. 12.2.3[INJ] key main screen
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.1.2 Parameter list
TEMP
Range: 0.0400.0 C, Default: 25.0 C
Set the temperature of the injection port.
Keep the injection port temperature as low as is practical to increase the service life of
the temperature sensor. In order to instantly vaporize samples inside the injection port,
set the injection port temperature approximately 30 C above the column oven
temperature (final temp). Due to the minute quantity of sample injected, the sample
vaporizes at temperatures lower than the boiling point of sample elements. To set the
injection port maximum temperature limit, refer to 16.6.4 Setting the maximum
temperature limits in 16.6 GC Configuration.
12.2.1.3 PF menu
PF menu Description
Reference
section
Print Prints the injection port temperature on Chromatopac.
Next Inj
Toggles among the setup screeens if two or more injection ports are
installed in this system.
The [INJ] key can also be used to switch screens.
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.2 Setting the flow rate with [FLOW] key
12.2.2.1 Screen description
Press the [FLOW] key to display the screen shown in Fig. 12.2.4 and to set the AFC
(advanced flow controller) parameters. The AFC controls the pressure and the flow rate
of the carrier gas.
12.2.2.2 Parameter list
INLET PRESS
Range: 0.0970.0 kPa (Refer to NOTE 1), Default: 100 kPa
Set the column inlet pressure.
This sets the initial temperature of a pressure program.
When the control mode is set to PRESS, the system controls the column inlet
pressure so that it remains constant during an oven temperature program.
COLUMN FLOW RATE
Range: (Refer to NOTE 2), Default: 1.00 ml/min
Sets the carrier gas flow rate at the capillary column outlet (atmospheric pressure at
25 C).
When you set the carrier gas flow rate, the system calculates the column inlet pressure
based on the inner diameter and the length of the column and the film thickness of the
column. The column flow rate is set separately so that the carrier gas flow rate desired
occures at the initial temperature in the oven temperature program.
LINEAR VELOCITY
Range: (Refer to NOTE 3), Default: 30.0 cm/s
Sets the average linear velocity of the carrier gas flowing in the capillary column.
When you set the linear velocity, the system calculates the column inlet pressure based
on the inner diameter and the length of the column and the film thickness of the column.
Fig. 12.2.4 [FLOW] key main screen
12 Injection Port
12.2 Split/Splitless Injection System
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The linear velocity is set separately so that the linear velocity desired occures at the ini-
tial temperature in the oven temperature program.
When the control mode is set to VELOCITY, the column inlet pressure automatically
changes so that the linear velocity remains constant even while the oven temperature
program is running.
SPLIT RATIO
Range: -1.0/0.09999.9, Default: -1.0
The split ratio is split flow rate / column flow rate.
When you set a split ratio, the system sets the total flow rate based on the calculated
carrier gas flow rate and split flow rate, so that the desired split ratio occurs at the oven
temperature.
Set the split ratio to -1.0 to fix the total flow rate regardless of the oven temperature.
TOTAL FLOW RATE
Range: 0.01200.0 ml/min (Refer to NOTE 1), Default: 500.0 ml/min
In split or splitless mode, the total flow rate is equivalent to column flow rate + split flow
rate + septum purge flow rate.
SPLIT MODE
Selection: SPLIT/SPLITLESS/DIRECT, Default: SPLIT
SPLIT: Controls the column inlet pressure and the total flow rate so that the
column inlet pressure and split ratio occur as specified.
SPLITLESS: Closes the split flow line during the sampling time so that the set column
inlet pressure is controlled by the Total Flow Controller.
Opens the split flow line and controls the Electronid Split Controller so that
the preset column inlet pressure occurs (Refer to Fig. 12.2.2.) after the
sampling time elapses.
DIRECT: Closes the split flow line and the set column inlet pressure (in pressure
mode) or the set total flow rate (in flow rate mode) occurs. When making
direct injection analyses, select WBI in the setup screen so that SPLIT
mode is not available.
SAMPLING TIME
Range: 0.009999.99 min, Default: 1.00 min
Sets the sampling time for splitless analysis.
The sampling time indicates the period of time after analysis starts until the split flow line
is opened.
When setting the sampling time, ensure that the program time is longer than the sampling time.
Otherwise, the sampling time connot function correctly.
CONTROL MODE
Selection: PRESS/VELOCITY/FLOW (for direct injection mode), Default: PRESS
When the injection mode is set to SPLIT or SPLITLESS
PRESS: Controls the system so that the column inlet pressure remains constant
during an oven temperature program.
VELOCITY: Controls the system so that the linear velocity remains constant during
an oven temperature program.
When the injection mode is set to DIRECT
PRESS: Controls the system so that the column inlet pressure remains constant
during an oven temperature program.
VELOCITY: Controls the system so that the linear velocity remains constant during
an oven temperature program.
NOTE
12 Injection Port
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CARRIER GAS TYPE
Selection: He/N2/H2/Ar, Default: He
Specify the carrier gas type supplied to the AFC.
This parameter is used for the measurement/control of the flow rate.
If this parameter is not set correctly, flow rate calculations may not be performed
correctly.
(Example: If this parameter is set to N2 when He is actually used, the displayed total
flow rate, column flow rate and linear velocity are lower than the actual values.)
1. Set the column inlet pressure and total flow rate so that they are within the ranges shown in
Fig. 12.2.5.
The ranges differ according to the columns to be used and purge flow rates.
2. The column flow rate ranges from 0 to the value at which the calculated column inlet pressure is
970 kPa or less and the calculated total flow rate is 1,200 ml/min.
3. The linear velocity ranges from 0 to the value at which the calculated column inlet pressure is
970 kPa or less.
Fig. 12.2.5Available setting ranges for the AFC
NOTE
360
ml/min
720
ml/min
1200
ml/min
290 kPa 590 kPa 970 kPa
Column inlet pressure
150 kPa
Available setting ranges (He, H2)
For He and H2
T
o
t
a
l
f
l
o
w
r
a
t
e
Primary
pressure
980 kPa
Primary
pressure
600 kPa
Primary
pressure
300 kPa
150
ml/min
300
ml/min
600
ml/min
290 kPa 590 kPa 970 kPa
Column inlet pressure
Available settable ranges (N2)
T
o
t
a
l
f
l
o
w
r
a
t
e
For N2
Primary
pressure
980 kPa
Primary
pressure
600 kPa
Primary
pressure
300 kPa
12 Injection Port
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12.2.2.3 PF menu
PF menu Description
Reference
section
Column
Sets inner diameter, length and film thickness of capillary column.
Values set here are used in column inlet pressure caluculations from
column flow rate or linear velocity (or vice versa).
If these parameters are not set correctly, calculations are not performed
correctly.
12.5.3
Gas Saver The gas saver saves carrier gas by reducing the split flow rate. 12.5.4
On/Off
Set the flow controller to be used to On. When the GC starts, the AFC in
the current analytical line which is set to be On is controlled.
Press Prog Sets the column inlet pressure program. 12.5.5
Flow Prog Sets the total flow rate program. 12.5.6
Split Prog Sets the split ratio program. 12.5.7
Purge Sets the septum purge flow rate. 12.5.8
Advanced
High Pressure Injection:
Sets high pressure injection, where the column inlet pressure is kept at a
high value for a certain period of time during injection.
Splitter Fix:
Keeps the split flow rate constant.
12.5.9
Offset
Performs offset calibration of the AFC sensor.
This calibration contributes to good reproducibility of results.
3.6
Next Flow
Toggles among the AFC set up screens if two or more AFCs are installed
in this system.
The [FLOW] key can also be used to switch screens.
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.3 Setting column parameters
For capillary columns, the column inner diameter, length, and film thickness are used to cal-
culate the column flow rate and linear velocity. Enter the column inlet pressure, and the col-
umn flow rate and linear velocity are calculated based on the column parameters.
Alternatively, by entering the column flow rate and linear velocity valves, the column param-
eters are used to calculate the corresponding column inlet pressure.
12.2.3.1 Screen description
Select [Column] (PF menu) from the [FLOW] key main screen to display the Column
Diam. screen shown in Fig. 12.5.5.
12.2.3.2 Parameter list
COLUMN I.D.
Range: 0.016.00 mm, Default: 0.32 mm
COLUMN LENGTH
Range: 0.1250.0 m, Default: 25.0 m
FILM THICKNESS
Range: 0.00300.00 m, Default: 0.50 m
Set the internal diameter, the length and film thickness of the capillary column in use.
These parameter values are used for calculation (or the backward calculation) of the
column head pressure based on the column flow rate or the linear velocity.
Fig. 12.2.6 Column setup screen
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.4 Gas saver
The gas saver function reduces the split ratio during a split of splitless analysis. This reduces
the amount of carrier gas flowing through the split flow line, conserving carrier gas.
Even though this can change the split ratio, the column inlet pressure is kept at a constant
value. In other words, changing the split ratio does not affect the carrier gas flow rate
through in the column.
12.2.4.1 Screen description
Select [Gas Saver] (PF menu) from the [FLOW] key to display the Gas Saver screen
shown in Fig. 12.5.6.
12.2.4.2 Parameter list
GAS SAVER
Selection: On/Off, Default: Off
Select On to use the gas saver function.
Select Off to disable the gas saver function.
GAS SAVER SPLIT RATIO
Range: 0.09999.9, Default: 5.0
Set the split ratio which will reduce the split flow to conserve carrier gas.
Setting 0 closes the split flow line.
GAS SAVER START TIME
Range: 0.009999.99 min, Default: 1.00 min
Specify the period of time after analysis starts until the split ratio switches to gas saver
mode.
This period of time should be longer than the time required for the sample to move from
the injection port to the column.
Setting the gas saves start time too early can provide unpredictable quantitation results.
Fig. 12.2.7 Gas saver setup screen
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.5 Pressure program
You can set a program to increase and decrease the column inlet pressure during analysis.
If high-boiling point contaminants are clunting shorlty after the target compounds, a pressure
program can be used so that the oven temperature does not need to be set higher than nec-
essary. This prolongs column service life.
12.2.5.1 Screen description
Select [Press Prog] (PF menu) from the [FLOW] key main screen when the control
mode is set to PRESS, to display the carrier press screen shown in Fig. 12.2.8
appears.
12.2.5.2 Parameter list
PRESS
Range: 0.0970.0 kPa (Refer to Fig. 12.2.5.), Default: 100 kPa
Set the initial pressure and the final pressure for each stage of the pressure program.
TIME
Range: 0.09999.99 min, Default: 1.00 min
Set the hold time for the initial pressure and the final pressure for each stage of the
pressure program.
RATE
Range: END/-400.00400.00 kPa/min, Default: END
Set the pressure program rate.
If you set the rate to 0, END appears and the program finishes at the previous ramp.
If you move the cursor to END and set any numeric value other than 0, the pressure
and the time for that ramp can be enterd.
The pressure increase/decrease program rate control range may be limited depending on the total flow
rate setup value, the column in use and the purge flow rate.
Fig. 12.2.8 Pressure program setup screen
NOTE
Up to 7 ramps of pressure
increase or decrease can be
set.
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.5.3 PF menu
12.2.5.4 Setting a pressure program
Q Screen terminology
<1-ramp pressure program>
Q Program creation
<1-ramp pressure program>
PF menu Description
Reference
section
Del Line Deletes a line at the current cursor position.
Ins Line Inserts a line in line at the current cursor position.
PRINT Prints the pressure program to a Chromatopac.
Fig. 12.2.9 Pressure program example
Initial pressure (PRSS)..... P1
Initial pressure hold time (TIME)...... a
Program rate (RATE).....
Final pressure (PRS)....... P2
Final pressure hold time (TIM)........ c
Pressure
P2
a
Program
starts.
Program
finishes.
Time
P 2 -P 1
b
b c
60 kPa(2 min)
100 kPa(5 min)
4 kPa/min
12 Injection Port
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12.2.6 Creating a Flow rate program
If the control mode is set to FLOW, increase and decrease the total flow rate during
analysis by making a flow rate program.
When you set a flow rate program for the APC, a corresponding pressure program is actu-
ally calculated based on of the pressure-flow rate calibration curve saved by the GC.
12.2.6.1 Screen description
Select [Flow Prog] (PF menu) from the [FLOW] key main screen while the control mode
is set to FLOW to display the Carrier Flow screen shown in Fig. 12.2.10.
12.2.6.2 Parameter list
FLOW RATE
Range: 0.00970.0 ml/min (Refer to Fig. 12.2.5.), Default: 50 ml/min
Set the initial flow rate and the final flow rate for each stage of the total flow rate
program.
TIME
Range: 0.09999.99 min, Default: 1.00 min
Set the hold time for the initial flow rate and the final flow rate for each stage of the flow
rate program.
RATE
Range: END/-400.00400.00 ml/min
2
, Default: END
Set the flow rate program rate.
If you set the rate to 0, END appears and the program finishes at the previous ramp.
If you move the cursor to END and set any numeric value other than 0, the pressure
and the time for that ramp can be entered.
The control range of the flow rate program may be limited depending on the column in use, purge flow
rate and gas restrictor.
Fig. 12.2.10 Flow rate program setup screen
NOTE
Up to 7 ramps of flow rate
increase/decrease can be set.
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.6.3 PF menu
12.2.6.4 Setting a flow rate program
Q Screen terminology
<1-ramp flow rate program>
Q Program creation
<1-ramp flow rate program>
PF menu Description
Reference
section
Del Line Deletes a line at the current cursor position.
Ins Line Inserts a line in line at the current cursor position.
Print Prints the flow rate program to a hromatopac.
Fig. 12.2.11Flow rate program example
Initial flow rate (FLOW).... F1
Initial flow rate hold time (TIME)...... a
Program rate (RATE)......
Final flow rate (FLW)........ F2
Final flow rate hold time (TIM)......... c
Flow rate
F2
F1
a
c
b
Program
starts.
Program
finishes.
Time
F 2 -F 1
b
20 ml/min(10 min)
30 ml/min(5 min)
3 ml/min
2
12 Injection Port
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12.2.7 Split ratio program
You can change the split ratio during a split analysis. In addition, you can set a split ratio
program after the sampling time has elapsed during splitless analysis.
The split ratio program and the gas saver perform basically the same operation. However,
the split ratio program is used for more general purposes.
12.2.7.1 Screen description
Select [Split Prog] (PF menu) from the [FLOW] key main screen when not in DIRECT
mode to display the Split Ratio screen shown in Fig. 12.2.12.
12.2.7.2 Parameter list
TIME
Range: 0.009999.99 min, Default: 0.00 min
Set this parameter to display the split ratio used previously in the Split Ratio column.
SPLIT RATIO
Range: -1.0/0.09999.9, Default: -1.0
Set the split ratio.
If the split ratio is set to -1.0, the total flow rate remains constant regardless of the
oven temperature.
12.2.7.3 PF menu
Fig. 12.2.12 Split ratio program setup screen
PF menu Description
Reference
section
Del Line Deletes a line at the current cursor position.
Ins Line Inserts a line in line at the current cursor position.
Print Prints the split ratio through to a Chromatopac.
A program can contain up to
7 ramps.
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.7.4 Setting a split ratio program
Q Screen terminology
<1-ramp program>
Q Program creation
<1-ramp program>
Fig. 12.2.13 Example of split ratio program
nitial ratio 'SPLT' S1
nitial program run time 'TME' a
Final ratio 'SPLT' S2
Split ratio
S2
S1
Program
starts.
Program
finishes.
Time
a
Split ratio = 60
Split ratio = 50
5.00 min
12 Injection Port
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12.2.8 Septum purge
Set the septum purge flow rate. The septum purge removes contamination from the injection
port at the septum.
The septum purge flow rate is set here.
12.2.8.1 Screen description
Select [Purge] (PF menu) from the [FLOW] key main screen to display the septum
purge screen shown in Fig. 12.5.13.
Fig. 12.2.14 Septum purge setup screen
12 Injection Port
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12.2.8.2 Parameter list
FLOW RATE
Range: Refer to Fig. 12.2.15, Default: 3.0 ml/min
Sets the septum purge flow rate.
12.2.8.3 PF menu
Fig. 12.2.15 Available setting range for the purge flow rate
PF menu Description
Reference
section
On/Off Set to On when the septum purge flow rate is applied
0
0
50
100
150
200
250
300
100 200 300 400 500
Column inlet pressure (kPa)
Setting range
P
u
r
g
e
f
l
o
w
r
a
t
e
(
m
l
/
m
i
n
)
12 Injection Port
12.2 Split/Splitless Injection System
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12.2.9 High pressure injection and splitter fix mode
Q High Pressure Injection
High pressure injection is a split/splitless injection method which keeps the column inlet
pressure at a value higher than the analysis pressure for a specified period of time while the
sample is injected. Then, the column inlet pressure returns to the normal analysis value.
High pressure injection is effective especially for the splitless injection system. High
pressure injections, can reduce the total gas volume and improve percent recovery valves.
Q Splitter Fix
If the injected sample consists of a solvent with a high vaporization expansion coefficient,
the pressure inside the injection port drastically increases when the solvent vaporizes. This
can result in too much solvent being diverted from the column, reducing sensitivity.
Sending power to the split flow valve at sample injection can keep the split ratio at its desig-
nated valve.
12.2.9.1 Screen description
Select [Advanced] (PF menu) from the [FLOW] key main screen when not in DIRECT
mode to open the advanced screen shown in Fig. 12.2.16.
Fig. 12.2.16Setup screen for high pressure injection and splitter fix mode
12 Injection Port
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12.2.9.2 Parameter list
Q High Pressure Injection
HIGH PRESS INJECTION MODE
Select One of the following three modes.
Off : Disables high pressure injection.
On : Sets the column inlet pressure to high value immediately.
Auto : Immediately sets the column inlet pressure to high pressure. When analysis is
finished and the GC returns to the ready status, the column inlet pressure
automatically increases.
HIGH PRESS INJECTION PRESS
Range: 0.0970.0 kPa (Refer to Fig. 12.2.5.), Default: 100.0 kPa
Set the column inlet pressure for high pressure injection.
HIGH PRESS INJECTION TIME
Range: 0.009999.99 min, Default: 1.00 min
Set the period of time after analysis starts until the column inlet pressure returns to the
original value.
Usually, set this equal to the sampling time.
Q Splitter Fix
SPLITTER FIX MODE
Selection: Off/On/Auto, Default: Off
Select one of the following three modes.
Off : Disables splitter fix mode.
On : Fixes the split flow line immediately.
Auto : Automatically enters splitter fix mode after analysis finishes and the system returns to
ready status.
FIX TIME
Range: 0.09999.99 min, Default: 0.10 min
Set the period of time to be in splitter fix mode.
When SPLITTER FIX MODE is set to On, indicate the period of time after SPLITTER FIX
MODE is set to On to exit splitter fix mode.
When SPLITTER FIX MODE is set to Auto, set the period of time after the analysis starts
to exit splitter fix mode.
Using splitter fix mode for long periods of time may interfere with constant pressure, negatively affect-
ing reproducibility of results.
HIGH PRESS INJECTION MODE = On HIGH PRESS INJECTION MODE = Auto
NOTE
145
12 Injection Port
12.3 12.
GC-2014
12.3Direct Injection System
Q Direct injection system
In a direct injection system, a wide-bore (0.53 mm or greater) column is used. Nearly the
entire amount of sample injected is inrtoduced on the column. This usually results in better
sensitivity than narrow-bore columns with split injections. However, peak shapes are broad,
which decreases resolution and can lead to a higher S/N ratio.
The direct injection system uses a WBI (wide-bore injection) injection port. When WBI is
specified, DIRECT injection mode is automatically used and split mode is not available on
the [INJ] key main screen.
Fig. 12.3.1
Control
Control
TFC
CARRIER
PURGE
PURGE VENT
Capillary column
12 Injection Port
12.3 Direct Injection System
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12.3.1 Setting the temperature
12.3.1.1 Screen description
Press the [INJ] key to display the injection port main screen shown in Fig. 12.3.2 and to
set the injection port temperature.
12.3.1.2 Parameter list
TEMP
Range: 0.0400.0 C, Default: 25.0 C
Set the injection port temperature.
Keep the injection port at the lowest practical temperature for the analysis; this prolongs
the service life of the temperature sensor. To instantly vaporize the injected sample, set
the injection port temperature approximately 30 C higher than the final column oven
temperature. Because the sample quantity is usually minute, the sample is vaporized at
temperatures lower than the boiling point of sample compounds. To set the maximum
temperature limit, refer to 16.6.4 Setting the maximum temperature limits in 16.6 GC
Configuration.
12.3.1.3 PF menu
Fig. 12.3.2[INJ] key main screen
PF menu Description
Reference
section
Print Prints the temperature program to a Chromatopac.
Next Inj
Toggles to the next setup screen when two or more injection ports are
installed in this system.
The [INJ] key can also be used to switch screens.
12 Injection Port
12.3 Direct Injection System
147
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12.3.2 Setting the flow rate
12.3.2.1 Screen description
Press the [FLOW] key to display the main Flow Screen shown in Fig. 12.3.3. Set the
AFC parameters to control the carrier gas pressure and the flow rate.
12.3.2.2 Parameter list
INLET PRESS
Range: 0.0970.0 kPa, Default: 100.0 kPa
Set the column inlet pressure.
When creating a pressure program, this specifies the initial pressure.
When the control mode is set to PRESS, the system controls the column inlet
pressure so that it remains constant during a temperature program.
Normally, when using a wide bore column, set the column inlet pressure to a low
pressure (2040 kPa).
COLUMN FLOW RATE
Default:(Refer to NOTE 1) 1.00 ml/min
Set the carrier gas flow rate at the capillary column exit (atmospheric pressure at 25 C).
When you set the carrier gas flow rate, the system calculates the column inlet pressure
based on the inner diameter, the length and the film thickness of the column. The col-
umn flow rate is set separately so that the carrier gas flow rate desired occurs at the ini-
tial temperature in the oven temperature program.
LINEAR VELOCITY
Default:(Refer to NOTE 2) 30.0 cm/s
Set the average linear velocity of the carrier gas flowing in the capillary column.
Fig. 12.3.3 [FLOW] key main screen
12 Injection Port
12.3 Direct Injection System
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When you set the linear velocity, the system calculates the column inlet pressure based
on the inner diameter, the length and the film thickness of the column. The linear velos-
ity is set separately so that the linear velocity desired occurs at the initial temperature in
the oven temperature program.
If you set the control mode to VELOCITY, the column inlet pressure automatically
changes so that the linear velocity remains constant during the oven temperature
program.
TOTAL FLOW RATE
Range: 0.01200.0 ml/min (Refer to Fig. 3.5.1), Default: 50.0 ml/min
Set the total flow rate, which is the sum of column flow rate + split flow rate + septum
purge flow rate.
CONTROL MODE
Selection: PRESS/VELOCITY/FLOW, Default: PRESS
PRESS: Controls the system so that the column inlet pressure remains constant during
an oven temperature program.
VELOCITY: Controls the system so that the linear velocity remains constant during an
oven temperature program.
FLOW: Controls the system so that the set flow rate remains constant.
CARRIER GAS TYPE
Selection: He/N2/H2/Ar, Default: He
Specify the carrier gas type supplied to the AFC.
This parameter is used for the measurement/control of the flow rate.
If this parameter is set incorrectly, flow rate calckulations may not be performed
incorrectly.
(Example: If this parameter is set to N2 when He is actually used, the displayed total
flow rate, column flow rate and linear velocity are lower than the actual values.)
1 The column flow rate ranges is from 0 to the value at which the calculated column inlet pressure is
970 kPa or less and the calculated total flow rate is 1,200 ml/min or less.
2 The linear velocity ranges is from 0 to the value at which the calculated column inlet pressure is
970 kPa or less.
12.3.2.3 PF menu
PF menu Description
Reference
section
Column
Sets inner diameter, length and film thickness of capillary column.
Values set here are used in column inlet pressure caluculations from
column flow rate or linear velocity (or vice versa).
If these parameters are not set correctly, calculations are not performed
correctly.
12.2.3
On/Off
Set the flow controller to be used to On. When the GC starts, the AFC in
the current analytical line which is set to be On is controlled.
Press Prog Sets the column inlet pressure program. 12.2.5
FLOW Prog Sets the total flow rate program. 12.2.6
Purge Sets the septum purge flow rate. 12.2.8
Offset
Performs offset calibration of the AFC sensor.
This calibration contributes to good reproducibility of results.
12.4
Next Flow
Toggles among the AFC setup screens if two or more AFCs are installed in
this system.
The [FLOW] key can also be used to Switch screens.
NOTE
149
12 Injection Port
12.4 12.
GC-2014
12.4AFC and APC Offset Calibration
The pressure and flow rate sensors of AFC and APC may become slightly off after long
periods of use. If the sensor values deviate, 0.5 kPa or 0.5 ml/min is indicated for
pressure or flow rate instead of zero even when there is no gas flowing.
In this case, perform the offset (zero point) calibration. Calibration is especially effective
when data reproducibility is important.
Calibration procedures are as follows.
1. Set the temperatures of the injection port, column oven, and detector low and wait until
they become 40 C or lower.
(AFC calibration is performed when there is no gas flowing. Stopping gas when parts'
temperatures are high may cause deterioration of columns.)
2. Press the [SYSTEM] key, select Start Seq (PF menu), and check the mode to start the
GC when the power is turned on. If it is not set to Manual Start, change it.
3. Turn off the power and reboot it.
Rebooting leaves the unit at the state of SYSTEM OFF.
Do not shut off gas supply by turning off the main valve or by any other measures.
Performing calibration without primary pressure makes the zero point off.
4. To perform AFC calibration, completely empty out the gas by detaching the septum of
the injection port.
To perform APC calibration, wait until when the pressure or flow rate does not fluctuate.
5. Press the toggle key on each flow controller's parameter setup screen until the Offset
PF menu is displayed. For AFC, press the [FLOW] key once and the toggle key twice.
6. Press Offset (PF menu).
The message Zero Calibration Start appears. Approximately 10 seconds later, the
message Zero calibration completed appears indicating that the calibration is
complete.
7. Return the septum of the injection port to its original position if it has been detached.
Fig. 12.4.1 (AFC) Fig. 12.4.2 (APC)
12 Injection Port
12.5 12.
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12.5Setting the Flow Rate Parameters
Q Linear velocity and carrier gas selection
In capillary analysis, the type and the flow rate of the carrier gas have a considerable effect
on the column efficiency. The figure below shows changes in the HETP (Height Equivalent
to Theoretical Plate) at different linear velocity valves for nitrogen, helium and hydrogen car-
rier gas.
Fig. 12.5.1 Effect on linear velocity and HETP for various carrier gases (H-V curve)
The graph above shows that the lowest HETP values are obtained when nitrogen is used as
the carrier gas and the linear velocity is set to a value a little less than 10 cm/s. However,
nitrogen is not a good carrier gas for capillary analysis for the following reasons.
(1) If the linear velocity deviates only slighty from the optimum value, the HETP increases
dramatically.
(2) To obtain the optional linear velocity, the flow rate must be low, resulting in long analysis
times.
Helium is frequently used as the carrier gas because the HETP is low over a considerably
wider linear velocity range starting at 20 cm/s.
The column efficiency of hydrogen is good at higher linear velocities than for helium. For this
reason, hydrogen can be used for rapid analyses. However, hydrogen is seldom used in
reality because it is extremely flammable, and therfore too dangerous.
Q Efficiency of an analysis
Usually, analyses are performed with a flow rate that is higher than the optimal flow rate, as
long as separation of conpounds is sufficient. This reduces the analysis time. For general
analyses on this system, setting the linear velocity to 30 cm/s is recommended.
The tables below show the column inlet pressure at which the linear velocity becomes
approximately 30 cm/s. Use the tables as the guideline for setting the column inlet pressure.
However, the inlet pressure also depends on the column type.
12 Injection Port
12.5 Setting the Flow Rate Parameters
151
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Example 1: Column oven temperature = 50 C(carrier gas = helium)
Example 2: Column oven temperature = 200 C (carrier gas = helium)
Fig. 12.5.2 shows the relationship between the column flow rate and the column inlet pressure.
60 d
4
P P0
2
P0
2
Fc 10
3
256 L P0
Fc : Column flow rate [ml/min]
d : Column I.D [mm]
L : Column length [m]
P : Column inlet pressure [kPa]
P0 : Column outlet pressure = atmospheric pressure [kPa]
: Viscosity coefficient (19.4 Pas (helium, 20 C))
Fig. 12.5.2
Length
30 m 60 m
I.D. of column Film thickness
0.25 mm 0.25 m 100 kPa 210 kPa
0.32 mm 0.25 m 60 kPa 120 kPa
0.53 mm 1.5 m 20 kPa 40 kPa
Length
30 m 60 m
I.D. of column Film thickness
0.25 mm 0.25 m 130 kPa 275 kPa
0.32 mm 0.25 m 80 kPa 160 kPa
0.53 mm 1.5 m 30 kPa 60 kPa
NOTE
12 Injection Port
12.5 Setting the Flow Rate Parameters
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153
13.1 13. 13.
GC-2014
13 Detector
13.1Hydrogen Flame Ionization Detector (FID)
13.1.1 Principle of FID operation
In the hydrogen flame ionization detector (FID), hydrogen gas is mixed with the column
outlet gas at a certain ratio as shown in Fig. 13.1.1.The gas mixture combusts in the air
atmosphere. An electrode exists at each end of the FID jet, and DC voltage is applied
between the electrodes.
If only pure carrier gas (nitrogen, helium or argon) and hydrogen gas are mixed, little current
is produced between the electrodes. When an organic compound is mixed with the carrier
gas, current is produced proportionally to the amount of organic compound present.
This is because ions (mainly carbon ions) are generated when an organic compound
combusts within the hydrogen flame, and the generated ions are captured by the collector.
For isomers, the ion quantity generated is almost proportional to the number of carbons
contained in the compound. However, carbon atoms in a C=O form do not create a signal.
The presence o halogens in the compound decreases sensitivity.
Because the ion current obtained by the FID is very low, it is amplified into a proper voltage,
then output to a Chromatopac or personal computer.
Fig. 13.1.1
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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13.1.2 Setting the detector
13.1.2.1 Screen description
Press the [DET] key to display the detector main screen shown in Fig.13.1.2. Here, set
the detector temperature, the detector gas flow rate, etc.
When the detector is configured in the analytical line, the output signal settings appear
in the lower portion of the screen.
13.1.2.2 Parameter list
DETECTOR CONTROLLER
Selection: On/Off, Default: On
When a detector is set to On, its current and voltage are controlled.
When a detector is configured in an analytical line and set to On here, the detector is
controlled and its signal monitored. However, even if a detector is set to Off, the gas
flow is controlled, and the temperature increases to the set value if the detector is
configured in an analytical line.
TEMP
Range: 0.0400 C, Default: 25.0 C
Set the detector temperature. Normally, set the detector temperature approximately
30 C higher than the final column oven temperature to prevent contamination by high
boiling point compounds.To set the maximum temperature limit, refer to 16.6.4 Setting
the maximum temperature limits in 16.6 GC Configuration.
FLAME (monitor only)
Selection: On/Off
Select On to ignite the flame.
Select Off to extinguish the flame.
(a) Dual FID (b) Single FID
Fig. 13.1.2 [DET] key main screen
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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GC-2014
SIGNAL POLARITY
(Displayed only when Dual is selected for the control mode of the dual FID)
Selection: +/-, Default: +
Set to + to output after subtracting the right side cell signal from the left side cell signal
of the dual FID and set to - for the opposite.
FILTER TIME CONSTANT
Selection: 4 ms/5 ms/10 ms/20 ms/50 ms/100 ms/200 ms/500 ms/1 s/2 s,
Default: 200 ms (single FID), 1 s (dual FID)
This constant affects the processing of the detector signal.
As the time constant increases, noise as well as the peak height are reduced.
Select the optimum value in accordance with the peak half width. (Refer to 13.3 Filter
Signal Time Constant.)
CONTROL MODE
Selection: Dual/single L/single R, Default: Dual
Set to Dual when connecting two columns to the dual FID and Single L or R when
connecting one column.
SIGNAL OUTPUT PORT
Selection: Off/Ch1/Ch2/Ch3/Ch4, Default: (Channel is automatically assigned.)
Select the digital and analog signals output channels. Four channels are available.
However, for analog output, only Ch1 and Ch2 are available as standard.
BACKGROUND SIG. SAVE
Selection: Off/Buff 1/Buff 2, Default: Off
Background baseline signals can be saved for the purpose of background subtraction.
BACKGROUND SIG COMP.
Selection: Off/Buff 1/Buff 2, Default: Off
Subtracts the saved background signal baseline from the actual baseline. This produces
a stable baseline despite considerable baseline fluctuations
DET SIG SUBTRACTION
Selection: Off/DET# 1/DET# 2/DET# 3/DET# 4, Default: Off
Subtracts the detector signal of one detector from the signal of another detector. This
function is mainly used in a dual column flow line to subtract the data acquired without
an injection from the data acquired with an injection. The background signal is elimi-
nated.
For the details on background save and background compensation, refer to 13.4
Background Compensation.
SIGNAL RANGE
Selection: 1/10
-1
/10
-2
/10
-3
/10
-4
, Default: /10
-1
Multiplies the analog signal by the coefficient 10
-x
for a linear analog signal type.
If the data processing unit is saturated, for example, change the setting from 1 to
10
-1
, from 10
-2
to 10
-3
. In case of the digital signal, the signal is always output
with 1.
SIGNAL ATTENUATION
Selection: 1/2
-1
/2
-2
/2
-3
/2
-4
, Default: /2
-1
Multiplies the analog signal by the coefficient 2
-x
for a wide analog signal type.
If the data processing unit is saturated, for example, change the setting from 1 to 2
-1
,
from 2
-2
to 2
-3
. In case of the digital signal, the signal is always output with 1.
ANALOG SIGNAL TYPE
Selection: Linear/Wide, Default: Linear
Set this item when the GC is connected to a Chromatopac in analog format.
Wide ... Select wide when connecting the GC to the C-R8A/C-R7A/C-R7A plus.
The GC outputs square root of the original signal to the Chromatopac, and the
received signals are squared in the Chromatopac.
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
156
GC-2014
When connecting the GC to a C-R7A/CR-7A plus for the first time, or replacing
the Chromatopac, set the detector signal output to Off and perform
calibration. (For the calibration procedure, refer to 2.2 Outputting Analog
Signals to the Chromatopac.)
Linear...Select linear when connecting the GC to any Chromatopac other than the C-
R8A/C-R7A/CR-7A plus.
When connecting the GC to the C-R8A/C-R7A/C-R7A plus and setting the
ANALOG SIGNAL TYPE to Linear, the optional signal cable (linear P/N 221-
47251-92) is required.
13.1.2.3 PF menu
PF menu Description
Reference
section
Ignite
Reduces the air flow rate, heats filament, and ignites detector when
pressed when FLAME was set to Off.
If AUTO IGNIT is set to On on the [SYSTEM] key screen, the detector is
automatically ignited after each setting reached the setting value.
13.2.2.4
Det Gas
Sets the flow rate of makeup gas, hydrogen and air if the advanced
Pressure Control (APC) is installed.
13.2.3
Ign. Set
If the Advanced Pressure Control (APC) is installed, you can set automatic
ignition and automatic re-ignition. Default value is On.
Next Det
Toggles to the setup screen of another installed detector.
The [DET] key can also be used to switch screens.
VLV On or
VLV Off
When the optional solenoid valve to shut off supply gas is installed,
hydrogen and air are shut off by the valve until ignition.
Opens the solenoid valve when VLV On is displayed and closes the valve
when VLV Off is displayed.
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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13.1.3 Setting the Detector Gas (manual flow controller)
Hydrogen and air are supplied to the FID as detector gas. For capillary analysis, makeup
gas is required to prevent peak tailing and optimize FID sensitivity.
GC-2014 has flow controllers according to models as described below.
Set the detector gas flow rate following the procedures described below.
1. Turn the main valve of the gas cylinder to supply gas to the GC.
2. Open the flow controller cover on the top of the back of the unit.
Layouts for the models with the dual FID and models with the single FID are as shown
in Fig. 13.1.3 (a) and Fig. 13.1.3 (b) respectively.
3. When the optional solenoid valve to shut off supply gas (P/N 221-70782-91) is installed,
hydrogen and air are shut off by the valve until ignition. To adjust the pressure, press the
[VLV On] key on the [DET] key main screen to open the solenoid valve.
4. Turn the pressure regulators to set the pressure as described below.
Hydrogen 55 kPa (Approx. 40 ml/min)
Air 40 kPa (Approx. 400 ml/min)
Makeup gas (nitrogen) 75 kPa (Approx. 30 ml/min)
Makeup gas (helium) 80 kPa (Approx. 30 ml/min)
Pressure-flow rate calibration curves for each flow controller are shown in Fig. 13.1.4. These curves
slightly differ according to units.
Models with the dual FID (GC-2014AF, GC2014ATF, etc.)
Two flow paths of manual flow controllers with hydrogen and air
Models with the single FID (GC-2014AFsc, etc.)
One flow path of manual flow controller with hydrogen and air
One flow path of manual flow controller for makeup gas
(a) Dual FID (b) Single FID
Fig. 13.1.3Manual flow controller for FID
Top
Bottom
Hydrogen
pressure meter
Right
Flow controller
for the right side FID
Left
Flow controller
for the left side FID
Back
Hydrogen
pressure regulator
Front
Air pressure regulator
Air
pressure meter
Top
Bottom
Hydrogen
pressure meter
Back
Hydrogen
pressure regulator
Front
Air pressure regulator
Air
pressure meter
Top
Makeup gas
pressure meter
Back
Makeup gas
pressure regulator
NOTE
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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Fig. 13.1.4 Pressure-flow rate calibration curves (examples)
O
6O
1OO
m!/m1n
2O 4O 6O 8O 1OO KPa
(a) Hydrogen
Hydrogen pressure
O
6OO
1OOO
m!/m1n
2O 4O 6O 8O 1OO KPa
(b) Air
Air pressure
O
1O
m!/m1n
2O 4O 6O 8O 1OO KPa
(c) Makeup gas (N2)
Makeup gas pressure
O
1O
2O 2O
8O 8O
4O 4O
6O 6O
6O 6O
m!/m1n
2O 4O 6O 8O 1OO KPa
(d) Makeup gas (He)
Makeup gas pressure
H
y
d
r
o
g
e
n
f
l
o
w
r
a
t
e
A
i
r
f
l
o
w
r
a
t
e
M
a
k
e
u
p
g
a
s
f
l
o
w
r
a
t
e
M
a
k
e
u
p
g
a
s
f
l
o
w
r
a
t
e
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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13.1.4 Setting the detector gas flows(APC)
The FID detector gas consists of makeup gas, hydrogen and air. The makeup gas is inert
gas supplied to the detector to prevent peak tailing and optimize FID sensitivity. Usually, the
carrier gas is used as the makeup gas. Hydrogen gas and air are supplied to be combusted
inside the detector, creating the FID flame.
13.1.4.1 Screen description
Select [Det Gas] (PF menu) from the [DET] key main screen to display the flow screen
shown in Fig. 13.1.5.
When the Start Flow status is selected on the [SYSTEM] key screen, the makeup gas
flow starts. Just before the ignition procedure begins, hydrogen and air flow starts.
Selecting Stop Temp/Det status from the [SYSTEM] key main screen, gas flow stop.
Fig. 13.1.5 Setting the detector gas flows
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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13.1.4.2 Parameter list
H2
Range: 0.0200.0 ml/min, Default: 40.0 ml/min(optimal flow rate)
MAKE UP
Range: 0.0100.0 ml/min, Default: 30.0 ml/min(optimal flow rate)
Makeup gas is inert gas to be supplied to the detector to optimize its sensitivity during
capillary analysis. Nitrogen and helium can be used for the FID. Using nitrogen is
recommended because it offers higher sensitivity. Set the value to zero for packed
analysis.
GAS TYPE
Selection: N2/He/Ar, Default: He
Set the type of gas used as the makeup gas.
Do not use hydrogen for make up gas.
Air
Range: 0.01000.0 ml/min, Default: 400.0 ml/min(optimal flow rate)
13.1.4.3 PF menu
PF menu Description
Reference
section
Next Flow
Switches screens to set detector gas for the left (L) and right (R) side
detectors during the dual mode of the dual FID with APC.
12.4
On/Off
Select Off to stop gas flow.
Select On to restart the gas flow.
Default value is On.
Offset
Performs offset calibration of APC sensor.
This calibration improves the reproducibility of results.
3.6
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
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13.1.5 Igniting and Extinguishing the FID
13.1.5.1 Confirmation prior to FID ignition
Confirm the following points prior to FID ignition.
1. Connect the column.
2. Specify the FID to be ignited in a flow line. (Refer to 8.3 Specifying the Analytical
Flow Line Components ([Line Config]))
3. Set the FID to be ignited to On. (Refer to 13.1.2 Setting the Detector.)
4. Turn the main valve of the gas cylinder to supply gas.
5. Set the flow rate of the detector gas. For APC, press [On/Off] (PF menu) on the
screen to set the detector gas so that all gas control is turned on.
(Refer to 13.1.3 Setting the Detector Gas (manual flow controller) or 13.1.4
Setting the detector gas flows(APC).)
13.1.5.2 FID ignition procedures
Q Automatic ignition
The system starts and the FID is ignited automatically.
1. Press the [SYSTEM] key and set the following parameters. Change other
parameters if necessary.
2. Start the GC.
GC starts when [Start GC] (PF menu) is pressed in manual starting and when the
power is turned on in automatic starting.
START TEMP/DET Yes
DETECTOR On
AUTO IGNITE On
(a) Main screen (b) [Start Seq] (PF menu)
Fig. 13.1.6 Setting starting procedures (automatic ignition)
13 Detector
13.1 Hydrogen Flame Ionization Detector (FID)
162
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3. After the GC starts, gas control starts. Temperature/detector control starts after the
start time passes. When the detectors temperature becomes READY, the FID is
ignited automatically.
Q Manual ignition
The FID is ignited by key operation.
1. Press the [SYSTEM] key and set the following parameters. Change other
parameters if necessary.
2. Start the GC.
GC starts when [Start GC] (PF menu) is pressed in manual starting and when the
power is turned on in automatic starting.
3. After the GC starts, gas control starts. Temperature/detector control starts after the
start time passes.
4. After the detectors temperature becomes 100 C or higher, press [Ignite] (PF
menu) on the [DET] key main screen.
START TEMP/DET Yes
DETECTOR On
AUTO IGNITE Off
(a) Main screen (b) [Start Seq] (PF menu)
Fig. 13.1.7 Setting starting procedures (manual ignition)
13 Detector
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If the detector is set to Off when setting GC starting procedures, the setting for all detectors specified in
a respective flow line automatically becomes Off.
Always set to On when only FID is used.
To set to Off while using detectors other than FID at the same time, set the detector to
On on the [DET] key screen and then operate the ignition.
1. The messages ignition finished and ignition finished (retried) mean that ignition has been carried
out properly.
2. The message DET#1, ignition failed or other similar messages mean that ignition has failed. In
this case, the units conditions are as follows.
Hydrogen and air continue to be supplied when the manual flow controller is used.
When the optional solenoid valve to shut off supply gas is installed, hydrogen and air are shut off by
the valve.
When the APC is used, APCs valve is closed to shut off hydrogen and air supply.
3. Potential causes of ignition failure are listed below. Remove the cause then ignite the FID.
Column is not connected.
Detector gas is not supplied.
Detector gas flow rate is not proper.
Unused detector (FID or FPD) is set to On.
FID jet is clogged. Clean or replace the FID jet.
Igniter filament is broken. Replace the igniter.
4. When the optional solenoid valve to shut off supply gas is installed or ignition is carried out
immediately after opening the gas cylinders main valve, the message (retried) or ignition failed
may be displayed because hydrogen in the piping is not completely replaced.
13.1.5.3 Extinguishing the FID
Q Manual flow controller
Extinguish the FID flame by closing the main valve of the hydrogen cylinder to shut off
gas supply.
Q When the manual flow controller and the solenoid valve to shut off supply gas are installed
Press [Stop GC] (PF menu) on the [SYSTEM] key main screen. The solenoid valves
close when the detector control ends to shut off gas supply, extinguishing the FID flame.
Q APC
Press [Stop GC] (PF menu) on the [SYSTEM] key main screen. APC control ends when
the detector control ends to shut off gas supply, extinguishing the FID flame.
To extinguish the flame before the GC stops, press the [DET] key, select [DET Gas] (PF
menu), and set the control of hydrogen and air to Off on the screen. Gas supply is shut
off, extinguishing the FID flame.
START TEMP/DET Yes
DETECTOR Off
AUTO IGNITE Off
NOTE
NOTE
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13.2Thermal Conductivity Detector (TCD)
13.2.1 Principle of TCD operation
The thermal conductivity detector (TCD) can detect all compounds except the carrier gas
itself.
The metallic TCD filament is heated by the application of current. The carrier gas used has a
high thermal conductivity, such as helium. As sample compounds pass the filament, the fila-
ment temperature increases, because the thermal conductivity of the sample compounds is
less than that of the carrier gas. The filament temperature changes affect its resistance; the
resistance is measured and produces a chromatogram.
A reference filament also exists, where only carrier gas flows, to eliminate background resis-
tance fluctions.
Fig. 13.2.1
The TCD sensitivity is proportional to the difference in thermal conductivity between the
sample and the carrier gas. Because the thermal conductivity of the sample is lower than
that of the carrier gas, the TCD sensitivity increases as the thermal conductivity of the carrier
gas increases.
For high sensitivity analysis, use helium with a purity of 99.9995 % or more.
Thermal conductivity k (x10
-4
Wm
-1
K
-1
) at room temperature, 300 K
Gas
Thermal
conductivity
Gas
Thermal
conductivity
Simple
compounds
He 1499
Inorganic
compounds
CO2 166.2
H2 1815 H2O 181
N2 259.8
Organic
compounds
acetone 115
Ar 177.2 hexane 128
Reference gas
TCD cell
Filament
Output signal
Carrier gas
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13.2.2 Setting the detector
13.2.2.1 Screen description
Press the [DET] key to display the Detector main screen shown in Fig. 13.3.2. Here, set
the detector temperature, the detector gas flow rate, etc.
When the detector is configured in the analytical line, the output signal settings appear
in the lower portion of the screen.
13.2.2.2 Parameter list
DETECTOR CONTROLLER
Selection: On/Off, Default: On
When a detector is set to On, its current and voltage are controlled.
When a detector is configured in an analytical line and set to On, the detector is con-
trolled and its signal monitored. However, the temperature increases up to the set value
if the detector is configured in the flow line even if detector control is Off.
TEMP
Range: 0.0400.0 C, Default: 25.0 C
Set the detector temperature. The TCD sensitivity is proportional to the difference in
temperature between the detector and the filament. Accordingly, the sensitivity
increases as the detector temperature decreases. However, the detector is normally set
approximately 10 C higher than the final column oven temperature: this prevents con-
tamination in the TCD cell.
To set the maximum temperature limit, refer to 16.6.4 Setting the maximum
temperature limits.
Fig. 13.2.2 [DET] key main screen
13 Detector
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SIGNAL POLARITY
Selection: +/-, Default: +
When analyzing compounds with a thermal conductivity higher than the carrier gas,
baseline peaks are inverted (negative). When this occurs, switch to a polarity of - to
produce positeve peaks.
CURRENT
Range: 0200 mA, Default: 0 mA
The TCD sensitivity is approximately proportional to the cube of the current.
If the sensitivity is insufficient, increase the current within the range shown in
Fig. 13.2.3. The maximum operating current is determined by the detector temperature
and the carrier gas type. Keeping the current highre than necessary shortens the fila-
ments life and can cause baseline drift.
Fig. 13.2.3Maximum operating current
CAUTION
If the current is turned on before the carriergas + make up gas has
completely replaced the air, the filament can be blown.
Ensure that the current is set to 0 at first. Press the [SYSTEM] key
main screen, allow carrier gas to flow for approximately 10 minutes,
then set the current.
CAUTION
To avoid broken filaments and poor performance, set the current
below the valves indicated by the curves below.
Current
(mA)
200
100
0 100 200 300 400
TCD temperature(
)
Carrier gas He
Carrier gas H2
Carrier gas N2
Carrier gas Ar
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FILTER TIME CONSTANT
Selection: 4 ms/5 ms/10 ms/20 ms/50 ms/100 ms/200 ms/500 ms/1 s/2 s, Default: 1 s
This constant affects the processing of the detector signal.
As the time constant increases, noise as well as the peak height are reduced.
Select the optimum value in accordance with the peak half width. (Refer to 13.3 Filter
Signal Time Constant.)
SIGNAL OUTPUT PORT
Selection: Off/Ch1/Ch2/Ch3/Ch4, Default: (Channel is automatically assigned.)
Select the digital and analog signals output Channels. Four channels are available.
However, for analog output, only Ch1 and Ch2 are available as standard.
BACKGROUND SIG. SAVE
Selection: Off/Buff 1/Buff 2, Default: Off
Background baseline signals can be saved for the purpose of background subtraction.
BACKGROUND SIG COMP.
Selection: Off /Buff 1/Buff 2, Default: Off
Subtracts the saved background signal baseline from the actual baseline. This pro-
duces a stable baseline despite considerable baseline fluctuations.
DET SIG SUBTRACTION
Selection: Off /DET#1/DET#2/DET#3/DET#4, Default: Off
Subtracts the detector signal of one detector from the signal of another detector.
For the details on background save and background compensation, refer to 13.4
Background Compensation.
SIGNAL RANGE
Selection: 1/10
-1
/10
-2
/10
-3
/10
-4
/, Default: 10
-1
Multiplies the analog signal by the coefficient 10
-x
for a linear analog signal type. If the
data processing unit is saturated, for example, change the setting from 1 to 10
-1
,
from 10
-2
to 10
-3
. In case of the digital signal, the signal is always output with 1.
SIGNAL ATTENUATION
Selection: 1/2
-1
/2
-2
/2
-3
/2
-4
/, Default: 2
-1
Multiplies the analog signal by the coefficient 2
-x
for a wide analog signal type. If the
data processing unit is saturated, for example, change the setting from 1 to 2
-1
,
from 2
-2
to 2
-3
. In case of the digital signal, the signal is always output with 1.
ANALOG SIGNAL TYPE
Selection: Linear/Wide, Default: Linear
Set this item when the GC is connected to a Chromatopac in analog format.
Wide ... Select Wide when connecting the GC to the C-R8A/C-R7A/C-R7A plus.
The GC outputs square root of the original signals to the Chromatopac, and the
received signals are squared in the Chromatopac.
When connecting the GC to a C-R7A/CR-7A plus for the first time, or replacing
the Chromatopac, set the detector signal output to Off and perform
calibration. (For the calibration procedure, refer to 2.2 Outputting Analog
Signals to the Chromatopac.)
Linear...Select linear when connecting the GC to any Chromatopac other than the C-
R7A/CR-7A plus.
When connecting the GC to the C-R8A/C-R7A/C-R7A plus and setting the
ANALOG SIGNAL TYPE to Linear, the optional signal cable (linear, P/N
221-47251-92) is required.
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13.2.2.3 PF menu
PF menu Description
Reference
section
Next Det
Toggles to the setup screeen of another detector.
The [DET] key can also be used to switch screens.
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13.2.3 TCD Zero Point Adjustment
Press [Zero Adj] (PF menu) on the [MONIT] key main screen to automatically start zero point
adjustment. When the TCD is used, the balance between sample and reference sides
becomes off after a column is replaced so the baseline may go off-scale. In this case, carry
out a zero-coarse-adjustment following the procedures described below.
TCD zero-coarse-adjustment is usually unnecessary when starting the unit after stopping it to leave the
lab on the previous day. It takes a while for the TCD baseline to stabilize. Even if the baseline is off-
scale when starting the unit, it goes close to zero when it stabilizes in many cases. Wait until the
baseline stabilizes.
1. Press [Zero Free] (PF menu) on the [MONIT] key main screen.
2. Turn the TCD zero-coarse-adjustment control shown on Fig. 13.2.4 to make the baseline close to
zero. It takes a while for the baseline to move after the control is turned. Turn the control slowly.
3. Press [Zero Adj] (PF menu) on the [MONIT] key main screen.
Fig. 13.2.4
NOTE
TCD zero -coarse
-adjustment control
13 Detector
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13.3Filter Signal Time Constant
Q Selecting the filter time constant
Normally, analysis can be performed with the time constant set to the default value (dual
FID, TCD: 1 s, single FID: 200 ms). In order to improve the S/N ratio, the time constant can
be changed by measuring the peak half width.
Fig. 13.3.1 shows the relationship between the peak half width and the time constant where
the S/N ratio is maximaized. For example, if the half width of a peak is 0.1 sec, the S/N
ratio is maximaized when the time constant is set to 20 ms.
Fig. 13.3.1Relationship between time constant and S/N ratio
Half width 10 s
Half width 1 s
Half width 0.1 s
4
m
s
5
m
s
1
0
m
s
2
0
m
s
5
0
m
s
1
0
0
m
s
2
0
0
m
s
5
0
0
m
s
1
s
2
s
Time constant
N
o
r
m
a
l
i
z
e
d
S
N
r
a
t
i
o
0
0.2
0.4
0.6
0.8
1
1.2
171
13 Detector
13.4 13.
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13.4Background Compensation
If the baseline drifts considerably during programmed temperature analysis, the baseline drift can
be saved as a background baseline in GCs waveform memory (background save). Afterwards,
the background can be subtracted from the signal (background compensation). The below is
background compensation procedures.
1. Set background storage.
Select where the background baseline
should be saved on the [DET] key main
screen. Either Buff 1 or Buff 2 can be
selected.
BACKGROUND SIG. SAVE Buff 1 (or Buff 2)
BACKGROUND SIG. COMP. Off
2. Execute analysis without sample injection. Baseline fluctuation is saved in Buff 1 or
Buff 2 as background.
3. Set background compensation.
Set the background to be subtracted as the
baseline fluctuation on the [DET] key main
screen.
BACKGROUND SIG. SAVE Off
BACKGROUND SIG. COMP. Buff 1 (or Buff 2)
4. Inject a sample and execute analysis. A signal after subtracting the background is
outputted.
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Fig. 13.4.1 Example of programmed analysis without compensation
Fig. 13.4.2Example of programmed analysis with compensation
14.1 14.
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14 Diagnosis
14.1Standard Diagnosis
Each part of the gas chromatograph is checked for problems with the self-diagnosis function.
Perform the standard diagnosis periodicaslly to maintain optimal performance and prevent failures.
14.1.1 Screen description
Select STANDARD DIAGNOSIS from the [DIAG] key main screen to display the Standard
Diagnosis screen shown in Fig. 14.1.1.
14.1.2 PF menu
Fig. 14.1.1 Diagnosis main screen
PF menu Description
Reference
section
Start Diag Starts standard diagnosis program. 14.1.5
Details
Displays result of the most recent diagnosis.
However, if standard diagnosis has not been executed since the power has
been turned on, default values are displayed.
[Print] (PF menu) prints out the displayed diagnosis results.
14.1.9
Diag Param
Determines setup values used for diagnostic reference and selects
diagnosis items.
14.1.3
14 Diagnosis
14.1 Standard Diagnosis
174
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14.1.3 Diagnosis Parameters
Press [Diag Param] (PF menu) from the Standard Diagnosis main screen to display the
Diagnosis Parameters screen shown in Fig. 14.1.2.
Select the items to be checked during the self-test.
Fig. 14.1.2Diagnosis setup screen
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175
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14.1.4 Diagnosis parameter list
For each item, specify whether it is to be checked or tested. Test items are marked Yes.
Items which are ignored are marked No. Each item is marked either Yes or No. For
example, if the septum counter is marked Yes, both the INJ1 and INJ2 will be chacked.
COUNTER FOR SEPTUM
COUNTER FOR INSERT
Verifies whether the preset number of injections has been exceeded.
The ANALYSIS COUNTER limit is displayed.
CRG USE TIME
Verifies whether the valve On time exceeds the preset operating time.
The COOLANT CONSUMPTION limit is displayed.
TEMP SENSOR USE TIME
The operating time for the temperature sensor in use at 300 C or above is displayed. Refer
to the guidelines for operating time.
TEMP SENSOR DIAG
Verifies whether spiking noise has been generated, to detect deterioration of the platinum
sensor.
LCD USE TIME
Verifies whether the accumulated backlight ON time exceeds the preset operating time.
The limit 15,000 hours.
FAN USE TIME
Verifies whether the accumulated fan operating time exceeds the preset operating time.
The limit is 43,800 hours.
DC VOLTAGE (5 VDC, 24 VDC, -15 VDC, FTD 24 VDC)
Verifies whether each DC voltage has exeeded its limit.
ROOM TEMPERATURE
Verifies whether the current room temperature is within the optimal range.
The range is 5 to 40 C.
ATMOSPHERIC PRESS
Verifies whether the atmospheric pressure is within the optimal range.
PRIMARY PRESS
Verifies whether the gas supply pressure is within the maximum set pressure.
CPU REGISTER
REAL TIME CLOCK REGISTER
Verifies that each register is correctly written and read.
DETECTOR ROM
Verifies that the data saved in the detector ROM is read correctly.
DETECTOR ADC REGISTER
Verifies that the data saved in the detector A/D converter register is read correctly.
DETECTOR HV SOURCE
Verifies whether the detector high voltage power supply is within the threshold.
CAUTION
At the time of Diagnosis, set the Split mode to SPLIT. When WBI
column is used, set the split mode to DIRECT.
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DETECTOR IGNITE
Checks that the ignition pulse is normal.
DETECTOR IGNITION
Verifies whether the ignition operation is normally executed.
ECD FREQUENCY
Verifies whether the frequency of the pulse voltage applied to the ECD is below the limit.
CARRIER GAS ROM, DETECTOR GAS ROM, APC ROM, AMC ROM
Verifies whether the data saved in the ROM on the flow controller PCB can be read correctly.
CARRIER GAS AD CONVERTER, DETECTOR AD CONVERTER,
APC AD CONVERTER, AMC AD CONVERTER
Verifies whether the contents of the A/D converter on the flow controller PCB can be read
correctly.
GAS CONTROL
Checks if carrier gas, detector gas, AUX APC, and AUX AMC are normally controlled.
OVER TEMP PROTECTION
Ensure that the overheat protection circuit is normal.
CPU PERIPHERAL
RESET IC
Verifies that the reset circuit works normally.
WATCH DOG TIMER
Ensures that the IC which checks for software problems is functioning normally.
ROM
Checks that the ROM is intact.
RAM
Verifies whether the RAM can be correctly written and read.
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177
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14.1.5 Starting the diagnosis
Press [Start Diag] (PF menu) from the standard diagnosis main screen shown in Fig. 14.1.1
to start diagnosis and to display the screen shown in Fig. 14.1.3.
14.1.6 PF menu
Fig. 14.1.3 Starting the Diagnosis
PF menu Description
Reference
section
Stop Diag
Stops the diagnosis.
If the program is stopped, items not yet executed are canceled.
14.1.7
Reset
Before stariting the IC diagnosis, the message Reset IC will be checked.
Press PF2 key. appears. Press [Reset] (PF menu) to check whether reset
IC is functioning normally.
Reset IC
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14.1.7 Stopping/exiting the diagnosis
Press [Stop Diag] (PF menu) during diagnosis to display the diagnosis stop screen shown in
Fig. 14.1.4.
When the diagnostics are allowed to complete, the total diagnosis results (Test Result) and
the number of abnormalities (Number of NG) are displayed.
14.1.8 PF menu
Fig. 14.1.4Diagnosis stops
PF menu Description
Reference
section
Details
When the diagnosis is stopped, diagnosis results up to that time are dis-
played.
When the diagnosis ends, the diagnosis results of all items are displayed.
Press [Print] (PF menu) to print out the displayed diagnosis results.
14.1.9
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179
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14.1.9 Diagnosis results
Press [Details] (PF menu) from the screen shown in Fig. 14.1.4 once the standard diagnosis
is have stopped or ended; the Test Result screen shown in Fig. 14.1.5 appears.
Press [Details] (PF menu) from the standard diagnosis screen shown in Fig. 14.1.4 to
display the results of the last test since the power was turned on. Once the power is turned
off, the diagnosis results are cleared.
14.1.10 PF menu
Fig. 14.1.5 Diagnosis results
PF menu Description
Reference
section
Print Prints out the results of the diagnosis to a Chromatopac.
14 Diagnosis
14.1 Standard Diagnosis
180
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Q diagnosis results
Good : Displayed when the diagnosis result satisfies the requirements.
Not Good : Displayed when the diagnosis result does not satisfy the require-
ments.
N/T (= Not Tested) : Displayed when the diagnostic test was stopped or when an item
is excluded from the test.
N/A (= Not Applicable) : Displayed when diagnostic test is disabled for the item (ignition
test for a TCD, for example).
N/S (= Not Selected) : Displayed when the diagnosis were not perfomed on an item
because it has not been configured in an analytical line.
Certain diagnosis items can be performed for components which
have not been configured. For example, for a detector not
configured in any line, Make Up Gas Control is not checked, but
its detector ROM check can be executed.
N/I (= Not Installed) : Displayed when the diagnosis item is not installed.
Q Troubleshooting items which are Not Good
Diagnosis item Countermeasures
SEPTUM COUNTER
Replace the septum. (Refer to 4.4 Septum in the
operation manual.)
INSERT COUNTER
Replace the glass insert. (Refer to 4.6 Glass
Insert in the operation manual.)
ROOM TEMPERATURE Check the operation range.
ATMOSPHERIC PRESS Check the operation range.
GAS PRIMARY PRESS
Increase supply pressure from the gas cylinder.
For example, adjust the regulator.
DETECTOR IGNITION Refer to 5.1 Troubleshooting operation manual.
ANY OTHER ITEM Contact your Shimadzu representative.
181
14 Diagnosis
14.2 14.
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14.2Log Reading Menu
14.2.1 Screen description
Select 2. LOG READING MENU from the [DIAG] key main screen to display the Log Read-
ing Menu screen shown in Fig. 14.2.1.
14.2.2 Parameter list
GC OPERATION LOG
Displays the power On/Off log and the system On/Off log.
ANALYSIS LOG
Displays the analysis log. This log records whether analyses were finished and whether con-
trols deviated from their target valves.
PARAMETER LOG
Displays the key operation log and the parameter change log.
ERROR LOG
Displays the log of displayed error messages.
DIAGNOSTIC LOG
Displays the diagnosis log.
Fig. 14.2.1 Log reading menu main screen
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14.2.3 GC Operation log
Select 1. GC OPERATION LOG to display the system On/Off log and the heater On/Off
log.
(1) Screen description
Select 2. LOG READING MENU from the [DIAG] key main screen, then select 1. GC
OPERATION LOG. The screen shown in Fig. 14.2.2 appears.
Up to 50 logs are stored. If the number of logs exceeds 50, existing logs are deleted
starting with the oldest.
If there are more items than can be displayed on one screen, scroll through the screen using the left
and right arrow keys.
(2) PF menu
Fig. 14.2.2 Operation log screen
PF menu Description
Reference
section
Clear Log
Deletes all displayed logs.
When [Clear Log] (PF menu) is pressed, the screen changes and the
message Clear log with PF2 appears. Press [Clear Log] (PF menu) to
clear the log.
Print Prints the the operation log to a Chromatopac.
NOTE
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14.2.4 Analysis log
When 2. ANALYSIS LOG is selected, the analysis log is displayed. This log records
whether analyses were allowed to finish and whether monitored valves exceeded their set
valves.
(1) Screen description
Select 2. LOG READING MENU from the [DIAG] key main screen, then select 2.
ANALYSIS LOG to display the screen shown in Fig. 14.2.3.
25545 logs are saved. The number of saved logs depends on the size of each log. If
the number of logs exceeds the capacity, existing logs are deleted starting from the
oldest.
During a temperature program, if the rate of temperature increase is too great, the GC may not be
within the Ready range. When this occurs, the analysis log shows Fail.
If there are more items than can be displayed on one screen, scroll through the screen using the left
and right arrow keys.
(2) PF menu
Fig. 14.2.3 Analysis log screen
PF menu Description
Reference
section
Clear Log
Deletes all displayed logs.
When [Clear Log] (PF menu) is pressed, the screen changes and the
message Clear log with PF2 appears. Press [Clear Log] (PF menu) to
clear the log.
Print Prints the analysis log to a Chromatopac.
NOTE
NOTE
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(3) Analysis log details
On the analysis log main screen, use the cursor to select a log item with on the right
and press the [ENTER] key to display the screen shown in Fig. 14.2.4.
The screen provides details about each error when the monitored value deviated from
the set value, and for which an alarm or warning was issued during the analysis.
Fig. 14.2.4 Details screen
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14.2.5 Parameter log
When 3. PARAMETER LOG is selected, parameter names and new values are
displayed when parameters are changed. In addition, the direct operation of valves, etc.
are also displayed.
(1) Screen description
Select 2. LOG READING MENU from the [DIAG] key main screen, then select 3.
PARAMETER LOG. The screen shown in Fig. 14.2.5 appears.
Up to 50 logs are saved. If the number of logs exceeds 50, existing logs are deleted
starting from the oldest.
If there are more items than can be displayed on one screen, scroll through the screen using the left
and right arrow keys.
(2) PF menu
Fig. 14.2.5 Parameter log screen
PF menu Description
Reference
section
Clear Log
Deletes all displayed logs.
When [Clear Log] (PF menu) is pressed, the screen changes and the
message Clear log with PF2 appears. Press [Clear Log] (PF menu) to
clear the log.
Print Prints the parameter log to a Chromatopac.
NOTE
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14.2.6 Error log
When 4. ERROR LOG is selected, the log of all errors which have been displayed is
shown.
(1) Screen description
Select 2. LOG READING MENU from of the [DIAG] key main screen, then select 4.
ERROR to display the screen shown in Fig. 14.2.6.
Up to 100 logs are saved. If the number of logs exceeds 100, existing logs are deleted
starting from the oldest.
If there are more items than can be displayed on one screen, scroll through the screen using the left
and right arrow keys.
(2) PF menut
Fig. 14.2.6 Error log screen
PF menu Description
Reference
section
Clear Log
Deletes all displayed logs.
When [Clear Log] (PF menu) is pressed, the screen changes and the
message Clear log with PF2 appears. Press [Clear Log] (PF menu) to
clear the log.
Print Prints the error log to a Chromatopac.
NOTE
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14.2.7 Diagnostic log
When 5. DIAGNOSTIC LOG is selected, the resulst of the standard diagnosis are
displayed. The results of the last diagnosis are shown in the [Details] (PF menu) screen
described in 14.1 Standard Diagnosis.
(1) Screen description
Select 2. LOG READING MENU from of the [DIAG] key main screen, then select 5.
DIAGNOSTIC LOG. The screen shown in Fig. 14.2.7 appears.
Up to 50 logs are saved. If the number of logs exceeds 50, existing logs are deleted
starting from the oldest.
If there are more items than items than can be displayed on one screen, scroll through the screen
using the left and right arrow keys.
(2) PF menu
Fig. 14.2.7 Diagnosis log screen
PF menu Description
Reference
section
Clear Log
Deletes all displayed logs.
When [Clear Log] (PF menu) is pressed, the screen changes and the
message Clear log with PF2 appears. Press [Clear Log] (PF menu) to
clear the log.
Print Prints the diagnosis log to a Chromatopac.
NOTE
14 Diagnosis
14.3 14.
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14.3Analysis Counter
Use the analysis counter to set the replacement timing of the septum, and the glass insert, when
the counter exeeds the limit, an error message is displayed.
14.3.1 Screen description
Select 3. ANALYSIS COUNTER from the [DIAG] key main screen to display the screen
shown in Fig. 14.3.1.
When the dual INJ (DINJ) is used, the number of analyses is indicated as follows:
Dual mode: The value counted on the L (left) inlet is indicated when the signal polarity of the detector
(DFID, DTCD) is +. The value counted on the R (right) inlet is indicated when the signal polarity is -.
Single mode: The value counted on the selected inlet (L or R) is indicated.
(a) Dual INJ (b) SPL
Fig. 14.3.1 Analysis counter screen
Computer for
Septum
Computer for
Insert
NOTE
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14.3.2 Parameter list
AOC WAIT
Selection: Yes/No, Default: No
When the threshold is exceeded during batch processing, select Yes to temporarily pause,
the AOC operation when the analysis counter has exeed the limit.
USE COUNTER
Selection: Yes/No, Default: Yes
ANALYSIS COUNTER
Selection: 0
SETTING TO WARN
Range: 09999, Default: 100
The septum/glass insert replacement interval depends on the type of analysis. Periodically replace the
septum and the glass insert even if the warning message is not displayed.
14.3.3 PF menu
PF menu Description
Reference
section
Reset Resets analysis number counter of the current item.
Next Displays the setup screen of the analysis counter of another injection port.
NOTE
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14.4Coolant Consumption Counter
The coolant consumption display allows you to confirm the total time that the CRG has been On
(The CRG is an optional accessory.)
If the coolant consumption exceeds the time limit specified (setting to warn), a warning message
is displayed. Replace the gas supply.
14.4.1 Screen description
Select 4. COOLANT CONSUMPTION from the [DIAG] key main screen to display the
Coolant consumption screen shown in Fig. 14.4.1.
Fig. 14.4.1 Coolant consumption sets screen screen
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14.4.2 Parameter list
USE COUNTER
Selection: Yes/No, Default : Yes
CONSUMPTION
Default: 0 min
The total time that the CRG is On is displayed.
Refer to 15.5 Setting the CRG Parameters.
SETTING TO WARN
Range: 09999 min, Default : 100 min
The coolant consumption time depends on the gas cylinder volume and the number of analyses which
requier CRG. Set the warning time according to the analysis conditions.
14.4.3 PF menu
PF menu Description
Reference
section
Reset Resets the Use counter.
NOTE
14 Diagnosis
14.5 14.
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14.5Standard Installation Test
After the system has been installed by your Shimadzu representative, the standard installation
test is performed to check whether the system is functioning properly.
14.5.1 Screen description
Select 5. STANDARD INSTALLATION from the [DIAG] key screen to display the Standard
installation screen shown in Fig. 14.5.1.
The installation test can be performed at any time to check for proper functioning. From this
screen, load the analytical conditions of the standard installation test.
14.5.2 PF menu
Fig. 14.5.1 Standard installation test main screen
PF menu Description
Reference
section
Load
Automatically sets the analytical conditions of the standard installation test.
When [Load] (PF menu) is pressed, TEST is displayed for the used file
name.
Unload Returns analytical conditions to their former status.
14 Diagnosis
14.5 Standard Installation Test
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14.5.3 Test procedure
(1) Specify the analytical conditions file of the standard installation test.
Example: Load File 1 using [File] (PF menu) of the [SET] key.
(2) Configure the injection port and the detector used to execute the standard installation
test in an analytical here.
However, if two or more analytical lines have been configured, the lowest No. analytical
line is set with the test conditions.
In the standard installation test, only one detector can be set per analytical line. If two or
more detectors are set, an error message appears.
(3) Set the dimensions of the column installed.
Example: Set the dimensions of the column using [Column] of the [FLOW] key.
(4) Press [Load] (PF menu) to load the analytical conditions of the standard installation test.
(5) If the analytical condition need to be changed for the installation test, change the
parameters.
(6) Make an injection, then verify whether the data has been acquired correctly.
(7) When analysis finishes, press [Unload] (PF menu) to return the analytical conditions to
their former status.
14 Diagnosis
14.6 14.
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14.6Peak Generator
Select 6. PEAK GENERATOR to generate electronic peaks to confirm of the operation of the
data processing unit.
14.6.1 Screen description
Select 6. PEAK GENERATOR from the [DIAG] key screen to display the Peak generator
screen shown in Fig. 14.6.1.
14.6.2 Parameter list
PEAK GENERATOR
Range: On/Off, Default: Off
MODE
Range: Noise/No Noise/Trunc, Default: Noise
Ch1Ch4 STANDARD SIGNAL
Range: On/Off, Default: Off
14.6.3 PF menu
Fig. 14.6.1 Peak generator setup screen
PF menu Description
Reference
section
Peak Info
Specify the parameters (retention time, full width at half height and peak
height) of the peaks to be generated.
15.1 15.
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15 Optional Devices
15.1Auto Injector Parameters
From the gas chromatograph, specify the parameters of the Shimadzu AOC-20i Auto Injector and the
AOC-20s Auto Sampler Carousel, which automatically inject liquid samples into the gas chromatograph.
For detailed setting procedures, refer to AOC-20 users manual.
15.1.1 Screen description
After installing the auto injector on the GC, access the line configuration screen from the
[SET] key, and then select AOC 1 for the analytical line. (Refer to 8.3 Specifying the
Analytical Flow Line Components ([Line Config])) Then, press the [OPTION] key. If the
screen shown in Fig. 15.1.1 does not appear, press the [OPTION] key again or [NEXT] (PF
menu) to display it.
The screen toggles among AOC parameters AUX temperature AUX APC AUX AMC
CRG screens in this order.
Q AOC STATUS
The AOC status can be monitored.
Fig. 15.1.1 AOC setup screen
Screen display Description
Inactive AOC is not operating.
Taking vial A vial is being picked up from the tray.
Preparation AOC is operating (before injection).
Rinse AOC is operating (after injection).
Putting vial A vial is being returned to the tray.
Wait AOC is waiting for analysis.
The AOC status is displayed.
15 Optional Devices
15.1 Auto Injector Parameters
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15.1.2 Parameter list
SAMPLE WASH
Range: 099, Default: 2
Set the number of times to rinse the syringe with sample before injection.
NUMBER OF INJECTION
Range: 099, Default: 1
Set the number of times the sample should be injected.
SAMPLE SIZE
Range: 0.18.0 l, Default: 1.0 l
Set the sample injection amount.
PRE SOLVENT WASH
Range: 099, Default: 0
Set the number of times to rinse the syringe with solvent before injection.
This item is valid only when the injection mode is set to 0 (normal).
SOLVENT WASH
Range: 099, Default: 1
Set the number of times to rinse the syringe with solvent after injection.
PUMPING
Range: 099, Default: 5
Set the number of times to raise and lower the plunger with the needle inside the sample to
eleminate syringe air bubbles.
VISCOSITY
Range: 0.099.9 sec, Default: 0.2 sec
During rinsing with sample and pumping, the system waits for the specified period of time.
When aspirating sample before injection, the system waits for either the valve set here or 4
seconds, which ever is longer.
The wait time during rinsing with solvent is always 0.2 seconds.
DWELL TIME
Range: 0.099.9 sec, Default: 0.0 sec
Set the length of time for the syringe to remain in the injection port after injection.
INJ. SPEED (PLUNGER)
Selecton: Slow/Middle/Fast, Default: Fast
Specifies the plunger speed during injection.
AOC POWER
Selection: On/Off, Default: On
Turns the AOC power on and off (built-in GC-2014 power supply).
15 Optional Devices
15.1 Auto Injector Parameters
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15.1.3 PF menu
PF menu Description
Reference
section
Start Starts AOC. The GC also starts when AOC injects a sample.
Stop
Temporarily stops the AOC.
If [Start] (PF menu) is pressed in stop status, the AOC resumes the opera-
tion before [Stop] (PF menu) was pressed.
Priority Sets up a Priority analysis. 15.1.4
Other Para Sets AOC options and customization. 15.1.7
Sampler Sets the auto sampler, sub injector and bar code reader. 15.1.10
Reset Resets AOC to the status before control was started.
Upload
Loads parameters from the AOC to the AOC setup screen of the gas
chromatograph.
Print Prints the parameters on the Chromatopac.
Next
Toggles the screen among AOC parameters AUX temperature AUX
APC AUX AMC CRG screens in this order.
15 Optional Devices
15.1 Auto Injector Parameters
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15.1.4 AOC priority analysis
Select [Priority] (PF menu) from the AOC main screen to display the AOC priority sample
screen shown in Fig. 15.1.2.
The batch can only be interrupted when the AOC is operating.
Enter the sample injection No., and press [Set] (PF menu).
15.1.5 Parameter list
INJECTION SAMPLE
INJECTION SAMPLE NUMBER
Enter the sample vial No. designated for priority analysis.
When an auto sampler carousel is not in use,
Short rack No. 16
Long rack No. 112
When an auto sampler corousel is installed, No. 1150 (maximum)
When an auto sampler carousel, the allowable vial No. range depends on the vial rack type
and the number of racks. A valve of 0 (default) indicates no priority sample.
Fig. 15.1.2 Priority analysis setup screen
NOTE
15 Optional Devices
15.1 Auto Injector Parameters
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15.1.6 PF menu
15.1.7 Other AOC parameters
Select [OtherPara] (PF menu) from the AOC main screen to display the other parameters
screen shown in Fig. 15.1.3.
Specify options and AOC custom parameters.
PF menu Description
Reference
section
Set
Analyzes the vial No. specified after the analysis of the current sample is
finished.
Fig. 15.1.3Additional AOC parameter setup
15 Optional Devices
15.1 Auto Injector Parameters
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15.1.8 Other AOC Parameter
INJ. SPEED (SYRINGE)
Selection: Slow/Fast, Default: Fast
Set the syringe injection speed.
USING 3 SOLVENT VIALS
Selection: Yes/No, Default: No
Specifies whether three solvent vials are present and the autosampler carousel is not in use.
This item is only available when USE OF THE SAMPLER in [Sampler] (PF menu) is set to
Not Use.
SOLVENT SELECT
Selection: All/A only/B only/C only, Default: All
This item is available when USING 3 SOLVENT VIALS is set to Yes or USE OF THE
SAMPLER in [Sampler] (PF menu) is set to Use.
All: Three solvent types are used.
A only: Only the solvent in the vial A is used.
B only: Only the solvent in the vial B is used.
C only: Only the solvent in the vial C is used.
For the details, refer to Fig. 3.4.1 in 3.4 Auto Sampler in the AOC-20 Users Manual.
AIR SUCTION
Selection: Yes/No, Default: No
Set whether or not 1 l of air is aspirated into the siringe after aspirating sample.
This type of injection is useful for samples with a wide boiling point range when compound
discrimination problems can occur.
PLUNGER SUCTION SPEED
Selection: Slow/Middle/Fast, Default: Fast
Set the plunger speed during sample injection.
SPEED OF PLUNGER
Selection: Slow/Middle/Fast, Default: Fast
Set the plunger speed during rinsing with sample or pumping.
SYRINGE HEIGHT ( )
Range: 020 mm, Default: 0 mm
Set the syringe height when it moves down to a sample vial (moves syringe up from default).
SYRINGE HEIGHT ( )
Range: 02 mm (1.5 ml vial)/010 mm (4 ml vial), Default: 0 mm
Set the syringe height when it moves down to a sample vial (moves syringe down from
default).
SYRINGE HEIGHT (INJ)
Range: 022 mm, Default: 0 mm
Set the syringe height when it moves down during sample injection (moves syringe up from
default).
CAUTION
When the column initial temperature is high or when a PEG-based,
polar column is used, the column life may be shortened by injecting
air.
15 Optional Devices
15.1 Auto Injector Parameters
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MULTI-INJ
Range: 199, Default: 1
Set the number of times to inject each sample.
KINDS OF VIALS
Selection: 1.5 ml/4 ml, Default: 1.5 ml
Specyfy the vial type.
RACK
Selection: Short/Long, Default: Short
Set the rack type.
KINDS OF THE SYRINGE
Selection: 10 l/50 l/250 l, Default: 10 l
Set the syringe type.
SUCTION VOLUME FOR WASHING
Selection: 80 %/60 %, Default: 80 %
Set the aspiration volume during sample wash and pumping.
RACK POSITION
Range: 02, Default: 1
Set the rack position while sampler is used.
15.1.9 PF menu
PF menu Description
Reference
section
Inj Mode For details, refer to 3.3.3 Injection mode in AOC-20 Users Manual.
15 Optional Devices
15.1 Auto Injector Parameters
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15.1.10 Auto-sampler carousel and other optional parameters
Select [Sampler] (PF menu) from the AOC main screen to display the sampler screen shown
in Fig. 15.1.4.
Specify the options installed on the AOC, such as sampler carousel.
When AOC1 and AOC2 are selected for the analytical line in Line configuration of the
[SET] key, both USE OF THE SAMPLER and USE OF THE SUB AOC are automatically
set to Use.
15.1.11 Parameter list
USE OF THE SAMPLER
Selection: Use/Not Use, Default: Not Use
USE OF THE SUB AOC
Selection: Use/Not Use, Default: Not Use(Set to Not Use because it is not used by GC-2014.)
BAR CODE READER
Selection: Use/Not Use, Default: Not Use
Select Use when the Bar Code reader is installed.
Fig. 15.1.4Sampler carousel and other options setup
203
15 Optional Devices
15.2 15.
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15.2Setting AUX Temperature
Temperature controller used for parts other than the column oven, injection port, and detector
can be set.
15.2.1 Screen description
When an optional device such as heater is installed, press the [OPTION] key to display the
screen shown in Fig. 15.2.1. If a different screen appears, press the [OPTION] key again or
[NEXT] (PF menu) to display the correct screen.
The screen toggles among AOC parameters AUX temperature AUX APC AUX AMC
CRG screens in this order.
15.2.2 Parameter list
TEMPERATURE SETTING VALUE
Range: 0.0400.0 C, Default: 25.0 C
15.2.3 PF menu
Fig. 15.2.1 Main screen to set AUX temperature
PF menu Description
Reference
section
Print Prints each temperature through a Chromatopac. 17.1
NEXT
Toggles the screen among AOC parameters AUX temperature AUX
APC AUX AMC CRG screens in this order.
On/Off Displays a sub screen to set a used unit to On. 15.2.4
15 Optional Devices
15.2 Setting AUX Temperature
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15.2.4 On/Off setting
When On/Off (PF menu) is pressed on the main screen to set AUX temperature, the
screen to set On/Off appears.
15.2.5 On/Off parameter list
TEMPERATURE CONTROL
Selection: On/Off, Default: On
Temperature is controlled when On is selected.
Fig. 15.2.2 Screen to set On/Off of AUX temperature
205
15 Optional Devices
15.3 15.
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15.3Setting the AUX APC Parameters
The pressure, the flow rate and the gas type can be set for the AUX APC.
15.3.1 Screen description
When the optional AUX APC is installed, press the [OPTION] key to display the screen
shown in Fig. 15.3.1. If a different screen appears, press the [OPTION] key again or [NEXT]
(PF menu) to display the correct screen.
The screen toggles among AOC parameters AUX temperature AUX APC AUX AMC
CRG screens in this order.
Fig. 15.3.1 AUX APC main screen
15 Optional Devices
15.3 Setting the AUX APC Parameters
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15.3.2 Parameter list
PRESS
Range: 0.0400.0 kPa, Default: 100 kPa
Set the pressure when the control mode is set to PRESS.
GAS TYPE
Selection: He/N2/H2/Ar, Default: He
Set the type of gas supplied to the APC. If the gas type is set incorrectly, the flow rate can
not be set as specified in FLOW mode. This is because a restrictor is used to calculate the
flow rate.
15.3.3 PF menu
PF menu Description
Reference
section
Offset
Performs offset calibration of APC sensor to improve the reproducibility of
results.
3.6
Next
Toggles among AOC parameters AUX temperature AUX APC AUX AMC
CRG screens
On/Off Set APC to be used to On. Default value is On.
207
15 Optional Devices
15.4 15.
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15.4Setting the AUX AMC Parameters
Flow rate and gas type can be set for the AUX AMC.
15.4.1 Screen description
When the DAFC unit on other configurations is set to "AMC, LR" and/or the optional AUX
AMC is installed, press the [OPTION] key to display the screen shown in Fig. 15.4.1. If a dif-
ferent screen appears, press the [OPTION] key again or [NEXT] (PF menu) to display the
correct screen.
The screen toggles among AOC parameters AUX temperature AUX APC AUX AMC
CRG screens in this order.
Fig. 15.4.1 AUX AMC main screen
15 Optional Devices
15.4 Setting the AUX AMC Parameters
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15.4.2 Parameter list
FLOW RATE
Range: 0.0100.0 ml/min, Default: 50 ml/min
Set the flow rate when the control mode is set to FLOW.
GAS TYPE
Selection: He/N2/H2/Ar, Default: He
Set the type of gas supplied to the AMC. This parameter is used to calculate the flow rate.
15.4.3 PF menu
PF menu Description
Reference
section
Offset
Performs offset calibration of AMC sensor to improve the reproducibility of
results.
Next
Toggles the screen among AOC parameters AUX temperature AUX
APC AUX AMC CRG screens in this order.
3.6
On/Off Set the AMC to be used to On. Default is On.
209
15 Optional Devices
15.5 15.
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15.5Setting the CRG Parameters
The CRG (option) allows temperatures below room temperature to be set. The CRG can be
connected to the column oven or the INJ2.
15.5.1 Screen description
Press the [OPTION] key from the [OPTION] key main screen, or press [NEXT] (PF menu)
until the CRG screen, shown in Fig.15.3.1, appears.
The screen toggles among AOC parameters setting AUX temperature AUX APC
AUX AMC CRG screens in this order.
If the CRG is turned off after a negative temperature valve has been set, the temperature cannot be
achieved, and the GC cannnot become ready. When turning off the CRG, ensure that the temperature
valve is set properly.
Fig. 15.5.1CRG main screen
NOTE
15 Optional Devices
15.5 Setting the CRG Parameters
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15.5.2 Parameter list
COLUMN OVEN
VALVE Selection: On/Off, Default: Off
CRG Selection: Use/Not Use, Default: Not Use
When the CRG is connected to the column oven, the column oven temperature
control range is extended to -99.0 +400.0 C from (room temperature + 4 C)
+400.0 C.
When using the CRG, set VALVE to On and CRG to Use.
When using valve control only, set VALVE to On and set CRG to Not Use.
INJ 2
VALVE Selection: On/Off, Default: Off
CRG Selection: Use/ Not Use, Default: Not Use
When the PTV is installed on INJ2, the injection port temperature control range is
extended to -99.0+400.0 C from 0.0400.0 C
When using the CRG, set VALVE to On and CRG to Use.
When using valve control only, set VALVE to On and set CRG to Not Use.
15.5.3 PF menu
PF menu Description
Reference
section
Next
Toggles the screen among AOC parameters AUX temperature AUX
APC AUX AMC CRG screens in this order.
16.1 16.
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16 Special Functions
16.1Time Scheduler
Use the Time scheduler to establish a weekly or daily schedule of automated GC operations.
16.1.1 description Screen
Select 1. TIME SCHEDULER from the [FUNC] key main screen to display the Time sched-
uler menu shown in Fig. 16.1.1.
16.1.2 Parameter list
MODE
Select whether the same schedule will be executed every day or a different schedule will be
executed on each day of the week.
EDIT
Edit the schedule.
START/STOP
Set the schedule start/stop procedure.
COPY
Copy the contents of a schedule to a specified schedule.
DELETE
Delete the contents of a specified schedule.
Fig. 16.1.1Time scheduler menu
16 Special Functions
16.1 Time Scheduler
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16.1.3 Setting the mode
Select 1. MODE from the time scheduler menu to display the mode setup screen shown in
Fig. 16.1.2.
Select whether to use the same schedule every day or to use a different schedule on each
day of the week. Up to 8 schedules can be set with the time scheduler.
When the time scheduler is operating, the mode cannot be changed.
Q Schedule number and day of the week
The table below shows the relationship between the schedule number and the day of the
week.
Fig. 16.1.2 Mode setup screen
Mode 1
(schedule number)
Mode 2
(day)
No. 0 Sun.
No. 1 Mon.
No. 2 Tue.
No. 3 Wed.
No. 4 Thu.
No. 5 Fri.
No. 6 Sat.
No. 7
NOTE
The schedule number can
be set only when in Number
mode.
16 Special Functions
16.1 Time Scheduler
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16.1.4 Editing a time schedule
Select 2. EDIT from the time scheduler menu to display the schedule number or the day of
the week setup screen shown in Fig. 16.1.3. Before editing a schedule, select the schedule
number or the day of the week, and press [Edit] (PF menu). Then, the schedule edit screen
shown in Fig. 16.1.4 appears.
You do not have to set schedules in the order of execution time. After editing time schedules,
they are automatically sorted. More than one schedule can be set to the same time. These
schedules will be executed at the same time.
16.1.5 PF menu
Fig. 16.1.3Schedule number selection screen Fig. 16.1.4 Schedule edit screen
PF menu Description
Reference
section
New Creates a new time schedule. 16.1.6
Del Line Deletes a schedule line at the current cursor position.
16 Special Functions
16.1 Time Scheduler
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16.1.6 Creating a new time schedule
Select [New] (PF menu) from the time schedule screen to display the Time Schedule screen
shown in Fig. 16.1.5.
Set an item using the [] and [] keys and [ENTER] key. When [Finish] (PF menu) appears
after you have set items, press [Finish] to validate the schedule.
In the upper half of the screen, the contents of the set schedule are displayed. In the lower
half of the screen, the schedule edit screen is displayed.
Up to 100 lines are available per schedule.
The schedule execution time range is from 00:00 to 23:59. The unit is 1 minute.
16.1.7 PF menu
Fig. 16.1.5 Creating a new schedule
PF menu Description
Reference
section
Finish Validates the time schedule.
Prev Page Returns to previous setup screen.
Next Page
Moves to next item.
The cursor can also be moved to next item by pressing [ENTER] key.
Cancel Cancels the time schedule currently being created.
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16.1 Time Scheduler
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16.1.8 Parameters available in the time scheduler
16.1.9 Changing schedule parameters
To change the contents of an existing time schedule, move the cursor using the [ ] and [ ]
keys to select the schedule to be changed, and press the [ENTER] key.
To change the time:
When the Time Schedule select screen appears, enter new numeric values and press
[Finish] (PF menu), if you would like to change only the time.
To change the parameters:
Move the cursor, change the parameter, and then press [Finish] (PF menu) to complete
the change.
To cancel any changes:
If you have changed the schedule but would like to return to the former schedule, press
[Cancel] (PF menu) before pressing [Finish] (PF menu). The schedule returns to its former
status.
Parameter Description
Stop
NUMBER
OF
TIMES
OF RUN
Time
scheduler
stop
Specifies the number of times the program can execute before
the schedule stops or switches to another file. If greater than 2,
The choices are Continuous or Pause at each run. For an
AOC, select Continuous. When Pause at each run is
chosen, the program executes at set intervals continuously at
set intervals.
If another program (such as a temperature program) is running
when time schedule execution time expires, priority is given to
the running program. When the current program finishes, the
time schedule stops or file is changed to another file.
Schedule
0-9 Load
GC Start/Stop Sets start/stop of gas chromatograph.
16 Special Functions
16.1 Time Scheduler
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16.1.10 Time schedule example
Example:7:00 System starts.
19:00 System stops.
First program Screen display
1. Time: 7:00
2. Start/stop
3. Start
Second program
4. Time: 19:00
5. Start/stop
6. Stop
7. Setting is completed.
16 Special Functions
16.1 Time Scheduler
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16.1.11 Starting/stopping a time schedule
Select 3. START/STOP from the time scheduler menu when no time schedule is executing
to display the screen shown in Fig. 16.1.6.
Select 3. START/STOP while a time schedule is executing to display the screen shown in
Fig. 16.1.7.
16.1.12 PF menu
Fig. 16.1.6 Schedule start screen Fig. 16.1.7 Schedule stop screen
PF menu Description
Reference
section
Start
Starts a time schedule.
This item is displayed when no time schedule is running.
If mode is set to number, the same schedule will be executed on
following day and beyond when schedule finishes.
If mode is set to day, the schedule for the current day is executed, and
the schedule for each day will be executed on the following day and
beyond.
Next
Runs the selected schedule on the following day.
If mode is set to day, the schedule for the next day is executed.
Stop
Stops the current schedule.
This item is displayed when a time schedule is running.
16 Special Functions
16.1 Time Scheduler
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16.1.13 Copying and deleting a time schedule
Select 4. COPY or 5. DELETE from the time scheduler menu screen to display the time
schedule copy screen or the time schedule delete screen shown in Fig. 16.1.8 or Fig. 16.1.9.
To copy, specify the copy source schedule and the copy destination schedule, then press
[Copy] (PF menu).
To delete, specify a schedule number to be deleted, then press [Delete] (PF menu).
A currently running schedule cannot be copied or deleted.
Fig. 16.1.8 Schedule copy screen Fig. 16.1.9 Schedule delete screen
NOTE
219
16 Special Functions
16.2 16.
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16.2Batch Schedule
Use the batch schedule to continuously and automatically perform analyses.
A batch is useful for switching methods automatically during the analyses.
16.2.1 Screen description
Select 2. BATCH from the [FUNC] key screen, the Batch screen shown in Fig. 16.2.1
appears.
Q AOC status
The AOC status is displayed on the Batch screen..
Fig. 16.2.1 Batch schedule screen
Screen display Description
Inactive AOC is not operating.
Taking vial Auto sampler arm is picking up a vial.
Preparation AOC is operating (before injection).
Rinse AOC is operating (after injection).
Putting vial Auto sampler arm is returning a vial to the
tray.
Wait AOC is waiting for analysis.
The AOC status is
displayed.
16 Special Functions
16.2 Batch Schedule
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16.2.2 Parameter list
Vial Initial No. and final vial No.
Example: 1-9 (Analysis starts from vial No. 1 and ends at vial No. 9.)
GC GC method file for analyses
DP Channel No. of chromatopac and file No.
Example: 1-5 (Channel 1 and data processing file No. 5 are used.)
This setting is ignored when using GC solution software.
#INJ Number of times to inject
Mk U is displayed when SAMPLE TYPE is set to Unknown.
S is displayed when SAMPLE TYPE is set to Standard.
CMD S is displayed when SLOPE TEST is set to On.
C is displayed when CLEAN UP is set to On.
16.2.3 PF menu
PF menu Description
Reference
section
Start Starts the batch schedule.
Stop Stops the batch schedule.
New Creates a new batch schedule.
16.2.4
16.2.7
Del line Deletes the line at the current cursor position.
Print Prints the schedule to a Chromatopac.
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16.2 Batch Schedule
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16.2.4 Creating a new batch schedule
Select [New] (PF menu) from the batch schedule screen to display the new batch schedule
screen shown in Fig. 16.2.2.
Set an item using the [ ] and [ ] keys and [ENTER] key. When [Finish] (PF menu)
becomes available and the items have been set, press [Finish] to validate the schedule.
At the top of the screen, the contents of the set schedule are displayed. At the bottom of the
screen, the schedule can be edited.
Up to 100 lines are available per schedule.
Fig. 16.2.2 New batch schedule screen
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16.2 Batch Schedule
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16.2.5 Parameter list
START VIAL NO.
Range:
1
Default: 0
FINAL VIAL NO.
Range:
1
Default: 0
1: With no auto sampler
Short rack ... 16
Long rack ... 112
With auto sampler 1150 (maximum)
When the auto sampler is used, the possible depends on the vial rack type and the number
of racks.
The default, 0, indicates that the setting is not given.
SAMPLE
Inject sample
The specified sample vial No. is analysed.
Without sample
Vials are not used for samples. Instead samples are introduced from a gas sampler with a
valve.
GC FILE NO.
Range: FILE 09, Default: FILE0
Set the file No. of the GC method to be used.
CHANNEL NO.
Range: Ch1/Ch2, Default: Ch 1
Set the channel No. connecting the GC to the Chromatopac. This setting is ignored when
using GC solution software.
DATA PROCESSOR FILE NO.
Range: FILE 09, Default: FILE0
Specify a date processor (Chromatopac) date integration file. This setting is ignored when
using GC solution software.
NUMBER OF INJECTION
Range: 099, Default: 0
Set the number of times to inject each sample.
SAMPLE TYPE
Unknown Select this item to analyze a sample of unknown concentration.
Analyze a standard and create a calibration curve before analyzing an unknown
sample.
Standard Select this item to analyze a standard of known concentration.
SLOPE TEST
Range: On/Off, Default: Off
When On is selected, the slope test is performed before running the batch schedule.
CLEAN UP
Range: On/Off, Default: Off
When On is selected, clean up is performed before running the batch schedule.
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16.2.6 PF menu
16.2.7 Editing a batch schedule
To change an existing batch processing schedule, move the cursor using the [ ] and [ ]
keys to the schedule to be edited and press the [ENTER] key. The schedule to be edited
appears on the edit screen.
To change the vial number, enter the new number from the edit screen and press [Finish]
(PFmenu).
To change the other parameters, move the cursor and make the change from the edit
screen, and then press [Finish] (PFmenu).
To cancel the edits and restore the original batch schedule, press [Cancel] (PFmenu) before
pressing [Finish](PFmenu).
PF menu Description
Reference
section
Finish Validates the schedule.
Prev Page Returns to previous setup screen.
Next Page Moves to setup screen for next item.
Cancel Cancels the schedule being created.
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16.2.8 Batch processing Setup example
Example Sample vials No. 1 to 3 are analyzed. The GC method file No. 2 is used. The
Chromatopac data processing file No. 0 is set to Ch 1.
A standard of known concentration is injected once.
Clean up is performed, but the slope test is not performed.
Screen display
1. Start vial No.: 1
Final vial No.: 3
2. GC file No.: FILE2
3. Data processing file No.:
Ch 1, FILE0
4. Number of injections: 1
Sample type: Standard
5. Slope test: Off
Clean up: On
6. The batch is set up.
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16.3 16.
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16.3Time Program
Use a time program to execute zero point adjustment and relay control during analysis.
16.3.1 Screen description
Select 3. TIME PROGRAM from the [FUNC] key screen to display the time program
screen shown in Fig. 16.3.1.
A time program starts as soon as analysis starts.
Time programs do not need to be set up in order. After you finish editing time programs, they
are automatically sorted.
More than one step can be set for the same time. The specified actions are executed at the
same time.
16.3.2 PF menu
Fig. 16.3.1 Time program main screen
PF menu Description
Reference
section
New Creates a new time program. 16.3.3
Del Line Deletes the time program line at the current cursor position.
Chng Line Moves the cursor to the next line.
Print Prints the program to the Chromatopac.
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16.3.3 Creating a new time program
Select [New] (PF menu) from the time program screen to display the time program edit
screen shown in Fig. 16.3.2.
Set an item using the [ ] and [ ] keys and the [ENTER] key. When [Finish] (PF menu)
becomes available and the items have been set, press [Finish] to validate the program.
At the top of the screen, the contents of the set program are displayed. At the bottom of the
screen, the program edit screen is displayed.
Up to 100 lines are available for one program.
The possible program execution time ranges from 0.00 to 9999.00 minutes.
16.3.4 PF menu
Fig. 16.3.2Time program edit screen
PF menu Description
Reference
section
Finish Validates the time program.
Prev Page Returns to previous setup screen.
Next Page Moves to next item.
Cancel Cancels the time program being created.
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16.3.5 Time Program parameters
NOTE 1) Relay description
AC On/Off: Turns the power supplied to the AC connector on the power controller PCB on/off.
Event of On/Off point: Turns the relay contact on the PRG PCB (option) on/off.
Event91 and Event92: Switches a-contact and b-contact of each relay on the CPU PCB
(standard).
Event of PRG: Switches a-contact and b-contact of each relay on the PRG PCB (option).
Blower, Cooling Fan, CRG INJ and CRG Column: Turns the power of each option on/off.
Parameter Description
Relay
NOTE 1)
Detector
Range
Sets range or attenuation for the detector configured in the
analytical line.
Polarity
Changes the polarity between + and - for TCD configured in the
analytical line.
Current Sets current for the detector configured in the analytical line.
NOTE 2)
Zero Adj
Turns on/off zero adjustment for the detector configured in the
analytical line.
Flame Ignites / Extinguishes the flame.
FTD
Turns on/off voltage feedback to make current constant for FTD
configured in the analytical line.
Detector controller
Turns on/off control of detector configured in the analytical line
during analysis program.
Flow
controller
Refer to
NOTE 3).
Splitter Ctrl Opens/closes splitter.
Flow controller On/Off
Turn carrier gas, septum purge, detector gas, APC, and AMC (AUX
AMC and AMC. LR) on/off.
High press inj mode Turns high pressure injection mode on/off.
Gas saver Turns gas saver function on/off.
Temperature
INJ1, INJ2, DET1, DET2,
AUX3, AUX4, AUX5
Use a time program to change temperature of heated zones, which
cannot be programmed.
Stop
NUMBER
OF TIMES
OF RUN
End of
program
Specify the number of times to execute the GC program. Then,
either the program stops or the next file is executed. If greater than
2, the choices are continuous or pause at each run. For an
AOC, select continuous. When pause at each run is selected,
the program executes continuously at set intervals.
If another program (such as a temperature program) is running
when time program execution time expires, priority is given to
running the program. When the current program finishes, the time
program stops or file is changed to another file.
0: FILE
09 Load
Other Set the parameter to input event No..(Refer to 17.4 Event No..)
Relay
Relay
Switch point
Event 91,92 V9192 Point A or B
PRG V9394 Point A or B
On/Off point Event 116 On or Off
AC On/Off
Oven Exhaust Fan On or Off
Cooling Fan On or Off
CRG INJ On or Off
CRG Colum On or Off
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NOTE 2) Current range
NOTE 3) When the dual AFC is used
1. There is no settings for splitter ctrl, high press inj mode, and gas saver.
2. Septum purge cannot be selected on flow controller On/Off.
16.3.6 Editing a time program
To change the contents of an existing time program, move the cursor using the [ ] and [ ]
keys to the program line to be edited changed and press the [ENTER] key.
To change only the time, enter the new time from the edit screen and press [Finish] (PF
menu).
To change the other parameters, move the cursor and make the changes from the edit
screen, and then press [Finish] (PF menu).
To cancel the edits and restore the original time program, press [Cancel] (PF menu) before
pressing [Finish] (PF menu).
Detector type Current
FTD 0.0010.00 (pA)
ECD 0.002.00 (nA)
TCD 0200 (mA)
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16.3.7 Time program setup example
Example 1: When both positive and negative peaks appear on the chromatogram
Four minutes after the program execution starts, the polarity of the detector DET
1 (TCD) is switched from plus to minus. Two minutes later (six minutes after the
program execution starts), the polarity is switched back to plus.
First program Screen display
1. Time: 4.0 min
2. Detector
3. Polarity
4. DET 1
5. - (minus)
Second program
6. Time: 6.0 min
Steps 24 are repeated.
7. + (plus)
8. The time program is set up.
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Example 2: Two AOC analyses use File No.0, then file No.1 is used.
(The execution time is set to 30 min.)
Screen display
1. Time: 30 min
2. Stop
3. Run: 2 times
4. File 1 is loaded.
5. Pause at each run(AOC)
6. The time program is set up.
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16.4 16.
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16.4Pre-Run Program
The Pre-Run program controls flow controllers and relays before the analysis starts.
16.4.1 Screen description
Select 4. PRE-RUN from the [FUNC] key screen to display the Pre-Run screen shown in
Fig. 16.4.1. A Pre-Run program is executed after the [START] key is pressed, but before an
analysis.
While the Pre-Run program is running, the elapsed time is displayed in the Time field on
the [MONIT] key screen.
Program steps do not need to be entered in order. After you finish editing the Pre-Run
program, programs are automatically sorted.
More than one step can be set for the same time. The specified actions are executed at the
same time.
16.4.2 PF menu
Fig. 16.4.1 Pre-Run program main screen
PF menu Description
Reference
section
New Creates a new Pre-Run program. 16.4.3
Del Line Deletes the program at the current cursor position.
Chng Line Changes over the screen of Pre-Run program every line.
Print Prints the program to the Chromatopac.
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16.4.3 Creating a new Pre-Run program
Create a Pre-Run program following the same procedure described in 16.3.3. Creating a
new time program in 16.3 Time Program.
The parameters are equivalent to those shown in 16.3.5. Time Program Parameters
except for STOP. The STOP parameter is described below.
Up to 100 lines are available for the Pre-Run program.
The possible Pre-Run program execution time ranges from 0.00 to 9999.00 minutes.
In the following case, AUTO of the STOP parameter is carried out when the pre-run program is fin-
ished.
There is no STOP parameter in the pre-run program.
Running the Batch Schedule.
16.4.4 Editing a Pre-Run program
To change the contents of the existing Pre-Run program, move the cursor using the [ ] and
[ ] keys to the program line to be edited and press the [ENTER] key.
To change only the time, enter the new time from the edit screen and press [Finish] (PF
menu).
To change the other parameters, move the cursor and make the changes from the edit
screen, and then press [Finish] (PF menu).
To cancel the edits and restore the original time program, press [Cancel] (PF menu) before
pressing [Finish] (PF menu).
16.4.5 After Pre-Run program is finished
When the Pre-Run program is finished, certain events automatically return to their pre-
programs status.
These events are listed below..
For details about the event No., refer to 17.4 Event No..
Parameter Description
End of
program
Auto
The AOC starts after the Pre-Run program is finished.
If there is no AOC, the GC starts.
Manual (Stop program)
After the Pre-Run program is finished, the system becomes
ready.
GC starts
After the Pre-Run program is finished, the GC starts.
For example, select this item to activate a gas sampler, switch the
valve and introduce the gas sample in to the GC as soon as the
program stops.
AOC/HSS starts
After the Pre-Run program is finished, the AOC/HSS starts.
After sample is injected, GC starts.
Clean up
After the Pre-Run program stops, clean up starts.
After clean up finishes, the system becomes ready.
Event No. Description
131134 Turn detector controller on/off.
141146 Turn carrier gas and septum purge on/off.
147158 Turn detector gas on/off.
171 Turns high pressure injection on/off.
181198 Turn AUX APC on/off.
201-210 Turn AUX AMC on/off.
NOTE
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16.4.6 Pre-Run Program set up example
Example: Switches B-contact of Event 91 four minutes in to the program.
Screen display
1. Time : 4.0 min
2. Relay
3. Relay
4. Switch point
5. Event 91, 92
6. Event 91
7. Point B
8. Setting is completed
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16.5Direct Operation
16.5.1 Screen description
Select 5. DIRECT OPERATION from the [FUNC] key screen to display the screen shown
in Fig. 16.5.1.
Input the event No. and press the [Execute] key to execute the specified event.
For a description of the event No., refer to 17.4 Event No..
16.5.2 Parameter list
EVENT
Range: -500+500, Default: ---
Runs the operation assigned to the event No.
Refer to 17.4 Event No..
16.5.3 PF menu
Fig. 16.5.1 Direct operation setup screen
PF menu Description
Reference
section
Execute
Runs the specified operation.
Input event No. to be run, and press [Execute] (PF menu).
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16.6 16.
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16.6GC Configuration
16.6.1 Screen description
Select 6. GC CONFIGURATION from the [FUNC] key screen to display the GC
configuration screen shown in Fig. 16.6.1.
16.6.2 Parameter list
DATE/TIME SETTING
Set the date and the time.
MAX. TEMPERATURE
Set the maximum temperature limit for each headed zone.
TRANSMISSION PARAMETER
Set the parameters related to transmission.
READY CHECK
Indicate the conditions, which should be satisfied in order for the system to be ready and the
STATUS light to illuminate.
SIGNAL SETTING
Set the signals which can be output from the gas chromatograph.
PORT NAME CUSTOMIZATION
Customize the names of various GC items.
LINK DEVICE CODE
Set the link device code the GC is linked to a Chromatopac.
Fig. 16.6.1 GC Configuration setup screen
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TEMPERATURE OFFSET
Set the temperature offset for each heated zone.
OTHER CONFIGURATIONS
Specify the configuration of miscellaneous setup items.
16.6.3 Setting the date and time
16.6.3.1 Screen description
Select 6. GC CONFIGURATION from the [FUNC] key screen, and then select 1.
DATE/TIME SETTING, to display the Date/Time setting screen shown in Fig. 16.6.2.
The date and the time can be set. This setting is automatically saved, even when the
GC power is off.
16.6.3.2 Parameter list
DATE
Range: 2000.01.012099.12.31
TIME
Range: 00:00:0023:59:59
Fig. 16.6.2 Date/time setup screen
The current date and time
are displayed.
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16.6.4 Setting the maximum temperature limits
16.6.4.1 Screen description
Select 6. GC CONFIGURATION from the [FUNC] key screen, and then select 2. MAX
TEMPERATURE to display the Max. Temperature screen shown in Fig. 16.6.3.
Set the maximum temperature limits of 8 heated zones.
16.6.4.2 Parameter list
COLUMN
Range: 0.0420.0 C, Default: 400.0 C
In order to protect the column, do not allow the maximum oven temperature to exceed
the maximum column temperature.
INJ1/DET1/DET2
Range: 10.0420.0 C, Default: 420.0 C
INJ2
Range: 0.0420.0 C, Default: 420.0 C
AUX3/AUX4/AUX5
Range: 10.0420.0 C, Default: 420.0 C
AUX3, AUX4 and AUX5 are available optionally.
If the are installed, the AUX temperature control unit (P/N 221-48458-91) is required.
16.6.4.3 PF menu list
Selection: Yes/No, Default: Yes
When Yes is selected, the Detector temperature setting value must be bigger than or
equal to the Oven temperature setting value.
When No is selected, the Detector temperature setting value may be smaller than the
Oven temperature setting value.
Fig. 16.6.3 Maximum temperature setup screen
PF menu Description
Reference
chapter
Protect Protection against contamination
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16.6.5 Setting transmission parameters
16.6.5.1 Screen description
Select 6. GC CONFIGURATION from the [FUNC] key screen, and then select 3.
TRANSMISSION PARAMETER, to display the Transmission Parameter screen shown
in Fig.16.6.4.
16.6.5.2 Parameter list
PROTOCOL
Selection: None/LEVEL1/LEVEL2/LEVEL3, Default: LEVEL2
BAUD RATE
Selection: 2400/4800/9600/19200/38400/57600/115200 bps, Default: 9600 bps
Set the communication speed.
STOP BIT
Selection: 1 bit/ 2 bit, Default: 1 bit
PARITY
Selection: NONE/EVEN/ODD, Default: NONE
STOP BIT and PARITY can be set when PROTOCOL is set to None or LEVEL1
or LEVEL2.
Set to EVEN in case of connecting a Chromatopac.
Refer to 2.3 Outputting Digital Signals to a Personal Computer and 2.4 Connecting a RS-232C
Cable to the Chromatopac C-R8A.
16.6.5.3 PF menu
Fig. 16.6.4Transmission parameter setup screen
PF menu Description
Reference
section
Apply Down loads the parameters immediately.
NOTE
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16.6.6 Setting the Ready Check Parameters
The Ready Check verifies whether the preset analytical conditions have been met.
When the selected items reach the specified settings, the STATUS light illuminates.
16.6.6.1 Screen description
Select 6. GC CONFIGURATION from the [FUNC] key screen, and then select 4.
READY CHECK, to display the ready check screen shown in Fig.16.6.5.
Set each parameter to yes or no. All parameters with yes must reach their initial
parameter starts in order for the GC to be ready and the STATUS light to turn green.
16.6.6.2 Parameter list
HEATER PORT
TEMP
Selection: Yes/No, Default: Yes
Indicate which headed zones should be included in the ready check.
CARRIER GAS
Selection: Yes/No, Default: Yes
SEPTUM PURGE
Selection: Yes/No, Default: Yes
Indicate which injection port septum purge flow lines should included in the check.
The displayed items depend on the injection port type.
DET FLOW GAS
MAKE UP
Selection: Yes/No, Default: Yes
HYDROGEN
Selection: Yes/No, Default: Yes
Fig. 16.6.5 Ready Check setup screen
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AIR
Selection: Yes/No, Default: Yes
Indicate which detector APC zones should be included in the check.
The displayed items depend on the detector type.
AUX APC
APC1APC15 PRESS
Selection: Yes/No, Default: Yes
This item is available only when optional APC units are installed.
AUX AMC
AMC1AMC10 FLOW
Selection: Yes/No, Default: Yes
This item is available only when optional AMC units are installed.
DETECTOR
CONTROLLER
Selection: Yes/No, Default: Yes
This item is available only when the FID is installed.
DRIFT
Selection: Yes/No, Default: Yes
This item compares the baseline drift to the drift limit for 10 minutes.
Once the GC becomes ready, the GC re-evaluates of the ready status 10 minutes later.
WAIT SIGNAL
Selection: Yes/No, Default: Yes
The wait signal applies to all detectors configured in analytical lines.
User-specified names are used in this screen.
16.6.6.3 PF menu
PF menu Description
Reference
section
Drift Set the baseline drift limit.
NOTE
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16.6.7 Parameter Configuration
Signals are output from four gas chromatograph channels.
To assign detector channels, see 13 Detector.
This section describes the detector signal configuration as well as the configuration of
various other parameters which can be monitored on the screen.
16.6.7.1 Screen description
Select 6. GC CONFIGURATION from the [FUNC] key screen, and then select 5.
SIGNAL SETTING, to display the signal settings screen shown in Fig. 16.6.6.
This screen allows you to adjust the GC signal parameters.
16.6.7.2 PF menu
Fig. 16.6.6 Signal setup screen
PF menu Description
Reference
section
Gain etc. Sets the signal gain and offset for each detector. 16.6.7.6
Data File
Sets the format of digital signals.
When GC is linked to a personal computer, this item is automatically set to
PC. When link is ended, this item automatically reverts to Chromatopac.
Det Sig
Sets signal output channels for all detectors.
The signal out put channels can also be specified for installed detectors
which have not been configured in an analytical line.
If two or more detectors are set to one channel, data can be output to
either channel without switching the output signal cable simply by changing
the analytical line configuration.