PerkinElmer CLARUS 600 GC User Manual Download Page 156

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Setting Up the Detectors

4-20

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

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ECD Overview

The Electron Capture Detector (ECD) is the most sensitive detector available for the

analysis of electrophilic compounds such as chlorinated hydrocarbons and pesticide

residues. It is concentration-sensitive and nondestructive.
The ECD cell contains a foil in a cylinder through which the carrier gas flows. The

coating of the foil's inner surface contains the radioactive isotope Nickel-63 and has

a nominal sensitivity of 15 mCi. To optimize detector response, make-up gas is

combined with column effluent.
Beta particles emitted from the isotope ionize the carrier gas. The resultant ions and

electrons travel to the collector anode assembly under the influence of a pulsed

polarizing voltage applied between the source and the collector. The pulse frequency

is varied to maintain a constant average current. The presence of an electron

absorbing species in the detector decreases the current as the absorbed electrons

form ions, which travel more slowly than electrons. The pulse frequency of the

Summary of Contents for CLARUS 600 GC

Page 1: ...CLARUS 600 680 GC User s Guide GAS CHROMATOGRAPHY ...

Page 2: ......

Page 3: ...Clarus 600 680 GC User s Guide ...

Page 4: ...o the implied warranties of merchantability and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may ...

Page 5: ...lossary of Chromatographic Terms 1 10 Touch Screen Navigation 2 1 Chapter Overview 2 3 Touch Screen 2 4 Tabs 2 6 Non Configured Devices 2 6 Non installed Devices 2 7 Run Button 2 8 Stop Menu 2 11 Signal Button 2 11 Heated Zones 2 13 Navigation Bar 2 16 Injectors 2 17 Program Buttons 2 18 Display Text 2 18 PSS 2 18 Packed Pkd 2 24 POC 2 28 Capillary Cap Injector 2 29 Oven 2 30 Aux Zone 2 31 Detecto...

Page 6: ...ng Mode 3 17 Inlet Temperature Programming Mode 3 18 Setting Up a One Ramp Injector Program 3 19 Viewing Setting Carrier Gas Pressure Flow Velocity 3 21 Setting Carrier Gas Pressure 3 23 Setting Carrier Gas Flow using PPC 3 25 Viewing Setting Carrier Gas Velocity 3 27 Setting the Septum Purge Mode and Offset 3 29 Setting Up Valves 3 37 Setting the Split Mode Using PPC 3 37 Set up the Splitless Mod...

Page 7: ... Setting Up a NPD 4 45 NPD Bead Activation Procedure 4 48 Setting up an FPD 4 55 FPD Overview 4 55 Setting Up the FPD 4 57 FPD Setup Summary 4 57 Configure the Linearizer and Signal Filter 4 57 Set the FPD Temperature 4 61 Detector Temperatures 4 72 Setting the Range 4 74 Setting the FID PID or NPD Range 4 74 Changing the FID PID or NPD Range During a Run 4 75 Setting the TCD Current Filament Curr...

Page 8: ...ules 6 49 Zeroing the PPC Gas Modules 6 49 Setting the Reference Temperature and Pressure 6 53 Calibrating the Carrier Gas Modules 6 54 Calibrating the Detector Gas Modules 6 57 Calibrating the Oven Temperature 6 60 Calibrate the Reference Thermometer 6 60 Place the Thermometer Probe in the Oven 6 61 Equilibrate the Oven Temperature 6 62 Enter the Required Offset Value 6 65 Remove the Thermometer ...

Page 9: ...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 7 16 Autosampler 7 22 Index ...

Page 10: ...viii ...

Page 11: ...Introduction 1 ...

Page 12: ...Introduction 1 2 ...

Page 13: ...ing options using the tools menus etc Chapter 3 Active Method This chapter contains step by step explanation of the active method Detailed information on setting up the autosampler is contained in this chapter Chapter 4 Setting Up the Detectors This chapter contains detailed information on setting up the detectors Chapter 5 Using the Method Editor This chapter describes how to modify save and use ...

Page 14: ...d to highlight special circumstances and warnings NOTE A note indicates additional significant information that is provided with some procedures CAUTION We use the term CAUTION to inform you about situations that could result in serious damage to the instrument or other equipment Details about these circumstances are in a box like this one WARNING We use the term WARNING to inform you about situat...

Page 15: ...ent 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: ...Flame Photometric Detector Gen generate Inj Vial injections per vial Int integrator kPa kilopascals NPD Nitrogen Phosphorus Detector PID Photoionization Detector Pkd packed injector POC Programmed On Column Injector PPC programmed pneumatic control Pre of preinjection syringe washes Psi or psig pounds per square inch gauge PSS Programmed Split Splitless Capillary Injector TCD Thermal Conductivity ...

Page 17: ...s with a solvent Post Inject The number of post injection syringe washes with a solvent Pumps The number of times the syringe draws up sample and evacuates it before acquiring the volume This is done to eliminate bubbles Mode The style of injection Fast Fast speed of the syringe during sample injection This is used to eliminate discrimination in the needle Normal Normal speed of the syringe during...

Page 18: ...ally limited by controlling throttling the intake of the ambient cold air used to cool the oven Detector background The detector output signal when no components are being eluted Equilibration The delay time after the method set points have been reached before the system becomes READY Flameout Detects if the flame is on to prevent injection into a nonfunctioning system and subsequent loss of sampl...

Page 19: ...dicates that all method parameters have reached their set points and that you can start your analysis Run The time from sample injection to the end of the oven temperature program Sleep mode The GC can be set to a predefined method for gas savings Temperature program PPC version only A program that specifies the rate of oven temperature increase from one plateau to the next and the time the oven t...

Page 20: ...e signal from the detector usually resulting from column temperature and or gas flow changes Blank run A run without the sample being injected Bleed The evaporation of the stationary phase from a column Capillary column wall coated open tubular column A small internal diameter column whose inside wall is coated with a liquid phase Carrier gas The mobile phase of the separation system An inert gas ...

Page 21: ... Usually defined as any signal that is as great as two times the noise level Also referred to as Minimal Detectable Quantity MDQ Mobile phase The gas which carries the solute sample along and over the column material This carrier gas is inert and usually helium nitrogen or hydrogen Noise Background signal fluctuations arising from a detector response This response is the result of the column insta...

Page 22: ...as syringes are available Tailing When a peak is not symmetrical or Gaussian shaped but the back end is broadened it is said to be tailing Temperature programming A technique commonly used to increase the rate of elution of the components After the sample is injected into the oven at a specific temperature the temperature program increases the oven temperature to the prescribed temperature at a de...

Page 23: ...Touch Screen Navigation 2 ...

Page 24: ...Touch Screen Navigation 2 2 ...

Page 25: ...use a stylus or you may like to touch the active areas of the touch screen Do not use sharp pointed objects A light touch is all that is needed You do not need to press forcefully on an active area Please note that when you touch an active area various processes are started in the instrument Some of these processes may take several seconds Be patient and wait for the process to complete before tou...

Page 26: ...t or stop actions or to display a dialog Option Buttons that you select drop down menu options from a list Boxes that you use to switch functions on or off and Radio Buttons that allow you to choose one of two or more options 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 M...

Page 27: ...e the ready not ready status A red blinking light indicates not ready and a steady green light indicates ready status Click here to view the Signal If a method is not running the screen will display a baseline The Title bar displays the name of the active method The Run button provides access to the Autosampler and Manual Inject settings Channel B appears above Channel A to emulate the order on to...

Page 28: ...ens 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: ...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 Touching the button prompts the following dialog box ...

Page 30: ...he Autosampler and Manual inject screens you must initiate a run from these screens However when the system is running the Stop button appears on all screens allowing you to Stop the run from anywhere in the application If the system is Paused the Resume button appears on all screens Autosampler Enabled When an Autosampler is enabled the Run button defaults to that screen The following screens sho...

Page 31: ...ed by default You can stop the countdown by pressing the Cancel button Manual Injection If no Autosampler is installed or configured the Run button displays the Manual injection screen The enable check box is selected by default Touching the start button initiates the countdown starting from 5 seconds When the countdown reaches 0 an audible beep prompts you to inject the sample The GC will then st...

Page 32: ...Touch Screen Navigation 2 10 Enabled Disabled When the Stop button is pressed an abbreviated Stop Menu appears ...

Page 33: ...Menu dialog and returns you to the Active Method Signal Button The Signal icon displays the graphic signal for the active method If the system is not running a baseline appears on the graph The Signal screen displays the selected detector signal over a fixed time period 2 minutes with you selecting the scaling factor using the up and down arrow buttons The raw signal is unprocessed and can appear ...

Page 34: ...Carrier Gas Pressure Using Manual Pneumatics AutoZero Button Autozeroes the selected detector Signal Plot The plot graph displays the signal from the selected detector in real time The window is 2 minutes wide The signal commences at the y axis and is plotted out to start 1 75 minutes The signal then scrolls back so the start is now 1 minute the last 0 75 minutes are displayed from there and the s...

Page 35: ...s well as a text label Heated zone buttons display a status light indicator in the lower right corner The indicator lights for individual zones follow the same convention as the system status light that appears in the Status bar Steady green indicates that the zone is ready A red blinking light indicates that the zone is not ready Injector and Detector Buttons The screen is organized with Channel ...

Page 36: ...ss 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 The active method screens include navigation icons on the title bar that allow you to access the same elements available from the Status screen ...

Page 37: ...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 The oven program screen displays the same tabs and navigation icons as the injector and detector active method screens Aux Zone Buttons If a heated Aux Zone is configured pressing the Aux button displays a screen that follows the same format as the injector ...

Page 38: ...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 Status Screen Active Method Navigation Bar ...

Page 39: ...ify the main components of an Active Method injector screen This example shows a screen for a PSS injector with PPC Injector Tab for Channel A PSSI selected Active Method Name Temp Ready Not Ready Light Carrier Gas Ready NotReady Light Carrier gas pressure flow or velocity Split Flow Ready Not Ready Split Flow actual value System Status Oven Program Step Time Date Display Split flow set value Carr...

Page 40: ...e setting the program button is grayed out In most cases fields with a deactivated program button are editable allowing you to modify the setting directly Display Text The text displayed next to the set point entry fields show the current values If the injector configuration allows you to display the value in other units such as velocity or flow the display text shows the actual values for all of ...

Page 41: ...ctor inlet temperature programs by selecting the program button on the active method screen is active Mode Description Inlet In the inlet programmed mode the injector is first heated to the injector temperature that is entered in the method The injector then follows the injector temperature program that you defined Oven The oven programmed mode is the default mode of operation In this mode the inj...

Page 42: ... actual temperature To modify the temperature program during a run touch the program button You can modify the temperature time or rate However if the program is currently in that step the changes will be ignored Isothermal Program If the program is isothermal the program button is grayed out and the top level field is active Changes entered in the field take effect immediately ...

Page 43: ...r 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 2 22 Touching the Program button next to the field displays the associated Carrier Pressure Program screen for the entry field value ...

Page 45: ...PC 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 The inlet system flow controller delivers the Total flow rate not the setpoint flow rate ...

Page 46: ...xed 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 1 Select Configuration from the Tools menu 2 Touch the Pneumatics button ...

Page 47: ...Clarus 600 680 GC User s Guide 2 25 3 Touch the PPC Connect button 4 Touch the OK button 5 Touch Carrier B to Configure your Packed column injector for PPC ...

Page 48: ...2 26 6 Select Pres Read from the drop down menu Then touch the OK button 7 Touch Close to close the Connect PPC Device screen 8 Touch OK on the Configuration PPC screen 9 Touch the B Injector button on the Configuration screen ...

Page 49: ...ure Injector B screen appears 11 Select Pressure or Flow from the 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: ... 28 POC 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 ...

Page 51: ...Clarus 600 680 GC User s Guide 2 29 Capillary Cap Injector 1 From the Configuration menu select Cap from the drop down list 2 Exit from Configuration and display the active method screen ...

Page 52: ...er of steps in the current program are deactivated In the example below step 2 is selected As soon as the user touches the OK button the change is implemented The graph in the capture on the right shows the immediate temperature rise and the departure from the program Graph and status bar show the oven is ready to run a program Touching the Go to button displays the Go to Temp dialog box to select...

Page 53: ...00 680 GC User s Guide 2 31 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 ...

Page 54: ...nfiguration settings The following screen shows the major components that apply to all detector screens The subsections that describe each detector type includes details about settings that are unique to that particular detector FID The FID Flame Ionization Detector uses a hydrogen and air flame to generate ions from the combustion of an organic compound The detector collects and measures the conc...

Page 55: ...tered baseline threshold level in mV If the threshold level is exceeded the flame is considered lit otherwise the Clarus GC detects that the flame is out and auto ignite automatically lights the flame before the start of a run 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...

Page 56: ... start of each run just prior to the instrument becoming READY However the manual flame ignition process performed by touching the Ignite button can be initiated at any time Auto ignite proceeds in the following sequence 1 When auto ignite begins the Clarus GC equilibrates 2 Once the two minutes of equilibration expire PRE RUN begins and the AutoSystem detects that the flame is not lit and indicat...

Page 57: ...larus 600 680 GC User s Guide 2 35 Configuration Settings The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method Configuration Screen ...

Page 58: ...onnected in a bridge circuit two in each channel The TCD is set up with the same amount of carrier gas flowing through both channels The presence of a sample component in the carrier gas flowing through the analytical channel changes the resistance of the filaments in that channel This unbalances the bridge and produces a signal proportional to the amount of sample The following screens show the A...

Page 59: ...tain a constant average current The presence of an electron absorbing species in the detector decreases the current as the absorbed electrons form ions which travel more slowly than electrons The pulse frequency of the polarizing supply is automatically controlled to maintain a constant current and is used to form the detector output signal The ECD works with nitrogen carrier or makeup gas or a ca...

Page 60: ...mer 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 The following screens show the Active Method screen and the corresponding settings in the Confi...

Page 61: ... 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 The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method Configuration Screen ...

Page 62: ...d the bead to produce a hydrogen plasma Stable intermediates are formed in the hydrogen plasma which then capture the electrons emitted from the bead to produce ions A polarizing field directs these ions to the collector electrode thereby creating a current which is amplified Sensitivity is affected primarily by the air flow and selectivity is affected primarily by the hydrogen flow The following ...

Page 63: ...o 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 The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method Configurat...

Page 64: ...ab 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 Delete button Always Clear button Always ...

Page 65: ...s automatically selected Up to 32 events can be specified The configured hardware determines which events are available Events that are not applicable should not be available The following table lists the available events The time range is 99 to 999 minutes Events occurring after the temperature program is complete are ignored Add The Add button displays settings that allow you to specify an event...

Page 66: ...ror 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 ...

Page 67: ...ar 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 ...

Page 68: ...Screen Navigation 2 46 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 ...

Page 69: ...timed event should have the same time as another timed event Time resolution is 0 01 minutes Timed Events may be entered and removed in any sequence Pressing the Clear button prompts a dialog box This action will clear the entire table Do you want to continue Yes No Timed Events are re ordered chronologically after each entry The capacity is 32 entries ...

Page 70: ...l 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 The current settings are changed via Timed Events Any settings may be changed during a run ...

Page 71: ...nd actual temperature To modify the temperature press the minus or plus button Touch OK to implement the value and close the dialog box Pneumatic Auxiliary Zones Up to four pneumatic zones can be set for PPC carrier gas control When one or more of the aux zones is configured the following button appears on the status screen The same button also appears on the Events screen Touching the button disp...

Page 72: ...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 ...

Page 73: ...Using the Active Method 3 ...

Page 74: ...Using the Active Method 3 2 ...

Page 75: ... operating parameters include the an oven temperature program injector temperature or injector temperature program detector temperature or detector temperature program carrier gas pressure set for pressure flow or velocity valve settings for example the operation of a gas sampling valve or split splitless operation of capillary column a timed events table and a variety of parameters for controllin...

Page 76: ...to perform you should now edit the Active Method to set your operating parameters Examples of how to perform the tasks listed below are described in the sections which follow You should of course substitute your values for ours Setting up oven temperature programs Setting injector temperatures programs PSS and POC Setting detector temperatures Viewing setting carrier gas pressure programs PPC View...

Page 77: ... before closing the oven door and elevating the oven temperature The Status screen icon buttons provide access to the active method parameters NOTE When you change an Active Method parameter the change goes into effect immediately For example if the system is READY and you change an injector temperature setpoint the status screen displays NOT READY until the new setpoint is reached ...

Page 78: ...e Oven program screen appears 3 Select a field by touching it and use the up and down arrow or keypad buttons to enter a temperature equilibration time and rate Enter a value of 0 in the Rate field to make that the last step You will then see the word END appear in the Rate field all the fields that follow are deactivated You must touch END and then touch the up arrow button to activate the next r...

Page 79: ...ms Longer equilibration times are recommended for initial oven temperatures of 50 C An equilibration time of 0 0 minutes can be used for isothermal methods Setting a Coolant Timeout Value The purpose of the coolant timeout value is to conserve coolant If you select a coolant timeout value when you configure the Clarus GC the coolant solenoid shuts off if a GC run is not started within this time pe...

Page 80: ...e cut in temperature range is 30 C 110 C We recommend that YOU NOTE THE AMBIENT TEMPERARTURE AND SET the cut in temperature 20 C above your current ambient temperature For example A room temperature of 20 C uses a default temperature of 40 C whereas a room temperature of 25 C uses a 45 C cut in temperature Examples for setting up isothermal 1 and 2 ramp programs follow NOTE Higher cut in temperatu...

Page 81: ...s for the Equilibration time Init specified in Oven Configuration screen and then becomes Ready For an isothermal run Init TIME 1 is equivalent to the total run time At the end of the time TIME 1 the system changes to Not Ready it equilibrates and then goes Ready To change the hold time Go to the Oven tab and enter a Time appropriate for your analysis for example 25 min NOTE Since a constant oven ...

Page 82: ...rease from the initial to the final oven temperature Init Rate 1 Final oven temperature Init 2 Isothermal time for the final temperature Init 2 Temperature increase of 0 C min which signifies the end of the RATE 2 step The following example shows how to convert an isothermal program into a one ramp program using the previous isothermal method oven temperature parameter as a starting point Paramete...

Page 83: ...ample are shown below Parameter Value Rate 2 4 C min Temp 3 100 C Time 3 5 min Rate 3 0 C min 1 From the oven tab enter a rate of 4 2 Enter a temperature of 100 3 Enter a time of 5 NOTE You can enter RATE 3 TEMP 4 and TIME 4 to set up a third ramp Holding an Oven Temperature While running a temperature program you can hold the oven temperature by setting it to the temperature of the unexecuted ste...

Page 84: ...he go to temp button to display the Go To Temp temperature screen 2 From this window touch the button for the temperature level that you want to hold Touch OK Modify the temperature on the Oven tab screen using the up and down arrow or keypad buttons When completed return to the system status screen ...

Page 85: ...perature 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 See the section on Timed Events ...

Page 86: ...ed and configured in position A front and a packed injector installed and configured in position B rear This section contains examples of how to Display injector temperature screens Change injector temperatures Turn injector heaters off Turn injector heaters on Set oven programming mode Set inlet programming mode Displaying Injector Temperature Screens From the System Status screen touch the injec...

Page 87: ...Clarus 600 680 User s Guide 3 15 The injector information displays ...

Page 88: ...ctor 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 2 Touch the Temp field and using the up and down arrow or keypad buttons increase the value to 255 ºC ...

Page 89: ...ows Parameter Value Temp 1 50 C Time 1 2 min Rate 1 5 C min Temp 2 240 C Time 2 10 min The initial injector temperature will be 55 C When the GC run begins the injector will hold this temperature for 2 minutes then it will ramp up to 245 C at 5 C min and hold for 10 min Figure 3 3 PSS oven mode temperature program NOTE Opening the oven door turns off the oven and the injector heater Also if you re...

Page 90: ...in the method The initial default values are Initial Temp 1 is 50 C Injection Time is 999 min and Inj Rate is 0 With non programmed injectors an entry of 0 turns the heated zone off With programmed injectors a temperature of 0 is possible Therefore when 0 is entered for the initial injector setpoint the following screen appears 1 From the selected injector tab screen make sure that the injector he...

Page 91: ... injector temperature Temp 2 Isothermal time for the final temperature Time 2 Temperature increase of 0 C min which signifies the end of the Rate 2 step The following example shows how to build a one ramp temperature program for your POC or PSS injector The parameter values used in the example are shown below Parameter Value Init Temp 60 C Init Time 0 min Init Rate 100 C min Inj Temp 2 250 C Inj T...

Page 92: ...to the System Status screen NOTE You can enter Rate 2 Temp 3 and Time 3 to set up a second ramp An entry of 999 for Rate 1 or 2 will cause the injector to ballistically heat up NOTE If the Injector Time is set with the default value of 999 the injector temperature will hold at the current temperature until the end of the oven program Otherwise the injector temperature will hold for the time you ha...

Page 93: ...d in PPC analysis Zero removes the flow controller from the GC method and sets the flow to 0 Flow enables the flow controller in the GC method and sets its initial flow to 30 of the nominal maximum flow rate according to the installed flow range element and carrier gas type The operator has the option to enter a different flow rate and enter a flow program When in the flow mode the PPC system also...

Page 94: ...er gas controller with a positive or negative ramp as required At the end of the GC oven program the carrier gas resets to the initial set point value in the method even if a carrier gas program is in progress The carrier gas also resets if the end of the carrier gas program occurs before the end of the oven program Carrier Gas Timed Events You can also use timed events to produce step changes in ...

Page 95: ...e on for pressure psi If the option for capillary control has been selected during configuration you can program the carrier gas according to one of three values pressure velocity or flow The carrier gas field on the injector tab screen displays the set point value The label below the field displays the current step The actual values for all the available configuration options are displayed to the...

Page 96: ... 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 CAUTION The ballistic mode of programming is not recommended Setting a program rate will be more reproducible 4 Touch Close to return to the injector screen ...

Page 97: ...s GC is configured with the PSS capillary mode on for flow If the option for capillary control has been selected during configuration you can program the carrier gas according to one of three values pressure velocity or flow The carrier gas field on the injector tab screen displays the set point value The label below the field displays the current step The actual values for all the available confi...

Page 98: ...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 A rate of 999 is a go to setting CAUTION The go to mode of programming is not recommended Setting a program rate will be more reproducible 4 Touch Close ...

Page 99: ...ured with the capillary mode on for velocity as shown by vel init displayed under the carrier gas field If the option for capillary control has been selected during configuration you can program the carrier gas according to one of three values pressure velocity or flow The Carrier Gas field on the injector tab screen displays the set point value The label below the field displays the current step ...

Page 100: ...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 A rate of 999 is a go to setting CAUTION The go to mode of programming is not recommended Setting a program rate will be more reproducible 4 Touch Close ...

Page 101: ...set 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 The Configure Injector screen appears ...

Page 102: ...am your capillary injector If you wish to program the Capillary control for more than just pressure skip to step 9 4 Under Flow Offset select either the Auto or Fixed The Auto mode is the preferred mode of operation If you want to shorten the overall run time at the expense of some area precision then use the Fixed mode ...

Page 103: ... value which is equal to the septum purge flow plus the column flow at the time of injection Since the system controls the total flow equal to the split vent plus septum purge plus column flow the septum purge is fixed and the column flow is controlled the difference between these two flows and the offset entered will go out the vent flow This will be consistent for each run 5 If Fixed is selected...

Page 104: ... dimensions and you can skip to step 12 After selecting Program you must enter your column dimensions as described in the following steps 9 Use the up and down arrow or keypad buttons to enter a Column Length which is measured in meters 10 Use the up and down arrow or keypad buttons to enter an Internal Diameter which is measured in micrometers not millimeters 11 Then view the calculated linear ga...

Page 105: ...ectly 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 To verify that you have entered the correct values you can measure the linear gas velocity by injecting methane and calculating the linear gas velocity ...

Page 106: ...d 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 If you select Ratio you enter the split ratio in your method The software controls the ratio and calculates the split flow 13 Select a Flow Offset of either Auto or Fixed ...

Page 107: ...s value should be equal to the septum purge flow plus the column flow If the wrong value is entered then the difference is added to or subtracted from the split vent flow so your actual split vent flow may be slightly higher or lower than the value entered in the method In both cases the split ratio is maintained for every injection If you want to save time from run to run select Fixed mode The Au...

Page 108: ... 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 See Chapter 7 for more details ...

Page 109: ... 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 Press Tools menu button and select Configuration The Configuration screen appears ...

Page 110: ...thod 3 38 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 ...

Page 111: ...lose 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 Touch the ratio field to modify the value OR If you configured the split mode for Flow the following screen appears ...

Page 112: ...ou set the split flow to zero the flow display shows column flow plus septum purge Common places for leaks would be the septum cap the O ring seal column connector etc See the Clarus Hardware Guide Chapter 8 for further information NOTE Please note that if the displayed value is much greater than the total flow defined as split flow and septum purge column flow this indicates a leak in the pneumat...

Page 113: ...ue increases the pressure flow velocity in the system at the time of injection to minimize the gas expansion in the injector liner and maximize the gas sample transfer onto the column Therefore you should use the highest pressure that your application will allow This provides better peak shapes better recovery and no discrimination for both low boiling and high boiling compounds This technique can...

Page 114: ...s that the sample can flow back into the injector and either be lost out the split vent or cause peak broadening Creating a Pressure Flow or Velocity Pulse Method 1 From the System Status screen touch the Injector button for which you wish to create a pressure flow or velocity pulse method The status screen similar to the one below for the selected injector appears 2 Touch the Events tab ...

Page 115: ...Clarus 600 680 User s Guide 3 43 3 Touch the Add button The Add Timed Event screen appears 4 Select Split A from the Event drop down menu ...

Page 116: ...arrow or keypad buttons to enter a flow value NOTE Values of 20 mL min and higher provide greater accuracy than values below 20 mL min 7 Touch OK You have now created a timed event set to turn on the split flow at 0 25 min 8 Touch the A Cap Injector tab The Injector status screen appears 9 Touch the Program button for the Carrier Gas field The Carrier Gas Pressure Program screen appears ...

Page 117: ... min 13 Touch the step 2 dialog box for pressure and use the up and down arrow or keypad buttons to enter the column operating pressure NOTE If you selected flow or velocity you should still follow the above procedure Just enter the appropriate flow or velocity values for your analysis NOTE If you are in the capillary mode and you set up the pressure mode first you can enter 70 psi and or 10 psi t...

Page 118: ...hen programmed at a controlled rate down to the initial or normal column operating pressure flow or velocity If you are using the autosampler at the end of the last sample in the sequence the Clarus MS will go Not Ready thereby sending a signal to the GC keeping it from coming Ready The External Ready must be connected See the Clarus 600 680 GC Installation Instructions 09936779 This keeps the GC ...

Page 119: ...Clarus 600 680 User s Guide 3 47 Setting the Timed Events 1 Touch the Events tab ...

Page 120: ...e the up and down arrow or keypad buttons to enter a negative Time for example 1 00 min for the event to occur prior to the GC coming ready Then press Enter The cursor moves to Event 5 Touch the Value dialog box and use the up and down arrow or keypad buttons to enter a value of 0 6 Touch OK The split flow will now turn off before the GC becomes ready so that at the time of injection the split flo...

Page 121: ...omatically turn the valve on The time depends on your sample solvent column etc Typical time values are between 0 25 and 2 0 minutes An optimum Time is the time that provides maximum area counts indicated by your data handling device with minimum solvent effect tailing 10 Touch the Value dialog box and use the up and down arrow or keypad buttons to enter a value of 50 mL min At the end of a run th...

Page 122: ... flow event time of 0 98 minutes At the end of a run the split flow resets to the original setting Setting a Value of 50 mL min minimizes contamination by keeping the splitter on during cool down NOTE The timed event that you set up or valve settings that you make become part of the method The timed event is automatically saved if you are editing the Active Method NOTE When operating in the splitl...

Page 123: ...tower can contain either a 0 5 5 0 or 50 0 µL syringe Figure 3 9 View of the Clarus GC with autosampler tower Autosampler Trays and Carousel 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 Thermostatting Tray Kit ava...

Page 124: ...Using the Active Method 3 52 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 ...

Page 125: ...e Vials Number of 2 mL Priority Vials 680 only 108 Standard 4 4 1 680 only 108 Tall 4 4 1 600 only 82 Standard 4 4 1 600 only 82 Tall 4 4 1 With the Tray Thermostatting Accessory Kit 600 680 82 Standard 4 4 1 Autosampler Touch Screen 1 You can access the Autosampler by selecting the Run button from the System Status Screen See screens below ...

Page 126: ...a method other than the current active method Start Button Touch the Start button to start a run The Start button is active whether or not the system is ready Issuing the start command before the system is ready gives users the flexibility to set up and run a method without having to wait for the system to attain ready status As soon as you touch OK the Start button changes to Stop whether or not ...

Page 127: ...he 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 Touching the Stop button before the system is running prompts the following dialog box Touch OK to cancel the run The status bar reflects that the system is running and the Start button changes to Stop ...

Page 128: ...top 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: ...m is selected by default The buttons for steps beyond the current program are deactivated To change the temperature touch the radio button and press OK Touching cancel retains the current setting and closes the dialog box Element Enabling by mode Enabling by state A S Program tabs Multi mode Always Method Always Not running auto or gc Start vial Multi Not running auto Stop vial Multi Always Inject...

Page 130: ...tions per vial and the starting and ending vial numbers As each program is run the system sets up the specified method as the Active Method While running in this mode the autosampler attempts at least one injection from each vial in the specified ranges NOTE The autosampler tray is keyed to fit correctly only in one direction When installed properly the tray is recessed slightly around the entire ...

Page 131: ...egin the autosampler run Autosampler Tasks Tab The Autosampler Tasks tab includes buttons to execute tasks such as Park and Clean Touch the Park button to park the autosampler tower NOTE If the syringe is directly over the injector you should move it by selecting Park Touch the Clean button to clean the syringe plunger with the solvent wash NOTE The Clean option is only available when the autosamp...

Page 132: ...the plunger from the syringe barrel 3 Wipe the plunger with a tissue soaked in an appropriate solvent Replace the plunger 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 Config ...

Page 133: ... between 1 and 15 This value is the number of seconds the plunger pauses at the top of stroke during sample acquisition NOTE You can obtain improved precision with viscous samples by using the 0 5 mL syringe and septa in the waste wash vials in place of the diffusion caps Using Solvent Pre Washes Pre washes refers to the number of solvent washes you want the system to perform prior to the pre inje...

Page 134: ...dle Septa are available for the waste vials and solvent wash vials by ordering P N N930 2780 We recommend using these septa in place of the diffuser caps when you are using Very viscous samples to wipe the sample off the outside of the syringe needle Toxic solvents and samples Very volatile solvents Multi Program Mode Waste Vials When operating in the Multi Program Mode the sample pre washes are e...

Page 135: ... PerkinElmer s Catalog service or visit us on line at www perkinelmer com NOTE When using mini vials it is not recommended to use pumps to acquire samples This assures that the sample will not be diluted by residual solvent in the syringe 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 enou...

Page 136: ...390 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 50 µL 0 63 mm O D N6101760 NOTE A 0 47 mm needle is required for use with the POC injector and 530 µm columns in the on column injection mode only You can achieve better precision in the on column injection mode when you use sample volumes of 1 0 µL or greater ...

Page 137: ...Setting Up the Detectors 4 ...

Page 138: ...Setting Up the Detectors 4 2 ...

Page 139: ...ere are exceptions The PPC module that controls the ECD is calibrated with nitrogen TCD is calibrated with helium PID is calibrated with helium If you intend to use a gas that is different from the gas used to calibrate the PPC module you must recalibrate the PPC module with the gas The instructional procedures in this chapter are written with the assumption that You know how to measure gas flows ...

Page 140: ...ol to the touch before you touch detectors injectors and their corresponding fittings Detailed procedures for turning heaters off and on are in the Hardware Guide Before you Install a Column If you have not read this chapter please do so before proceeding A column has been installed carrier gas flow or pressure has been set and all connections have been leak tested The PPC modules have been calibr...

Page 141: ...rily by the hydrogen flow The detector linearity is affected by the air flow The FID has flameout detection and an auto ignite feature Flameout detection occurs 0 5 minutes into the PRE RUN time and it measures the user entered baseline threshold level in mV If the threshold level is exceeded the flame is considered lit otherwise the Clarus GC detects that the flame is out and auto ignite automati...

Page 142: ...ected to the FID and all fitting connections have been leak tested WARNING Turn off the hydrogen gas before disconnecting a column from the FID When two FIDs are installed but only one FID has a column connected to it plug the inlet of the FID without a column with a 1 8 inch stainless steel plug P N N930 0061 to prevent hydrogen from back diffusing into the oven Since in the manual pneumatics ver...

Page 143: ...rom the Clarus GC touch screen Each PPC module is calibrated at the factory with the gas air and hydrogen that it controls therefore to set the gas flow simply follow this procedure Turn on the air at the source and adjust the line pressure to 70 90 psig 1 Turn on the hydrogen at the source and adjust the line pressure to 70 90 psig 2 Press the Tools button and select Configuration The Configurati...

Page 144: ...Setting Up the Detectors 4 8 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: ...pad buttons to enter a flameout detection level in mV for example 0 3 mV NOTE You must set a Flameout value in millivolts mV for the FID auto ignition feature to work For example 0 3 mV Flameout detection occurs 0 5 minutes into the PRE RUN time and measures the user entered baseline threshold level in mV In this example 0 3 mV is used If the 0 3 mV threshold level is exceeded the flame is conside...

Page 146: ...ed on the base of the detector and capped with a stainless steel Swagelok Plug before attempting to ignite 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: ...may not auto ignite if your carrier gas flow is 60 mL min or higher The PPC version of the FID has flameout detection and an auto ignite feature Flameout detection occurs 0 5 minutes into the PRE RUN time and it measures the user entered baseline threshold level in mV If the threshold level is exceeded the flame is considered lit otherwise the Clarus GC detects that the flame is out and auto ignit...

Page 148: ... appears If auto ignition is attempted with the FID gases set to zero flow the message No ignition Flame gases are off appears on the screen To proceed go to the Configuration screen and reset the air and hydrogen to their 450 and 45 mL min flowrates To Auto Ignite The auto ignition process only occurs before the start of each run just prior to the instrument becoming READY However the manual flam...

Page 149: ... 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 CAUTION 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 Flame ignition may not occur if your carrier gas flow is 60 mL min or h...

Page 150: ...perature display 4 Touch the Ignite button Note the signal level in mV before the flame ignites 5 Upon pressing the Ignite button the air flow turns off for 15 seconds Flame Ignition 1 appears in the status bar and the glow plug begins to glow Glow Plug Ignitor Figure 4 2 Location of the FID glow plug ignitor 6 When you hear a POP observe the Signal level in mV as it increases on the screen and re...

Page 151: ...ly ignite the flame NOTE To prevent condensation from forming on the FID always turn off the flame both the hydrogen and air before cooling the detector or turning off the Clarus GC Using the FID in Corrosive Environments If you are analyzing samples such as chloroform methylene chloride etc that produce corrosive by products we recommend installing the piece of vent tubing P N 0250 6490 supplied ...

Page 152: ...r 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 4 Route the end of the tubing through the hole in the detector cover as you close the detector cover 5 Connect one end of a length of vent tubing to this piece of tubing and place the other end in a vent hood ...

Page 153: ...ed zone Call your PerkinElmer Representative Instrument shutdown also occurs if there is a PRT Platinum Resistance Thermometer or MPU Micro Processor Unit failure In these cases the following error message is displayed INSTRUMENT SHUTDOWN xxxxx PRT ERROR where xxxxx is the failed zone Call your PerkinElmer Representative NOTE The detector gas modules have been set to OFF at the factory for both ma...

Page 154: ... list of the Agreement States which have been granted authority by the U S Nuclear Regulatory Commission to regulate the possession and use of radioactive material It is required that you are familiar with regulation 10 C F R Section 31 5 Supplement 1 Following are summaries of its requirements Labels Do not remove any of the labels attached to the ECD cell or any of the labels attached to your Cl...

Page 155: ...rson be exposed to radiation Other Requirements Regulation 10 C F R Section 31 5 see Appendix I does not permit you to abandon the ECD cell or export it It may not be transferred except to a person specifically licensed to receive it Within thirty days of such a transfer you must report to the Director of Nuclear Material Safety and Safeguards U S Nuclear Regulatory Commission Washington D C 20555...

Page 156: ...ophilic compounds such as chlorinated hydrocarbons and pesticide residues It is concentration sensitive and nondestructive The ECD cell contains a foil in a cylinder through which the carrier gas flows The coating of the foil s inner surface contains the radioactive isotope Nickel 63 and has a nominal sensitivity of 15 mCi To optimize detector response make up gas is combined with column effluent ...

Page 157: ... up gas A cross section view of an ECD is shown below Figure 4 6 Electron Capture Detector ECD If you are using the ECD with a packed column check to see whether the optional Flow Readout was calibrated with nitrogen or argon methane carrier gas If not select the appropriate carrier gas To function properly the total carrier gas flow through the detector should be 30 mL min or more Where required ...

Page 158: ...using the ECD You can correct this situation by installing a glass lined receiver P N N6000968 The glass lined receiver terminates in a 1 16 inch fitting so that it can accept capillary columns with an i d of 530 microns or less If you suspect that the background is caused by column liquid phase bleeding install the glass lined receiver in the detector base Then insert the column end just beyond t...

Page 159: ...ases should be used Whenever a column is disconnected from an ECD the ECD should first be cooled to avoid oxidation of the Nickel foil Vent the ECD Outlet NOTE If venting the ECD effluent is required attach an additional piece of tubing to the tubing that is connected to the ECD outlet This does not affect the performance of the ECD 1 Open the detector cover see the following figure to expose the ...

Page 160: ...o the ECD 6 Thread the vent tubing through the detector cap and insulating cover as you position them over the ECD 7 Secure the insulating cover to the Clarus GC with the two screws previously removed 8 Thread the tubing through the hole in the detector cover then close the detector cover This hole is either directly above the ECD or at the rear of the detector cover depending on the detector conf...

Page 161: ... how to set the make up gas With PPC pneumatics the make up gas is set from the Clarus GC keyboard The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure To set the make up gas 1 Set the make up line pressure to 60 90 psig 2 In the System Status screen touch the ECD button 3 In the ECD Tab change the Make Up field touch the Tools butto...

Page 162: ...n 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 ...

Page 163: ... 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 6 Touch OK when finished ...

Page 164: ...gas plus sample flowing through an analytical channel see the following figure Four tungsten rhenium filaments are connected in a bridge circuit two in each channel The TCD is set up with the same amount of carrier gas flowing through both channels The presence of a sample component in the carrier gas flowing through the analytical channel changes the resistance of the filaments in that channel Th...

Page 165: ...the difference in thermal conductivity between the carrier gas and the component NOTE To prevent TCD filament damage shut off the filament current before disconnecting columns or turning off gas flows To set up a TCD read the TCD setup summary then follow the steps TCD Setup Summary To set up a TCD Ensure that a column is installed Turn on the oven and detector heaters Equalize the makeup and refe...

Page 166: ...CD 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 ...

Page 167: ... of 5 mL min to each of the two detector channels Set the Makeup and Reference Gas With PPC pneumatics the reference gas is set from the Clarus GC touch screen Also PPC pneumatics provide you with TCD filament protection by monitoring the carrier gas leak tests or monitoring the gas through the alarm feature and shutting down the TCD current if a gas leak or no gas at all is detected The PPC modul...

Page 168: ...e 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 ...

Page 169: ...ample and reference gas channels you must select the necessary detector gas sources As shipped from the factory the sample channel is Carrier 2 and the reference gas channel is the detector Reference Gas In some cases with Arnel configurations for example the TCD could be sourced with both a Carrier gas as well as an Aux gas in GSV applications half the run could look at the Carrier and half could...

Page 170: ... 120 3 160 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 Balance the Bridge 1 In the System Status Screen touch the Signal button to display the Signal screen This will allow you to observe the signal as you adjust the potentiometer ...

Page 171: ...s indicated by a constant reading on the display 5 Reset the potentiometer to produce a reading between 0 0 and 20 0 mV Using a TCD with the Autosampler or GSV When using a TCD with an autosampler or a GSV Gas Sampling Valve at high sensitivity a minor baseline upset may occur at the time of injection If the signal goes below zero create an Autozero timed event to re zero the detector back before ...

Page 172: ...otoionization 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 Figure 4 13 Cross section view of a PID ...

Page 173: ...IDs may be operated at 350 C for short periods of time with a subsequent loss in lamp life The PID is equipped with a glass lined inlet and exhaust that permits series operation with another detector Figure 4 14 PID installed in the Detector 2 position PID Setup To set up a PID read the PID setup summary then follow the steps PID Setup Summary To set up a PID Turn on the oven and the detector heat...

Page 174: ...rn On the Oven and the Detector Heaters NOTE A PID can only be installed in the Detector 2 position rear 1 Close the oven door This turns on the oven heater 2 From the System Status screen touch the PID button 3 In the PID page touch the temp field and use the up and down arrow or keypad buttons to add a PID temperature appropriate for the analysis to be run ...

Page 175: ...gas is required when using capillary columns at low flows 10 mL min or less Since a PID is concentration sensitive make up gas flow should be kept to a minimum to obtain the best peak shapes and sensitivity NOTE Use make up gas only if you are using a capillary column at flows of 10 mL min The following procedures describe how to adjust the make up gas using PPC pneumatics ...

Page 176: ...if you are using a reference gas other than helium 1 With the make up gas is set from the Clarus GC touch screen The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure 2 To set the Make up and Reference gases touch the Tools button in PID screen and then touch Configuration from the drop down menu ...

Page 177: ... 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 however the noise level may increase 5 Use the up and down arrow or keypad buttons to set the Offset to 5 6 When all the settings are appropriate for your analysis touch OK The PID scre...

Page 178: ... the system to stabilize until the background signal is steady Optimize the Lamp Intensity 1 As shown in the screen above go to the Atten Attenuation field Touch the downward arrow and select an attenuation value of 32 2 Make sure AutoZero is off 3 Locate the lamp intensity control knob see Figure 4 14 and slowly turn it clockwise increasing the signal until the background signal on your integrato...

Page 179: ...the noise is between 1 and 1 5 of full scale at an attenuation of x8 Setting Up a NPD WARNING To avoid injury Do Not Nitrogen Phosphorus Detectors NPD use hydrogen gas Before you turn on the hydrogen gas to the NPD ensure that a column is connected to the NPD fitting inside the oven Turning on the hydrogen gas without first connecting a column to the NPD could create the possibility of an explosio...

Page 180: ...column flow changes may produce a negative baseline drift The detector operates by electrically heating a glass bead that contains an alkali metal to the point where it emits electrons A mixture of hydrogen gas and air flows around the bead to produce a hydrogen plasma Stable intermediates are formed in the hydrogen plasma which then capture the electrons emitted from the bead to produce ions A po...

Page 181: ...and air flow as described below then condition the bead Set the Hydrogen Flow and Air Flow for PPC The pneumatics consists of PPC modules where the plasma gases are adjusted and set from the Clarus GC keyboard The PPC modules are calibrated at the factory to set the flows for an analysis follow the procedure below 1 Turn on the hydrogen at the tank and adjust the line pressure to 60 90 psig 2 Turn...

Page 182: ...4 46 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 ...

Page 183: ...s Guide 4 47 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: ...timum flow provides the best sensitivity signal to noise selectivity and bead life Any changes to these flows will affect all of these parameters Also when using capillary columns makeup gas is not required NPD Bead Activation Procedure Packed Column Setup Disconnect column and cap the oven end of the detector The recommended Detector Cap Nut is in the 1 8 in Plug Kit P N N9300061 Capillary Column...

Page 185: ... to stabilize WARNING If a capillary column is used and is not disconnected from the detector a high detector temperature can cause bleed at the detector junction with the column Make certain the detector temperature is lower than the maximum temperature recommended for the capillary column of your application Set the hydrogen and air flow as follows Air to 100 mL min Hydrogen to 2 0 mL min NOTE H...

Page 186: ...background value that occurs with the bead off 12 Open the detector cover see Figure 4 28 and locate the bead potentiometer dial see the following figure If the NPD is detector 1 front position the potentiometer is located on the left side of the panel If the NPD is detector 2 rear position the potentiometer is located on the right side of the panel Figure 4 30 Location of the Potentiometer Dial ...

Page 187: ...ce the potentiometer to 750 10 After 1 minute reduce the potentiometer down to 700 11 For Capillary columns Wait 10 minutes go to the NPD detector screen then adjust the potentiometer so that the NPD baseline response reads around 0 5 mV on Range 1 Then set the desired column flow for the application to be run For Packed Columns 12 Allow the baseline to stabilize for 30 minutes Wait 10 minutes go ...

Page 188: ...abilized it is ready for operation If you are unable to achieve adequate sensitivity for your standard increase the background of the NPD Increasing intervals of 0 25 mV are recommended Adjust the background setting to achieve the sensitivity required for your samples For example if you have a concentrated sample such as drugs it can be analyzed with a background of 0 25 0 50 mV If you have a low ...

Page 189: ...use for long periods of time for example over the weekend Reactivate a Used NPD Bead To increase the bead life turn off the bead if the NPD is not continually in use When you turn off the bead keep the detector temperature hydrogen flow and air flow set to operating conditions If the column remains connected to the injector and detector in the oven make sure the carrier gas is flowing through the ...

Page 190: ...st to simply lower the potentiometer setting to 600 and maintain the detector temperature at 200 deg C or greater If the NPD detector will not be in use for an extended period simply turn the potentiometer to zero To reuse the bead follow the activation procedure Loss in sensitivity the NPD bead is a consumable and will experience a loss in sensitivity over time Often adequate sensitivity can be r...

Page 191: ...atics version the hydrogen needle valve has been factory set to a very low setting Set both the hydrogen and air inlet pressures to 30 psig then measure and set the flows as stated in this chapter NOTE The PPC pneumatics detector gas modules have been set to OFF at the factory FPD Overview In the Flame Photometric Detector FPD the column effluent is mixed with hydrogen and then burned in air Light...

Page 192: ...Setting Up the Detectors 4 56 A cross section view of an FPD is shown below Figure 4 31 Flame Photometric Detector FPD ...

Page 193: ...unction of the square of the sample quantity injected That is if twice as much sample is injected the response is quadrupled When the linearizer is turned on the software calculates the square root of the signal and sends that value to the integrator or recorder NOTE If Linearization is set to ON the Autozero function must be checked off on the FPD tab screen NOTE If Linearization is set to ON set...

Page 194: ...Setting Up the Detectors 4 58 2 The FPD page is now visible ...

Page 195: ... Guide 4 59 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 ...

Page 196: ...een 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 If you want to improve the signal to noise change the setting to 800 msec Then run your standard and observe that the signal remains the same and the noise improves ...

Page 197: ...en 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 Do not enter any value less than 250 C 1 From the System Status screen touch the FPD button 2 The FPD tab page is now visible ...

Page 198: ...an the highest temperature of your oven program Set the Hydrogen Flow and Air Flow for PPC The PPC pneumatics consists of PPC modules to set the hydrogen and air gases from the Clarus GC touch screen The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure 1 Turn on the air at the source and adjust the pressure to 70 90 psig 2 Turn on th...

Page 199: ...Clarus 600 680 User s Guide 4 63 4 The FPD tab page is now displayed ...

Page 200: ...Detectors 4 64 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 ...

Page 201: ...pad buttons to change the value to 90 mL min 8 To change the filter value touch the Filter field and use the up and down arrow or keypad buttons to set the value appropriate for your analysis The default setting 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 r...

Page 202: ...Setting Up the Detectors 4 66 7 Touch OK when completed Turn On the Photomultiplier Tube 1 From the System Status screen touch the FPD button ...

Page 203: ...Guide 4 67 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 ...

Page 204: ...etting as the photomultiplier tube ages and the signal diminishes The signal to noise ratio may vary with each photomultiplier tube therefore increasing the voltage may not increase the signal to noise ratio After installing a replacement photomultiplier tube the noise should be about 2 when the Clarus GC integrator output is set to attenuation 8 x8 and the Linearizer off See the Clarus 600 680 GC...

Page 205: ... 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 Use the up and down arrow or keypad buttons to enter a setpoint of at least 100 C this is the minimum entry for a FPD in the temp field ...

Page 206: ...t NOTE If you find it difficult to light the flame rotate the FPD cap so that the FPD outlet faces the front or left side of the instrument Figure 4 33 Ignitor assembly positioned on the FPD outlet 8 Remove the ignitor assembly from the FPD outlet If the flame is lit the signal on the Autozero screen should increase and remain greater than the noted amount Confirm that the flame is lit by holding ...

Page 207: ...WARNING The FPD outlet is hot To prevent injury never place your hand over the FPD outlet 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 ...

Page 208: ... 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 In the System Status screen touch the ECD button 2 In the ECD screen you will see the Make Up field to change the setting touch Tools and touch Configuration from the drop down menu ...

Page 209: ...ield 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 The message on the button will toggle to either on or off and will be visible on the screen ...

Page 210: ...ing you to the FID tab screen page 2 To change the range touch the Range field Select a range from the drop down menu for the detector FID PID and NPD range options are 1 or 20 where 1 is the most sensitive setting and 20 is 20 times less sensitive The value that you enter will always be used unless you change it on the Event page For certain analyses such as those for trace or concentrated compon...

Page 211: ...un 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 1 Touch the Event tab to view and change a range during a run 2 Touch the Add button to show the following screen ...

Page 212: ...Setting Up the Detectors 4 76 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 ...

Page 213: ...5 Enter a value for the AutoZero A by touching the Value field Then using the up and down arrow buttons enter On or Off 6 When completed touch OK to close the screen 7 When a run is started the system uses the initial range of 1 for 2 minutes then switches to a range of 20 for the duration of the run When the run completes the system switches back to the initial value of 1 When completed touch OK ...

Page 214: ...e the temperature and current must be off 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 TCD range options are Off 40 80 120 and 160 maximum sensitivity and 40 80 120 or 160 A negative value reverses the polarity ...

Page 215: ...o bridge current are shown below Table 4 3 Correlation Between Bridge Current and Range Bridge Current mA Range Entry Off 0 40 1 80 2 120 3 160 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: ...our 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 chapter Practical Hints section To automatically change the range from 2 to 2 after 3 minutes into the run 1 From the System Status screen touch the TCD button 2 In the TCD tab page touch the Events tab ...

Page 217: ...Clarus 600 680 User s Guide 4 81 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 ...

Page 218: ...ect 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 When the run is completed the system switches back to the initial value in this case 2 ...

Page 219: ...you are running complex analyses such as those requiring detector switching you may wish to route the signal to either channel Rerouting Output Assume that Detector 1 is an FID whose output is going to an integrator in this example the integrator is output A Detector 2 is a TCD whose output is going to a recorder in this example the recorder is output To reroute the FID output A to the integrator ...

Page 220: ...Setting Up the Detectors 4 84 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 ...

Page 221: ...positive 6 Touch OK to return to the Events tab page 7 Once in the FID page touch the System button to return to the System Status screen 8 In the System Status screen touch the TCD button The TCD page will appear Touch the Events tab 9 In the Events screen touch the A button The Timed Events screen will appear In the drop down menu for Events and touch Output B 10 Touch the Time field and use the...

Page 222: ...etector 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 NOTE Detector routing remains in effect until changed If two detectors are installed but only one configured then the output of the configured detector is sent to both output channels ...

Page 223: ...alues to the next highest power of 2 For example if you go to the Atten field and select 1 then an attenuation of 32 appears on the screen The range of attenuation values that may be used is 1 65 536 Raising the attenuation decreases the signal to the recorder Lowering the attenuation amplifies the signal to the recorder To change an attenuation value an FID detector is used as an example 1 From t...

Page 224: ...age 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: ... the sample with the highest concentration must not exceed the 1 V signal When using a flame ionization detector FID if you operate at range x1 and attenuation x64 and the signal saturates exceeds 1 V then use range x20 and determine the appropriate attenuation value from x64 to x1 that produces a reasonable size peak When using a nitrogen phosphorus detector NPD the same will apply When using an ...

Page 226: ...lly attenuation for an integrator need only be performed once To obtain the most satisfactory results it is recommended that attenuation be carried out under actual operating conditions prior to running your first sample Valid attenuation values when an integrator is configured are 1 2 4 8 16 32 and 64 The greater the attenuation the smaller the degree of detector signal amplification Attenuation ...

Page 227: ...nal 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 From the System Status screen touch the TCD button 2 In the TCD tab page touch the Atten field and use drop down menu to change the value ...

Page 228: ...Setting Up the Detectors 4 92 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 ...

Page 229: ...stem will autozero the detector to the offset specified during configuration whenever the system becomes READY or when a run is started The example below uses the ECD detector but the following procedure can also all the detectors 1 In the System Status screen touch the ECD button 2 In the ECD Tab you will see the AutoZero field To turn on the AutoZero touch the field and a check mark will appear ...

Page 230: ...Setting Up the Detectors 4 94 NOTE When Autozero is Off the output signal is never autozeroed ...

Page 231: ...Using the Method Editor 5 ...

Page 232: ...Using the Method Editor 5 2 ...

Page 233: ...Clarus 600 680 GC User s Guide 5 3 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: ... and edit the first five methods The fifth method is reserved for TotalChrom and may be overwritten If you attempt to overwrite the method it will retain the name External to remind you that this is a possibility You cannot access the Default method This method is used by the system to populate a method with default values when the New Method menu option is selected The default settings are the sa...

Page 235: ...Clarus 600 680 GC User s Guide 5 5 Method Edit Mode When you touch Method Editor from the Tools menu a screen similar to the status screen appears ...

Page 236: ...an Aux button appears on the method edit screen The Method Edit screens are similar to the Active Method screens with the following differences The run and signal icons on the top navigation bar are absent No configuration information appears No ignite button on the FID screen No status bar or current information The Start and Tools menu button in the bottom bar are replaced with the File menu but...

Page 237: ... 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 Touching the Oven button displays the oven screen in Method Edit mode ...

Page 238: ... 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 The Method Name field is not active until you select an option from the File menu ...

Page 239: ...tore and delete methods The Exit Editor option closes the Method Edit screen and displays the view that appeared when the user invoked the Method Editor Tools option During a run the Activate menu option is grayed out since you cannot activate a different method during a run New Method When you need to develop a new method select New Method from the pop up File menu If your current method has not ...

Page 240: ...10 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 The Save As dialog reappears ...

Page 241: ... and displays the name untitled After defining the values for the new method touch the Method Name field to display the Save As dialog box Assign a name to the new method and save the changes Open Method Touching the Open Method option prompts the following warning box only if changes have been made since the last save If you touch Yes the Save As dialog appears When the Open option is selected th...

Page 242: ...ut 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 No dialog box appears if a name appears in the Method Name field If the Method Name field is empty either from generating a New Method or from entry into the Method Editor the Save As dialog box appears ...

Page 243: ...ent method The list of method names always displays External in the last position If you do not change the name or select another method from the list clicking OK prompts the dialog box to confirm that the existing method will be overwritten Clicking Yes overwrites the stored method with the new method pneumatics with the same name To assign a new method name touch the name field to invoke the alp...

Page 244: ...keypad and displays the Save As dialog box with the name entered in the name field Touching Cancel closes the keypad and displays the Save As screen The name field is not modified The External method is always the last entry in the list The External method cannot be renamed but it may be overwritten Touching OK saves the edited method under the assigned name The name is added to the list and the S...

Page 245: ...el 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 When you select a method and press OK the Save As screen appears with the new method name in the field You can now press OK to save the method in the available position ...

Page 246: ...tton or OK to prompt the memory full error again Activate This command is deactivated while the system is running When the command is available the Activate option applies the currently edited method conditions and name to the active method The method editor mode retains control If the method is not named the Save As dialog box opens for you to select a method from the list Delete Touching the del...

Page 247: ...ected method and close the dialog box Exit Editor The Exit Editor option closes the Method Edit screens and restores the Active Method Touching Exit Editor invokes the following dialog box Pressing the Yes button closes the dialog box and displays the active method screens Pressing the No button closes the dialog box and retains the Method Editor mode ...

Page 248: ...Using the Method Editor 5 18 ...

Page 249: ...Using the Tools Menu 6 ...

Page 250: ...Using the Tools Menu 6 2 ...

Page 251: ...d settings such as Method Editor Configuration Maintenance and Utilities To display the menu touch the Tools button 1 To access the Tools menu display the System Status screen as shown below 2 Touch the Tools button shown above and the Tools menu appears You are now able to select any of the options displayed in the menu ...

Page 252: ...Tools Menu 6 4 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: ... 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 The list box displays the contents of the selected log The logs are not editable ...

Page 254: ...ion that prompts the reminder When the criteria are met a dialog box displays the message The last item accessed is automatically selected The tasks are listed in the order they were entered Use the scroll bar to display additional entries Each entry includes the name of the task and the Count at which it is set to prompt a reminder message The buttons below the list allow the user to add edit and...

Page 255: ...enance 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 3 Enter a message by touching the Message field This displays the alphanumeric keypad for you to enter a message ...

Page 256: ...Tools Menu 6 8 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 9 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: ...od of time Instead of turning off the injector heater you may find it more convenient to deconfigure the unused injector When you do this the injector temperature screen for the deconfigured injector will not appear in the method Every Clarus GC has been configured at the factory for the specific injector s that have been installed You can check the injector configuration of your Clarus GC from th...

Page 259: ... 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 The example below shows None selected ...

Page 260: ...n in this case If the Capillary Control mode is set for flow or velocity the radio buttons for Program and Oventrack are deactivated If the mode is set for pressure and the Oventrack radio button is selected the column dimension fields are deactivated In this case the pressure is entered in the method and the software maintains the column flow based on the initial oven temperature and pressure Whe...

Page 261: ...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 The field label changes from Leak Limit to Offset Program Mode Configuring the injector for the Program mode displays the following ...

Page 262: ... 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 When using a mass spectrometer select the Vacuum Compensation checkbox ...

Page 263: ...tor 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 This example shows that POCO a programmable on column injector is selected as the Type on the Configuration screen ...

Page 264: ...e 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 Make your settings then touch the OK button Then touch the Close button to exit configuration ...

Page 265: ...s Guide 6 17 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: ...cted it turns black The default value is 0 The Offset range is 10 to 10 C Enter the Offset temperature and allow the oven temperature to equilibrate for at least 30 minutes The displayed temperature will approach 100 00 C or the oven temperature you entered and the thermometer readout will approach a value close to 100 00 C Coolant If you have an optional coolant select the type installed its targ...

Page 267: ...ng Selecting this check box allows you to enable or disable the Soft Cooling function Checking or un checking this check box will not lose the previous settings Rate This user entered value limits the cool down rate Note that this is not a negative temperature program rate but just a means of ensuring that the rate does not exceed the entered value once cooling is initiated Limit This user entered...

Page 268: ...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 If Yes is selected the Define Gas Sources screen appears and you configure an available flow module In this example you will define a detector ...

Page 269: ...ser s Guide 6 21 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 ...

Page 270: ...nu 6 22 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 ...

Page 271: ...Clarus 600 680 GC User s Guide 6 23 The following series of screens show the configuration screen for each detector TCD ECD ...

Page 272: ...Using the Tools Menu 6 24 PID NPD ...

Page 273: ...Clarus 600 680 GC User s Guide 6 25 FPD Output Configured ...

Page 274: ...Using the Tools Menu 6 26 External Configuration If an external amplifier is installed a screen similar to the following appears Run AutoSampler ...

Page 275: ...if filled with solvent and emptied to waste after sample injection The first half of these washes is taken from solvent vial 1 or 3 The second half from solvent vial 2 or 4 The default is 2 Permissible entries are 0 to 15 Injection Mode Fast 30 milliseconds Not available when a 50 0 syringe is installed Normal injection takes about 1 second Slow takes about 7 5 second Auto resume provides option f...

Page 276: ...8 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 ...

Page 277: ...d 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 Language drop down menu Touch the language option The list box closes and the selected language is immediately displayed throughout the application Brightness field The field is selected ...

Page 278: ...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 To set the Date and Time highlight the field then use the up and down arrow or keypad buttons to enter the values ...

Page 279: ... 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 4 Select whether you want these start up settings to Repeat Once or Always ...

Page 280: ...leep 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 Select the After field then set the time after which sleep will by using the up and down arrow or keypad buttons ...

Page 281: ...terface 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 To access the PPC Settings press the pneumatics icon button on the Configuration screen The pneumatic configuration screen appears and displays a number of buttons to represent different types of settings ...

Page 282: ...Using the Tools Menu 6 34 PPC Configure ...

Page 283: ...ontrolling software to recognize a specific PPC module that is installed at a specific location This is necessary so that the software can control the installed hardware The PPC board has 12 sockets to which various injector and detector modules are connected The socket locations and descriptions are listed in the following table and shown in the following figure Table 6 1 Injector and Detector So...

Page 284: ...y on the PPC board The PPC modules for the split splitless capillary Cap injector or PSS injector split vent connections that correspond to injectors 1 and 2 or the pressure readout that corresponds to a packed column injector Pkd or POC injector installed in socket 1 and 2 are connected to sockets 11 J20 and 12 J21 respectively on the PPC board The PPC modules for detectors 1 and 2 are connected ...

Page 285: ...de panel Phillips Screws 3 PPC Control Board J10 J12 J14 J16 J18 J20 J11 J13 J15 J17 J19 J21 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: ... 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 PPC Connect Press the PPC Connect button The following message appears to caution users that modifying the settings can have a negative impact on the operation of the PPC system Press OK and the main Connect PPC Devices screen...

Page 287: ...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 Also the Detector A and B buttons show PID and ECD icons respectively Touching a Carrier Detector or Aux icon button displays a dialog that allows this device to be defined ...

Page 288: ...Using the Tools Menu 6 40 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 ...

Page 289: ...unctions for this logical position This is explained in more detail in a later section For a Carrier a Detector flow module is invalid and is not offered Note that at this point the only available position for the primary module is 0 the undefined state Once a function is selected for the primary module in this case Carrier flow the position list is updated to offer only those positions consistent...

Page 290: ...dule 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: ...K 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 Select Split Ctrl control The secondary module for Carrier B is now enabled but inspection shows that there are no suitable modules available for assignment ...

Page 292: ...nt 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: ...a Detector flow module The following screen shows that once Detector flow has been selected the position combo box is recalculated and offers positions 3 and 4 Once Position 3 is assigned to the primary module however this location is no longer available for use with the secondary module Press OK to implement the changes and return to the connect screen In the example shown in the following screen...

Page 294: ... 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 If Aux 1 is pressed before setting up the carriers and detectors a more complete list is offered as shown in the screen on the right ...

Page 295: ... 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 For a carrier this means scanning through all of the locations looking for ones that the hardware test has shown to contain CARR or PRES modules and that have not been assigned to another logical location ...

Page 296: ...Using the Tools Menu 6 48 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 ...

Page 297: ...s in your laboratory In the factory the TCD reference gas and the PID make up gas have been calibrated with helium and the ECD make up gas with nitrogen Zeroing and calibrating PPC modules consists of the following steps Zeroing the PPC gas modules Gas turned off Setting the reference temperature and pressure Calibrating the PPC carrier gas modules and or PPC detector gas modules Gas turned on The...

Page 298: ...s PID Makeup Gas Make sure that the gas supply to the Clarus GC is turned off at this time Ensure that the pressure in the lines has completely bled down by loosening the restrictor on the rear of the PPC module that you are calibrating see the following with a 1 2 inch socket wrench or open end wrench Refer to above table for a listing of the injectors and detectors with the corresponding PPC gas...

Page 299: ...es 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 Select any of the other tabs to Zero another Channel carrier gas detector or Aux ...

Page 300: ... 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 controller has two pressure transducers per module whereas the other modules only have one In the carrier flow module pressure transducer A reads the differential pressure across the flow measuring device restrictor and transducer B reads the i...

Page 301: ...ssure values are set at the factory We recommend leaving these parameters set to the factory default values Temp 25 C and Press 14 7 psi If you wish to use your own flow measuring device and know the temperature and pressure at which your flow measuring device was calibrated then enter the values as described in this procedure To set the reference temperature and pressure 1 From the Configuration ...

Page 302: ...sure that all the gas flows up through the detector and not into the oven If you are using a packed injector or programmed on column injector you can disconnect the column and measure the flow at the exit of the injector If you are using a capillary injector or programmed split splitless injector you must remove the column Cap the injector exit in the oven and measure flows at the split vent exit ...

Page 303: ...results before you begin to calibrate you 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 Select OK ...

Page 304: ... the restrictor with a different one The number is stamped into the restrictor CAUTION If you are performing this calibration procedure and you do not have a column connected to the detector you must plug the detector fitting in the oven with an Swagelok 1 8 inch cap before proceeding This will ensure that all the gas flows up through the detector and not into the oven CAUTION All carrier gas modu...

Page 305: ...the restrictor installed is not the same as the restrictor number entered then the actual measured flow will not match 20 of the setpoint value This indicates that there is a problem The number displayed next to Hi on the screen is the value that the software interprets as the actual flow This number will always equal the setpoint if control is possible If you set the flow higher than what is poss...

Page 306: ...sing a make up gas other than nitrogen To calibrate a detector gas module 1 Ensure that the gases connected to the Clarus GC have been turned on and stabilized for at least 15 minutes before you begin calibration Ensure that no detector flame is lit before calibrating 2 To eliminate the column flow from the detector gas calibration disconnect the column from the detector and cap the detector fitti...

Page 307: ...ou do not touch the field the original value will remain and not change 6 Enter Zero 0 for the detector gas setpoints If you are using a FID NPD or FPD enter 0 for both air and hydrogen detector gas setpoint 7 When you have added all the appropriate values touch OK If you have an ionization detector for example FID NPD or FPD you must repeat this process for the hydrogen gas also The other detecto...

Page 308: ...tored in a reserved area of the battery backed memory Required Equipment A calibrated precision platinum resistance thermometer with 0 01 C readout and a probe capable of insertion into the GC oven The following steps summarize how to calibrate the oven temperature 1 Calibrate the reference thermometer 2 Place the thermometer probe in the oven 3 Equilibrate the oven temperature 4 Enter the require...

Page 309: ...llow the oven to cool 2 Remove the left side instrument cover Note the location of three approximately 1 inch diameter holes that correspond to the holes on the left side of the oven One or more of these holes may be occupied by gas sampling valves Figure 6 5 Left panel removed to reveal left side of the oven exterior 3 Insert the temperature probe through the exposed white insulation covering one...

Page 310: ...obe 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 Close the oven door then turn the GC and thermometer on From the System Status screen press the oven button ...

Page 311: ...Clarus 600 680 GC User s Guide 6 63 2 Touch the Tools button and select Configuration in the drop down menu 3 Press on the Oven button on the Configuration screen ...

Page 312: ...ow 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 ...

Page 313: ...displayed temperature will approach 100 00 C or the oven temperature you entered in step 4 and the thermometer readout will approach a value close to 100 00 C Enter the Required Offset Value 1 After the temperature has stabilized subtract the thermometer reading from the actual oven temperature shown on the previous screen 2 Using the plus and minus keys enter a value into the above screen then pr...

Page 314: ...he 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: ...ser s Guide 6 67 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 ...

Page 316: ...lated and inserted into the two unselected fields For example the example in the above screen will allow you to enter an inlet pressure and calculate the flow rate and velocity from this and the other entries Use the up and down arrow or keypad buttons to add the flow rates 5 Press the Split button and the next screen appears This screen allows you to calculate the split flow settings may The Clos...

Page 317: ...pported If the value scrolls below 1m then the units should change to mm 1 to 1000 in 1mm increments The default value will be 30m For the calculation this value should be converted to cm Diameter Column diameter should be entered in µm 1 to 1000µm in 1µm increments The default will be 320µm Value converted to cm for calculations Temp Normal GC oven temperature range in C 99 to 450 C in 1 C increm...

Page 318: ... Configuration screens for the rest of the user interaction The range for this field will be 0 to 100 psi abs in 0 1psi increments or 0 to 689 kPa abs in 1kPa increments The default will be Ambient 14 7psi abs or 101kPa abs Suggested Velocity A display only field that shows the recommended carrier gas velocity range from the selected carrier gas name Inlet Press This is a selectable field this is ...

Page 319: ...w rate This field will take its initial value from the Main Screen Flow field The same range and units will apply If the value is changed in this field the entry in the Main Screen will also be updated and the input pressure velocity and t0 will be recalculated Split flow rate This field will use mL min units 0 to 500mL min range in 1ml min increments The default will be 50mL min Column i d This f...

Page 320: ... that the split dynamics occur at an elevated pressure pI and elevated temperature injector temperature The flow rates Fa and Fs are at ambient pressure and temperature The same factors would be applied to each to convert these flows to the true values inside the injector and so they would be cancelled out in this equation ...

Page 321: ...ngth 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 The following screen appears ...

Page 322: ...round 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 The Background Bakeout tool is always enabled Detector A and Detector B need to be labeled with the installed detector names The Calibration checkboxes are enabled if a detector is installed in that posit...

Page 323: ... only the most recent profile is used for compensation One background profile is stored for each detector Calibration and compensation can be applied independently to each detector output signal Note Calibration run time must be greater than 2 minutes Calibration Menu Options Once The background profile will be calibrated once and stored This profile is applied automatically to all manual or autos...

Page 324: ...e 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 Touch the Stopwatch icon button 4 The following screen appears ...

Page 325: ...Clarus 600 680 GC User s Guide 6 77 Program Max Oven Program Rates 1 Touch the Program icon button 2 The following screen appears ...

Page 326: ...elease 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: ...larus 600 680 GC User s Guide 6 79 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 ...

Page 328: ...Using the Tools Menu 6 80 About Touch About to display version information To access About from the System Status screen touch Tools menu and then touch About ...

Page 329: ...Setting up a Typical Analysis 7 ...

Page 330: ...Setting up a Typical Analysis 7 2 ...

Page 331: ...ee the earlier chapters in this guide on the Active Method Method Editor and Tools Menu The Clarus GC can have many configurations For the purpose of this chapter we are assuming the following configuration Injector B is packed Pkd Injector A is programmed split splitless capillary injector PSS One detector is a thermal conductivity detector TCD The other detector is a flame ionization detector FI...

Page 332: ...e 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 Repeat the same procedure for the time and rate As shown in the example below this analysis has been set to have an initial temperature of 75 ºC and it is held at this temperature for 1 minute then goes up 10 deg...

Page 333: ...Clarus 600 680 GC User s Guide 7 5 ...

Page 334: ... 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 2 Next set the carrier gas by touching the Program button to display the Carrier Pressure Program screen ...

Page 335: ...ide 7 7 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: ...l Analysis 7 8 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: ...jector 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 4 When done touch the Close button 5 Touch the Carrier Gas Program button This displays the Carrier Pressure Program screen ...

Page 338: ... 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 8 Touch Close when you have entered all the parameters ...

Page 339: ...urn black Then use the up and down arrow or keypad buttons to set to the required temperature for your application 3 Set the Atten attenuation and Range by touching the arrow button and selecting a value from the drop down list as shown in the example below This example also shows that the Heater is off 4 If you require the heater on for your analysis just touch the Heater button and it will toggl...

Page 340: ...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 7 If the Gas flows Output Offset Filter and Flameout have to be changed touch the Tools button and then touch Configuration on the displayed menu ...

Page 341: ... 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: ...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: ...t 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 When completed touch OK to return to the Event tab Repeat this procedure until you have added all the timed events for your procedure 10 Once all the fields have been set as required by your application touch the ignite button on the FID tab screen to ignite the FID ...

Page 344: ...he 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 3 Repeat the same procedure for the Attn attenuation and Current As shown in the example below this analysis has the heater off ...

Page 345: ...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 6 The gas flows output offset and filter are shown above as reference fields and they cannot be changed in this screen ...

Page 346: ...Setting up a Typical Analysis 7 18 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 ...

Page 347: ...pplication requires 9 Once you have modified the Configuration screen touch OK and the new values will now be visible on the TCD tab screen 10 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 348: ...e 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 12 When completed touch OK to return to the Event tab Repeat this procedure until you have added all the timed events for your procedure ...

Page 349: ...Clarus 600 680 GC User s Guide 7 21 13 Once all the fields have been set as required by your application for the TCD touch the Clarus GC icon on the screen ...

Page 350: ...creen 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 When the count down goes to zero the analysis will begin If you need to stop the autosampler run touch the Stop button ...

Page 351: ... 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: ...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 6 After you touch OK on the Autosampler Configuration screen the main autosampler screen will appear again Touch Start to begin the run Touch the Signal icon to get to the Signal screen...

Page 353: ...arus 600 680 GC User s Guide 7 25 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 ...

Page 354: ...Setting up a Typical Analysis 7 26 ...

Page 355: ...Index ...

Page 356: ...I 2 ...

Page 357: ...arrier gas 6 54 detector gas 6 58 CAP abbreviation 1 6 Carrier Gas PPC velocity viewing setting 3 27 Changing TCD polarity 4 80 Chromatographic terms glossary 1 10 Cmptr abbreviation 1 6 Column Flow Calculator 6 67 Column Length Calculator 6 73 Configuration 6 10 Configuring injectors 6 10 Connect PPC module socket descriptions 6 35 Conventions Notes cautions and warnings 1 4 text 1 4 Coolant cut ...

Page 358: ...splay text 2 18 PSS 2 18 split flow 2 23 temperature program 2 19 Inlet temperature program setting up 3 6 Int abbreviation 1 6 Integrator noise 4 90 Isothermal temperature program setting up 3 8 K kPa abbreviation 1 6 L Labels Warning Signs 1 5 Logout 6 79 M Maintenance 6 6 Method Editor 6 4 file menu 5 9 mode 5 5 overwriting the active method 5 9 Multiprogram mode 3 58 Multi ramp temperature pro...

Page 359: ...itless Injection 3 41 Priority sample inserting 3 62 Psi abbreviation 1 6 psig abbreviation 1 6 PSS abbreviation 1 6 R Reference Pressure setting 6 53 Reference Temperature setting 6 53 Release 6 78 Rerouting detector output 4 83 S Screen abbreviations 1 6 Septum Purge Mode PPC viewing setting 3 29 Setting injector temperature 3 14 Setting up isothermal temperature program 3 8 multi ramp temperatu...

Page 360: ...emperature and pressure setting 6 53 utilities 6 66 Touch Screen 0 3 2 4 autozero button 2 12 aux zone button 2 15 heated zones 2 13 ignite button 2 12 injector and detector buttons 2 13 manual injection 2 9 oven button 2 15 run button 2 8 signal button 2 11 signal display and scaling 2 12 signal plot 2 12 zero display button 2 13 Typical Analysis autosampler 7 22 detectors 7 11 7 16 injectors 7 6...

Page 361: ......

Page 362: ...kinElmer 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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