Page 1 GAS CHROMATOGRAPHY 600/680 GC LARUS User’s Guide...
Page 2 ...
Page 3 Clarus 600/680 GC User’s Guide...
Page 4 The information contained in this document is subject to change without notice. Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no warranty of any kind with regard to this document, including, but not limited to, the implied warranties of merchantability and fitness for a particular purpose.
Page 5: Table Of Contents
Table of Contents Introduction ........................1-1 About This Manual ......................1-3 Conventions Used in this Manual ..................1-4 Notes, cautions and warnings ................... 1-4 Warning Signs on the Instrument..................1-5 Screen Abbreviations ....................... 1-6 Glossary of Clarus GC Terms ..................1-7 Autosampler Terms ......................
Page 6 Events Tab ......................2-42 Timed Events Table ....................2-43 Using the Active Method ....................3-1 Overview .......................... 3-3 Editing the Active Method ....................3-4 Getting Ready to Edit the Active Method ................ 3-5 Setting Up Oven and Inlet Temperature Programs ............3-6 Configuring the Equilibration Time (Init) ..............
Page 7 FID Overview ........................4-5 Setting Up an FID ..................... 4-6 Automatically Ignite the Flame ................4-11 Manually Ignite the Flame ..................4-13 Using the FID in Corrosive Environments ............. 4-15 Setting up an ECD ......................4-17 United States Government Regulations for ECDs ..........4-17 Special Instructions for ECD Cell Purchasers ............
Page 8 Method Editor ........................5-3 Method Edit Mode ......................5-5 Oven Settings ......................5-7 Managing Methods ......................5-9 File Menu ........................5-9 Using the Tools Menu ....................6-1 Tools Menu ........................6-3 Method Editor ........................6-4 Event Log ......................... 6-5 Maintenance ........................6-6 Configuration .........................
Page 9 Setting up a Typical Analysis ..................7-1 System Status Screen ....................... 7-4 Injector Settings ....................... 7-6 Packed Column (PKD) Injector ................7-6 Programmed Split/Splitless (PSS) Injector ............... 7-8 Detector Settings ......................7-11 Flame Ionization Detector (FID) ................7-11 Detector .......................... 7-16 Thermal Conductivity Detector (TCD) ..............
Page 10 viii...
Page 11: Introduction
Introduction...
Page 12 Introduction...
Page 13: About This Manual
Clarus 600/680 GC User’s Guide About This Manual This guide is divided into following chapters: Chapter 1 Introduction This chapter contains a brief introduction to the Clarus GC, the conventions and warnings used in the manual. Chapter 2 Touch Screen Navigation This chapter contains information that introduces you to the look and feel of the touch screen.
Page 14: Conventions Used In This Manual
Normal text is used to provide information and instructions. text refers to text that is displayed on the screen. Bold All eight-digit numbers are PerkinElmer part numbers unless stated otherwise. Notes, cautions and warnings Three terms, in the following standard formats, are also used to highlight special circumstances and warnings.
Page 15: Warning Signs On The Instrument
Clarus 600/680 GC User’s Guide Warning Signs on the Instrument For detailed safety information see the Safety Practices chapter in the Clarus 600/680 GC Customer Hardware and Service Guide (P/N 09936781). Caution, hot surface. Caution, risk of electric shock. Caution, laser radiation hazard. Caution (refer to accompanying documents).
Page 16: Screen Abbreviations
Introduction Screen Abbreviations AUX – Auxiliary zone Cap – capillary split/splitless injector Cmptr – computer Ctrl – syringe control parameters ECD – Electron Capture Detector FID – Flame Ionization Detector FPD – Flame Photometric Detector Gen – generate Inj/Vial – injections per vial Int –...
Page 17: Glossary Of Clarus Gc Terms
Clarus 600/680 GC User’s Guide Glossary of Clarus GC Terms The glossary of Clarus GC terms are divided into two types: • Autosampler Terms • Instrument-Specific Terms Autosampler Terms Term Description Washes Washing the syringe. Pre-Wash The number of prewashes of sample to prime the syringe (no pumping).
Page 18: Instrument-Specific Terms
Introduction Instrument-Specific Terms Term Description Attenuation The amplification of the detector output signal. Background A routine that automatically subtracts a stored calibrated compensation baseline profile from the signal generated during a GC run. Ballistically Changing the oven temperature as quickly as possible to reach a set point.
Page 19 Clarus 600/680 GC User’s Guide Term Description Parameter An independent variable used to specify a condition to be met. Programmable Pneumatic Control PPC Pre-run The time after equilibration during which negative-time events are executed. PPC version only. Sample management system. PreVent...
Page 20: Glossary Of Chromatographic Terms
Introduction Glossary of Chromatographic Terms Adsorption – A process that occurs at the surface of a liquid or solid as a result of the attractive forces between the adsorbent and the solute. These forces may be physical or weakly chemical. Analysis –...
Page 21 Clarus 600/680 GC User’s Guide pressure is calculated. This is dependent on the capillary control mode and installed pressure or split control option. Flow rate – The mass flow of carrier gas or detector gas in milliliters per minute. Ghost peaks – Peaks that are not due to sample components, for example, peaks produced by carrier gas impurities, septum, or components from previous analyses.
Page 22 Introduction 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.
Page 23: Touch Screen Navigation
Touch Screen Navigation...
Page 24 Touch Screen Navigation...
Page 25: Chapter Overview
Clarus 600/680 GC User’s Guide Chapter Overview You operate the Clarus GC using the touch screen on the front of the GC. The touch screen is the interface between you and the instrument, enabling you to control the Clarus GC in order for you to perform your analyses easily and conveniently.
Page 26: Touch Screen
Touch Screen Navigation Touch Screen The main display area on the touch screen is referred to as screens. You use various screens to set up your Clarus GC to perform the analyses. These screens contain: Entry fields which allow you to make entries, •...
Page 27 Clarus 600/680 GC User’s Guide The following Status Screen shows the different sections of the user interface. The Status Screen displays icons that provide quick access to major areas of the system. The injector and detector buttons show graphic representations of the devices for each channel.
Page 28: Tabs
Touch Screen Navigation Tabs Some of the active method screens include tabs to allow you to switch views associated with a specific channel. Non-Configured Devices If a device is installed but not configured, or configured as None, both the graphic and light are grayed out. Touching the button prompts the following dialog box.
Page 29: Non-Installed Devices
Clarus 600/680 GC User’s Guide The following screen capture shows the drop down list on the injector Configuration screen used to set a device to None. Non-installed Devices If a device is not installed, a grayed out deactivated button with no indicator light appears in the designated position.
Page 30: Run Button
Touch Screen Navigation Run Button The Run button displays the Manual injection and Autosampler settings if the device is enabled. The bottom bar on these screens includes the Start button. When the system is running, the Start button changes to the Stop button. Since the Start button is only available on the Autosampler and Manual inject screens, you must initiate a run from these screens.
Page 31 Clarus 600/680 GC User’s Guide When the GC is ready, touch the Start button to begin the run. If you touch Start before the system is ready, the run will start when the system reaches the ready status. When the Autosampler is disabled, touching the Run button displays the Manual inject screen.
Page 32 Touch Screen Navigation Enabled Disabled When the Stop button is pressed, an abbreviated Stop Menu appears. 2-10...
Page 33: Stop Menu
Clarus 600/680 GC User’s Guide Stop Menu Stop Immediately – Touching this button immediately stops the Active Method and closes the Stop Menu dialog.. Go to a temp, program step – Displays the Go to Temp dialog for you to select the step you wish to go to at this time.
Page 34 Touch Screen Navigation The name of the channel appears on the top left of the screen. Detector controls include Ignite and Autozero. Display controls include scaling and zeroing. Ignite Button Pressing the Ignite button starts the ignition sequence for a PPC-enabled FID. During ignition the plot and signal level are active.
Page 35: Heated Zones
Clarus 600/680 GC User’s Guide Zero Display Button The Zero Display button offsets the current signal level to 5% f.s.d. on the display. Heated Zones The Status screen displays graphic icons to represent the devices installed in the system. Each type of injector and detector is represented with a customized graphic as well as a text label.
Page 36 Touch Screen Navigation the active method settings for each device. Touching a device icon displays the selected screen as well as a row of tabs to allow easy access to the injector, oven, detector, and events for that channel. Touching the alternate channel icon on the top navigation bar displays the active screen and associated tabs for the other channel if it is installed and configured.
Page 37 Clarus 600/680 GC User’s Guide Oven Button Clicking the oven button provides access to the oven program settings and graph. You can set 1 to 10 program steps and up to 9 ramp rates. Use the up and down scroll buttons to the right of the oven entries to view program steps 5 – 10. If both channels are running and the Oven is accessed from the Status screen, it defaults to Channel A.
Page 38: Navigation Bar
Touch Screen Navigation Navigation Bar The navigation bar provides icons to allow users to seamlessly toggle between channels as well as access the same main areas of the system available from the status screen. The following diagram shows the navigation bar of an Active Method with the corresponding icons on the status screen.
Page 39: Injectors
Clarus 600/680 GC User’s Guide Injectors The injector elements that appear on a particular injector screen depend on injector types as well as selected configuration options. Some injector types offer a variety of options while others are more limited. The labels in the following screen capture identify the main components of an Active Method injector screen.
Page 40: Program Buttons
Touch Screen Navigation Program Buttons The program button appears next to the temperature and Carrier Gas fields for a programmable PSS or POC injector. If the program button associated with a value is active, the entry field is grayed-out. You must go to the program screen to modify the settings.
Page 41 Clarus 600/680 GC User’s Guide Configuration Options The following screens show the configuration choices and how they correspond to the entry fields in the active method. Configuration Screen Active Method Temperature Program You can set injector (inlet) temperature programs by selecting, the program button on the active method screen is active.
Page 42 Touch Screen Navigation The temperature graph displays the set point value. The label below the graph displays the current step. The text to the left of the graph displays the actual temperature. To modify the temperature program during a run, touch the program button. You can modify the temperature, time, or rate.
Page 43 Clarus 600/680 GC User’s Guide Carrier Gas Program The Carrier Gas options for PSS include flow, velocity, or pressure. If the option for Capillary Control is selected, you can program the carrier gas according to one of the three values. The following example shows that Pressure was selected as shown in the following Configuration screen: The corresponding actual values for the other units appear as read-only text on the screen as shown in the following Active Method screen.
Page 44 Touch Screen Navigation Touching the Program button next to the field displays the associated Carrier Pressure Program screen for the entry field value. 2-22...
Page 45 Clarus 600/680 GC User’s Guide Capillary Control Off The following screens are examples when Capillary Control is off Split Flow The PPC system adds the split flow offset to the method's split flow rate setpoint to obtain the Total split flow rate delivered to the inlet system. The total value is equal to the setpoint flow rate (the flow at the column entrance) plus the offset flow rate.
Page 46: Packed (Pkd)
Touch Screen Navigation Packed (Pkd) The packed column injector has a fixed (non-programmable) temperature field. The carrier gas can be programmed by Pressure or flow. The following procedure shows how to navigate through the screens to configure PPC for a packed column injector.
Page 47 Clarus 600/680 GC User’s Guide 3. Touch the PPC Connect button. 5. Touch Carrier B to Configure your Packed column injector for PPC. 4. Touch the OK button. 2-25...
Page 48 Touch Screen Navigation 6. Select Pres Read from the drop- 9. Touch the B Injector button on the down menu. Then touch the OK Configuration screen. button. 7. Touch Close to close the Connect PPC Device screen. 8. Touch OK on the Configuration PPC screen.
Page 49 Clarus 600/680 GC User’s Guide 10. The Configure Injector B screen 11. Select Pressure or Flow from the appears. drop-down menu. 12. To exit out of Configuration, touch the OK button then touch the Close button. 13. Display the active method and view the B-Pkd injector parameters as shown on the right.
Page 50: Poc
Touch Screen Navigation The packed on co lumn injector can be programmed by Inlet (POCI) or Oven (POCO). The POC injector is configured and controlled according to the same parameters as the PSS injector. Packed On Column Inlet Packed On Column Oven 2-28...
Page 51: Capillary (Cap) Injector
Clarus 600/680 GC User’s Guide Capillary (Cap) Injector 1. From the Configuration menu, 2. Exit from Configuration and select Cap from the drop-down display the active method screen. list. 2-29...
Page 52: Oven
Touch Screen Navigation Oven The Oven Temperature Program provides fields and a graph that reflect the current temperature program as shown in the screen on the left below. Pressing the Go to button invokes a dialog box that allows users to raise the temperature to a value associated with another step.
Page 53: Aux Zone
Clarus 600/680 GC User’s Guide Aux Zone If the GC is configured with an auxiliary zone, the button appears on the status screen. Touching the Aux button displays a dialog box with the setpoint and actual temperature. 2-31...
Page 54: Detectors
Touch Screen Navigation Detectors Detector screens provide you with a way to set and control a number of parameters during a run, such as temperature, range, and attenuation. Other active elements include a Heater Off button to turn off the detector and an AutoZero check box.
Page 55 Clarus 600/680 GC User’s Guide in the sample. The FID active method screen varies depending on whether the detector is configured with manual or programmable pneumatics. This section describes the screen components for each type of configuration. Touching the Ignite button allows you to light the FID flame. Auto-Ignition The PPC controlled FID has flameout detection and an auto-ignite feature.
Page 56 Touch Screen Navigation After the flame ignites, the FID output level is monitored to confirm ignition before producing a READY signal. If ignition is not confirmed, the ignition process repeats up to two more times if needed. If ignition is not achieved after three attempts, the flame gases are set to off and a dialog box appears displays the following message: “Flame 1 or 2 failed to ignite.”...
Page 57 Clarus 600/680 GC User’s Guide Configuration Settings The following screens show the Active Method screen and the corresponding settings in the Configuration screen. Active Method Configuration Screen 2-35...
Page 58: Tcd
Touch Screen Navigation 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. Four tungsten-rhenium filaments are connected in a bridge circuit, two in each channel.
Page 59: Ecd
In order to prevent a Thermal Runaway risk, the GC shuts down if any heated zone exceeds 470º C. If this occurs, the following message appears: Warning Instrument Shutdown Thermal Runaway xxxxxx zone Call your PerkinElmer service representative 2-37...
Page 60 Instrument Shutdown xxxx zone PRT error Call your PerkinElmer service representative 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.
Page 61: Pid
Clarus 600/680 GC User’s Guide The Photoionization Detector (PID) is designed to allow the effluent from a chromatographic column to be ionized by ultraviolet light (provided the ionization potential of the effluent is less than that of the UV source). The current produced by the ion flow is measured by the detector and is proportional to the concentration of the ionized material.
Page 62: Npd
Touch Screen Navigation The nitrogen phosphorus detector (NPD) is a highly specific thermionic detector for organically bound nitrogen and phosphorus. 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.
Page 63: Fpd
Clarus 600/680 GC User’s Guide In the Flame Photometric Detector (FPD), the column effluent is mixed with hydrogen and then burned in air. Light emitted from the flame passes through a lens, a filter, and to a photomultiplier tube, which generates an electrical signal. The Flame Photometric Detector is used for detecting sulfur, phosphorus, or tin compounds, which produce chemiluminescent reactions with emissions at wavelengths characteristic of the S2, Sn, and HPO species.
Page 64: Timed Events
Touch Screen Navigation Timed Events Events Tab The Events tab displays the timed events table and buttons, valves, and Aux gas controls. Element Enabling Timed events table Always Aux gas button PPC configuration Relays Always (see below for details) Insert button Always Edit button Always...
Page 65: Timed Events Table
Clarus 600/680 GC User’s Guide Timed Events Table The timed events table displays the time, name, and value of each event. Timed events may be added and removed while the GC is running. The next event to be executed is automatically selected. Up to 32 events can be specified. The configured hardware determines which events are available.
Page 66 Touch Screen Navigation Error Messages Edit Touching this button displays the active method page for editing timed events. If the GC is running, then edited events at times before the run time at which the edited list is accepted do not occur until the next run. 2-44...
Page 67 Clarus 600/680 GC User’s Guide Delete Clear Touching the Clear button deletes the contents of the entire event table. A dialog box confirms the action. Pressing Yes clears the table. Touching the No button closes the dialog box and retains the contents of the Events table. If the table is empty, the following Error message appears: 2-45...
Page 68 Touch Screen Navigation Value The value box function depends on the event. For some events, such as Carrier X, a numeric value is required. For others, such as TCD polarity, a choice between two options is required. 2-46...
Page 69 Clarus 600/680 GC User’s Guide The PreVent/ProTect/MS Vent valves are never operated during a run and are not required in the Timed Events list. • No timed event should have the same time as another timed event. • Time resolution is 0.01 minutes. •...
Page 70 Touch Screen Navigation Relays They appear as set in the configuration screen. User can turn on the initial and/or current settings by touching the check box. If GC is Ready, changing the initial setting will change the current setting. The initial settings are stored in the method and are only changed if the user modifies them.
Page 71 Clarus 600/680 GC User’s Guide Aux Zones Heated Aux Zone If the GC is configured with an auxiliary zone, the activated button appears on the status screen. Touching the Aux button displays a dialog box with the setpoint and actual temperature.
Page 72 Touch Screen Navigation Aux Zones that have been set in PPC configuration display the configured unit type and include a status indicator light. The initial values can be modified via timed events. The current value is shown next to the initial value field. 2-50...
Page 73: Using The Active Method
Using the Active Method...
Page 74 Using the Active Method...
Page 75: Overview
Clarus 600/680 User’s Guide 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, the fifth method is reserved for TotalChrom (external computer controlled software) and may be overwritten.
Page 76: Editing The Active Method
Using the Active Method Editing the Active Method If you have read and used the chapters in this manual sequentially, as recommended, by now you have probably installed and conditioned one or two columns, and set up one or two detectors. Also, you were probably not aware at the time that you modified certain Active Method parameters.
Page 77: Getting Ready To Edit The Active Method
Clarus 600/680 User’s Guide Getting Ready to Edit the Active Method  Close the oven door. NOTE: If a column has been installed, make sure you have carrier gas flow through the column before closing the oven door and elevating the oven temperature. The Status screen icon buttons provide access to the active method parameters.
Page 78: Setting Up Oven And Inlet Temperature Programs
Using the Active Method Setting Up Oven and Inlet Temperature Programs You can set up ramp programs (they are Init (1), 2, 3, through 10) using the Clarus GC software. 1. From the System Status screen touch the oven button to display the oven program screen.
Page 79: Configuring The Equilibration Time (Init)
Clarus 600/680 User’s Guide Figure 3-1. Typical temperature program steps. Before you actually set up an oven temperature program, you should decide on the Equilibration Time you need and change the default value if necessary (see below). Configuring the Equilibration Time (Init) When you change the oven temperature setpoint, the system heats or cools the oven to the new setpoint, then equilibrates the column(s) for the specified Equilibration Time before the instrument becomes READY.
Page 80: Setting A Coolant Cut-In Temperature
Using the Active Method NOTE: When using a POC or PSS injector with the subambient accessory, the injector temperature must not be set below the oven temperature. You can minimize coolant consumption if using the oven subambient with the PSS or POC installed but not being used, by deconfiguring the PSS or POC.
Page 81 Clarus 600/680 User’s Guide To set up an isothermal program: 1. From the Oven tab set the initial temperature 1 to 75 ºC using the up and down arrow or keypad buttons. 2. Enter a temperature setpoint appropriate for your analysis, for example, 100 °C. NOTE: The oven status changes to Not Ready.
Page 82: Setting Up A One-Ramp Temperature Program
Using the Active Method NOTE: You can set the rate to 0 but 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: •...
Page 83: Holding An Oven Temperature
Clarus 600/680 User’s Guide 3. Enter a ramp initial rate 1 of 2 C/min. ° 4. For Temp 2, enter a temperature of 70 °C. 5. Enter a time of 10 min. Setting Up a Multiramp Temperature Program The following example shows how to expand the above one-ramp program to a two-ramp program.
Page 84 Using the Active Method 2. After you touch oven button the Oven tab screen appears. Next, touch the go to to display the Go To Temp (temperature) screen. temp button 2. From this window touch the button for the temperature level that you want to hold. Touch OK.
Page 85 Clarus 600/680 User’s Guide The oven heats ballistically to the temperature value for oven Temp 2 and holds, instead of executing the time associated with oven Temp 2. Figure 3-2. Oven Temperature Program for Rate 1. To hold the oven program at a specific time during or before a run, use an oven HOLD timed event.
Page 86: Setting Injector Temperatures
Using the Active Method Setting Injector Temperatures Packed, Capillary (Split/Splitless), Programmed On-Column, and Programmed Split/Splitless The examples in this section were derived by editing the Active Method with a capillary injector installed and configured in position A (front), and a packed injector installed and configured in position B (rear).
Page 87 Clarus 600/680 User’s Guide The injector information displays: 3-15...
Page 88: Turning Injector Heaters On Or Off
Using the Active Method Turning Injector Heaters On or Off  To turn the Heater Off touch the check box. As the injector cools off, the injector temperature is displayed on the above screen. Changing Injector Temperatures 1. To turn the heaters on and modify temperatures, make sure the Heater Off check box does not display a check mark.
Page 89: Oven Temperature Programming Mode
Clarus 600/680 User’s Guide Oven Temperature Programming Mode In this mode the POC or PSS injector is configured as Oven. The injector temperature is set to the oven temperature plus 5 °C. This is the default mode and the easiest mode to operate in.
Page 90: Inlet Temperature Programming Mode
Using the Active Method Inlet Temperature Programming Mode The inlet temperature programming mode is used when the POC or PSS injector is configured as Inlet. In this mode, the injector follows the injector temperature program that you entered in the method. The initial default values are: Initial (Temp 1) is 50 °C, Injection Time is 999 min, and Inj Rate is 0.
Page 91: Setting Up A One-Ramp Injector Program
Clarus 600/680 User’s Guide Setting Up a One-Ramp Injector Program To set up a one-ramp injector program, enter the following parameters: • Initial injector temperature (Init Temp) • Isothermal time for the initial temperature (Init Time) • Rate of temperature increase from the initial to the final injector temperature (Init Rate) •...
Page 92 Using the Active Method 3. The temp program screen appears for the selected injector. Use the up and down arrow buttons or numeric keypad button to program the temperature, time and rate. Refer to the table on the previous page for some examples for values to set up a one ramp injector program.
Page 93: Viewing/Setting Carrier Gas Pressure/Flow/Velocity
Clarus 600/680 User’s Guide Viewing/Setting Carrier Gas Pressure/Flow/Velocity NOTE: For a description of programmable pneumatics control (PPC), refer to “PPC Fundamentals” In the Hardware Guide. PPC enables you to select and set the carrier gas Pressure, Flow, or Velocity. In all three modes, you can operate at a constant pressure, flow, or velocity or at a programmed pressure, flow, or velocity.
Page 94 Using the Active Method Initial Carrier-Gas Setpoint The carrier gas mass-flow controller receives set points of flow or pressure depending on the configured carrier gas mode. The program calculates the initial set point from the active GC method. The initial set point is established upon setting up a method, ending a run, or resetting the GC.
Page 95: Setting Carrier Gas Pressure
Clarus 600/680 User’s Guide Setting Carrier Gas Pressure To view or set the carrier pressure: 1. From the System Status screen touch the corresponding Injector button (A or B) for which you want to set the carrier pressure. The injector screen appears. In this example, the Clarus GC is configured with the PSS capillary mode on for pressure (psi).
Page 96 Using the Active Method 3. Touch the field, ranging from the Initial field to the step 4 field, and use up and down arrow or keypad buttons to enter a pressure, hold time and rate. NOTE: The rate for the range is 0 (end) to 99. A rate of 999 is a ballistic setting (maximum).
Page 97: Setting Carrier Gas Flow Using Ppc
Clarus 600/680 User’s Guide Setting Carrier Gas Flow using PPC To view or set the carrier flow: 1. From the System Status screen touch the Injector button (for example, Pkd or Cap) corresponding to the injector you wish to set the carrier gas flow. The tab for the selected injector appears: In this example, the Clarus GC is configured with the PSS capillary mode on for flow.
Page 98 Using the Active Method The Carrier Pressure Program window appears: 3. Touch to highlight each individual field, ranging from the Initial field to the step 4 field, and use up and down arrow or keypad buttons to enter a pressure, HOLD time and HOLD rate. NOTE: The rate for the range is 0 (end) to 99.
Page 99: Viewing/Setting Carrier Gas Velocity
Clarus 600/680 User’s Guide Viewing/Setting Carrier Gas Velocity You can view/set carrier gas velocity using PPC. To view or set the carrier gas velocity: 1. From the System Status screen touch corresponding Injector button for which you wish to set the carrier gas velocity. The page for the selected injector appears: In this example, the Clarus GC is configured with the capillary mode on for velocity (as shown by vel.-init displayed under the carrier gas field).
Page 100 Using the Active Method The Carrier Velocity Program window appears: 3. Touch each individual field, ranging from the Initial field to the step 4 field, and use up and down arrow or keypad buttons to enter a velocity, equilibration time and rate. NOTE: The rate for the range is 0 (end) to 99.
Page 101: Setting The Septum Purge Mode And Offset
Clarus 600/680 User’s Guide Setting the Septum Purge Mode and Offset To set the septum purge and offset: 1. Touch Tools button and select Configuration from the drop down menu. The Configuration screen appears: 2. Touch the button corresponding to the injector you want to modify (A-Injector or B-Injector).
Page 102 Using the Active Method 3. From the Capillary Control drop down menu select Pressure. Now you can only pressure program your capillary injector. If you wish to program the Capillary control for more than just pressure skip to step 9. 4.
Page 103 Clarus 600/680 User’s Guide We recommend that if you are operating with a split vent flow of 50 mL/min or less, select the Auto mode. Before each injection in the Auto mode, the system briefly closes the split vent and measures the total flow. With the split vent off this flow is the column flow plus the septum purge flow.
Page 104 Using the Active Method From the Carrier Control drop-down menu select from the following options: Off, Pressure, Flow, or Velocity. 8. Select either Program or Oventrack. However, if you select the Oventrack The following screen shows Program mode you do not need to enter column dimensions, and you can selected: skip to step 12.
Page 105 Clarus 600/680 User’s Guide The Column Carrier Gas Calculator screen appears: NOTE: If you incorrectly enter a column length or internal diameter, the resulting flow and pressure may be incorrect. For example, a 0.25 mm column may actually be 0.22 mm.
Page 106 Using the Active Method column length (cm) Retention Time of Methane (sec) 12. Return back to the Configure Injector screen and select either a Flow or Ratio Split Mode. If you select Flow, you will enter a split flow in your method. The software controls and calculates the split ratio.
Page 107 Clarus 600/680 User’s Guide In the Auto mode, the system performs a PreRun for one minute before it becomes READY, the split vent is closed, and the system measures the septum purge flow plus the column flow. This is referred to as the “offset.” The septum purge flow is controlled but not user selectable;...
Page 108 Using the Active Method If Fixed is selected use the up and down arrow or keypad buttons to enter an offset value in mL/min. 15. Press OK. NOTE: The Clarus PPC split pneumatics adds the septum purge offset to the split vent setpoint to obtain the total split system flow rate.
Page 109: Setting Up Valves
Clarus 600/680 User’s Guide Setting Up Valves The Clarus GC operates six internal solenoid valves. You can initially configure valves from the Configuration screen by selecting the Relays button. To change valve settings for your current method use the Timed Events screen and touch the Relays button. Setting the Split Mode Using PPC To set the split mode: 1.
Page 110 Using the Active Method 2. Touch the Injector button for the corresponding injector which to configure the split mode. The Configure Injector screen appears. 3. Touch the Capillary Control check box. Select either a Flow or Ratio Split mode. 3-38...
Page 111 Clarus 600/680 User’s Guide 4. Touch OK. The Configuration screen appears. 5. Touch Close. 6. On the System Status screen, touch the corresponding Injector button. The active method screen appears: The screen above displays the Split mode configured for Ratio. 7.
Page 112 Using the Active Method The Total Flow (split vent + septum purge + column) is displayed as a non- editable text field. The septum purge flow is factory preset to ~3.0 mL/min. It is not user adjustable. If you set the split flow to zero, the flow display shows column flow plus septum purge.
Page 113: Set Up The Splitless Mode For A Cap Or Pss Injector
Clarus 600/680 User’s Guide Set up the Splitless Mode for a CAP or PSS Injector The Splitless Mode is used for trace analyses. Most of the sample is transferred onto the column, then the split vent is opened, thereby venting any sample remaining in the injector liner.
Page 114 Using the Active Method the injector. It is important not to program the pressure (flow, velocity) down too quickly or ballistically, since this can cause backflush of the column. This means that the sample can flow back into the injector and either be lost out the split vent or cause peak broadening.
Page 115 Clarus 600/680 User’s Guide 3. Touch the Add button. The Add Timed Event screen appears: 4. Select Split A from the Event drop-down menu. 3-43...
Page 116 Using the Active Method 5. Touch the Time dialog box and use the up and down arrow or keypad buttons to enter a time of .25 minutes. 6. Touch the Value dialog box and use the up and down arrow or keypad buttons to enter a flow value.
Page 117 Clarus 600/680 User’s Guide 10. Touch the Initial pressure dialog box and use the up and down arrow or keypad buttons to enter a pressure value (for example 70). 11. Touch the Initial time dialog box and use the up and down arrow or keypad buttons to enter an initial time.
Page 118 Using the Active Method avoid this, the setup procedure is slightly different than the above procedure. When using a mass spectrometer, you would not want the initial pressure to be too high, because at the end of the GC run all parameters are set back to their initial values, and the higher pressure could cause damage to the vacuum system.
Page 119 Clarus 600/680 User’s Guide Setting the Timed Events 1. Touch the Events tab. 3-47...
Page 120 Using the Active Method 2. Touch Add. The Add Timed Event screen appears. 3. From the Event drop down menu select Split A (if the injector is installed in position A) or Split B (if the injector is installed in position B). 4.
Page 121 Clarus 600/680 User’s Guide 8. From the Event drop down menu select Split A (if you have the injector configured for position A) or Split B (if you have the injector configured for position B). 9. Touch the Time dialog box and use the up and down arrow or keypad buttons to enter a positive time for the event (for example, 2.00).
Page 122 Using the Active Method If you are using pressure pulse injection, you must set the split flow on just prior to when the inlet pressure begins to drop to the operating setpoint. CAUTION For example, if the inlet pressure is programmed to start decreasing one minute after injection, use a split flow event time of 0.98 minutes.
Page 123: Contolling The Autosampler
The Clarus 600 GC can use only the 82-vial standard tray or the 82-vial tall tray. The Clarus 680 GC is designed to use the large capacity 108-vial tray for standard vials or the 108-vial tray for tall vials. There is also an 82-vial...
Page 124 Using the Active Method Figure 3-10. Sample Tray and Carousel. 82-Vial Standard Tray 108-Vial Standard Tray 108-Vial Tall Tray and Carousel (for non-PerkinElmer vials) 3-52...
Page 125: Autosampler Touch Screen
Clarus 600/680 User’s Guide Clarus GC Tray Capacity Vial Height Number of Number of Number of Model of 2 mL Sample 4 mL Wash 4 mL Waste 2 mL Priority Vials Vials Vials Vials 680 only Standard 680 only Tall 600 only Standard 600 only...
Page 126: Start Button
Using the Active Method 2. In the next screen touch the Autosampler radio button to the right of the Type heading. The Autosampler screen contains three tabs. The first two tabs display identical screens for setting Program 1 and 2, allowing you to sequence two methods. The Tasks tab displays buttons to perform tasks such as Park, Clean, and specify a priority injection.
Page 127: Stop Button
Clarus 600/680 User’s Guide • When the GC oven starts to program, the Start Out signal will be asserted for 1 second. • The Ready Out signal will be asserted only when the GC is fully equilibrated and the GC has reached full Ready status. Stop Button As soon as the Start button is touched, the Stop button appears on all top level screens.
Page 128 Using the Active Method Touching the Stop button displays the following start menu dialog box: Stop Immediately – The Autosampler stops and the stop buttons turns to Start. Stop at the end of this run – The user can allow the current run to complete and then stop the Autosampler sequence.
Page 129 Clarus 600/680 User’s Guide Pause after this run - The system may be paused to stop any further injections until resumed by the user. When the system is paused, the Stop button turns to Resume on all top level screens. Go to a temp, program step –...
Page 130 Using the Active Method Autosampler Buttons Run options include selecting the run type, method, autosampler parameters, and run start/stop/program controls. The various controls, contents and enabling are configuration and mode dependent. 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.
Page 131 Clarus 600/680 User’s Guide 3. Highlight the Vials, Vol and Injections/Vail fields and use the plus minus buttons to input the correct amount. 4. Select either Injector A or B. 5. Touch Start when you are ready to begin the autosampler run. Autosampler Tasks Tab The Autosampler Tasks tab includes buttons to execute tasks such as Park and Clean.
Page 132 4. Pull and expel the same solvent through the barrel several times. 5. Replace the syringe using the procedure in the preceding section. NOTE: Only syringes distributed by PerkinElmer should be used with the Clarus GC. Plungers are not interchangeable from syringe to syringe.
Page 133 Clarus 600/680 User’s Guide Auto Resume Check the Auto Resume checkbox to allow the autosampler program to automatically resume where it left off should a power failure occur. Running Viscous Samples The Clarus GC allows you to vary the length of time the plunger pauses at the top-of- stroke when acquiring samples.
Page 134: About Waste And Wash Vials
Using the Active Method This option instructs the autosampler to interrupt the vial injection sequence and inject a "Priority" vial that has been placed in the "Priority" position of the turntable. The priority vial will be injected after completion of the current run. After the priority vial has been injected (in accordance with the current program parameters), and the priority run completed, the program continues with the next injection in sequence.
Page 135: About Sample Vials
Only PerkinElmer vials should be used with the Clarus GC. 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.
Page 136: Available Syringes
Using the Active Method Available Syringes The following syringes are available for the Clarus GC: Syringe Part Number 5-µL (0.63 mm O.D.) Teflon-tipped plunger (Std) N6101390 0.5-µL (0.63 mm O.D.) N6101252 0.5-µL (0.47 mm O.D.) N6101253 5-µL (0.63 mm O.D.) N6101251 5-µL (0.47 mm O.D.) N6101380...
Page 137: Setting Up The Detectors
Setting Up the Detectors...
Page 138 Setting Up the Detectors...
Page 139: Overview
Clarus 600/680 User’s Guide Overview This section contains procedures for setting up the following detectors: FID (flame ionization) PID (photoionization) ECD (electron capture) NPD (nitrogen phosphorus) TCD (thermal conductivity) FPD (flame photometric) The instructions provided in this chapter describe how to set detector gases that are controlled by PPC modules.
Page 140 Setting Up the Detectors 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.
Page 141: Fid Overview
Clarus 600/680 User’s Guide 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, generating ions. The ions are collected and measured by the detector, with their concentration proportional to the amount of compound present.
Page 142: Setting Up An Fid
Setting Up the Detectors Setting Up an FID To set up an FID that uses PPC modules, first read the FID Setup Summary, then follow these procedures. To avoid injury, Do Not turn on the hydrogen gas unless a column is connected to the FID and all fitting connections have been leak tested.
Page 143 Clarus 600/680 User’s Guide FID Setup Summary To set up the PPC FID: • Set the air and hydrogen flows. • Automatically ignite the flame. Manually ignite the flame. Set the Air and Hydrogen Flows The FID pneumatics utilizes two PPC modules: one to control the air and the other to control the hydrogen.
Page 144 Setting Up the Detectors NOTE: The screen above shows that an FID is installed in Channel A. 4. Select a filter value from the Filter drop-down menu.
Page 145 Clarus 600/680 User’s Guide The default setting is 200 milliseconds. To improve the signal-to-noise, change the setting to 800 milliseconds. This improves the noise but broadens the peak shapes. If you want a faster detector response, change the setting to 50 milliseconds;...
Page 146 Setting Up the Detectors A column must be installed on the base of the detector and capped with a stainless steel Swagelok Plug before attempting to ignite CAUTION the flame. 7. Touch the Set Point dialog box for the H2 flow and use the numeric keypad or the up and down arrow buttons to set the Hydrogen flow to 45 mL/min.
Page 147: Automatically Ignite The Flame
Clarus 600/680 User’s Guide 8. Press OK. Automatically Ignite the Flame How Auto-Ignition Works To ensure proper auto-ignite FID operation, make sure your column is positioned in the FID 2.75 inches (70 mm) from the back of the column nut. CAUTION The flame may not auto-ignite if your carrier gas flow is 60 mL/min or higher.
Page 148 Setting Up the Detectors With the FID temperature set, the air and hydrogen flows set, and auto-ignition activated by setting a positive mV value for the flame offset, the FID attempts auto- ignition at -0.5 min. before the system becomes ready. At this Pre-run time the status bar flashes “...
Page 149: Manually Ignite The Flame
Clarus 600/680 User’s Guide confirm that the flame is lit. If a lighted flame is not confirmed, the Clarus GC repeats the ignition process up to two more times. Manually Ignite the Flame You can manually ignite the flame at any time by following this procedure. Before trying to ignite the flame, make sure that you have sufficient combustion gases and they are turned on at the source, and make sure that the flows are set as described earlier in this section.
Page 150 Setting Up the Detectors ° NOTE: For proper ignition to occur, the FID must be heated to at least 100 2. Touch the temp field and use the up and down arrow or keypad buttons to enter a setpoint of at least 100 C, or enter a value 50 °...
Page 151: Using The Fid In Corrosive Environments
Clarus 600/680 User’s Guide 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 forms on the object if flame ignition has occurred. The FID outlet is hot! To prevent injury, never place your hand over the FID outlet.
Page 152 Setting Up the Detectors The FID outlet is hot! To prevent injury, never place your hand over the FID outlet. WARNING 2. Lift open the detector cover. 3. Cut the piece of tubing (P/N 0250-6490) to a length of 4-inches and firmly insert one end of the tubing into the top of the FID.
Page 153: Setting Up An Ecd
U.S. Nuclear Regulatory Commission (NRC) and/or in some states by the equivalent state agency. For further information on obtaining a license, contact PerkinElmer, Shelton, Connecticut Customer Service department or the NRC Material Branch Office of Nuclear Materials, Safety and Safeguards, Washington, DC 20555.
Page 154: Special Instructions For Ecd Cell Purchasers
Special Instructions for ECD Cell Purchasers (Who are not Specifically Licensed to Handle Radioactive Materials) The PerkinElmer Electron Capture Detector (P/N N610-0063, 120 V or N610-0134, 230 V) contains 15 mCi of Nickel-63 (Ni 63), a radioactive material. Your possession and use of this detector is governed by 10 C.F.R.
Page 155 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.
Page 156: United Kingdom Regulations
Setting Up the Detectors United Kingdom Regulations In the U.K., registration is required under the Radioactive Substances Act of 1960, for anyone keeping or using radioactive materials. Application should be made to any one of the following governing bodies: ENGLAND Department of the Environment Queen Anne's Chambers Tothill Street...
Page 157 Clarus 600/680 User’s Guide 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.
Page 158: Ecd Set Up
Setting Up the Detectors NOTE: If you want to switch between an 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 NOTE: To minimize detector contamination, run the ECD hot, at a temperature of at least 375 ºC.
Page 159 Clarus 600/680 User’s Guide NOTE: Because an ECD is extremely sensitive, contamination from any part of the system can add to the background and noise. To help assure a clean system the injector and detector should be baked-out and both packed and capillary columns thoroughly conditioned before use.
Page 160 Setting Up the Detectors 4. Attach the outer metal sleeve of the vent tubing (P/N N610-0161) to the ECD Outlet. Figure 4-8. Connecting vent tubing to the ECD outlet. 5. Press down and turn the metal sleeve on the end of the vent tubing to secure it to the ECD.
Page 161 Clarus 600/680 User’s Guide Adjust the Make-up Gas Flow 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 CAUTION other than nitrogen. The following procedures describe how to set the make-up gas.
Page 162 Setting Up the Detectors 4. In this Configuration screen touch the A-ECD button. The following screen appears: The Filter default setting is 200 milliseconds. If you want to improve the signal- to-noise, change the setting to 800 milliseconds; however, the noise improves 4-26...
Page 163 Clarus 600/680 User’s Guide but the peak shapes broaden. If you want a faster detector response, change the setting to 50 milliseconds; however, the noise level may increase. 5. To change the Make Up gas flow in this Configuration screen, use the up and down arrow or keypad buttons.
Page 164: Setting Up A Tcd
Setting Up the Detectors Setting up a TCD NOTE: The PPC pneumatics detector gas modules have been set to OFF at the factory. TCD Overview The Thermal Conductivity Detector (TCD) is a dual-channel detector that 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).
Page 165: Tcd Setup
Clarus 600/680 User’s Guide TCD Setup 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.
Page 166 Setting Up the Detectors 2. In the TCD tab page touch the temp field and use the up and down arrow buttons or the numeric keypad to enter a TCD temperature appropriate for the analysis to be run. 3. The detector heater can be turned on or off by touching the Heater On/Off button. 4-30...
Page 167 Clarus 600/680 User’s Guide Equalize the Makeup and Reference Gas Flows The following procedures describe how to adjust the makeup and reference gas using PPC pneumatics in the Clarus GC. The TCD flow module for reference gas is calibrated with helium at the factory.
Page 168 Setting Up the Detectors This displays the Configuration screen page. 2. Touch the TCD button to display the TCD configuration screen. The following example shows the TCD configuration settings and how they correspond to the TCD active method screen. TCD Active Method TCD Configuration Screen 4-32...
Page 169 Clarus 600/680 User’s Guide 3. In the TCD Configuration screen set the Make-up gas and Reference gas line flows to 30 mL/min using the up and down arrow buttons or the numeric keypad. 4. As shown in the example above, use the up and down buttons or the numeric keypad to set the filter to 200 and the Output to 5.When all the settings are appropriate for your analysis touch OK.
Page 170 Setting Up the Detectors The correlation between bridge current and range is in Table 4-2: Table 4-2. Correlation Between Bridge Current and Range Bridge Current (mA) Range Entry ±0 ±1 ±2 ±3 ±4 NOTE: Entering a negative number reverses the detector polarity. For examples of reversing the polarity, see the Clarus 600/680 GC Customer Hardware and Service Guide, Maintenance Chapter, section “Practical Hints.”...
Page 171: Using A Tcd With The Autosampler Or Gsv
Clarus 600/680 User’s Guide 2. Allow the system to stabilize for about 20 min, then open the detector cover. 3. Locate the TCD Balancing Potentiometer (see Figure 4-11). Adjust the potentiometer until the Autozero display reads between 0.0 and 20.0 mV. 4.
Page 172: Setting Up A Pid
PPC pneumatics. PID Overview The PerkinElmer Photoionization Detector (PID) is designed to allow the effluent from a chromatographic column to be ionized by ultraviolet light (provided the ionization potential of the effluent is less than that of the UV source). The current produced by the ion flow is measured by the detector and is proportional to the concentration of the ionized material.
Page 173: Pid Setup
Clarus 600/680 User’s Guide A cross section view of a PID is shown in the above figure. Figure 4-14 is an illustration of an installed PID. º NOTE: The optimum operating temperature for a photoionization detector is 250 C. PIDs °...
Page 174 Setting Up the Detectors Adjust the make-up gas flow if using a capillary column at flows of ≤10 mL/min. • Turn on the UV lamp. • Optimize the lamp intensity. Turn On the Oven and the Detector Heaters NOTE: A PID can only be installed in the Detector 2 position (rear). 1.
Page 175 Clarus 600/680 User’s Guide 4. If you require the heater on for your analysis just touch the heater button and it will toggle to heater on. Adjust the Make-up Gas Make-up gas is required when using capillary columns at low flows (10 mL/min or less).
Page 176 Setting Up the Detectors The PID flow module for make-up gas is calibrated with helium gas at the factory. You must recalibrate the PID flow module if you are using a reference gas other than helium. CAUTION 1. With the make-up gas is set from the Clarus GC touch screen. The PPC modules are calibrated at the factory;...
Page 177 Clarus 600/680 User’s Guide This displays the PID Configuration screen: 3. In the PID Configuration screen set the Make-Up gas line pressures to 60 - 90 psig by using the up and down arrow or keypad buttons. 4. As shown in the example above, use the up and down arrows to set the Filter to 200.
Page 178 Setting Up the Detectors 2. Turn the lamp intensity control knob fully counterclockwise. 3. Turn the UV lamp switch ON. 4. From the PID Tab make sure that AutoZero is off (the box is not checked). If it is On, touch the field to remove the check mark. 5.
Page 179: Setting Up A Npd
Clarus 600/680 User’s Guide Figure 4-17. A typical intensity signal. 4. Repeat steps 2 through 4 at different attenuations using the highest lamp intensity that corresponds to the lowest background signal. NOTE: If optimizing the lamp intensity cannot be done easily using the above procedure, increase the lamp intensity until the noise is between 1% and 1.5% of full scale at an attenuation of x8.
Page 180: Npd Overview
Setting Up the Detectors Turn off the hydrogen gas before disconnecting a column from the NPD. When two NPDs are installed, but only one NPD has a WARNING 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.
Page 181: Setting Up A Npd
Clarus 600/680 User’s Guide reduce bead performance and life. Although these solvents may still be used, they should be avoided whenever possible. Figure 4-26. Nitrogen Phosphorus Detector (NPD). Setting Up a NPD To set up a NPD using PPC modules, set the hydrogen and air flow as described below, then condition the bead.
Page 182 Setting Up the Detectors 3. In the System Status screen touch the NPD button. The following screen appears: 4. To set the air and hydrogen touch the Tools button in NPD screen and touch Configuration from the displayed menu. The Configuration displays: 4-46...
Page 183 Clarus 600/680 User’s Guide This displays the NPD Configuration screen: 5. In the NPD Configuration screen, set the Air to 450 mL/min and the Hydrogen flow to 45 mL/min by touching the field and using the up and down arrow or keypad buttons.
Page 184: Npd Bead Activation Procedure
Setting Up the Detectors 6. Set the Filter to 200. The default setting for the filter is 200 milliseconds. If you want to improve the signal-to-noise, change the setting to 800 milliseconds; however, the noise improves but the peak shapes broaden. If you want a faster detector response, change the setting to 50 milliseconds;...
Page 185 Clarus 600/680 User’s Guide 1. Obtain a stopwatch or use the stopwatch function in the GC Utilities screen. 2. Open the oven door and allow the oven to cool. 3. Using a 7/16-inch wrench, loosen and remove the column nut from the detector fitting.
Page 186 Setting Up the Detectors 11. From the system status screen touch the signal icon to display the detector background. 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. 12.
Page 187 Clarus 600/680 User’s Guide Activating the NPD Bead The bead requires an activation step prior to use. Do not inject a sample during Activation. To Activate the bead, carefully follow this procedure in sequential steps below: 1. Turn the bead potentiometer dial clockwise to apply current to the bead. 2.
Page 188 Setting Up the Detectors 15. Make sure the column flow is properly set. Touch the signal icon display the detector background produced by carrier gas flow. The bead background will be less due to cooling effects. 16. Turn the bead potentiometer dial clockwise until you achieve a reading of 0.25 mV above the "off"...
Page 189 Clarus 600/680 User’s Guide 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.
Page 190 Setting Up the Detectors Column bleed: Material from the column can effect bead lifetime. Keep the maximum oven temperature as low as possible for each application. Between run operation: If the NPD bead is not in use for a few days it is best to simply lower the potentiometer setting to 600 and maintain the detector temperature at 200 deg.
Page 191: Setting Up An Fpd
, Sn, and HPO species. A filter that isolates sulfur emissions (P/N N6000637) is supplied with the detector. Another filter that isolates phosphorus emissions (P/N N6000981) and a filter that isolates tin emissions (P/N L4145472) are available from PerkinElmer at www.perkinelmer.com. 4-55...
Page 192 Setting Up the Detectors A cross section view of an FPD is shown below. Figure 4-31. Flame Photometric Detector (FPD). 4-56...
Page 193: Setting Up The Fpd
Clarus 600/680 User’s Guide Setting Up the FPD To set up a FPD using PPC modules, follow the steps below. FPD Setup Summary To set up a FPD: • Configure the linearizer and signal filter. • Set the FPD temperature. •...
Page 194 Setting Up the Detectors 2. The FPD page is now visible. 4-58...
Page 195 Clarus 600/680 User’s Guide 3. For Linearizer the default value is Off. To change the value to On touch the Tools button in FPD tab screen and touch Configuration from the displayed menu. 4. This will bring you to the Configuration screen page. 4-59...
Page 196 Setting Up the Detectors 5. Touch the FPD button to display the NPD configuration screen. 6. In this screen touch the Linearize check box to turn it On. This is indicated by a check in the box. 7. Set the Filter to 200. The default setting is 200 msec.
Page 197: Set The Fpd Temperature
Clarus 600/680 User’s Guide 8. When all the settings are appropriate for your analysis touch OK. The FPD tab screen will be now visible and the changes you made in the configuration screen will be shown. Set the FPD Temperature NOTE: When using the FPD with Turbochrom Version 3.1 or earlier, OMEGA, or the Model 1020/1022 (software Version 7.10 for the SX or Version 6.5 for GC Plus), the FPD temperature values must be entered between 250 °C and 450 °C only.
Page 198 Setting Up the Detectors NOTE: For proper ignition to occur, the FPD must be heated to at least 250 °C. 3. Touch the temp field and use the up and down arrow or keypad buttons to enter a setpoint of at least 250 C (this is the minimum entry for a °...
Page 199 Clarus 600/680 User’s Guide 4. The FPD tab page is now displayed. 4-63...
Page 200 Setting Up the Detectors 5. To change the gas flow values touch the Tools button in FPD tab screen and touch Configuration from the displayed menu. This displays the Configuration screen. This displays the FPD Configuration screen. 4-64...
Page 201 Clarus 600/680 User’s Guide 6. On this page touch the FPD button to get to the FPD Configuration screen. 6. Touch the Hydrogen field and use the up and down arrow or keypad buttons to change the value to 75 (to 75 mL/min). 7.
Page 202 Setting Up the Detectors 7. Touch OK when completed. Turn On the Photomultiplier Tube 1. From the System Status screen touch the FPD button. 4-66...
Page 203 Clarus 600/680 User’s Guide 2. The FPD tab page is now visible. 3. To turn on the photomultiplier tube touch the Tools button in FPD tab screen and touch Configuration from the displayed menu. This will bring you to the Configuration screen page. 4-67...
Page 204 Setting Up the Detectors 4. On this page touch the FPD button to display the FPD Configuration page. 5. In the PMT Voltage field set the percentage (see note below) by using the up and down arrow or keypad buttons. This will turn on the photomultiplier tube.
Page 205 Clarus 600/680 User’s Guide Ignite the Flame 1. Open the electronics cover to access the ignitor assembly. Figure 4-32. Ignitor assembly. 2. From the system status screen touch the FPD button. 3. The FPD tab page is now visible. NOTE: For proper ignition to occur, the FPD must be heated to at least 250 °C. 4.
Page 206 Setting Up the Detectors , or enter a temperature that is 50 C higher than the highest ° temperature of your oven program. 5. Close the oven door. Wait for the FPD 1 temperature to become READY. 6. Position the ignitor assembly on the FPD outlet (see the following figure). 7.
Page 207 Clarus 600/680 User’s Guide The FPD outlet is hot! To prevent injury, never place your hand over the FPD outlet. WARNING NOTE: To prevent condensation on the FPD, always turn off the flame (hydrogen and air gases) before cooling the detector or turning off the Clarus GC. 4-71...
Page 208: Detector Temperatures
Setting Up the Detectors Detector Temperatures To display or change detector temperatures and turn the detector heaters on or off can be done from one screen in the Clarus GC. The example shown below assumes that the Clarus GC has an ECD detector. 1.
Page 209 Clarus 600/680 User’s Guide 3. In the ECD page touch the temp field and use the up and down arrow or keypad buttons to set an ECD temperature appropriate for the analysis to be run. 4. To turn the heater on or off just touch the Heater button .
Page 210: Setting The Range
Setting Up the Detectors Setting the Range Setting the FID, PID, or NPD Range FID, PID, or NPD range is set from the FID, PID, or NPD Range screen. initial The example below uses FID but the following procedure can also be used for PID or NPD.
Page 211: Changing The Fid, Pid, Or Npd Range During A Run
Clarus 600/680 User’s Guide Changing the FID, PID, or NPD Range During a Run To automatically change the range from 1 to 20 after 1 minutes into the run. The example below uses FID but the following procedure can also be used for PID or NPD.
Page 212 Setting Up the Detectors 3. In the Add Timed Event screen enter an Event by touching the down arrow in the Event field to view the other ranges. Select the one you need by touching it. 4-76...
Page 213 Clarus 600/680 User’s Guide 4. Enter a time by touching the Time field and using the up and down arrow or keypad buttons, enter the time required for your analysis. This will change the time for AutoZero A as shown. 5.
Page 214: Setting The Tcd Current (Filament Current)
Setting Up the Detectors Setting the TCD Current (Filament Current) When the detector is not in use the temperature and current must be off. CAUTION 1. From the System Status screen touch the TCD button 2. In the TCD tab page touch the Current field and use the drop down menu to change the value.
Page 215 Clarus 600/680 User’s Guide The TCD range values corresponding to bridge current are shown below: Table 4-3. Correlation Between Bridge Current and Range Bridge Current (mA) Range Entry ±1 ±2 ±3 ±4 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.
Page 216: Changing Tcd Polarity During A Run
Setting Up the Detectors Changing TCD Polarity During a Run TCD Range timed events are restricted to changing TCD polarity. For example, if an initial range is four, then an event can only be entered for +4 or −4. Examples for using polarity changes are given in Clarus 600/680 GC Customer Hardware and Service Guide, “Maintenance”...
Page 217 Clarus 600/680 User’s Guide 3. In the Events tab touch the Add button. 4. Using the up and down arrow or keypad buttons enter a time of three minutes into the Time field. 4-81...
Page 218 Setting Up the Detectors 5. Using the drop down menu in the Value field select a value of -2. 6. When completed touch OK to close this screen. 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.
Page 219: Routing Detector Output
Clarus 600/680 User’s Guide Routing Detector Output The Clarus GC contains one analog data output channel for each installed detector amplifier board. You can attach an integrator or recorder to either output channel Normally the detector output would go to the device configured for that channel. However, if you are running complex analyses, such as those requiring detector switching, you may wish to route the signal to either channel.
Page 220 Setting Up the Detectors 3. In the Events screen touch the Add button. The Timed Events screen will appear. In the drop down menu for Events and touch Output A. 4-84...
Page 221 Clarus 600/680 User’s Guide 4. Touch the Time field and use the up and down arrow or keypad buttons to input a time that the FID’s output will go to the integrator. 5. Touch the value field and use the drop down to select a negative value (detector A is negative, detector B is positive).
Page 222 Setting Up the Detectors 11. Touch the value field and use the drop down to select a positive value (detector 1 is negative, detector 2 is positive). 12. Touch OK to return to the TCD page. 13. Once in the TCD page touch the System button to return to the System Status screen.
Page 223: Attenuating Detector Signals Going To A Recorder
Clarus 600/680 User’s Guide Attenuating Detector Signals Going to a Recorder The purpose of attenuation when a recorder is attached and configured is to bring a peak on scale by amplifying a weak signal or reducing an overly strong signal. Attenuation in this case affects only the presentation of the signal.
Page 224 Setting Up the Detectors 3. After this is done you may continue with another tab page or touch the System button to return to the System Status screen. A table listing attenuation vs. the maximum detector signal producing 100% deflection on a 1 mV-recorder is provided in the Clarus 600/680 GC Customer Hardware and Service Guide, Maintenance chapter, section “Practical Hints.”...
Page 225: Optimizing A Detector Signal To An Integrator For Maximum Sample Dynamic Range
Clarus 600/680 User’s Guide Optimizing a Detector Signal to an Integrator for Maximum Sample Dynamic Range The Clarus GC contains improved electronics which significantly reduce amplifier noise. This allows you to amplify the detector signal without getting a large increase in the noise level. Therefore, it provides excellent minimal detection (signal to noise) for all Clarus GC detectors.
Page 226: Matching Detector Signals With Your Integrator
Setting Up the Detectors Matching Detector Signals with Your Integrator The following procedure should be followed if you are operating your detector near the minimal detectable quantity level. This will ensure that the integrator is not filtering the signal coming from the Clarus GC. The purpose of attenuation when an integrator is attached and configured is to assure that the GC output is above the noise level of the integrator.
Page 227 Clarus 600/680 User’s Guide Figure 4-40. An example of detector noise. A table listing attenuation vs. the maximum detector signal producing a 1-V output to an integrator is provided in the Clarus 600/680 GC Customer Hardware and Service Guide, Maintenance chapter, section “Practical Hints.” To change an attenuation value: 1.
Page 228 Setting Up the Detectors NOTE: 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. 4-92...
Page 229: Autozeroing A Detector
Clarus 600/680 User’s Guide Autozeroing a Detector Each configured detector is equipped with digital autozeroing capability. As long as Autozero is On (indicated by a check mark in the box), the system will autozero the detector to the offset specified during configuration whenever the system becomes READY or when a run is started.
Page 230 Setting Up the Detectors NOTE: When Autozero is Off, the output signal is never autozeroed. 4-94...
Page 231: Using The Method Editor
Using the Method Editor...
Page 232 Using the Method Editor...
Page 233: Method Editor
Clarus 600/680 GC User’s Guide Method Editor To access the Method Editor display the System Status screen: From this screen touch the Tools button (as shown above). This displays the following options:...
Page 234 Using the Method Editor To access Method Editor, touch Tools menu and touch the first option, Method Editor. The Method Editor screens are similar to the Active Method screens. The differences are noted in this section. You can access and edit the first five methods. The fifth method is reserved for TotalChrom and may be overwritten.
Page 235: Method Edit Mode
Clarus 600/680 GC User’s Guide Method Edit Mode When you touch Method Editor from the Tools menu, a screen similar to the status screen appears.
Page 236 Using the Method Editor The buttons with icons provide access to the injector, detector, oven, and aux settings associated with the Active Method in the method mode. If an Aux temperature is configured, an Aux button appears on the method edit screen. The Method Edit screens are similar to the Active Method screens with the following differences: •...
Page 237: Oven Settings
Clarus 600/680 GC User’s Guide The following screens show the differences between the two modes( Active Method and Method Editor). The first screen below shows the PSS active method screen. The second screen, that follows, shows the screen in Method Edit mode. Active Method Screen Method Edit Mode Oven Settings...
Page 238 Using the Method Editor You can program up to 10 oven steps by touching the field and using the up and down arrow or keypad buttons to enter a value. After entering all of your settings, touch the File button. This displays a pop-up File menu with options to create, modify, and save methods.
Page 239: Managing Methods
Clarus 600/680 GC User’s Guide Managing Methods The name of the active method is grayed-out in the file name list that appears for Delete, Open, Activate, and Save As. If you enter the same name as the active method, the following message appears: File Menu The pop up File menu includes options to create, modify, store, and delete methods.
Page 240 Using the Method Editor You can either assign a Name to the current method by touching the Name field and use the displayed Data Entry keypad. When done typing a name, in this example I typed name, then touch the OK button.
Page 241 Clarus 600/680 GC User’s Guide To save it, touch OK or touch Cancel to close the Save As dialog box When the dialog box closes, the GC is in the New Method mode and the fields are populated with default values. The Method Name field is activated and displays the name “untitled.”...
Page 242 Using the Method Editor Touch the method name and OK to populate the method edit screens with the values from the selected method. If you choose Cancel, or touch the OK button without selecting a method, the dialog box will close and the operation will be ignored. Save The Save command saves the previously opened and optionally modified method under the same name.
Page 243 Clarus 600/680 GC User’s Guide Save As.. The Save As command saves the current method under a new or existing name. Touching this option displays the Save As dialog box. The Name field displays the name of the current method. The list of method names always displays “External”...
Page 244 Using the Method Editor Although a new method name field displays the name “untitled,” the field to enter the new name is blank. The Method Name field displays each character as it is touched starting from the center of the field. The name can be comprised of any combination of letters and numbers and is limited to 13 characters.
Page 245 Clarus 600/680 GC User’s Guide Pressing Continue returns control to the previous screen. You can select a name or cancel out of the process. If five methods are already stored, entering a new name will prompt the following dialog box: If you press Yes, the method list appears.
Page 246 Using the Method Editor If you press No, the Save As… dialog box displays the same fully populated list of methods. The new method name is still in the Name field. You can press Cancel to return to Method Edit mode and access the File button, or OK to prompt the memory full error again.
Page 247 Clarus 600/680 GC User’s Guide Select a name from the list. The selected name appears in the Method Name field. Touch the OK button to delete the selected method and close the dialog box. Exit Editor The Exit Editor option closes the Method Edit screens and restores the Active Method.
Page 248 Using the Method Editor 5-18...
Page 249: Using The Tools Menu
Using the Tools Menu...
Page 250 Using the Tools Menu...
Page 251: Tools Menu
Clarus 600/680 GC User’s Guide Tools Menu The Tools pop-up menu provides options to a number of Clarus GC features and settings, such as , and . To Method Editor, Configuration, Maintenance Utilities display the menu, touch the Tools button: 1.
Page 252: Method Editor
Using the Tools Menu Method Editor To access Method Editor, touch the Tools button and then touch the first option, Method Editor. For detailed Method Editor information see Chapter 4, Using the Method Editor in this guide.
Page 253: Event Log
Clarus 600/680 GC User’s Guide Event Log To access Event Log, from the System Status screen, touch the Tools button and touch the second option in the list, Event Log. In the Event Log screen you can select either the Autosampler or current Run log.
Page 254: Maintenance
Using the Tools Menu Maintenance To access the Maintenance screen, from the System Status screen, touch the Tools button and then touch Maintenance. The maintenance feature provides you with the ability to set up to eight task reminders. For each item, you can enter the name of the task and specify the condition that prompts the reminder.
Page 255 Clarus 600/680 GC User’s Guide 1. To add an entry, touch the New button. The New Maintenance Task screen appears. The interval options are: Injections, Hours, and Days: 2. Touch the Count (interval) field and then enter a value using up and down arrow or keypad buttons.
Page 256 Using the Tools Menu Type the message. For example, Change Septum 4. Click OK to save the message. 5. If a maintenance task has already been assigned to the selected number, a dialog box will ask if you want to overwrite it.
Page 257 Clarus 600/680 GC User’s Guide 6. When done, touch the Close button. 7. When the Count value equals the number assigned to the task, a dialog box displays the reminder. 8. Touch OK to close the reminder.
Page 258: Configuration
Using the Tools Menu Configuration To access Configuration, from the System Status screen, touch the Tools menu and select Configuration. The Configuration screen appears. This section describes how to configure and then shows the various GC configuration screens. Injectors (Deconfiguring and Configuring Injectors) Occasions may arise when you may not be using one of the injectors for an extended period of time.
Page 259 Clarus 600/680 GC User’s Guide Deconfiguring the detectors also deconfigures the detector’s PPC control. You must reconfigure the PPC control when restoring the detector configuration. 1. Touch the A-Injector button. The Configure Injector A appears. 2. Select the Injector Type from the drop-down list: The Type options are: None, Packed, Cap, GSV, PSSI, and POC.
Page 260 Using the Tools Menu PSS - Programmed Split/Splitless Injector The PSSI injector includes a Capillary Control option If the Capillary Control mode is selected the following additional parameters are displayed (shown below in the bordered area) and the Capillary Control can be configured for pressure, flow, and velocity. When set for inlet programming, the injector is first heated to the injector temperature entered in the method and then follows the injector temperature program.
Page 261 Clarus 600/680 GC User’s Guide The Flow Offset radio buttons are active with or without capillary control. The options include Auto, which is the default setting, and Fixed. When Auto is selected, enter the value for the Leak Limit. The Fixed option allows you to enter the split flow offset directly.
Page 262 Using the Tools Menu Oventrack Mode Configuring the injector for Oventrack mode, means that the injector set point equals the oven set point plus 5 and the Column Length and Split Mode fields are not used. Also on the Active Method screen, the Program button next to the temperature field is deactivated as shown below.
Page 263 Clarus 600/680 GC User’s Guide Packed Injector 1. This example, shows that Pkd (a packed column injector) is selected as the Type on the Configuration screen. 2. Make your settings then touch the OK button. Then touch the Close button to exit configuration. POC- Programmable On Column Injector 1.
Page 264 Using the Tools Menu 2. Make your settings then touch the OK button. Then touch the Close button to exit configuration. Capillary – Split/Splitless Injector 1. This example, shows that Cap (a Capillary Split/Splitless injector) is selected as the Type on the Configuration screen. 2.
Page 265 Clarus 600/680 GC User’s Guide GSV – Gas Valve 1. This example, shows that GSV (a gas sampling valve) is selected as the Type on the Configuration screen. 2. Make your settings then touch the OK button. Then touch the Close button to exit configuration.
Page 266: Oven
Using the Tools Menu Oven Use the oven configuration screen to set up oven parameters. This example shows a temperature limit of 300 °C and an Equilibration rate of 1.0 mL/min. Calibration When the Calibration Offset field is selected it turns black. The default value is 0.
Page 267 Clarus 600/680 GC User’s Guide Soft Cooling Soft-cooling is a technique whereby, the cooling rate of the GC oven is initially limited by throttling the intake of the ambient (cold) air used to cool the oven. This is done by limiting the rate of cooling. Press the Soft Cooling button to display the Soft Cooling screen.
Page 268: Detectors
Using the Tools Menu Detectors FID Disabled When you touch the OK button, the system launches a status query to the PPC connect module to ascertain whether a PPC flow module has been assigned to the FID. If no flow module has been assigned, a dialog box appears. If No is selected, the dialog box closes.
Page 269 Clarus 600/680 GC User’s Guide When the PPC gas source is defined, touch the OK button to validate the settings and the FID detector configuration screen appears. Touch the OK button to close this screen then touch the pneumatics button 6-21...
Page 270 Using the Tools Menu Touch the PPC Connect button, touch OK to clear the caution screen, then touch the button for the PPC device you want to connect. In this example the FID. Select the Det Flow or None for Air and Hydrogen and touch OK. 6-22...
Page 271 Clarus 600/680 GC User’s Guide The following series of screens show the configuration screen for each detector. 6-23...
Page 272 Using the Tools Menu 6-24...
Page 273 Clarus 600/680 GC User’s Guide Output Configured 6-25...
Page 274: Run/Autosampler
Using the Tools Menu External Configuration If an external amplifier is installed a screen similar to the following appears: Run/AutoSampler 6-26...
Page 275 Clarus 600/680 GC User’s Guide Pre-wash is number of times the syringe is filled with the sample and emptied to a waste vial before a sample is acquired for injection. The default is 2. Permissible entries are 0 to 15. Pump is the number of times the syringe is filled with the sample before it is acquired for injection.
Page 276: Setup
Using the Tools Menu Setup The Key Clicks check box is selected by default. The Enable Password check box is deselected by default. If the check box is enabled, the default password is “Clarus.” Touch the Set button to display the password dialog box. 6-28...
Page 277 Clarus 600/680 GC User’s Guide Touch the New field. The alphanumeric keypad appears for you to enter the password. Passwords are limited to eight characters and are case sensitive. Enter the password and touch OK, or touch the x (close symbol) or Cancel to close the keypad and continue setup.
Page 278 Using the Tools Menu Use the up and down arrow or keypad buttons to increment the brightness values up or down. The settings take effect immediately. Date/Time Set 1. Touch the Date/Time button to display the Time and Date screen. 2.
Page 279 Clarus 600/680 GC User’s Guide Startup 1. Touch the Startup button to display the Startup screen. 2. Select the Method field, then using the arrow button select your desired method. 3. To set the Date and Time, highlight the field, then use the up and down arrow or keypad buttons to enter the values.
Page 280 Using the Tools Menu Sleep 1. Touch the Sleep button to display the Sleep screen. 2. Select the Method field then using the arrow button select your desired method. This now enables the displayed fields for edit. Value range is 6-999. 3.
Page 281: Pneumatics
Clarus 600/680 GC User’s Guide Pneumatics The parameter tables show the connection between the values shown on the screen and the underlying parameter interface that communicates to the GC. The dependency column summarizes major issues such as if a parameter is not available or hidden when PPC is not fitted.
Page 282 Using the Tools Menu PPC Configure 6-34...
Page 283: Connecting The Ppc Modules
Clarus 600/680 GC User’s Guide Connecting the PPC Modules The Clarus GC PPC modules have been properly installed and configured at the factory for your specific combination of injectors and detectors. The configuration information is stored in a reserved area of the battery-backed memory; however, if the memory lost the PPC module connect configuration or if you installed a new PPC module by purchasing an add-on kit, you must follow the procedure(s) listed in this section.
Page 284 Using the Tools Menu A flow or pressure module can be connected to positions 1 – 8. Split vent modules or pressure modules can only connect to positions 9 – 12. The PPC modules for injectors 1 and 2 carrier gas connections are connected to sockets 1 (J10) and 2 (J11), respectively, on the PPC board.
Page 285 Clarus 600/680 GC User’s Guide PPC Control Board PPC Control Board (Note: Disconnect the grounding wire inside panel to remove this right-side panel.) Phillips Screws (3) Right-Side Panel Figure 6-1 The PPC board installed in the Clarus GC. Your Clarus GC has been properly configured (connected) at the factory. However, you can check the configuration to become familiar with the procedure in the event that you need to reconfigure (reconnect).
Page 286 Using the Tools Menu For example, if a capillary injector is installed (split/splitless (CAP) or programmed split/splitless (PSS)), then Split is configured to notify the Clarus GC software that a capillary PPC module is installed. If a packed injector (Pkd) or programmed on-column (POC) injector is installed, Flow is configured to notify the software that a PPC flow module is installed.
Page 287 Clarus 600/680 GC User’s Guide The screen includes icon buttons to identify the logical PPC devices. The displayed carrier icons are taken from the currently configured injector for the corresponding channel. The detector icons are taken from the currently configured detectors. In the above screen Carrier A and B buttons show the PSS injector icon and the packed column injector icon respectively.
Page 288 Using the Tools Menu Touching the Carrier A icon displays the following dialog box: Since the PPC has yet to be configured the primary module is undefined and the secondary module entry is disabled. 6-40...
Page 289 Clarus 600/680 GC User’s Guide The primary entry is expected to be the module function. The following screen shows the full potential range available for the primary module function. The available range of functions is calculated by combining the set of potential functions from each of the uncommitted positions with the valid set of functions for this logical position.
Page 290 Using the Tools Menu The secondary module is now enabled. This will only be the case if the primary module is set to Carrier Flow or Split Control. The following screen shows that the second module can be configured as either Pressure readout or Split control under these conditions.
Page 291 Clarus 600/680 GC User’s Guide In this case the secondary module is left unconfigured (None). Touch OK to close the dialog box and implement the settings. Touch the Carrier B button on the Connect PPC Device screen to display the associated settings.
Page 292 Using the Tools Menu Press OK to close the dialog box and implement the changes. The Connect PPC Device screen appears. Dialog: Define Detector If Detector A is selected on the Connect PPC Device the dialog shown below pops up. Since the PPC has yet to be configured the primary module is undefined and the secondary module entry is disabled.
Page 293 Clarus 600/680 GC User’s Guide Note that the dialog title bar contains the detector name and that the primary and secondary function boxes are now labeled with the default gases for this type of detector. For a detector that only requires a single gas – ECD, PID, and External - the secondary module line is hidden.
Page 294 Using the Tools Menu Press OK to apply these changes. Define Aux Touch Aux 1 to display the dialog box. In the example shown, in the following screen capture on the left, since all of the available modules have been assigned no options are available.
Page 295 Clarus 600/680 GC User’s Guide For each function, position pair the same basic calculation is used to identify what modules are available and what locations are available once the module type has been selected. To identify the types of module available, first identify the set of available locations that contain one of the acceptable set of modules for this logical position.
Page 296: Reference Settings
Using the Tools Menu Reference Settings Relays The Relay settings are accessed from the Tools Menu System option screen. Use the drop down screen to set the type of valve. 6-48...
Page 297: Zeroing And Calibrating The Ppc Modules
Clarus 600/680 GC User’s Guide Zeroing and Calibrating the PPC Modules The Clarus GC gas modules have been calibrated at the factory and are ready to use. For good laboratory practices and your own internal validation protocol, you may wish to recalibrate at installation with your own flow measuring device. All carrier gas modules have been calibrated at the factory with helium.
Page 298 Using the Tools Menu Table 6-2. Injector/Detector and Corresponding PPC Module Gas Function Injector/Detector PPC Module Gas Function Packed Column and POC Injector Carrier Gas Capillary and PSS Injector Carrier Gas and split flow FID, NPD, FPD Both air and hydrogen gases Makeup Gas Reference Gas Makeup Gas...
Page 299 Clarus 600/680 GC User’s Guide To zero the carrier and detector gases: 1. From the PPC screen touch the PPC Configure button. To proceed, touch OK on the Caution message. 2. Select the channel you need (in this example Channel A tab is selected). Touch the Zero button.
Page 300 ± is still outside the range of 3 psi, contact your local PerkinElmer Service Engineer. The module identifier 1A is defined as follows: The number (1 – 12) indicates the specific PPC module. The letter A or B indicates the pressure transducer within that module. The flow...
Page 301: Setting The Reference Temperature And Pressure
Clarus 600/680 GC User’s Guide Turn on the carrier gas and allow at least one minute for the line pressure to stabilize and purge the lines before CAUTION selecting Calibrate from the display. Setting the Reference Temperature and Pressure The reference temperature and pressure values are set at the factory. We recommend leaving these parameters set to the factory (default) values (Temp °...
Page 302: Calibrating The Carrier Gas Modules
Using the Tools Menu 2. In PPC Reference Conditions screen add the reference temperature and pressure using the plus minus buttons. Touch OK when completed. Calibrating the Carrier Gas Modules If you are performing this calibration procedure and you do not have a column connected to the detector, you must plug the CAUTION detector fitting in the oven with an Swagelok 1/8-inch cap before...
Page 303 Clarus 600/680 GC User’s Guide To obtain the correct results, before you begin to calibrate you CAUTION must first Zero the Gas Modules. 1. From the PPC screen touch the PPC Configure button. Touch OK on the Caution message. 2. Select the channel you need (in this example Channel A tab is selected). Touch the Calibrate button.
Page 304 Using the Tools Menu 3. In the Calibrate screen use drop down menu to select the proper carrier gas and use the plus minus buttons to input the other values needed. In this example, the injector is a capillary split/splitless and the restrictor installed is a number 6.
Page 305: Calibrating The Detector Gas Modules
Clarus 600/680 GC User’s Guide The Set value displayed on the screen is 60% of the flow range available at the current gas supply pressure. The value displayed is from a lookup table based on the restrictor installed, the type of carrier gas, the ambient temperature, and the gas supply pressure.
Page 306 Using the Tools Menu The TCD and PID flow module for reference gas is calibrated with helium at the factory. You must recalibrate the TCD and PID flow CAUTION module if you are using a reference gas other than helium. The ECD flow module for make-up gas is calibrated with nitrogen at the factory.
Page 307 Clarus 600/680 GC User’s Guide 4. Select Detector tab. Touch the Calibrate button. Select OK. 5. In the Calibrate screen use drop down menu to select the proper carrier gas and use the plus minus buttons to input the other values needed. Remember only touch the fields that need to be changed.
Page 308: Calibrating The Oven Temperature
Using the Tools Menu Calibrating the Oven Temperature The Clarus GC oven temperature is controlled by a sophisticated software routine that permits adjustment of the actual oven temperature inside the oven up or ° down within a ±10 C window. This calibration utility is intended for applications which require precisely matching oven temperatures across several Clarus GCs, such as the determination of retention indices.
Page 309: Place The Thermometer Probe In The Oven
Clarus 600/680 GC User’s Guide Place the Thermometer Probe in the Oven The thermometer probe must be placed as close as possible to the same position in each GC oven to be calibrated. Access to the CAUTION oven is provided on the left-side oven wall. Turn off the power and allow the oven to cool.
Page 310: Equilibrate The Oven Temperature
Using the Tools Menu 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. Figure 6-6 Holes on the left side of the oven exterior. Equilibrate the Oven Temperature 1.
Page 311 Clarus 600/680 GC User’s Guide 2. Touch the Tools button and select Configuration in the drop down menu. 3. Press on the Oven button on the Configuration screen. 6-63...
Page 312 Using the Tools Menu ° 4. From the window, shown below, set the oven temperature of 100 C or use another temperature if desired by using the plus and minus buttons. 5. Single Point is the default setting. When the Single Point Calibration radio button is selected, the Offset field is active and the GC Tune drop 6-64...
Page 313: Enter The Required Offset Value
Clarus 600/680 GC User’s Guide down field is inactive. (GC Tune is only available if it is downloaded. A successful tune must be performed in order for GC tune to be enabled. Only those channels for which a valid tune exists will be available on the drop down list.
Page 314: Utilities
Using the Tools Menu Utilities 1. To reach the Utilities screen of the Tools Menu go to the System Status screen and select Utilities from the tools menu. 2. Touch the following icon on the Utilities screen to access the Column Flow Calculator, the Column Length Calculator, the Background Compensation, Stopwatch, or Program (Max Oven Program Rates).
Page 315: Column Flow Calculator
Clarus 600/680 GC User’s Guide Column Flow Calculator The capillary column gas flow rate “calculator” allows you to automatically calculate the correct gas flow rate. 1. Touch the Column Flow Calc icon button 2. The following screen appears. 6-67...
Page 316 Using the Tools Menu 3. Input the column length, column diameter, column temperature, carrier gas name, and outlet pressure. 4. One of the following is selected: Inlet Pressure, Flow Rate, and Velocity/t0. A value is entered into the selected field and results are calculated and inserted into the two unselected fields.
Page 317 Clarus 600/680 GC User’s Guide Column Flow Calc Main Screen Length This field is normally entered in meters (1 to 1000 in 1m increments). The calculator should also support techniques such as PreVent and heart-cutting etc. and so shorter columns/tubes should be supported. If the value scrolls below 1m, then the units should change to mm (1 to 1000 in 1mm increments).
Page 318 Using the Tools Menu Name The name of the carrier gas is selected in order to apply the correct viscosity coefficients and suggested column carrier gas velocities as shown in the Table. Screen Name η Suggested ,Pa.s Velocity, cm/s Helium 0.000018662 0.646 20 to 40...
Page 319: Split Flow Calculations Screen
Clarus 600/680 GC User’s Guide The carrier gas flow rate is in units of mL/min (1 to 100mL/min in 0.1mL/min increments). There is no default as this field will be already filled by a previous calculation result. Velocity This is a selectable field and, if selected, the t0 field is also enabled for input. The Inlet Press and Flow fields are deselected and are display only.
Page 320 Using the Tools Menu Split flow ratio Value displayed to nearest integer. Dimensionless units. Split velocity ratio Note that the split dynamics occur at an elevated pressure, p and elevated temperature (injector temperature). The flow rates, Fa and Fs are at ambient pressure and temperature.
Page 321: Column Length Calculator
Clarus 600/680 GC User’s Guide Column Length Calculator 1. The Column Length Calculator displays the correct Length of tubing that should be inserted into an injector or detector as measured from the back of the nut. Touch the Column Length Calc icon button 2.
Page 322: Background Compensation
Using the Tools Menu Background Compensation Background compensation is a routine that automatically subtracts a stored baseline profile from the signal generated during a GC run. 1. Touch the Background Compensation icon button 2. The following screen appears. Background compensation is a routine that automatically subtracts a stored baseline profile from the signal generated during a GC run.
Page 323 Clarus 600/680 GC User’s Guide Type, Method, and Start are always enabled, so that a bakeout can be performed with a mass spec or other system with zero detectors. Before background compensation can be applied to a detector output signal, the baseline profile must be calibrated.
Page 324: Stopwatch
Using the Tools Menu Stopwatch The Stopwatch computes the flow rate that corresponds to the entered volume flowing during the timed interval. The start button resets the timer to zero and starts timing. While timing, the start button caption changes to Stop. 3.
Page 325: Program (Max Oven Program Rates)
Clarus 600/680 GC User’s Guide Program (Max Oven Program Rates) 1. Touch the Program icon button 2. The following screen appears. 6-77...
Page 326: Release
Using the Tools Menu Release… To access Release, from the System Status screen, touch Tools menu and press the Release. The following screen will appear select either Yes or No. If you select Yes the instrument will be released from its external control. If you select No the screen will close.
Page 327: Logout
Clarus 600/680 GC User’s Guide Logout… To access Logout, from the System Status screen, touch Tools menu and press the Logout. Touching Logout displays the splash screen for the Clarus 600 or Clarus 680. 6-79...
Page 328: About
Using the Tools Menu About Touch About to display version information. To access About, from the System Status screen, touch Tools menu and then touch About. 6-80...
Page 329: Setting Up A Typical Analysis
Setting up a Typical Analysis...
Page 330 Setting up a Typical Analysis...
Page 331 Clarus 600/680 GC User’s Guide This chapter gives you a brief overview on how to run a typical analysis on your Clarus GC. For more detailed information on the different screens and parameters discussed in this chapter see the earlier chapters in this guide on the Active Method, Method Editor and Tools Menu.
Page 332: System Status Screen
Setting up a Typical Analysis System Status Screen Everything starts from the system status screen. 1. Touch the Oven button to display the oven information. 2. The oven information is now visible. To program the oven temperatures touch the temperature field and it will turn black (highlighted). Then use the up and down arrow or keypad buttons to set to the required temperature for your application.
Page 333 Clarus 600/680 GC User’s Guide...
Page 334: Injector Settings
Setting up a Typical Analysis Injector Settings Packed Column (PKD) Injector 1. After entering the oven settings, touch Injector B (the Pkd tab) and then touch the Temp field. The field is highlighted to indicate that it is selected. Use the up and down arrow or keypad buttons to enter the proper initial temperature for your application.
Page 335 Clarus 600/680 GC User’s Guide 3. Touch the Initial psi field to select it. Next use the up and down arrow or keypad buttons to enter the proper carrier gas pressure for your application. 4. When done touch the Close button and the following screen appears:...
Page 336: Programmed Split/Splitless (Pss) Injector
Setting up a Typical Analysis Programmed Split/Splitless (PSS) Injector 1. To select Injector A touch the icon in the active method screen or the PSS button on the System Status screen. Once you touch the button the following screen appears.
Page 337 Clarus 600/680 GC User’s Guide 3. Touch the Temperature Program button (to the right of the temperature field. This displays the Injector Temperature Program screen. Here you can set an injector temperature program for your analysis. The following example shows an analysis that uses the same injector temperature (250 °C) throughout the analysis.
Page 338 Setting up a Typical Analysis 6. Select the Initial psi field. Use the up and down arrow or keypad buttons to set the carrier gas pressure to the required pressure for your application. 7. Repeat the same procedure for the time and rate. As shown in the example, this analysis has been set to have an initial temperature of 255 ºC and it is held at this temperature for 60 minutes then going up 2 degrees.
Page 339: Detector Settings
Clarus 600/680 GC User’s Guide Detector Settings Flame Ionization Detector (FID) 1. Touch the FID button on the Status Screen. 2. To program the temperature in the FID tab touch the Temperature field and it will turn black. Then use the up and down arrow or keypad buttons to set to the required temperature for your application.
Page 340 Setting up a Typical Analysis 5. To autozero the detector baseline touch the AutoZero field for the check off to appear (in this example AutoZero is used). 6. The Gas flows, Output, Offset, Filter, and Flameout are shown above as reference fields and they cannot be changed in this screen.
Page 341 Clarus 600/680 GC User’s Guide The Configuration screen appears: 8. As shown in the screens below the Configuration screen allows you to modify the Filter, Flameout, Gas Flows and Output fields as your application requires. Once you have modified the Configuration screen touch OK and the new values will now be visible on the FID screen.
Page 342 Setting up a Typical Analysis 8. If timed events have to be added or modified in the Active Method touch the Events tab to get to this screen. The Events tab accesses the timed events table and buttons, valves, and Aux gas controls. Timed events may be added and removed while the GC is running.
Page 343 Clarus 600/680 GC User’s Guide 9. Touch the Add button to add a timed event to the run. In the Event field select the type of event from the drop down menu. Use the up down arrows to input the amount of time for this event in the time field. In the value field use the drop down menu to insert the correct value.
Page 344: Detector
Setting up a Typical Analysis Detector Thermal Conductivity Detector (TCD) 1. Touch the TCD button on the Status Screen to display the TCD tab. 2. To program the temperature in the TCD tab touch the Temperature field and it will go black. Then use the up and down arrow or keypad buttons to get to the required temperature for your application.
Page 345 Clarus 600/680 GC User’s Guide 4. If you require the heater on for your analysis just touch the Heater button and it will toggle to heater on. 5. To have the detector autozero the baseline to a fixed amount touch the AutoZero field for the check off to appear (in this example AutoZero will not be used, it is not checked off).
Page 346 Setting up a Typical Analysis 7. If the gas flows, output, offset and filter have to be changed touch the Tools button and touch Configuration from the drop down menu. The Configuration screen appears: 7-18...
Page 347 Clarus 600/680 GC User’s Guide 8. Touch the TCD button and as shown in the screens below the Configuration screen will allow you to modify the gas flows, output, offset and filter fields as your application requires. 9. Once you have modified the Configuration screen touch OK and the new values will now be visible on the TCD tab screen.
Page 348 Setting up a Typical Analysis 11. Touch the Add button to add a timed event to the run. In the Event field select the type of event from the drop down menu. Use the up down arrows to input the amount of time for this event in the time field. In the value field use the drop down menu to insert the correct value.
Page 349 Clarus 600/680 GC User’s Guide 13. Once all the fields have been set as required by your application for the TCD, touch the Clarus GC icon on the screen. 7-21...
Page 350: Autosampler
Setting up a Typical Analysis Autosampler 1. Touch the Run button to display the Autosampler setting screen. 2. The Autsosampler screen allows you to select the method from the drop down window. Once you select the method you want to use for your application, the injection count down will begin.
Page 351 Clarus 600/680 GC User’s Guide 3. If you need to modify the method for running the autosampler or enable the autosampler touch the Tools button and from the drop down menu touch Configuration. 4. Touch the Run button on the Configuration screen. The following screen displays.
Page 352 Setting up a Typical Analysis 5. In the Autosampler Configuration screen check off the Enable Autosampler field by touching it. If your application requires Recycling and/or Auto Resume touch the field to check off. Use the drop down window to set the volume and mode type. For the Syringe wash use the plus/minus buttons to modify the fields of Viscosity Control, Solvent Pre- wash, Pre-Inject, Post-Inject and Pump.
Page 353 Clarus 600/680 GC User’s Guide 7. On the Signal screen you will be able to observe the peaks as they are coming out during the analysis. If at any time you need to stop the analysis touch the Stop button. 7-25...
Page 354 Setting up a Typical Analysis 7-26...
Page 355: Index
Index...
Page 357 Clarus 600/680 GC User’s Guide Cmptr, abbreviation, 1-6 Column Flow Calculator, 6-67 Abbreviations, screen, 1-6 Column Length Calculator, 6-73 About This Manual, 1-3 Configuration, 6-10 Active Method Configuring editing, 3-4 injectors, 6-10 parameters Connect, PPC module editing, 3-4 socket descriptions, 6-35 Attenuating Conventions detector signal, 4-87, 4-90...
Page 358 Index abbreviation, 1-6 Isothermal temperature program auto-ignition, 4-9 setting up, 3-8 overview, 4-5 setting up PPC, 4-6 File Menu, 5-9 kPa, abbreviation, 1-6 Flow Programming, 1-11 Flowmeter attaching to an ECD, 4-24 Labels Warning Signs, 1-5 abbreviation, 1-6 Logout, 6-79 cross-sectional view, 4-56 igniting the flame, 4-69 overview, 4-56...
Page 359 Clarus 600/680 GC User’s Guide Oven temperature program Reference Temperature setting up, 3-6 setting, 6-53 setting up a multi-ramp, 3-11 Release, 6-78 setting up a one-ramp, 3-10, 3-19 Rerouting setting up isothermal, 3-8 detector output, 4-83 Overview ECD, 2-37, 4-20 FID, 4-5 Screen FPD, 4-56...
Page 360 Index setting up PPC, 4-31 manual injection, 2-9 using with autosampler, 3-63, 4-35 oven button, 2-15 Temperature program run button, 2-8 isothermal signal button, 2-11 setting up, 3-8 signal display and scaling, 2-12 setting up a multi-ramp, 3-11 signal plot, 2-12 setting up a one-ramp, 3-10, 3-19 zero display button, 2-13 Temperature Programming, 1-12...
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Page 362 PerkinElmer Life and Analytical Sciences 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.

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Clarus 600 gc

PerkinElmer CLARUS 680 GC User Manual

Introduction

Touch Screen Navigation

Using the Active Method

Setting up the Detectors

Using the Method Editor

Using the Tools Menu

Setting up a Typical Analysis

Index

Quick Links

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Summary of Contents for PerkinElmer CLARUS 680 GC