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CLARUS 400/480 GC
Software Guide
Clarus 400/480 GC
Software Guide
Release History
Part Number
Release
09936812
Publication Date
February 2010
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Table of Contents
Introduction ................................................................................................... 9
About This Manual ....................................................................................... 11
Manual Conventions and Screen Abbreviations ........................................... 13
Manual Conventions .............................................................................. 13
Screen Abbreviations ............................................................................. 13
Glossary of Clarus GC Terms ....................................................................... 15
Autosampler Terms ............................................................................... 15
Instrument-Specific Terms .................................................................... 16
Glossary of Chromatographic Terms ............................................................ 17
Symbols Located on the Clarus 400/480 GC ................................................ 20
System Description...................................................................................... 21
Introduction ................................................................................................... 23
Overview of the Clarus 400/480 GC............................................................. 24
About the Keyboard ...................................................................................... 26
About the Screen ........................................................................................... 27
Function Key Descriptions ........................................................................... 28
Method Function Key ............................................................................ 29
System Function Key ............................................................................. 29
Auto(sampler) Function Key ................................................................. 30
Background Function Key ..................................................................... 30
Control Key Descriptions ............................................................................. 31
Run Key ................................................................................................. 31
Reset Oven Key ..................................................................................... 31
Status Escape Key.................................................................................. 32
Delete Key ............................................................................................. 32
Entry Keys .................................................................................................... 33
Parameter Keys ............................................................................................. 34
Status, Menus and Screens ......................................................................... 35
Overview ....................................................................................................... 37
Turning on the System .................................................................................. 38
System Status ................................................................................................ 39
Checking the Status of Individual Items ....................................................... 41
Checking the Oven Temperature ........................................................... 41
Checking the Injector Temperature ....................................................... 41
Checking the Detector Temperature ...................................................... 42
Checking the Carrier Gas Pressure or Flow........................................... 42
Action Menus ................................................................................................ 44
Scrolling Through Menu Pages ............................................................. 44
Selecting an Option................................................................................ 44
3
Introduction
11
Introduction
Chapter 2
Chapter 3
Status, Menus, and Screens introduces you to the look and feel
of Clarus GC user interface. It shows you how to turn on the
GC, check the status, and perform fundamental operations such
as changing parameters, selecting options, etc.
Chapter 4
Chapter 5
Chapter 6
Chapter 7
Chapter 8
Chapter 9
Appendix
Index
12
Individual keys are displayed in the text by enclosing the name of the key in square brackets.
For example, [Oven Prog], [Enter], [->Set], [Method], [System], [1], [8], etc.
All temperatures are in degrees Celsius (C).
Screen displays are presented throughout the text as a double-lined box:
Method 1
READY
75
Screen Abbreviations
Autosamp autosampler
AUX Auxiliary zone
Cap capillary split/splitless injector
Cmptr computer
Ctrl syringe control parameters
ECD Electron Capture Detector
Equil equilibration
Extrn external
FID Flame Ionization Detector
Gen generate
GSV gas sampling valve
Inj injector
Inj/Vial injections per vial
Int integrator
kPa kilopascals
NPD Nitrogen Phosphorus Detector
OnCol on column
13
Introduction
Ovn oven
Paus pause
Pkd packed injector
Pre # of preinjection syringe washes
Pres pressure
Prg autosampler program
Pri priority sample vial
Psi or psig pounds per square inch (gauge)
Rec recorder
Resm resume
Stpwtch stopwatch
TCD Thermal Conductivity Detector
14
Autosampler Terms
Instrument-Specific Terms
Autosampler Terms
Term
Description
Washes
Pre
Post
Pumps
Mode
Fast
Normal
Slow
Solv
Visc
15
Introduction
Instrument-Specific Terms
Term
Description
Background
compensation
Ballistically
Detector
background
Equilibration
The delay time after the method set points have been reached
before the system becomes READY.
Isothermal method
Method
Negative-time
event
Parameter
Pre-run
Range
Ready
Run
Sleep mode
Timed Events
Zone
16
17
Introduction
Linearity Quantitatively all detectors will produce a linear response with respect to solute
concentration over a defined range, for example, the Linear Range.
Liquid phase The material in the column that causes the components to separate because of
partitioning of the components between the mobile phase (carrier gas) and the stationary
phase (liquid phase).
Lowest limit of detection The smallest amount of sample that can be detected by the
detector being used. Usually defined as any signal that is as great as two times the noise
level. Also referred to as Minimal Detectable Quantity (MDQ).
Mobile phase The gas which carries the solute (sample) along and over the column
material. This carrier gas is inert and usually helium, nitrogen, or hydrogen.
Noise Background signal fluctuations arising from a detector response. This response is the
result of the column installed, carrier gas purity, electronic components, etc. The
response of any detector is defined by the signal-to-noise ratio.
Partition Coefficient The differential solubility of a substance in two different phases. In
the case of gasliquid chromatography, the sample components reach an equilibrium
between the gas phase (mobile) and the liquid phase (stationary). Each component has a
different partition coefficient thus causing separation in the column.
Resolution The degree of separation between two peaks.
Retention time The time interval from the point of injection to the appearance of the peak
maximum, of a components signal.
Septum Silicone rubber material placed in the injection port through which the injection is
made. When the needle is withdrawn, the silicone rubber reseals, thus not allowing any
sample or carrier gas to escape.
Stationary phase The liquid or solid adsorbent portion of the column that retains
components passing through the GC column.
Syringes Precision dispensing devices used to deliver sample to the GC. Liquid and gas
syringes are available.
Tailing When a peak is not symmetrical or Gaussian shaped but the back end is broadened,
it is said to be tailing.
Temperature programming A technique commonly used to increase the rate of elution of
the components. After the sample is injected into the oven at a specific temperature, the
temperature program increases the oven temperature to the prescribed temperature at a
defined rate (in C/min).
18
Unretained peak A component that is not retained by the column. The time taken for an
unretained sample to pass through the column is the same time as the time taken for the
carrier gas to pass through.
19
Introduction
PNEUMATIC SYMBOL
LEGEND
CARRIER
FLOW / PRESSURE
FID
TCD
NO CONNECTION
20
DETECTOR MAKE-UP/
REFERENCE FLOW
HYDROGEN
AIR
NPD
SPLIT FLOW
ECD
System Description
22
Introduction
The Clarus 400 and Clarus 480 Gas Chromatograph is a dual-channel, temperatureprogrammable stand-alone gas chromatograph (GC). It is available in many configurations, such
as with or without, an autosampler and a variety of injector/detector combinations to provide you
with total GC flexibility. The Clarus GC is microprocessor controlled, where you enter the
operating parameters from the color-coded keyboard and view the prompting text and monitor
instrument functions on a large two-line vacuum fluorescence display.
23
System Description
The FID, ECD, TCD, or the NPD, may be installed in either the front or the rear detector
position.
Each installed detector has one analog output which may be attached to either an integrator or
recorder. Signals may be routed under instrument control.
Either none, one, or two packed column injectors; none, one, or two capillary column
injectors; or one of each injector type may be installed. Capillary column injectors consist of
the conventional split/splitless injector (CAP).
Up to two gas sampling valves may be installed.
The Clarus 400 and Clarus 480 GC is a manual pneumatics instrument.
The carrier gas and detector gas controls are built into the pneumatics control panel on the
Clarus GC. The carrier gas controls are used to set the flow for packed injectors and the
pressure for CAP injectors. The detector gas controls are used to set the hydrogen and air for
FID and NPD reference for TCD; and make-up gas for the ECD. Figure 2 is an example of a
dual-channel pneumatics control panel with Channel 1 containing a capillary injector and a
FID and Channel 2 containing a packed injector and an ECD.
For each channel, the injector-pneumatic controls are on the left and the detector-pneumatic
controls are on the right.
24
Channel 1
Channel 2
25
System Description
Note:
Function keys
Parameter keys
Entry keys
Control keys
As you run this instrument you will see software functions on the display that are
not supported by the Clarus GC. Please ignore these functions and continue with your
analysis.
An audible short beep sounds every time a key is pressed. A long beep sounds when an error
has been made. The key groups and their locations are illustrated in Figure 3.
Function Keys
Method
System
Auto
BackGround
Run
Parameter Keys
Entry Keys
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Control Keys
26
Ready
245 C
The screen displays status information, error messages, and interactive menus (method,
system, configuration, autosampler, and background).
27
System Description
Method
System
Auto
BackGround
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
28
Run
0 no
Pressing [Method] displays the first page of the two-page Method Menu.
Method 1
Setup Edit
Active
Copy
>
Method 1
Gen Delete
Active
Print
>
The commands in the Method Menu provide utilities for managing and editing methods.
Procedures for using these utilities are given in Controlling the Clarus 400/480 GC chapter.
The following table is a brief description of these utilities.
Command
Description
Setup
Edit
Copy
Gen
Delete
Lock >
System Control
Stpwtch Extrn Prnt
>
The commands in the System Control menu provide a number of system utilities.
Procedures for using these utilities are given in chapter 9, System Utilities. A brief
description of these utilities follows.
29
System Description
Command
Description
Config
Selecting this option puts the system into the Configuration Mode.
The configuration menus allow you to specify configuration details
for a variety of hardware options.
Lock
Stpwtch
Extrn
>
A/S Stopped
Park Clean
Print >
The top line displays the autosamplers status (for example, Stopped). The bottom line
displays menu options.
Autosampler details are too specialized and extensive to be described in this chapter. All
details are provided in Chapter 7, Controlling the Autosampler.
Pressing [Background] displays the Background menu on the bottom line and the
background status on the top line.
Background 1
Off
Calibrate
Detailed procedures for using this function are given in chapter 8, Background
Compensation.
30
Method
System
Auto
BackGround
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
Run
0 no
Run Key
Press the [Run] key to start a GC run after manually injecting a sample, continue to run after
an oven hold, or to initiate calibrating a background. Details for using [RUN] for the latter
purpose are given in chapter 8, Background Compensation.
System Description
Select 1 to stop a run and reset the instrument to the initial method conditions. Additional
details are given in chapter 6, Controlling the Clarus 400/480 GC.
The [Status Escape] key is used to escape from various environments. The top level to
which you can escape is the System Status screen.
Method 1
READY
75
A screen similar to that above appears if you escape from the Method, System, Autosampler,
or Background menus.
If you press [Status Escape] a second time, the screen displays the Run End Time, as shown
below.
Method 1
END
READY
13.0m
Delete Key
Use this key to delete a timed event or oven temperature program step.
32
Entry Keys
Method
System
Auto
BackGround
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
Run
0 no
33
System Description
Parameter Keys
Method
System
Auto
BackGround
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
Run
0 no
34
36
Overview
This chapter introduces the Clarus 400/480 GC software and includes examples of how to:
Check the status of individual items such as the oven temperature, injector
temperature, etc.
A basic knowledge of the procedures in this chapter is required before you can perform the
tasks in the remaining chapters. We therefore recommend that you duplicate the examples
shown as closely as possible.
The examples shown in this chapter were prepared with a Clarus 400 GC containing the
following detectors and injectors:
Note:
As you run this instrument you will see software functions on the display that are
not supported by the Clarus 400/480 GC. Please ignore these functions and continue with
your analysis.
CAUTION
37
On/Off Switch
NOT RDY
40
If an error message appears instead of the above screen, refer to the Clarus 400 /480 GC
Hardware Guide, Troubleshooting chapter.
38
System Status
Upon initial startup, the Clarus GC monitors the carrier gas inlet pressure. If this pressure is less
than 50 psi, the following message occurs.
Warning: Car1 Inlet
< 50 psi, Press CE
After you press CE, this message will not occur again, even if you did not correct the
situation.
Also at this time, the oven, injector(s), and detector(s) start heating to the set points specified
in the Active Method. Until all components reach their set points, the system is not ready for
an injection to be made. This is indicated by the message NOT RDY on the upper right
corner of the screen.
The system indicates the components that are not ready by displaying and blinking their
abbreviated names on the bottom line of the System Status screen. The bottom line also
shows the actual oven temperature and continuously updates it.
There is room on the screen for only three abbreviated names. As a component reaches its set
point, its abbreviated name disappears from the screen and is replaced by the next name in the
priority list that is not ready. The priority display order is as follows:
Det (detector temperature) If two detectors are installed, the appearance of "Det"
indicates that either or both detectors are not ready.
Inj (injector temperature) If two injectors are installed, the appearance of "Inj"
indicates that either or both injectors are not ready.
Gas (carrier gas flow/pressure) For the Clarus 400/480 GC, if a capillary injector
and a packed injector with the Optional Flow readout are both installed, the
appearance of "Gas" indicates that the carrier gas pressure/flow for one or both
injectors has not been adjusted to the set point.
39
Ext appears if the device attached to the READY IN terminal (for example, a data
handling system) is not ready. Please refer to the Clarus 400/480 Installation
Instructions for details.
When all components are READY, the system starts equilibrating and the NOT RDY
message changes to EQUILIB.
Method 1
-1.5 min
EQUILIB
75
The clock counts down until the equilibration time has elapsed. The Clarus GC is now
ready for a sample injection shown by displaying READY in the upper right corner of
the screen.
Method 1
40
READY
75
On each menu, the set point is displayed on the bottom line and the actual value (which is
continuously updated) is displayed on the top line.
If the items set point and actual value are not equal (within a specified tolerance), then that
item is NOT READY and its abbreviated name appears on the System Status screen.
The above example shows that the temperature of the oven has not reached the set point
of 75 C.
Press [Inject Prog]. A menu for the injector installed in position 1 (front) appears.
Cap 1 NOT RDY 110
Temperature
150
The above example shows that the temperature of the capillary injector installed in
position 1 has not reached the set point.
41
If a second injector is installed, you can check its temperature status by pressing
[Inject Prog] again.
Pkd 2 NOT RDY 160
Temperature
200
The above example is for a packed injector installed in position 2 (rear).
Press [Detect Control]. A menu for the detector installed in position 1 (front) appears.
FID 1 NOT RDY 120
Temperature
165
The above example shows that the temperature of the FID detector installed in position 1
has not reached the set point.
If a second detector is installed you can check its temperature status by pressing
[Detect Control] again.
ECD 2 NOT RDY 160
Temperature
200
The above example is for an ECD installed in position 2.
A capillary injector is installed in position 1. A screen appears that shows the actual pressure
(top line) and the set point (bottom line). Examples of a NOT RDY and a READY screen
are shown below:
Pres 1 NOT RDY
10.2
Set
25.4 psi
Pres 1
Set
25.4
25.4 psi
1. Press [Carrier Prog] again to display the carrier gas screen for the injector installed in
position 2. The screen below shows that a packed injector with the optional Flow
Readout is installed in position 2.
42
25
30mL
The procedure for setting carrier gas pressure is given in Clarus 400/480 GC Hardware
Guide Chapter 5, Installing a Capillary Column on a Capillary Injector. The procedure
for setting carrier gas flow is presented in Chapters 4 and 5 in the Clarus 400/480 GC
Hardware Guide.
43
Action Menus
An action menu is a display that contains options. When you select an option and press
[Enter], the microprocessor carries out the selected option.
To see an action menu, press [Method]. Page 1 of the Method menu appears.
Method 1
Active
Setup Edit
Copy >
This is the first page of a two-page menu. A menu contains a second page if the
character > appears on the far right of the bottom line.
Note:
When the Clarus GC is under external control (for example, Turbochrom) the method menu
is not available from the GC keyboard.
To see the second page, press [->Set] several times to scroll the
cursor ( ) off the right side of the display and onto the next page.
Method 1 Active
Gen Delete Print >
Selecting an Option
When an action menu is displayed, the cursor ( ) appears on the bottom line to the left of the
default option. For example:
Method 1 Active
Setup Edit Copy >
1. To select a default option, simply press [Enter].
2. To select another option, press [->Set] until the cursor is on the left of the desired
option. To complete the selection, press [Enter].
44
If you select the wrong item, press [CE] before pressing [Enter] to restore the
cursor to its original position.
Press [Status Escape] to escape from a menu. This displays the next higher menu of the
System Status screen.
Method 1
Note:
READY
75
You may have to press [Status Escape] several times to display the status screen.
45
Input Screens
An input screen is one in which data are entered or modified. To see an example of an input
screen, press [Oven Prog]. A screen similar to the following appears:
Oven
TEMP 1
75
75
46
Initial Setup
Procedures
48
Your Clarus GC has been configured at the factory to correctly reflect the installed injectors
and detectors. However, there are operational parameters that you must configure before
using your Clarus GC. This chapter familiarizes you with the steps necessary to configure
your Clarus GC by using a typical configuration example.
Configuration Basics (on the next page), provides you with the background information
needed to perform the following tasks. More specifically, in this chapter you will learn how
to:
49
Configuration Basics
Before configuring the Clarus GC, take time to familiarize yourself with the keyboard by
noting the location of the keys and how the keys are grouped. The following illustration
shows the key group locations on the Clarus 400/480 GC keyboard:
Function Keys
Method
System
Auto
BackGround
Run
Parameter Keys
Entry Keys
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Control Keys
As you run this instrument you will see software functions on the display that are
not supported by the Clarus 400/480 GC. Please ignore these functions and continue with
your analysis.
Before configuring your Clarus GC you can become familiar with all of the configuration
screens (menus) by first entering the Configuration Mode (by pressing [System] [Enter]) and
50
then repeatedly pressing [Enter] to view each screen. When viewing the last configuration
screen, pressing [Enter] returns you to the initial configuration screen. The total number of
configuration screens that appear depend on the particular hardware installed.
Once familiar with the overall configuration of your Clarus GC, you can go directly to most
configuration screens by doing the following.
To display a screen containing the
following information:
[Oven Prog]
[Time]
Sleep Time
[Time] [Time]
Start Time
Coolant Type
[Rate]
Injector Type
[Inject Prog]
[Carrier Prog]
Detector Settings
[Detect Control]
Output to a recorder/integrator
[Output]
Output Offset
[Auto Zero]
Autosampler Mode
[Auto]
51
Lock >
Config
PSIG Flow
Note:
None
kPa
PSIG
Flow
52
Lock >
System Control
Stpwtch Extern >
If you want to display the second page, press [->Set] three times to display the screen on
the right.
Note:
Whenever you see " > " displayed on the screen, it indicates that there are additional menu
selections. Press the [->Set] key repeatedly to display those selections.
2. To enter the Configuration mode, if necessary, press [->Set] to move the cursor to the
left of Confg (as shown above), then press [Enter].
If the autosampler is installed, the
following screen appears:
Automation Configure
None AutoSamp
53
Lock >
A single autosampler program that specifies which injector is to be used, the size
of the injection, and the number of injections per vial. Samples are injected
sequentially starting with the first occupied vial position. The GC is controlled
by the parameters in the Active Method.
Multi
The autosampler runs two programs consecutively. Each program specifies: the
method to be used (each program can use a different method if desired), which
injector to use, the size of the injection, the number of injections per vial, and the
starting and ending vial numbers. As each program is run, the system sets up the
specified method as the Active Method. While running in this mode, the
autosampler attempts at least one injection from each vial in the specified ranges.
Upon powerup, the Clarus GC sets up the method that was running when the power was lost
and runs it one time without injecting a sample. If any automation sequence was
interrupted, it is resumed.
7. Press [Status Escape] to return to the System Control menu or press [Enter] to display
the Oven Maximum Temperature Limit screen.
55
Config
No
3. If you wish to calibrate, press [Yes/ 1] [Enter] "Calibrating the Oven Temperature," in
Chapter 13 otherwise press [No / 0] [Enter].
The Oven Equilibration Time screen appears:
Oven
Config
Equil. Time 2.0 m
The oven equilibration time is the amount of time you wish to equilibrate the oven at the
current temperature after it had cooled down or changed from the initial temperature.
The default value is 2.0 minutes.
4. Type an equilibration time (in minutes), then press [Enter].
5. Press [Status Escape] to return to the System Control menu or press [Enter] to display
the next configuration screen.
56
CAUTION
After the Clarus GC is idle with no keyboard or chromatographic activity for a period of time
longer than the specified sleep time, the sleep method automatically sets up. The Clarus GC
top level status screen displays with a status of SLEEP instead of READY with the sleep
method number displayed as the active method number.
While running the sleep method, the [Run] key is inactive and the GC is NOT READY to any
interconnected devices such as data handling systems. To exit the sleep mode, set up a new
method or start an automated analysis.
To define a sleep time:
1. Copy or generate and then save a method to an unused method number, for example,
Method 3. Then edit that method by entering the parameters for a sleep condition.
2. If necessary, display the Sleep Time screen by pressing [System] [Enter] [Oven Prog]
[Enter] [Enter] [Enter].
The Sleep Time screen appears:
Sleep Time
Set
Config
Off
3. Type a sleep time value between 5 and 999 minutes (typing a 0 turns off the sleep
mode). Then press [Enter].
57
Config
The Sleep Method screen contains the numbers of the saved methods. The above screen
shows that methods 1, 2, 3, and 5 are saved.
4. Select a sleep method from the available stored GC methods in memory. For example, since
you saved the sleep method as Method 3, select Method 3. Then press [Enter].
5. Press [Status Escape] to return to the System Control menu or press [Enter] to display
the Heating Delay screen.
58
59
Config
Yes
Hr:
00:
Dy:
00:
Mo:
00:
Yr:
00
3. Press [->Set] to move the cursor to each of the positions, then enter the correct value for
each parameter. The hours (Hr) range is 1-24. After typing the year (Yr), press [Enter]
to accept the setting.
The Startup Time screen appears:
Startup Time
Set a time?
Config
No
Hr:
00:
Dy:
00:
Mo:
00:
Yr:
00
5. Press [->Set] to move the cursor to each position, then enter the correct value for each
parameter. The hours range is 1-24. After typing the year, press [Enter] to accept the
setting. After typing the year, press [Enter] to accept the setting, then press [Enter].
The following screen appears with the available methods that you have created and stored
(saved):
60
StartUp
1
Meth Config
5
Rept
Config
Always
7. Press [->Set] to select your choice, then press [Enter] to accept the value. Press [Status
Escape] to return to the System Control menu.
61
Configuring an Injector
Your Clarus GC is configured for the installed injectors at the factory; however, if you need
to view or change the injector configuration follow this procedure.
To configure an injector:
1. Press [System] [Enter] [Inject Prog].
The first injector configuration screen appears:
Injector 1
Config
None Pkd Cap GSV >
The position of the cursor tells you the type of injector installed in position 1. The above
screen shows that a capillary injector is installed in position 1.
2. To change the injector configuration, press the [->Set] key the number of times necessary to
select the type of injector you want to configure for position 1.
3. Press [Enter].
4. Press [Enter].
The following screen appears:
HEADSPACE
Installed?
Config
No
If Headspace is installed in your system, press [Yes/ 1] and the following screen appears:
HS40
Car1 Car2
Config
Both
62
1 Config
PSIG Flow
The optional readout was configured before shipment from the factory.
2. Press the [->Set] key two times to move the cursor to the left of PSIG, if it is not already
there and press [Enter].
3. You can press [Enter] proceed to configure valves or press [Status Escape] to return to
the main screen.
Configuring the Carrier Gas for Packed Inlets
1. Press [System] [Enter] [Carrier Prog].
The Gas Display screen appears:
63
Gas Display 1
None kPa
Note:
Config
PSIG Flow
The optional readout was configured before shipment from the factory.
2. Press the [->Set] key three times to move the cursor to the left of Flow, if it is not already
there.
3. Press [Enter] and a screen similar to the following appears:
Carrier
He
Gas 1
N2 H2
Config
Ar/Ch4
4. Move the cursor with the [->Set] key to the left of the carrier gas you are using, then
press [Enter]. If you are using helium, just press [Enter].
The following screen appears:
Carrier Gas 1
Calibrate Flow ?
Config
No
He
Hi=100
The optional Flow Readout is calibrated in the factory using Helium carrier gas. If you are
using a carrier gas other than Helium, you must select the gas as shown in the above
example. You do not have to recalibrate.
If you install a 0-20 mL/min flow element, you must recalibrate. Refer to Calibrating the
Flow Readout, Chapter 9 for this procedure.
6. Press [Enter] to display the Carrier Gas 2 Config screen or press [Status Escape] to
return to the main menu.
64
Configuring Valves
To configure a valve:
Method 1
READY
35
65
Configuring Detectors
Determining the Number, Type, and Position of Installed Detectors
This procedure describes how to configure detectors using a typical example: an FID in
position 1 and an ECD in position 2:
1. If necessary, press [System][Enter][Detect Control].
If a detector is installed in position 1, an appropriate screen appears. For example, if a
FID is installed in position 1, the following screen appears:
Detector 1
FID
Config
Output
2. Press [Enter].
The FID Filter screen appears:
FID 1 Filter
50 200
Config
800
The default setting is 200 milliseconds. If you want to improve the signal-to-noise,
change the setting to 800 milliseconds. The noise improves, but the peak shapes broaden.
A setting of 50 gives a faster detector response, but it may increase the noise level.
3. Press [->Set] to select a filter value, then press [Enter].
The FID Flameout detection screen appears:
FID 1
Flameout
Note:
Config
0.3 mV
You must set a Flameout value in millivolts (mV) for the FID auto-ignition feature to work.
For example, 0.3 mV.
Flameout detection occurs 0.5 minutes into the PRE-RUN time and it measures the userentered baseline threshold level in mV. In this example 0.3 mV are used. If the 0.3 mV
threshold level is exceeded, the flame is considered lit; otherwise, the auto-ignite sequence
begins to automatically ignite the flame.
4. Type a flameout detection level in mV (for example, 0.3 mV) and press [Enter] to accept
the entry. Press [Enter] again to display the next screen.
66
The screen to set the air flow (Air Set) appears. The actual flow is on the top line and the
setpoint flow value is to the right of the cursor on the bottom line.
FID 1
0
Air
Set 0 mL
Type 450 to set the FID 1 air flow to 450 mL/min then press [Enter].
5. Press [Enter].
The screen to set the hydrogen flow (H2 Set) appears. The actual flow is on the top line
and the setpoint flow is on the bottom line.
FID 1
H2
0
Set 0 mL
Config
AUX
67
CAUTION
8. Press [Enter] to display the detector gas flow screen or press [Status Escape] to return to
the main menu.
68
In either case the Output 2 screen appears, but only if a detector has been installed in
position 2 (rear).
Output 2
Recorder
Config
Integrator
2. Configure a recorder or integrator for Output 2 using the same procedure as for Output 1.
3. Press [Enter] to display the Integrator 1 Configuration Offset screen or press [Status
Escape] to return to the main menu.
69
Config
5.0 mV
If you configured Output 1 as a recorder, the Offset parameter screen appears as shown
below:
Rec 1
Offset
Note:
Config
5%
Config
5%
2. Press [Enter] to display the Detector 1 Configuration screen or press [Status Escape]
to return to the System Control menu.
To change an offset value for Output 2 above:
1. Type in the new value, then press [Enter].
Note:
The offset values are not applied to the digital computer signal; they are only applied to the
analog outputs.
2. Press [Enter] to display the initial Automation Configure screen or press [Status
Escape] to return to the main menu.
70
Configuring a Printer
The print options that are displayed on various menus do not appear unless a printer is
configured.
To configure a printer:
1. If necessary, press [System] [System].
Page 2 of the System Control menu appears:
System
Control
Stpwtch Extern >
2. Press [->Set] [Enter].
The following screen appears:
External Device
None Printer Cmptr
3. Select Printer and press [Enter].
Printer Baud
3 12
24
Note:
X1
48
00
96
The values in the above menu and those below are default values for most serial printers.
Check the manual supplied with your printer and make the required changes.
4. Press [Enter].
The following screen appears:
Printer
Data
7
Bits
8
5. Press [Enter].
Printer
Even
Parity
Odd
None
6. Press [Enter].
71
Printer
1
Stop
2
Bits
7. Press [Enter].
8. Press [Status Escape] to return to the System Control menu.
72
Setting Up
Detectors
74
You know how to measure gas flows using a flowmeter with the Clarus GCs
built-in stopwatch. If not, prior to continuing, please read "Using the Built-in
Stopwatch" in Chapter 4, "Before You Install a Column."
WARNING
Note:
The instant the Clarus GC is turned on, the oven, injector(s), and
detector(s) begin to heat up rapidly. To avoid injury, turn off all
heaters and allow their respective zones to become cool to the touch
before you touch detectors, injectors, and their corresponding fittings.
Detailed procedures for turning heaters off and on are in Chapter 3,
"Before you Install a Column" In the Clarus 400/480 GC Hardware
Guide. If you have not read Chapter 3, please do so before
proceeding.
A column has been installed, carrier gas flow or pressure has been set, and all
connections have been leak tested.
As you run this instrument you will see software functions on the display that are
not supported by the Clarus GC. Please ignore these functions and continue with your
analysis.
75
Setting Up Detectors
Setting up a FID
WARNING
The detector gas modules have been set to OFF at the factory.
CAUTION
76
FID Overview
Flame Ionization Detectors (FID) are mass sensitive and used for the destructive analysis
of organic compounds.
As the sample enters the detector, it is mixed with hydrogen and then burned in air,
thereby generating ions. The ions are collected and measured by the detector, with their
concentration proportional to the amount of compound present. Ion collection is
enhanced by a polarized electric field that is created by applying a negative voltage (200
V) to the jet tip. The detector sensitivity is affected primarily by the hydrogen flow.
A cross section view of a FID is shown below.
Amplifier
Connector
Ignitor
Polarizing Pin
Collector
Flame Jet
Air In
Hydrogen In
Flame Jet
Extension
Detector
Fitting
77
Setting Up Detectors
1.
78
Detector Cover
79
Setting Up Detectors
2. Insert the end of the flowmeter tubing into the FID adapter (P/N N610-3119,
supplied in the shipping kit). Then insert the adapter into the FID collector.
See the following figure.
FID Collector
2.
To adjust the combustion gases, the manual pneumatics consist of an on/off needle valve
for air and on/off regulator for hydrogen mounted on the pneumatics control panel.
CAUTION
80
AIR
81
Setting Up Detectors
CAUTION
The outer knob is the on/off knob and it must be turned fully on for
complete flow. In the case of the pressure regulator, if this knob is
only partially opened, the flow will be less than the setting made
when the knob was fully opened.
4. To access the adjustment screw, remove the protective cap from the hydrogen
pressure regulator.
5. Insert the hex wrench (P/N 0990-7235) in the adjustment screw and turn it clockwise a
few turns.
For safety reasons, the hydrogen pressure regulator is set to a very low flow before it
is shipped from the factory.
6. Display the Stopwatch screen by pressing [System] [System] [Enter].
Stopwatch
0.00 min
Flow
Vol 1
All gases exit through the top of the FID. If you use a flowmeter to measure the air and
hydrogen gas flows with a column connected to the FID and the carrier gas flowing,
remember to subtract the carrier gas flow from the total measured flow.
8. Repeatedly adjust the hydrogen flow and measure the flow until you obtain a flow
rate of about 45 mL/min.
Note:
Both the carrier gas and hydrogen gas exit through the FID. For satisfactory operation
of the FID, a flow rate of 45 mL/min of hydrogen is required. If a column is connected to
the FID, and the carrier gas is set and flowing, you should add the carrier gas flow rate
to the required hydrogen flow. For example, if the carrier gas flow is 30 mL/min, adjust
the hydrogen flow until the measured total flow rate (combined carrier gas and
hydrogen) is about 75 mL/min (45 mL/min of hydrogen plus 30 mL/min of carrier gas).
9. Turn off the hydrogen flow by turning the outer ring of the hydrogen control valve
completely clockwise.
82
3.
1. Turn on the air at the source. Adjust the line pressure to 30 psig.
2. Make certain that the flowmeter is still attached to the FID collector.
3. Start the air flowing by turning the outer ring of the air control valve (see Figure 14)
fully counterclockwise.
4. Remove the protective cap from the air control valve.
The stopwatch screen should still be displayed.
5. Measure the flow rate.
For best accuracy, use a soap bubble flowmeter volume that gives a reading of at
least 30 seconds.
6. Repeatedly adjust the air flow by turning the needle valve with a small screwdriver
(P/N 0990-7273) and measure the flow until you achieve a flow rate of about 450
mL/min.
Note:
Both the carrier gas and air exit through the FID. For satisfactory operation of the FID,
a flow rate of 450 mL/ min of air is required. If a column is being used with the FID, and
the carrier gas has been set and is flowing, the carrier gas flow rate should be added to
the required air flow. For example, if the carrier gas flow is 30 mL/min, adjust the air
flow until the measured total flow rate (combined carrier gas and air) is about 480
mL/min.
7. Turn off the air flow by turning the outer ring of the air control valve completely
clockwise.
8. Replace the air control valve protective cap, remove the flowmeter, and replace the
FID cap.
9. Press [Status Escape].
83
Setting Up Detectors
CAUTION
4.
If at any time the line pressure is changed from 30 psig, you must
remeasure and adjust the air flows.
1. Press [Detect Control] until the appropriate FID Temperature screen appears:
FID 1
NOT RDY
Temperature
Note:
35
100
For proper ignition to occur, the FID must be heated to at least 100 C.
2. Enter a setpoint of at least 100 C, or enter a value 50 C higher than the highest
temperature of your oven program.
3. Close the oven door. Wait for the FID 1 temperature to become READY:
FID 1
READY
Temperature
100
100
4. Turn on the hydrogen by turning the outer knob of the hydrogen pressure regulator
valve fully counterclockwise.
CAUTION
The outer knob is the on/off knob and it must be turned fully on for
complete flow. In the case of the pressure regulator, if this knob is
only partially opened, the flow will be less than the setting made
when the knob was fully opened.
5. After purging the FID with hydrogen for a minimum of 60 seconds, press [Detect
Control] once or twice until your FID is displayed. Then press [Enter]. The
following screen appears:
(Note the signal level in mV before the flame ignites.)
84
FID 1 Signal
0.00 mV
Push Set to Ignite
6. Press the [->Set] key.
Method
System
Auto
BackGround
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
Run
0 no
85
Setting Up Detectors
86
0.05mV
on
The signal level shown in this screen is at the range that you set so if you have set a
range of 10, the signal will be 10 times smaller.
You can also confirm that the flame is lit by holding a shiny object (such as a mirror
or small wrench) over the FID outlet. Condensation will appear on the object if
ignition has occurred.
The FID outlet is hot! To prevent injury, never place your hand over
the FID outlet.
WARNING
CAUTION
87
Setting Up Detectors
CAUTION
The flame will not ignite with this vent tubing installed. To ignite
the flame, you must first remove the vent tubing, ignite the flame,
and then replace the vent tubing.
The FID outlet is hot! To prevent injury, never place your hand over
the FID outlet.
WARNING
88
Setting up an ECD
WARNING
CAUTION
The detector gas modules have been set to OFF at the factor.
CAUTION
89
Setting Up Detectors
CAUTION
Labels
Do not remove any of the labels attached to the ECD cell or any of the labels attached to
your Clarus GC that refer to the ECD cell. Follow all instructions and abide by all
precautions provided by the labels and in user instruction manuals referred to by the
labels.
90
Leak Testing
You are obligated under federal and state regulations to make certain that the ECD cell is
wipe tested for leakage of radioactive materials at intervals of no longer than six months,
and that the analysis of these wipe tests is conducted by a person specifically licensed to
do so, either by the U.S. Nuclear Regulatory Commission or by an Agreement State. The
analyses can be performed by the firm listed below:
National Leak Test Center
P.O. Box 486
North Tonawanda, New York 14120
If a leak test detects more than 0.005 mCi of removable radioactive material on the surface
of an ECD cell, or if the cell itself is damaged in such a way as to indicate that it may no
longer adequately shield the radioactive material inside, you must immediately suspend
operation of your chromatograph until the cell has been repaired or disposed of by a person
specifically licensed to do so. Any such incident must be reported by you to the Regional
Office, Inspection and Enforcement, U.S. Nuclear Regulatory Commission.
Please read NRC Regulation 10 C.F.R. Section 20.402 and 20.403 (see the Appendix in
the Clarus 400/480 GC Hardware Guide). These describe your duties should the
radioactive material (Ni 63) in the ECD cell be lost, stolen, or released, or should any
person be exposed to radiation.
Other Requirements
Regulation 10 C.F.R. Section 31.5 (see the Appendix in the Clarus 400/480 GC Hardware
Guide) does not permit you to abandon the ECD cell or export it. It may not be transferred
except to a person specifically licensed to receive it. Within thirty days of such a transfer,
you must report to the Director of Nuclear Material Safety and Safeguards, U.S. Nuclear
Regulatory Commission, Washington, D.C. 20555, the name and address of the transferee.
However, no report is needed to transfer a used or defective ECD cell to PerkinElmer in
order to obtain a replacement. You may transfer the ECD cell to another general licensee,
like yourself, only when it remains at the same location to which it was shipped by
PerkinElmer. Give the transferee a copy of these instructions and the regulations in
Appendix I, and report to the commission as required in Regulation C.F.R. Section 31.5.
91
Setting Up Detectors
The ECD cell may only be removed for repair from the
chromatograph if a specific license has been obtained, THE CELL
SHOULD NEVER BE DISMANTLED.
WARNING
SCOTLAND
WALES
Welsh Office
Cathay's Park
Cardiff, CF1 3NG
NORTHERN
IRELAND
Ministry of Development
Parliament Building
Storemont
Belfast, Northern Ireland
92
ECD Overview
The Electron Capture Detector (ECD) is the most sensitive detector available for the analysis
of electrophilic compounds such as chlorinated hydrocarbons found in pesticide residues. It
is concentration-sensitive and nondestructive.
The ECD cell contains a nickel foil in a cylinder through which the carrier gas flows. The
coating of the foil's inner surface contains the radioactive isotope Nickel-63 and has a
nominal sensitivity of 15 mCi. To optimize detector response, make-up gas is combined
with column effluent.
Beta particles emitted from the isotope ionize the carrier gas. The resultant ions and
electrons travel to the collector anode assembly under the influence of a pulsed polarizing
voltage applied between the source and the collector. The pulse frequency is varied to
maintain a constant average current. The presence of an electron absorbing species in the
detector decreases the current as the absorbed electrons form ions, which travel more slowly
than electrons. The pulse frequency of the polarizing supply is automatically controlled to
maintain a constant current and is used to form the detector output signal.
The ECD works with nitrogen carrier or makeup gas or a carrier or makeup gas mixture
of 95% argon/5% methane. When using capillary columns at low flows (5 mL/min or
less), helium or hydrogen may be used as the carrier gas provided nitrogen or
argon/methane is used as the make-up gas. A cross section view of an ECD is shown
below.
93
Setting Up Detectors
Collector (Anode)
To Amplifier
63
Ni Foil (Source)
Makeup Gas In
Column Connection
If you want to switch between a FID and an ECD, when using the same packed column
injector, use nitrogen as the carrier gas for both detectors. Argon/methane is not
recommended for use with an FID because it produces a high background, more noise,
and a wandering baseline.
94
CAUTION
CAUTION
95
Setting Up Detectors
Setting Up an ECD
To set up a ECD, read the ECD setup summary, then follow the steps.
CAUTION
1.
CAUTION
1. Open the detector cover (see the following figure) to expose the top of the ECD.
96
Insulating Cover
Detector Cap
Screw
Screw
97
Setting Up Detectors
Vent Tubing
ECD Outlet
98
2.
The following procedures describe how to set the make-up gas in the Clarus GC.
CAUTION
The ECD flow module for make-up gas is calibrated with nitrogen
gas at the factory. You must recalibrate the ECD flow module if
you are using a make-up gas other than nitrogen.
CAUTION
ECD Make-Up
Figure 20. The ECD make-up gas control valve for an ECD.
99
Setting Up Detectors
The make-up gas control valve consists of an outer ring (used to turn the make-up gas
completely off or on), a protective cap, and an inner needle valve (used to adjust the flow
of make-up gas). Removing the cap exposes the needle valve adjustment screw. To set
flow, use a small thin screwdriver (P/N 0990-7273, supplied in the shipping kit) to turn
the adjustment screw. Turn the screwdriver counterclockwise to increase the flow or
clockwise to decrease the flow.
You should only adjust make-up gas flow after a column has been installed and the
carrier gas flow or pressure has been set to the value required for the analysis.
Make-up gas need not be added when using packed columns, where the carrier gas flow
is 30 mL/min or higher.
To adjust the make-up gas:
1. Turn the outer ring of the make-up valve fully clockwise.
2. Display the built-in stopwatch by pressing [System] [System] [Enter].
3. Measure the column flow rate and make certain that it is set to the desired value.
For best accuracy, use a soap bubble flowmeter volume that gives a reading of at
least 30 seconds.
4. Turn the outer ring of the make-up valve fully counterclockwise.
5. Remove the protective cap from the make-up valve.
6. Repeatedly adjust the make-up gas (turn the needle valve using the screwdriver (P/N
0990-7273) counterclockwise to increase the flow, clockwise to decrease the flow).
Adjust the total flow until it equals 30 mL/min or higher.
Note:
The lower the total flow, the better the sensitivity, provided that peak shape is
maintained.
7. Replace the cap on the make-up gas valve and disconnect the flowmeter.
100
Setting Up a TCD
The detector gas modules have been set to OFF at the factory.
CAUTION
TCD Overview
The Thermal Conductivity Detector (TCD) is a dual-channel detector which measures the
difference in thermal conductivity between carrier gas flowing through a reference
channel and carrier gas plus sample flowing through an analytical channel (see the
following figure).
Four tungsten-rhenium filaments are connected in a bridge circuit, two in each channel.
The TCD is set up with the same amount of carrier gas flowing through both channels.
The presence of a sample component in the carrier gas flowing through the analytical
channel changes the resistance of the filaments in that channel. This unbalances the
bridge and produces a signal proportional to the amount of sample.
Reference Out
Reference In
Carrier Out
Carrier In
Setting Up Detectors
Setting Up a TCD
Setting up a TCD requires that you equalize carrier gas flows through both channels,
followed by balancing the current through the two filaments. The TCD is nondestructive
and can be used in series with other detectors. The TCD is a universal detector that is
concentration sensitive. The TCD sensitivity depends on the filament current, component
concentrations, and the difference in thermal conductivity between the carrier gas and the
component.
CAUTION
To set up a TCD, read the TCD setup summary, then follow the steps.
1.
102
35
Off
3. Type a TCD temperature appropriate for the analysis to be run, for example, 250 C.
TCD 2 NOT RDY
Temperature
45
250
4. Press [Enter].
Wait for the detector temperature to stabilize; as "NOT RDY" will disappear from the
above screen.
2.
The following procedures describe how to adjust the makeup and reference gas in the
Clarus GC.
CAUTION
The TCD flow module for reference gas is calibrated with helium
gas at the factory. You must recalibrate the TCD flow module if
you are using a reference gas other than helium.
For optimum performance, apply a minimum flow of 5 mL/min to each of the two
detector channels.
103
Setting Up Detectors
Balance
Potentiometer
Reference Outlet
Analytical Outlet
104
Reference
Flow Knob
TCD Ref Flow
3.
1. Select a bridge current range using the criteria in the following table.
CAUTION
105
Setting Up Detectors
Up to 100 C
Up to 300 C
Up to 350 C
Up to 350 C
Recommended Operating
Temperatures for the Following
Detectors
N2
Argon
Do not Use 4
Do not Use 3
Up to 110C
Up to 350 C
Do not Use 4
Do not Use 3
Do not Use 2
Up to 350 C
Range Entry
0
1
2
3
4
Entering a negative number reverses the detector polarity. For examples of reversing the
polarity, see Chapter 8, Practical Hints in the Clarus 400/480 GC Hardware Guide.
1. Press [AutoZero] [AutoZero]. The Autozero screen appears and displays the value of
the background signal.
TCD 2 A/Z
Initial
106
334.5 mV
On
2. Allow the system to stabilize for about 20 min, then open the detector cover.
3. Locate the TCD Balancing Potentiometer (see Figure 8-14). Adjust the
potentiometer until the Autozero display reads between 0.0 and 20.0 mV.
4. Wait for drifting to stop as indicated by a constant reading on the display.
5. Reset the potentiometer to produce a reading between 0.0 and 20.0 mV.
107
Setting Up Detectors
Setting Up a NPD
To avoid injury, Do Not turn on the hydrogen gas unless a column is
connected to the NPD and all fitting connections have been leak
tested.
WARNING
WARNING
Turn off the hydrogen gas before disconnecting a column from the
NPD.
When two NPDs are installed, but only one NPD has a column
connected to it, plug the inlet of the NPD without a column with a
1/8-inch stainless steel plug (P/N N930-0061) to prevent hydrogen
from back-diffusing into the oven.
Since in manual pneumatics, the hydrogen pressure regulator and the
air needle valve have been turned off prior to shipment, first set the
hydrogen and air inlet pressures to 30 psig. Then measure and set the
gas flows as described in this chapter.
The detector gas modules have been set to OFF at the factory.
CAUTION
108
NPD Overview
The nitrogen phosphorus detector (NPD) is a highly specific thermionic detector for
organically bound nitrogen and phosphorus.
CAUTION
The detector operates by electrically heating a glass bead, that contains an alkali metal, to the
point where it emits electrons. A mixture of hydrogen gas and air flows around the bead to
produce a hydrogen plasma. Stable intermediates are formed in the hydrogen plasma which
then capture the electrons emitted from the bead to produce ions. A polarizing field directs
these ions to the collector electrode, thereby creating a current which is amplified. Sensitivity
is affected primarily by the air flow, and selectivity is affected primarily by the hydrogen
flow.
A cross-sectional view of a NPD is shown in the following figure.
CAUTION
109
Setting Up Detectors
To The
Amplifier
Bead Transformer
Assembly
Collector
Bead
Flame
Jet
Air
In
Hydrogen
In
Column
Connector
110
CAUTION
AIR
111
Setting Up Detectors
Removing the cap exposes the adjustment screw, which is used to control the gas flow. To
set the air, use a small thin screwdriver to turn the needle valve adjusting screw
counterclockwise to increase the flow and clockwise to decrease the flow. To set the
hydrogen, use a hex wrench to turn the adjustment screw clockwise to increase the flow and
counterclockwise to decrease the flow. The on/off regulator has an internal restrictor to allow
low flows (3 mL/min or less) with an inlet of 30 psig. Turn the on/off regulator knob
clockwise to increase the flow and counterclockwise to decrease the flow.
1.
Detector Cover
112
This exposes the NPD bulkhead fittings shown in the following figure.
Red Sticker
Bulkhead Fittings
Hydrogen Line
Air Line
The hydrogen line is marked with a red sticker. The air line is unmarked.
2. Disconnect the hydrogen line by loosening the nut that connects the
hydrogen line to the bulkhead fitting with a 7/16-inch wrench.
2.
Note:
For safety reasons, the hydrogen pressure regulator is set in the off position (turned
completely clockwise) before it is shipped from the factory.
1. Turn on the hydrogen gas at the tank and adjust the line pressure to 30 psig.
2. Connect the tubing from a flow meter to the end of the
hydrogen line at the NPD. It is marked with a red sticker.
3. Turn the hydrogen pressure regulator outer knob fully counterclockwise to open it.
113
Setting Up Detectors
CAUTION
The outer knob is the on/off knob and it must be turned fully on for
complete flow. In the case of the pressure regulator, if this knob is
only partially opened, the flow will be less than the setting made
when the knob was fully opened.
4. To expose the adjustment screw, remove the protective cap from the hydrogen pressure
regulator.
5. Insert the hex wrench in the adjustment screw and turn it clockwise to increase the flow.
6. Display the Stopwatch screen on the Clarus GC by pressing [System] [System] [Enter].
Stopwatch
0.00 min
Flow
Vol 1
7. Measure the flow rate. See "Using the Built-in Stopwatch" in Chapter 9, System
Utilities.
For best accuracy, use a soap bubble flowmeter volume that gives a reading of at least 30
seconds.
8. Continue adjusting the hydrogen flow until you obtain a flow rate of between 1.5 and 2
mL/min.
3.
Note:
For safety reasons, the air needle valve is set in the off position (turned completely clockwise)
before it is shipped from the factory.
1
Turn on the air at the source and adjust the line pressure to 30 psig.
2. Connect the flowmeter to the end of the air line that is near the NPD.
3. Start the air flowing by turning the outer ring of the air control valve fully
counterclockwise (see Figure 25).
4. Remove the protective cap from the air control valve.
The stopwatch screen should still be displayed.
5. Measure the flow rate. For details, see "Using the Built-in Stopwatch" in Chapter 9,
System Utilities.
114
For best accuracy, use a soap bubble flowmeter volume that gives a reading of at least 30
seconds.
6. Adjust the air flow by turning the needle valve with the screwdriver.
Continue to measure and adjust the air flow until you obtain a flow rate of about 100 5
mL/min.
1. Disconnect the flowmeter and reconnect the air line to the detector bulkhead.
Make sure the air line is connected to the unmarked bulkhead fitting.
2. Connect the hydrogen line (red sticker) to the detector bulkhead.
Make sure the hydrogen line is connected to the bulkhead fitting marked with a red
sticker.
CAUTION
CAUTION
Any time the line pressure is changed from 30 psig, you must remeasure and adjust the air flows.
115
Setting Up Detectors
CAUTION
The flows listed in the above procedures for hydrogen and air are
optimum for both capillary and packed column flow rates. The
optimum flow provides the best sensitivity (signal to noise),
selectivity, and bead life. Any changes to these flows will affect all
of these parameters.
Also when using capillary columns, makeup gas is not required.
5. Close the oven door. Maintain a carrier gas flow through the column.
6. Install the bead in the conventional manner according to the installation procedure in
the GC Hardware Guide. Make sure that the bead does not contact any other surfaces.
7. Set the following conditions in the following order:
WARNING:
Set the Detector temperature to 150 deg. C. or greater. Wait for the detector
temperature to stabilize.
If a capillary column is used and is not disconnected from the detector, a high detector
temperature can cause bleed at the detector junction with the column. Make certain
the detector temperature is lower than the maximum temperature recommended for
the capillary column of your application.
-
NOTE: Hydrogen flow accuracy is critical to proper NPD bead activation. Make certain that
the H2 flow is within 0.5 mL/min, or closer, to the H2 set point of 2.0 mL/min. Check
with a calibrated flow meter at the detector bulkhead that the flow is accurate if
activation problems occur.
NOTE:
Ensure that the hydrogen line is well purged of entrained air before you make the
final setting of hydrogen flow. Failure to purge the gas line from the hydrogen
supply (tank or generator) will result in an incorrect flow setting for operation and
can lead to poor operating performance and reduce bead life.
When the bead is off, the background value should be 0 0.25 mV. Write down the
background value that occurs with the bead off.
5. Open the detector cover (see Figure 4-26) and locate the bead potentiometer dial see (the
following figure).
117
Setting Up Detectors
If the NPD is detector 1 (front position), the potentiometer is located on the left side
of the panel. If the NPD is detector 2 (rear position) the potentiometer is located on
the right side of the panel.
119
Setting Up Detectors
16. Turn the bead potentiometer dial clockwise until you achieve a reading of 0.25 mV
above the "off" reading with the detector range set to x1.
17. Once the system has stabilized, it is ready for operation.
If you are unable to achieve adequate sensitivity for your standard, increase the
background of the NPD. Increasing intervals of 0.25 mV are recommended.
Adjust the background setting to achieve the sensitivity required for your samples.
For example, if you have a concentrated sample, such as drugs, it can be analyzed
with a background of 0.25 0.50 mV. If you have a low-level sample, such as
pesticides, it may require a setting as high as 1 2 mV. To get the maximum life
from your NPD bead, operate at the lowest setting to achieve your required
sensitivity.
NOTE: (1) The bead will be stable after operating for several hours, but it will drift in time. At the
start of each day, adjust the background reading to the setting you are using and allow a few
minutes for it to stabilize.
(2) Due to the loss of alkali metal with use, the nature of the bead is to drift over time. We
strongly recommend using an internal standard for quantitative analysis.
(3) The bead can operate at higher background settings. The higher the setting, the greater the
signal and noise. Therefore, the signal to noise ratio will not increase dramatically. Operate at
the lowest possible setting to achieve the required sensitivity; this will also prolong the life of
the bead.
120
NOTE: The bead should be turned off by turning the bead potentiometer dial fully counterclockwise
before you turn off the Clarus GC. Remember that the bead has a finite life. You can extend
the bead life by turning the bead off when it is not in use for long periods of time (for
example, over the weekend).
121
Setting Up Detectors
122
Controlling the
Clarus 400/480 GC
124
Overview
The Clarus GC is controlled by a collection of operating parameters called the Active Method.
You can prepare and save up to five methods and make any one of them the Active Method.
However, Method 5 is typically reserved for external computer control of the Clarus GC. If you
are not controlling your Clarus GC from an external computer, you can use Method 5 in the
same way as you would use your other four methods.
Clarus GC operating parameters include such things as an oven temperature program; injector
temperature or detector temperature or a timed events table, and a variety of parameters for
controlling data output.
Active Method parameters are always saved when you turn the Clarus GC off, and
automatically reloaded when you turn it back on.
This chapter contains the following sections:
Method Utilities
125
Function Keys
Method
System
Auto
BackGround
Run
Parameter Keys
Entry Keys
Oven
Temp
Time
Rate
Inject
Temp
Carrier
Gas
Valve
Detect
Temp
Range
Output
on yes
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Control Keys
Only the Active Method can be edited directly from the parameter keys without going through
the Method menu. To view and edit a Stored method, see Editing a Stored Method. To
generate a new method, see Generating a Method.
The parameter keys are linked in sequence from left to right, top to bottom. To display the
first parameter screen, press [Oven Prog]. To display subsequent screens, press [Enter].
After selecting a parameter screen, the remaining parameter screens are arranged in a loop.
After displaying the last parameter screen, pressing [Enter] displays the first parameter
screen. You don't have to view the parameters in sequence. To view a specific parameter
screen, simply press the appropriate parameter key.
126
The following table lists the GC tasks and their corresponding parameter keys:
GC Task
Parameter Key
[Inject Prog]
[Detect Control]
[Carrier Prog]
[Carrier Prog]
Setting up valves
[Valve]
[Range]
[Range]
[Output]
[Atten]
Autozeroing a detector
[AutoZero]
[Events]
127
The following sequence of method parameter screens was obtained by first pressing [Oven
Prog], then repeatedly pressing [Enter] to display subsequent screens.
Oven
TEMP 1
READY
75
75
Oven
READY
TIME 1
0.00m
999.9m
Oven
READY
RATE 1
75
End
Cap 1
READY
Pkd 2
READY
Temperature
Temperature
128
125
125
150
150
Setting up valves
Autozeroing a detector
Up to this point, you have read Chapters 1 through 8, just installed a column, set up the
carrier-gas pressure or flow, and set up your detector. If this is the case, all gases are turned
on at the gas source, and the Clarus GC is on. If you have just set up an FID, you should
have ignited the flame.
Following the last of the above tasks is a section called "Method Utilities." It shows you how
to generate, set up, copy, delete, edit, and print a method.
Depending on what has occurred before you got to this chapter, the oven door may or may
not be closed. To make it easier for you to follow the examples presented in this chapter:
1. Close the oven door.
A status screen appears that is similar to one of the following:
129
Method 1 READY
75
Both the NOT RDY and READY status screens display the current active method
number. In the above example, Method 1 is the Active Method.
2. If you press [Status Escape] a second time, the total analysis time is displayed.
Whether the system is ready or not, you can proceed to the next section.
Note:
When you change an Active Method parameter, the change goes into effect immediately. For
example, if the system is READY and you change an injector temperature setpoint, the status
screen displays NOT RDY until the new setpoint is reached.
Note:
Config
2.0m
If the Equilibration Time is satisfactory, press [Status Escape]. Otherwise, type in a new
time, then press [Enter] [Status Escape].
75
75
80
100
131
For an isothermal run, TIME 1 is equivalent to the total run time. At the end of the time
(TIME 1), the system changes to NOT RDY, it equilibrates, and then goes READY.
To change the hold time:
3. Press [Enter].
Oven
TIME 1
0.00m
999.9m
4. Enter a hold time appropriate for your analysis, for example, 25 min.
Oven
TIME 1
0.00m
25.0m
5. Press [Enter].
Oven
RATE 1
Note:
100
End
Since a constant oven temperature is maintained for isothermal operation, the rate of
temperature increase must be set to 0 . If the Active Method you are editing is already
isothermal, the RATE parameter will have been properly set at 0 and is indicated on the
screen by the word "End." If other than an isothermal program has been previously set up, a
value will appear on the screen. For example:
Oven
RATE 1
132
100
2 /m
Note:
Whenever a RATE is set to 0, any subsequent program steps, if present, are deleted from
the Active Method.
Setting Up a One-Ramp Temperature Program
Setting up a one-ramp program requires entering the following information in the sequence
shown:
Rate of temperature increase from the initial to the final oven temperature (RATE 1)
Temperature increase of 0 C/min which signifies the end of the RATE 2 step.
The following example shows how to convert an isothermal program into a one-ramp
program using the previous isothermal method oven temperature parameter as a starting
point.
Parameter
Value
TEMP 1
50 C
TIME 1
5 min
RATE 1
2 C/min
TEMP 2
70 C
TIME 2
10 min
RATE 2
End (0 C/min)
133
NOT RDY
100
100
NOT RDY
90
50
3. Press [Enter].
Oven
TIME 1
NOT RDY
0.00m
25.0m
NOT RDY
75
End
NOT RDY
60
50
NOT RDY
0.00m
0.00m
NOT RDY
51
End
134
Value
RATE 2
4 C/min
TEMP 3
100 C
TIME 3
5 min
RATE 3
0 C/min
If the RATE 2 screen is not on the display, press [Rate] twice to display it.
Oven
RATE 2
NOT RDY
60
End
NOT RDY
60
70
0.00m
0.00m
50
End
4. If "End" is not shown, press [0] [Enter] or [Delete] [Enter] to end the temperature
program.
Note:
You can enter RATE 3, TEMP 4, and TIME 4 to set up a third ramp.
135
The examples in this section were derived by editing the Active Method with a capillary
injector installed and configured in position 1 (front), and a packed injector installed and
configured in position 2 (rear).
This section contains examples of how to:
136
150
150
2. To display the injector 2 screen, press [Enter], or press [Inject Prog] again.
165
275
The status changes to NOT READY until the injector heats up to the new temperature.
The screen then appears as shown below:
Cap 1
Temperature
275
275
325
325
325
0
137
295
Off
As the injector cools off, the injector temperature is displayed on the top line of the above
screen.
30
Off
25.4
25.0 psi
The screen displays a digital pressure readout of the actual pressure (top line) and the set
pressure (bottom line).
Note:
The Pressure Readout display units are configured by PerkinElmer as psi. If you want to
change the units to kPa, refer to Chapter 9, System Utilities.
2. If your Clarus GC has a second capillary injector, you can view its pressure screen by
pressing [Enter] from the first pressure display or [Carrier Prog] twice if another
parameter is on the screen.
To adjust the carrier gas pressure:
1. Type in a new setpoint value, for example, 20, then press [Enter].
The screen changes to:
138
Pres 1
Set
Note:
NOT RDY
25.4
20.0 psi
When the setpoint is greater than zero, the Clarus GC compares the setpoint and actual
pressure reading. If the actual pressure is not within the READY window, the "NOT RDY"
status appears. When the inlet pressure is within the READY window, NOT RDY disappears
from the screen.
SPLIT FLOW
Pressure
Control
Knob
CARRIER PRESSURE
Fixed
Auto is the default and recommended for split operation, especially at split vent flows of
50 mL/min or less.
3. Press [->Set] to select the Fixed septum purge mode.
4. Enter the offset in mL/min:
139
Septum Purge 1
Flow
3.0 mL/min
Setting Up Valves
The Clarus GC operates six internal solenoid valves. Procedures for setting up Valves 1 or 2
for Split/Splitless operation controlled by manual pneumatics are provided in Chapter 5,
"Installing a Capillary Column" In the Clarus 400/480 GC Hardware Guide.
There are up to six valve screens, one for each configured valve. The specific valve screen is
displayed by pressing [Valve] one to six times. Alternately, you can display the screen for
Valve 1, then repeatedly press [Enter], to view subsequent screens.
An example of a valve screen configured capillary injector (CAP) is shown below:
Split 1
Initial
Note:
OFF
OFF
The examples shown below assume that the Clarus GC is READY, an FID has been installed
and configured in position 1 (front), a TCD has been installed and configured in position 2
(rear).
This section contains examples of how to:
FID 1
Temperature
150
150
2. To display the detector 2 screen, press [Enter] or press [Detect Control] again.
165
275
The status changes to NOT RDY until the detector heats up to the new temperature. The
screen then appears as shown below:
FID 1
Temperature
275
275
325
325
325
3. Press [Enter].
The screen changes to:
141
TCD 2
Temperature
295
Off
As the detector cools off, the detector temperature is displayed on the top line of
the above screen.
Turning Detector Heaters On
1. Display the appropriate detector screen, for example:
TCD 2
Temperature
Off
30
20
20
FID and NPD range options are 1 or 20, where 1 is the most sensitive setting and 20 is 20
times less sensitive.
To change the initial setting to 1:
142
FID 1 Range
Initial
The value that you enter will always be used unless you change it with a timed event.
For certain analyses such as those for trace or concentrated components, you may wish to
change the Range during a GC run. You can do this with a Timed Event. The following
example illustrates this.
Event
Value
Event
Value
3. Press [Range].
The screen changes to:
TIME
2.00
Event
Range 1
Value
1
The range shown is the initial value in the Active Method for detector 1. If detector 2 is
required, press [Range] a second time.
4. Press [20] [Enter].
The screen changes to:
TIME
2.00
Event
Range 1
Value
20
143
When a run is started, the system uses the initial range of 1 for 2 minutes, then
switches to a range of 20 for the duration of the run. When the run is completed, the
system switches back to the initial value of 1.
5. Press [Status Escape] to leave the timed event screen.
Range
TCD range options are 0 (Off), 1, 2, 3, 4 (maximum sensitivity) and 1,2, 3, or -4. A
negative value reverses the polarity.
The TCD range values corresponding to bridge current are shown below:
Table 9-1. Correlation Between Bridge Current and Range
Range Entry
Off
40
80
120
160
0
1
2
3
4
2
2
The initial setting is the range that is used at all times unless the polarity is
changed with a timed event during a GC run.
144
Event
Value
Event
Value
Event
Range 2
Value
2
The Range value shown is the initial value in the Active Method.
4. Press [2] [Enter].
The screen changes to:
TIME
3.00
Event
Range 2
Value
2
When a run is started, the system uses the initial range of 2 for 3 minutes, then reverses the
polarity for the duration of the run. When the run is completed, the system switches back
to the initial value, in this case 2.
5. Press [Status Escape] to leave the timed event screen.
145
Rerouting Output
Assume that:
TCD 2
TCD 2
Detector routing remains in effect until changed. The [Output] key is inactive unless two
detector amplifiers are configured as live detectors, and neither is configured as "Output." If
two detectors are installed but only one configured, then the output of the configured detector
is sent to both output channels.
146
Event
Value
Event
Value
3. Press [Output].
The screen changes to:
TIME
5.00
Event
Output1
Value
TCD 2
The above shows that the TCD output is going to channel 1 (the integrator). Enter the
number of the detector whose output you want sent to the integrator.
4. Press [1].
The screen changes to:
TIME
Event
5.00 Output1
Value
FID 1
When the run starts, the TCD output goes to the integrator. After 5 minutes, the FID
output goes to the integrator. When the run is complete, the TCD output goes to the
integrator.
5. Press [Status Escape].
147
2048
2048
148
149
Attenuation of detector signals may be changed during a GC run with a timed event. At the
end of the GC run, the initial attenuation value is automatically restored.
150
Autozeroing a Detector
Each configured detector is equipped with digital autozeroing capability. As long as
Autozero is On, the system will autozero the detector to the offset specified during
configuration (see Chapter 3, Initial Setup Procedures) whenever the system becomes
READY or when a run is started. You can turn Autozero On or Off from the Autozero
screen.
To view the Autozero screen:
?
Press [AutoZero].
1.09 mV
On
The actual value of the detector signal is displayed on the top line.
To manually autozero the detector:
?
Press [->Set].
Autozeroing can be set or turned off during a GC run with a timed event.
Note:
The events that may be included and the parameter keys that must be pressed to insert the
name of that event and its current value into the table are listed below:
Event
Value
2. Enter the time into the run that you want the event to occur, for example, 1.00 min, then
press [Enter].
The cursor moves to the Event field:
152
Time
1.00
Note:
Event
Value
Permissible time entries are from 99.00 to 999.00 minutes. Events may be entered that are
0.01 minutes apart.
3. Press an appropriate parameter key, for example, [Range]:
Time
1.00
Event
Range 1
Value
20
153
Event
Value
Event
Value
3. Press an appropriate parameter key. For example, capillary injector (CAP), press
[Valve].
The screen changes to:
Time
2.00
Event
Split1
Value
ON
Event
Value
Event
Value
154
Time
3.00
Event
Atten 1
Value
2048
75
75
Time
Event
1.00
2.00
3.00
Value
Range 1
Split1
Atten 1
20
On
2048
Event
Value
2. Press [Enter].
If timed events values exist, the first line of the table is displayed:
Time
1.00
Event
Range 1
Value
20
155
Event
Value
2. Type the time of the event you want to display, for example, 3. The line for that time
appears:
Time
3.00
Event
Atten 1
Value
2048
156
CAUTION
Use this feature only when you perform manual injection. If you use
the oven "Hold" feature with the autosampler, it will prevent the
Clarus GC from coming ready and therefore prevent it from
injecting!
Using a timed event to hold the oven temperature program will keep the GC in a "holding
pattern" until you press [Run].
Typically use this feature in conjunction with the splitter valve by setting the split valve
initially to OFF. This keeps the splitter valve closed (saving carrier gas) until the [Run] key
is pressed.
1.
Press [Valve].
The following screen displays:
Valve 1
Off
Initial
2. Press [Events].
A blank timed events screen appears:
Time
Event
Value
Event
Hold
Value
Event
Valve 1
Value
157
Event
1.00
Hold
0.99
Valve 1
Value
On
At one minute before the GC becomes "ready" (1.00), it will "Hold" at the current
settings until you press the [Run] key. Then at 0.99 min before "ready," the split vent
valve opens.
Note:
You must press the [RUN] key again, at the moment the injection is made, in order to start the
run.
158
Method Utilities
The software provides utilities for performing the following tasks:
Copying a method
Deleting a method
Printing a method
Procedures for performing the above tasks are given in the subsections that follow.
To perform the above tasks you must first display the Method menu by pressing
[Method]. Page 1 of the Method menu appears:
Method 1
Setup Edit
Active
Copy >
Method 1
Gen Delete
Active
Print >
Generating a Method
The Gen option on page 2 of the Method menu allows you to generate a new method, using
default parameters as a starting point. To perform this task:
1. Display page 2 of the Method menu.
Method 1
Gen Delete
Active
Print >
159
Except for the top line, all parameter screens have the same appearance as those in the
Active Method. Procedures for viewing and editing parameters are identical to those
discussed above for the Active Method.
3. When you have completed entering the parameters, press [Status Escape].
The following menu appears:
Method
Save
Generated
Setup Discard
Note:
Gen
Method as #
4
5
Generated
Setup Discard
160
Method
Save
Generated
Setup Discard
Setup
Generated
Discard
2. Press [Enter].
Active
Copy >
2. Select Setup. A menu displaying the numbers of all Stored Methods as well as the
Active Method appears:
Setup Method #
1
2
The cursor is positioned to the left of the method number that is active.
3. Select the number of the method to be set up, then press [Enter]. For example, if you
select 2 and then press [Enter], the System Status screen appears displaying the method
number that has been made active. For example,
161
75
Copying a Method
1. Display page 1 of the Method menu.
Method 1
Setup Edit
Active
Copy >
Active
Print >
2. Select Delete.
A screen displaying the Stored Method numbers is seen. The Active Method and Stored
Methods specified in an autosampler program (see Chapter 7, "Controlling the
Autosampler") cannot be deleted. Their numbers are not displayed:
162
Delete Method #
2
3
4
Active
Copy >
(# 4)
200
Method # 4 Edited
Save
Abandon
5. Select the appropriate option, then press [Enter]. Abandon discards the edit and the
method is not changed.
Printing a Method
Note:
A printer must be attached and configured (see Configure a Printer in Chapter 4).
1. Display page 2 of the Method menu.
2. Select Print, then press [Enter].
The following appears:
Print Method #
1
2
3
4
164
Controlling the
Autosampler
166
Overview
Notes: 1. The autosampler will not respond to commands if the autosampler door is opened.
2. Only sample vials and syringes distributed by PerkinElmer should be used with the Clarus
GC.
3. Syringe plungers are not interchangeable from syringe to syringe.
The autosampler contains three basic parts: a syringe tower, a carousel, and a sample tray (see
following two figures). The syringe tower can contain either a 0.5-, 5.0-, or 50.0-L syringe.
The sample tray contains positions for eighty-two 2-mL sample vials. The turntable contains
one priority sample vial, four 4-mL waste vials, and four 4-mL wash vials.
Syringe Tower
167
168
Clarus GC
Model
Tray Capacity
of 2 mL Sample
Vials
Vial Height
Number of
4 mL Wash
Vials
Number of
2 mL Priority
Vials
480 only
108
Standard
480 only
108
Tall
400 only
82
Standard
400 only
82
Tall
82
Standard
169
The autosampler can be configured to operate in one of two modes, Single- or MultiProgram.
Multi-Program Mode In this mode, the autosampler runs two programs consecutively.
Each program specifies: the method to be used (each program can use a different method
if desired), which injector to use, the size of the injection, the number of injections per
vial, and the starting and ending vial numbers. As each program is run, the system sets
up the specified method as the Active Method. While running in this mode, the
autosampler attempts at least one injection from each vial in the specified ranges.
The remainder of this chapter includes the following procedures and topics:
Note:
The autosampler tray is keyed to fit correctly only in one direction. When installed properly,
the tray is recessed slightly around the entire Clarus GC top. If installed 180 out of position,
the tray will be angled (not lying flat) across the top of the instrument and will not allow the
tower to pass over it.
170
1. Press [Auto].
A/S
STOPPED
Prg Ctrl
START >
2. Select Ctrl, then press [Enter].
The "Fast" injection speed is not available when a 50.0-L syringe is installed.
Do not use the "Fast" mode with the 0.47-mm O.D. needle.
CAUTION
172
CAUTION
For on-column injection, the autosampler must be equipped with the 0.47mm O.D. needle.
173
1.
174
Config
Off
Config
Auto 1 2 3 4 5
2. Select Auto or a specific method number, then press [Enter].
If you select Auto, then upon powerup, the Clarus GC will set up the method that
was running when the power was lost and run it once without injecting a sample. The
automation sequence that was interrupted is resumed.
If you select a specific method (1-5), then upon powerup, the Clarus GC will set up
that method and run it once without injecting a sample. The automation sequence
that was interrupted is resumed.
2.
1. Press [Auto].
Page 1 of the 2-page Autosampler Menu appears:
A/S STOPPED
Prg Ctrl START >
2. Press [Enter].
The following screen appears:
Injector L Inj/Vial
1.0 1
175
3. Enter the injector # to be used (for example, 1 for position 1 or 2 for position 2), then
press [->Set].
The cursor moves to L.
Injector L Inj/Vial
1 1.0 1
If a 0.5- L syringe has been configured, you may enter a volume from 0.0 to 0.5
L in steps of 0.1 L.
If a 5- L syringe has been configured, you may enter a volume from 0.0 to 5.0 L
in steps of 0.5 L.
If a 50- L syringe has been configured, you may enter a volume from 0.0 to 50.0
L in steps of 5.0 L.
176
3.
Set Up a Method
If you want to run the Clarus GC under the control of a method other than the current Active
Method, follow this procedure. Otherwise skip to step 4 (Start the Autosampler).
1. Press [Method] [Enter].
If the Active Method is Method # 1, a screen similar to the following appears:
Setup Method #
1 2 3 4 5
The above example assumes that you have created and saved five methods.
2. Select the desired method #, then press [Enter].
3. Press [Auto] to display the Autosampler Menu.
A/S
STOPPED
Prg Ctrl START >
4.
STOPPED
Select START, then press [Enter]. The autosampler starts and a screen similar to
the following appears:
A/S
V01 Inj01
Prg Ctrl Paus STOP >
The top line displays the autosampler status, namely:
177
1.
178
Auto Program
Auto Resume
Config
Off
Config
Off
2.
1. Press [Auto].
Page 1 of the 2-page Autosampler menu appears:
A/S
Prg
STOPPED
Ctrl START >
2. Press [Enter].
The following screen appears:
Edit Program #
2
3. Press [Enter].
The following screen appears:
Prog Meth Start Stop
1 1 01 82 >
4. Type the # of the method to be used [for example, 0 (Off) through 5], then press [Enter]
[->Set].
Note:
To select a method in this screen, you must have previously saved the method.
179
Note:
If a 0.5- L syringe has been configured, you may enter a volume from 0.0 to
0.5 L in steps of 0.1 L.
If a 5- L syringe has been configured, you may enter a volume from 0.0 to 5.0
L in steps of 0.5 L.
If a 50- L syringe has been configured, you may enter a volume from 0.0 to
50.0 L in steps of 5.0 L.
180
STOPPED
3.
4.
1. Press [Auto].
Page 1 of the 2-page Autosampler menu appears:
A/S
Prg
Ctrl
STOPPED
START >
181
A/S
Prog1 V01 Inj01
Prg Ctrl Paus STOP>
The top line displays the autosampler status, namely:
182
STOPPED
Ctrl Start >
Solv Visc
0
>
5. Select Visc.
6. Enter a value between 1 and 15. This value is the number of seconds the plunger
pauses at the top-of-stroke during sample acquisition.
Note:
You can obtain improved precision with viscous samples by using the 0.5-mL syringe and
septa in the waste/wash vials in place of the diffusion caps.
184
The Clean option is only available when the autosampler has stopped.
2. Select Clean, then press [Enter].
The following appears:
A/S Cleaning Syringe
Prg Ctrl STOP
The system performs the number of solvent washes specified in the Post parameter of the
Syringe Wash screen shown below:
Pre
2
Pump Post
6
2
185
Only syringes distributed by PerkinElmer should be used with the Clarus GC. Plungers are
not interchangeable from syringe to syringe.
Printing
If a printer is connected and configured, you can print the contents of an autosampler
program or programs, or an Automation Log.
1. Select the Print option from page 2 of the Autosampler menu by pressing [Auto] [Auto].
A/S
STOPPED
Park Clean Print >
2. Select Print, then press [Enter].
The following menu appears:
Print Automation
Programs
Log
3. To print the autosampler programs, select Programs and then press [Enter].
4. To print the autosampler log, select Log and then press [Enter] to display the following
menu:
Print Automation Log
No Once Always
186
Select Always to automatically print the Log after all programs have been completed,
or upon stopping the autosampler.
#/Vial:
Inlet:
uL
1.0
Vial #
Injections
1
2
3
0
Status
ok
No vial
187
STOPPED
If the syringe is directly over an injector, you should move it by selecting Park from the above
menu.
188
189
Very viscous samples (to wipe the sample off the outside of the syringe needle).
Single-Program Mode
Waste Vials
When operating in the Single-Program Mode, the sample pre-washes are emptied into waste
vial #1 and #3 (alternating from one injection to the next). The solvent post-washes are
emptied into waste vial #2 and #4 (alternating from one injection to the next).
Wash Vials
When using solvent washes, injection 1 uses solvent from solvent wash vial #1, injection 2
uses solvent from wash vial #2, injection 3 uses solvent from wash vial #3, injection 4 uses
solvent from wash vial #4, injection 5 uses solvent from wash vial #1, etc.
Multi-Program Mode
Waste Vials
When operating in the Multi-Program Mode, the sample pre-washes are emptied into waste vial
#1 for program 1 and waste vial #3 for program 2. The solvent post-washes are emptied into
waste vial #2 for program 1 and #4 for program 2.
Wash Vials
Program 1 splits between solvent wash vials #1 and #2. For example, if four washes are
required, two will be taken from vial #1, and two will be taken from vial #2.
190
Program 2 splits between solvent wash vials #3 and #4. For example, if five washes are
required, three will be taken from vial #3, and two will be taken from vial #4.
1. When using mini-vials, it is not recommended to use pumps to acquire samples. This
assures that the sample will not be diluted by residual solvent in the syringe.
2. Only PerkinElmer vials should be used with the Clarus 400 GC.
3. Adjust the crimper so that it does not deform the vial cap and septum, but crimps the vial
cap tight enough so that you cannot turn the cap. An improperly adjusted crimper cam cause
the autosampler to malfunction.
191
Available Syringes
The following syringes are available for the Clarus 400/480 GC:
Syringe
Part Number
N6101390
N6101252
N6101253
5- L (0.63 mm O.D.)
N6101251
5- L (0.47 mm O.D.)
N6101380
N6101760
192
Background
Compensation
194
Overview
Background compensation is a routine that automatically subtracts a stored baseline profile
from the signal generated during a GC run.
Before background compensation can be applied to a detector output signal, the baseline
profile must be calibrated. The [Background] key controls both calibration and
compensation.
Calibration involves running a blank using your temperature program. Once run, the
background profile is stored. This profile is overwritten if calibration is rerun, thus only the
most recent profile is used for compensation.
One background profile is stored for each detector. Calibration and compensation can be
applied independently to each detector output signal.
Note:
195
Background Compensation
Note:
Off
2. Select Cal, then press [Enter]. The Background Calibration Menu for detector 1
appears.
Calibrate B/G 1
Off Once Multiple
To display the Calibration Menu for detector 2, press [Background] [Background].
196
Multi The system runs the calibration method over and over again until you turn off
calibration in the Calibration Menu. You may wish to use this option, for example, to
condition a column overnight.
Note:
The system stores only the most recent calibrated background profile.
Off Select this option to turn calibration off.
3. Select "Once" or "Multiple," then press [Enter].
A screen similar to the following appears.
Background 1 Off
Off Calibrate
4. Then press [Status Escape].
When equilibration is complete, the System Status screen appears. For example,
B/G Cal
READY
75
5. Press [RUN].
The system runs the oven temperature program once or multiple times and stores the
baseline profile. In Multi, press [Run] to initiate the start of automatic cycling.
197
Background Compensation
198
System Utilities
Overview
The software contains utilities that enable you to:
Note:
As you run this instrument you will see software functions on the display that are
not supported by the Clarus 400/480 GC. Please ignore these functions and continue with
your analysis.
You access these utilities from the System Control menu. To display the System Control
menu, press [System]. The first page of the two page System Control menu appears.
System Control
Confg
Lock >
System Control
Stpwtch Extrn
Prnt >
201
System Utilities
Flow
Vol 1
Flow
Vol 10
202
Stopwatch
0.50 m
Flow 2.0
Vol 10
Flow 4.0
Vol 10
The Stopwatch is a lap counter. As it runs, the time and flow are displayed on the screen. By
pressing [Enter], you can freeze this display without stopping the Stopwatch from counting.
This allows you to read the carrier gas flow for a specific point in time. When you press
[Enter] a second time, the display is updated to the current time and flow and continues to
reflect this information until you stop it again.
203
System Utilities
System Control
Stpwtch Extern >
2. If necessary, press [->Set] to move the cursor to the left of Confg (as shown above), then
press [Enter] to enter the Configuration mode.
If the autosampler is installed, the
following screen appears:
Automation Configure
None Autosamp
204
[Oven Prog]
[Time]
Sleep Time
[Time] [Time]
Start Time
Injector Type
[Inject Prog]
Detector Settings
[Detect Control]
Output to a recorder/integrator
[Output]
Output Offset
[Auto Zero]
Autosampler Mode
[Auto]
205
System Utilities
CAUTION
This example uses a packed column. Before proceeding, determine whether the packed
column is in position 1 or 2 using the procedure previously described.
1. Open the oven door.
2. Turn on the Clarus GC, if it is not already on, and wait for the following screen to appear:
OVEN DOOR OPEN
Press CE to Continue
3. Press [CE].
A screen similar to the following appears:
Method 1
Ovn
206
OVN OFF
55
Notice that as the oven cools down, the actual temperature is continuously updated on the
bottom line.
4. Wait for the oven fan to turn off.
The oven fan automatically turns off when the oven temperature drops to 40 C.
5. Connect a soap bubble flowmeter to the packed injector fitting inside the oven.
To minimize the possibility of melting the tubing, we recommended using Tygon tubing
to make the connection.
Note:
The flow of carrier gas through a packed injector is controlled by the flow control knob on
the pneumatics control panel (see the following figure).
207
System Utilities
7. Turn the flow control knob fully clockwise until it is completely closed.
8. Press [System] [System] [Enter].
The Stopwatch screen appears:
Stopwatch Flow
0.00 min Vol 1
9. Measure the flow rate.
Ideally, it should be zero, but some flow controllers may produce a small flow when
turned off.
10. Press [CE] to reset the stopwatch.
11. Press [System] [Enter] to enter the configuration mode. Using the [Carrier Prog] key,
select the appropriate screen.
Gas Display 2 Config
None kPa psig Flow
12. Press the [->Set] key to move the cursor to Flow, if it is not already there.
13. Press [Enter]
A screen similar to the following appears:
Carrier Gas 2 Config
Calibrate Flow ? No
14. Press [On/Yes 1].
The screen changes to:
Carrier Gas 2 Config
Calibrate Flow ? Yes
15. Press [Enter].
The following screen appears:
Carrier Gas
He
N2
H2
Config
Ar/CH4
16. Select the carrier gas you are using, then press [Enter].
208
Flow 2
HI=100
He
17. Type the flow value measured in step 9, then press [Enter].
18. Turn the flow control knob counterclockwise to start the carrier gas flowing.
19. Measure and adjust the flow to one of the following:
Note:
Flow 2
HI=100
He
The element symbol on the above screen is that for the carrier gas selected in step
16.
21. Select HI, then press [Enter].
Calib.
LO=0
Flow 2
He
HI=100
22. Type the flow just measured, then press [Enter] [Status Escape].
209
System Utilities
System Control
Stpwtch Extrn Prnt>
System
Runlog
210
Selecting Always prints the run log after each run is terminated.
System Control
Stpwtch Extrn Prnt>
System
Runlog
211
System Utilities
System Control
Stpwtch Extrn Prnt>
When the keyboard is locked, the function and parameter keys are read-only. Methods and
configuration may be displayed but not altered. If you forget the code, the instrument must
be turned off and then on again to free the keyboard. If external computer control is
activated, the keyboard is locked by the computer. You need not enter any code to lock the
keyboard. Just pressing [Enter] will lock the keyboard. If you lock the keyboard by pressing
[Enter], pressing [Enter] will unlock it.
212
1.
2.
CAUTION
213
System Utilities
Figure 40 Left panel removed to reveal left side of the oven exterior.
3. Insert the temperature probe through the exposed white insulation covering one of the
holes so that the probe tip is positioned in the center of the oven cavity.
Note which hole you used and measure the length of the probe that protrudes into the
oven. Use the same position for subsequent oven calibrations.
214
3.
100.00
0.00
215
System Utilities
The above screen shows the time-averaged actual oven temperature in the upper right,
and the current temperature offset in the lower right.
8. Allow the oven temperature to equilibrate for at least 30 minutes. The displayed
temperature will approach 100.00 C (or the oven temperature you entered in step 2),
and the thermometer readout will approach a value close to 100.00 C.
4.
5.
100.10
-1.45
216
217
System Utilities
218
219
System Utilities
For example, if detector 1 has been configured as an FID, the following screen appears:
Detector 1 Config
FID
Output
To deconfigure this detector:
1. Select Output, then press [Enter].
The screen appears as shown below:
Detector 1 Config
FID
Output
2. Press [Enter].
As a result of the deconfiguration, detector 1 is removed from the method and its detector
temperature screen will no longer appear in the method.
Note:
If one of the detectors has been deconfigured, analog data from the remaining detector will
be routed to both output channels. Both detectors should not be deconfigured at the same
time.
220
Follow the above steps to enter the configuration mode. Choose [Detect Control], select
FID, then press [Enter] [Status Escape].
Appendix:
Configuration Menus
The menu examples in this appendix were prepared with a Clarus equipped with the
autosampler and the following detectors and injectors:
The Clarus used also has an integrator connected to Output 1 and a recorder connected to
Output 2.
223
>
2. Press [Enter].
The first configuration menu appears:
Automation Configure
None Autosamp
You can display the configuration menus for your system sequentially by pressing
[Enter] each time you wish to move from one menu to the next. Notice that the menus
are on a loop, i.e., after displaying the last menu, pressing [Enter] redisplays the first
menu.
The following section shows examples of configuration menus.
224
A/S Syringe
Config
0.5L 5.0L 50L
Auto Program
Auto Resume
Config
Off
Oven Maximum
Temp Limit
Oven Temp
Calibrate ?
Config
No
Oven
Config
Equil. Time
2.0m
Config
CO2
Injector 1
Config
None Pkd Cap GSV
Coolant
None
LN2
Injector 2
None Pkd
Config
350
Config
Cap GSV
Valve 1
Config
None Valv Split GSV
Valve 2
Config
None Valv Split GSV
Valve 3
Config
None Valv Split GSV
Valve 4
Config
None Valv Split GSV
Detector 1
FID Output
Config
Detector 2
ECD Output
Config
Output 1
Config
Recorder Integrator
Output 2
Config
Recorder Integrator
225
Integrator 1
Offset
Detector 2
ELCD
Extn
Config
0.5mV
Config
Output
Recorder
Offset
Config
5.0 %
ELCD 2
Config
Heat Detector
No
Depending on the menu and the item selected, additional menus may appear. These have
been previously described where appropriate.
* The Aux(iliary) Heater is reserved for use with PerkinElmer supplied accessories.
The menu does not appear if a TCD is configured into the system.
226
[Oven Prog]
[Time]
Coolant Type
[Rate]
[Time] [Enter]
Injector Type
[Inject Prog]
Detector Settings
[Detect Control]
Output to a recorder/integrator
[Output]
Output Offset
[Auto Zero]
Autosampler Mode
[Auto]
Pressing a parameter key multiple times allows you to step through the options for that key.
For example, press [Detect Control] twice to see the options for the second detector, if
installed.
227
228
Index
A
Abbreviations, screen, 13
About
the keyboard, 26
Active Method
editing, 129
parameters
editing, 129
examples, 128
viewing, 126
Adjusting
carrier gas pressure, 138
Attenuating
detector signal, 148, 149
Auto-ignition, FID, 66
Autosampler
configuring, 54
configuring syringe size, 55
controlling, overview, 167
Function key, 30
run
pausing, 187
resuming, 187
stopping, 188
starting, 177, 181
tasks
cleaning the syringe, 185
pausing autosampler run, 187
resuming autosampler run, 187
tower, parking, 188
tray, 167
turntable, 167
using with TCD, 107, 192
vials, waste & wash, 190
Autozeroing a detector, 151
B
Background Calibration Menu, 196
Background calibration options
multi, 197
off, 197
Index
once, 196
Background compensation
calibrating baseline profile, 196
glossary, 16
overview, 195
turning off, 198
turning on, 198
Background menu, 196
Balancing TCD bridge current, 106
Baseline profile, calibrating, 196
Bridge current vs. range, 106
C
Calibrating
baseline profile, 196
optional flow readout, 206
oven temperature, 213, 216
reference thermometer, 213
CAP, abbreviation, 13
Carrier gas
checking status, 42
configuring pressure display for manual
pneumatics, 52
Carrier gas pressure
adjusting, 138
configuring display for manual pneumatics, 52
displaying, 138
viewing, 138
Changing
detector temperature, 141
injector temperature, 137
TCD polarity, 145
Chromatographic terms, glossary, 17
Clarus
controlling, 125
Cleaning the syringe, 185
Clock, setting, 60
Cmptr, abbreviation, 13
Combustion
control valves, FID, 81
needle valves, FID, 81
Configuration
displaying menus, 51
entering, 53
printing, 211
Configuration Menus
displaying, 204
Configuration Mode
entering, 204
230
escaping, 126
Configuring
autosampler, 54
clock, 60
detectors, 219
equilibration time, 131
injectors, 62, 217
integrator, 69
Integrator/Recorder offsets, 70
manual pneumatics carrier gas pressure display,
52
multi program mode, 178
oven, 56
printer, 71
recorder, 69
startup time, 60
valves, 65
Control key
Delete, 32
Run, 31
Control valves
combustion, 81
Conventions, 13
Copying a Method, 162
Ctrl, abbreviation, 13
D
Deconfiguring
detectors, 219
injectors, 217
Delete control key, 32
Deleting
a Stored Method, 162
timed event, 156
Detector
attenuating
signal to a recorder, 148
signal to an integrator, 149
autozeroing, 151
configuring, 66, 219
cover, 78
heater
turning off, 141
turning on, 142
output
rerouting, 146
rerouting using a timed event, 147
routing, 146
temperature
E
ECD
abbreviation, 13
adjusting make-up gas, 100
outlet, 97
overview, 93
setting up, 96
setting up manual pneumatics, 99
setup summary, 96
venting the outlet, 96
Entering parameters
multi program mode, 179
single program mode, 175
Entry keys, 33
Off/No, 33
On/Yes, 33
Equil, abbreviation, 13
Equilibration
screen, 40
Equilibration time
configuring, 131
Extrn, abbreviation, 13
F
FID
abbreviation, 13
adjusting air flow, 83
adjusting hydrogen flow, 81
attaching a flowmeter, 78
auto-ignition, 66
cross sectional view, 77
range changing, 143
range setting, 142
setting up manual pneumatics, 78
Flow controller
See optional flow readout:, 206
G
GC tasks vs. parameter keys, 127
GC temperature program steps, 130
Gen, abbreviation, 13
Generated Method
saving, 160
setting up, 160
Ghost Peaks, 17
Glossary
autosampler terms, 15
chromatographic terms, 17
GSV, abbreviation, 13
H
Hydrogen flow
adjusting, 81
I
Inj, abbreviation, 13
Inj/vial, abbreviation, 13
Injector heater
turning off, 137
turning on, 138
Injector temperature
changing, 137
checking status, 41
displaying, 137
setting, 136
Injectors
configuring, 62, 217
Inlet temperature program
setting up, 130
Int, abbreviation, 13
Integrator
231
Index
configuring, 69
Integrator noise, 149
Isothermal temperature program
setting up, 131
K
Key
Autosampler function, 30
Method function, 29
parameter, 34
System function, 29
Keyboard
about the, 26
locking, 212
unlocking, 212
kPa, abbreviation, 13
L
Leaving
timed events screen, 155
Locking the keyboard, 212
M
Make-up gas
adjusting for an ECD, 100
control valve, 99
needle valve, 99
Menu
about, 44
auto(sampler), 30
background, 196
background calibration, 196
escaping from, 45
Injector, 62
Output, 69
printer, 71
selecting an option, 44
System Control, 29, 53, 201, 204
Menu, overview, 37
Method
copying, 162
printing, 164
setting up, 177
Method function key, 29
Method Menu, 159
Method utilities+, 159
Mode
232
configuration, 204
Multi program mode
configuring, 178
entering parameters, 179
running samples, 178
Multiprogram mode, 170
Multi-ramp temperature program
setting up, 135
N
NPD
adjusting the air flow, 114
adjusting the hydrogen flow, 113
bead activation, 116
reactivating a used bead, 121
setting up manual pneumatics, 111, 112
NPD, abbreviation, 13
O
Off/No entry key, 33
Offset screen, 70
Offsets
configuring Integrator/Recroder offsets, 70
On/Off Switch, 38
On/Yes entry key, 33
OnCol, abbreviation, 13
One-ramp temperature program
setting up, 133
Option, selecting from a menu, 44
Optional flow readout, calibrating, 206
Output Menu, 69
Oven
calibrating the temperature, 216
calibrating the temperature,, 213
checking temperature status, 41
configuring, 56
setting a heating delay time, 59
setting equilibration time, 56
turning on, 102
Oven temperature program
setting up, 130
setting up a multi-ramp, 135
setting up a one-ramp, 133
setting up isothermal, 131
Overview
AutoSystem XL GC, 23
ECD, 93
TCD, 101
P
Parameter keys, 34
method, 126
Parameter screens, 126
Parameters
Active Method
examples, 128
viewing, 126
injection mode, 172
syringe wash, 171
Parking, autosampler tower, 188
Paus, abbreviation, 14
Pkd, abbreviation, 14
POC
configuring, 62
Inlet Programmed Mode, 62
Oven Programmed Mode, 62
Pre
See syringe wash parameters, 171
Pre, abbreviation, 14
Pres, abbreviation, 14
Pressure display, configuring for manual
pneumatics, 52
Prg, abbreviation, 14
Pri, abbreviation, 14
Printer
configuring, 71
menu, 71
Printing
Configuration, 211
run log, 210
Priority sample, inserting, 188
Psi, abbreviation, 14
psig, abbreviation, 14
PSS
configuring, 62
Inlet Programmed Mode, 62
Oven Programmed Mode, 62
Pump
See syringe wash parameters, 171
R
Recorder
configuring, 69
Rerouting
S
Saving
Generated Method, 160
Screen
abbreviations, 13
Clock, 60
equilibration, 40
Offset, 70
Sleep Time, 57
stopwatch, 202
Syringe Wash, 171
timed events, 152
leaving, 155
Screens
about, 46
changing values, 46
Screens, overview, 37
Septum Purge Mode (PPC)
viewing/setting, 139
Set entry key, 33
Setting
detector temperature, 140
FID range, 142
injector temperature, 136
TCD range, 144
Setting up
Generated Method, 160
isothermal temperature program, 131
multi-ramp temperature program, 135
one-ramp temperature program, 133
PPC valves, 140
Stored Method, 161
Setup summary
ECD, 96
FID with manual pneumatics, 78
NPD with manual pneumatics, 112
TCD, 102
Single program mode, 170
233
Index
entering parameters, 175
running samples, 174
Sleep Time
creating a sleep method, 57
setting, 57
Startup time, setting
configuration, 60
Status
system, 39
Status checking
carrier gas, 42
detector temperature, 42
injector temperature, 41
oven temperature, 41
Status, overview, 37
Stopping, autosampler run, 188
Stopwatch
setting, 202
Stored Method
deleting, 162
setting up, 161
Stpwtch, abbreviation, 14
Syringe
cleaning, 186
configuring autosampler syringe size, 55
Syringe tower, 167
Syringe wash
parameters, 171
screen, 171, 183, 184
System Control Menu, 29, 53, 201, 204
System function key, 29
System status, 39
System utilities, 201, 220
System, turning on, 38
T
TCD
abbreviation, 14
attaching a flowmeter, 104
balancing the bridge, 106
overview, 101
234
polarity
changing, 145
range
setting, 144
range vs. bridge current, 144
setting up manual pneumatics, 103
using with autosampler, 107, 192
Temperature program
isothermal
setting up, 131
setting up a multi-ramp, 135
setting up a one-ramp, 133
Temperature program steps, 130
Temperature Programming, 18
Timed event
adding, 154
deleting, 156
entering, 152
Timed events screen, 152
leaving, 155
Timed events table
building, 151
displaying, 155
editing, 156
going directly to a line, 156
Tray, autosampler, 167
Turntable, autosampler, 167
U
Unlocking the keyboard, 212
Utilities, system, 201, 220
V
Valves
combustion, FID, 81
configuring, 65
Valves (PPC)
setting up, 140
PerkinElmer
710 Bridgeport Avenue
Shelton, CT 06484-4794, U.S.A.
Internet: http://www.perkinelmer.com
email: info@perkinelmer.com
PerkinElmer is a registered trademark of PerkinElmer, Inc.