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Chapter 5
Split/Splitless Injector (S/SL)

S/SL Injection Techniques

102

Instruction Manual

Figure 5-5. Split Injection Technique

The major advantage of split injection is and the ability to introduce samples over
a wide range of concentrations. Peak shapes are very sharp due to the rapid
sample introduction into the column.

1. Carrier Gas Inlet

3. Septum Purge Line

2. Split Line

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Summary of Contents for FOCUS GC

Page 1: ...Thermo Scientific FOCUS GC Gas Chromatograph Instruction Manual PN 31709412 Revision May 2007 HOME ...

Page 2: ...ly complete and accurate information however Thermo Fisher Scientific assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this manual or the information contained therein even if this information is properly followed and problems still arise This publication is not part of the Agreement of Sale between Thermo Fisher Scientific ...

Page 3: ... calibration changes and repairs have been carried out by authorized personnel and if the local installation complies with local law regulations the instrument is used according to the instructions provided and if its operation is only entrusted to qualified trained personnel Thermo Electron S p A is not liable for any damages derived from the non compliance with the aforementioned recommendations...

Page 4: ...iv InstructionManual ...

Page 5: ...xiv Chapter 1 FOCUS GC Description 25 Instrument Overview 26 FOCUS GC Components 26 Pneumatic Compartment 26 Analytical Unit 26 Electronic Compartment 27 Status Panel and Keypad 27 Gas Control 27 Carrier Gas Control 27 Detector Gas Control 28 Column Oven 28 Injector 28 Split Splitless S SL Injector 28 Purged Packed Column PPKD injector 29 Columns 29 Detector 29 Flame Ionization Detector FID 29 The...

Page 6: ...ng Valve Overview 40 Chapter 2 The FOCUS GC User Interface 41 Overview 42 The Display 42 The Display LEDs 44 The FOCUS GC Keypad 45 Parameters Entry 46 User Interface Main Menu 47 Oven 47 Inlet 48 Carrier 48 Detector 48 No Detector 49 External Detector 49 Signal 49 External Detector 50 Autosampler 50 Sequence 50 Others 51 Configuration 51 When to Configure 51 Configuration Menu 52 Oven Configurati...

Page 7: ...61 Run Time Events 62 Run Log 64 Time 66 Valves 67 Info Diagnostics 68 Chapter 3 Gas Control 71 Gas Supplies 72 Carrier Gas Regulation 75 Detector Gas Regulation 75 Measuring Gas Flow 78 Carrier Gas Parameters 80 Flow Mode 80 Constant Flow 80 Constant Pressure 80 Chapter 4 Column Oven 83 Column Oven Overview 84 Oven Safety 85 Column Oven Configuration 86 Oven Parameters 87 Chapter 5 Split Splitles...

Page 8: ... Column 125 Introduction 126 Capillary and Wide bore Columns 126 Using Correct Fittings 126 Column Ferrules 126 Packed Columns 128 Metric Packed Columns 128 Using Correct Metric Fittings 128 Imperial Packed Columns 129 Using Correct Imperial Fittings 129 Installation 132 Keeping Leaks Under Control 146 Column Evaluation 146 Identifying and Removing Leaks 146 Expected K Factor 150 K Factor Tables 1...

Page 9: ...tivity Detector TCD 171 TCD Overview 172 TCD Gas Supplies 174 Columns 175 TCD Operating Modes 175 Constant Temperature 175 Constant Voltage 175 Selecting TCD Operating Parameters 177 Using the CT Mode 177 Using the CV Mode 177 Suggested Operating Values 178 TCD Menu 179 Detector Signal Parameters 181 Chapter 10 Autosamplers 187 Autosampler Overview 188 Sequence of Sample 188 Autosampler Configurat...

Page 10: ...Inject with an Autosampler enabled 213 Run 213 Chapter 12 Checkout Using FID with S SL 215 SOP number P0407 05 E 31 May 2006 216 Scope 216 Preliminary Operations 216 Parts Referenced 218 Analytical Conditions Required for FID S SL 219 Chapter 13 Checkout Using TCD with S SL 229 SOP number P0473 04 E 02 May 2007 230 Scope 230 Preliminary Operations 230 Parts Referenced 232 Analytical Conditions Req...

Page 11: ...dard Septum 262 When Cleaning or Replacing the Liner 262 If the Glass Liner Breaks Inside the Injector 263 Related Operating Sequences 263 Maintaining a PPKD Injector 276 When replacing the septum 276 When replacing the liner 276 Maintaining a FID 282 FID Troubleshooting 295 Change in Sensitivity 295 Gases 295 Flame Ignition 296 Maintaining a TCD 298 TCD Troubleshooting 300 Sensitivity 300 Baselin...

Page 12: ...pter 16 LAN Option Set up 321 Introduction 322 IP Address and LAN Communication Port 322 Reset Button 323 Network Cables 323 Set Up 324 Appendix A Customer Communication 337 How To Contact Us 337 Reader Survey 338 Glossary 339 Index 345 ...

Page 13: ... and menus This chapter contains also instructions to set up the software on your GC either to match the installed hardware or to reflect your preferences Chapter 3 Gas Control contains information on controlling and programming the carrier and detector gas flows to the FOCUS GC Chapter 4 Column Oven describes the features of the FOCUS GC column oven Chapter 5 Split Splitless Injector S SL describ...

Page 14: ... TCD with the Split Splitless Injector S SL Chapter 14 Checkout Using TCD with PPKD contains the operating procedure to check the Thermal Conductivity Detector TCD with the Purged Packed Injector PPKD Chapter 15 Maintenance and Troubleshooting contains information and operating sequences to perform the necessary maintenance of the instrument and also information concerning troubleshooting in case ...

Page 15: ...tles displayed on the computer screen or on a digital display This symbol illustrates menu paths to select such as File Open KEY NAME Bold uppercase sans serif font indicates the name of a key on a keyboard or keypad such as ENTER CAUTION This symbol alerts you to an action or sequence that if performed improperly could damage the instrument NOTE This symbol alerts you to important information rel...

Page 16: ...bol indicates the presence of flammable materials This symbol indicates the presence of radioactive material This symbol indicates an operation or sequence that must not be performed by the user A Thermo Fisher Scientific authorized Customer Support Engineer must perform this sequence This symbol indicates all metal objects such as watches and jewelry must be taken off This symbol indicates an eye...

Page 17: ...anual xvii This symbol indicates the user must wear protective shoes when performing the sequence This symbol indicates the user must wear protective clothing when performing the sequence This symbol indicates the user must wear gloves when performing the sequence ...

Page 18: ...s used on Thermo Fisher Scientific instruments Only a few of them are used on the FOCUS GC gas chromatograph Symbol Description Direct Current Alternating Current Both direct and alternating current Three phase alternating current Earth ground terminal Protective conductor terminal Frame or chassis terminal Equipotentiality On Supply Off Supply 3 ...

Page 19: ... for specific Warning or Caution information to avoid personal injury or damage to the product Caution risk of electric shock Caution hot surface Caution refer to accompanying documents In position of a bistable push control Out position of a bistable push control Symbol in compliance to the Directive 2002 96 EC on Waste Electrical and Electronic Equipments WEEE placed on the european market after...

Page 20: ...rmore Thermo Fisher Scientific part numbers PN for the paper copy manuals are provided for each book title Site Preparation and Installation Manual PN 317 094 11 This manual and diskette describes how to set up a workspace for the FOCUS GC and how to connect the FOCUS GC to the gas supplies and peripheral devices FOCUS GC Instruction Manual PN 317 094 12 This manual provides descriptions of the FO...

Page 21: ...85 Voltage variations not exceeding of the nominal value Transients according to installation categories II Degree of pollution according to IEC 664 3 7 3 2 Technical Features The following table summarizes the major technical features of the FOCUS GC Features Description External Interface RS232 Serial Line LAN Optional Power Supply 120 Vac 50 60 Hz 1600 VA 230 Vac 50 60 Hz 1600 VA Dimensions 680...

Page 22: ...ifications Before using chemicals please read the hazard indications and information reported in the Safety Sheet supplied by the manufacturer referring to the relevant CAS Chemical Abstract Service number Use of Gases WARNING Before using gases carefully read the hazard indications and information reported in the Safety Sheet supplied by the manufacturer referring to the CAS Chemical Abstract Ser...

Page 23: ...ocal regulations Make sure the gas supply is turned completely off when connecting hydrogen lines Perform a bubble test to ensure that the hydrogen lines are leak tight before using the instrument Perform this test after the pressure test described in the Testing for Leaks paragraph in FOCUS GC Site Preparation and Installa tion Guide Manual Repeat this test to eliminate all leaks Ensure your GC c...

Page 24: ...ut the room The reliability of the sensor depends on careful maintenance After the sensor is in use you must periodically check its operating performance and calibration as recommended by the manufacturer Refer to your hydrogen sensor s instruction manual for maintenance guidelines WARNING Never use hydrogen in FOCUS GC unless your GC oven has a hydrogen sensor installed Thermo Fisher Scientific C...

Page 25: ...verview of the features and options of the FOCUS GC gas chromatograph After each brief description of a FOCUS GC component you will find references to chapters in this manual containing more detailed information Chapter at a Glance Instrument Overview 26 GC Parts Description 31 ...

Page 26: ...pneumatic compartment contains the pneumatic gas control circuits The carrier gas control circuit is completely electronic digital pneumatics while the detector gas control circuit is conventional analog pneumatics Analytical Unit The analytical unit consists of two subcompartments the column oven the injector and detector compartment 1 Pneumatic Compartment 3 Electronic Compartment 2 Analytical U...

Page 27: ... for carrier gas control and conventional pneumatics for detector gases control Carrier Gas Control Carrier gas is controlled electronically through an electronic pneumatic control module Digital Pressure Flow Control DPFC mounted in the pneumatic compartment DPFC Module The DPFC module features the following constant pressure or constant flow operating modes inlet pressure control in kPa psi or b...

Page 28: ...n factory prior shipment and remains always at the set flow DGFC gas flow can be automatically switched on and off by using the FOCUS GC keypad Refer to Chapter 3 Gas Control Column Oven The FOCUS GC column oven has a high degree of thermal stability and fast heating and cooling The air circulation in the oven ensures the column is kept in a thermally homogenous and stable zone This provides more ...

Page 29: ...tor PPKD Columns The column is where the chromatographic separation of the sample occurs Several types of columns are available for different chromatographic applications capillary columns wide bore capillary columns packed column Refer to Chapter 7 Column Detector FOCUS GC is designed to operate with the following detectors Flame Ionization Detector FID This is one of the most used detectors in G...

Page 30: ... only provides the heating through the base body the gas supply and the signal analog to digital conversion for acquisition Instrument Automation FOCUS GC contains several automated features for running the GC communicating with other analysis equipment and interacting with a data system Autosampler Interface The TriPlus AI 3000 AS 3000 AS 2000 or HS 2000 autosampler can be connected to the GC Ref...

Page 31: ...is paragraph gives you a detailed description of the instrument components Front Panel Figure 1 2 FOCUS GC Front Panel It comprises Column Oven Status Panel and keypad Electronic Compartment 1 Column Oven Door 3 Status Panel and Keypad 2 Column Oven Door Push Button 4 Electronic Compartment 1 2 3 4 ...

Page 32: ...olumn oven door by pushing the relevant button Figure 1 3 Column Oven Internal View Refer To Chapter 4 Column Oven User Interface User interface shown in Figure 1 4 has three components a two line display display LEDs showing the instrument s status and a keypad for data entry Figure 1 4 FOCUS GC User Interface Refer To Chapter 2 The FOCUS GC User Interface ...

Page 33: ... compartment shown in Figure 1 5 comprises Low Voltage Section Mains Voltage Section Figure 1 5 Example of Electronic Compartment Low Voltage Section It contains the electronic circuits to operate and control the instrument WARNING A Li 3 V 220 mA h unrechargeable battery is present on the Main Board The battery replacement must be performed only by specialized technical personnel High Voltage Sec...

Page 34: ...tage section is provided of a series of protection fuses as reported in the following table Power Supply Breaker 120 Vac 15A 230 Vac 7A Fuse Type Protection F1 F2A IEC 127 I 5 x20 mm Injector heater element F2 T1 6A IEC 127 III 5 x20 mm 230 Vac Main power Breaker 120 Vac Main power Breaker F3 F2A IEC 127 I 5 x20 mm Auxiliary heater element F4 F0 63A IEC 127 I 5 x 20 mm Oven fan motor F5 F0 63A IEC...

Page 35: ...nnections 1 Carrier Gas Inlet Port 2 Detector Gas Inlet Ports 3 Servo Air Inlet port for GSV 4 Gas Sampling Valve Sample In Out Ports 5 Oven Exhaust Vent Area 6 Electrical connections REF MAKE UP CARRIER SERVO AIR max 500 kPa OUT SAMPLE EXT DET 10V 1V 0V GND AIR H2 MAKE UP IN SAMPLE WARNING HIGH TEMPERATURE OVEN EXHAUST AIR DO NOT PLACE TEMPERATURE SENSITIVE MATERIAL NEAR OPENINGS 2 2 H SENSOR 100...

Page 36: ...tion menu The following gives a brief conversion guide for the most commonly used pressure units 100 kPa 1 bar 14 51 psi Detector Gases Inlet Ports They are located on the middle upper part of the instrument rear panel Detector gas inlet ports are directly connected to the DGFC module WARNING Pressure of the supply gas lines should be set to a minimum of 400 kPa 60 psi to ensure the regulation of ...

Page 37: ... details refer to Gas Sampling Valve Overview Electrical Connections Electronic connections al located on the rear part of the electronic compartment As shown in Figure 1 7 Figure 1 7 Electrical Connections 1 Breaker marked POWER to switch the instrument On Off Position I instrument ON Position O instrument OFF 2 120 or 230 Vac 50 60 Hz Main socket marked 3 9 pin connector marked AUTOSAMPLER to di...

Page 38: ...sily recognizable by the presence on the GC rear panel of a RJ45 connector 2 LEDs for LAN activity and a reset button The FOCUS LAN sampler is shipped with a default IP address which may not match the LAN needs of the sites where the sampler must be installed To change the default values contact your LAN administrator and ask for the IP address to be assigned the netmask and eventually the port Th...

Page 39: ... during cooling down cycles Do not expose gas tanks or bottles chemicals regulators electrical cords or other temperature sensitive items to oven exhaust Top Panel Top panel is shown in Figure 1 8 Figure 1 8 Top Panel It comprises S SL or PPKD injector port Split and Purge lines vent FID or TCD detector For details refer to the following Chapters Split Splitless Injector S SL Purged Packed Column ...

Page 40: ...s sampling a 6 port valve is used A wide range of sampling loops allows the analysis of different sample volumes NOTE A sampling loop with 1 mL of volume is provided in the standard outfit The sampling loop is installed directly on the valve The switching between load sample and inject sample position and vice versa is controlled through the FOCUS GC keypad or through the GC method created with th...

Page 41: ...s and menus This chapter contains also instructions to set up the software on your GC either to match the installed hardware or to reflect your preferences Chapter at a Glance Overview 42 User Interface Main Menu 47 Configuration 51 Configuration Menu 52 Run Time Events 62 Run Log 64 Time 66 Valves 67 Info Diagnostics 68 ...

Page 42: ...us a keypad for data entry Figure 2 1 illustrates the complete FOCUS GC user interface Figure 2 1 The FOCUS GC User Interface The Display The display shows the menus you use to control the GC parameters settings and configuration options The data entry keys allow you to scroll through set and modify the menu information Figure 2 2 shows the components of a typical menu display ...

Page 43: ...ich is the setpoint that is edited Scroll Indicator This item is found in the upper right corner of the display It indicates that not currently visible menu items exist It appears in three ways indicating that you can scroll downward indicating that you can scroll upward indicating that you can scroll in either direction Currently Visible Menu Parameters The display shows four lines of a menu at a...

Page 44: ...to make a run for example when the setpoint oven temperature has not been reached It remains lit if any additional equilibration time has been configured It blinks when the GC has one or more error conditions Standby Prep Run This LED lights when the GC is in Standby waiting to be advanced to the Ready status It blinks when the GC prepares for a run for example during switching of valves required ...

Page 45: ... device such as an autosampler has been programmed the system automatically starts after injection The red STOP key has the following functions stops a run in progress resets the FOCUS GC from READY to NOT READY The STATUS key displays the instrument status includes the Not Ready messages The HOME key opens Main Menu and comes back to the returns precedent page menu The SCROLL UP and SCROLL DOWN a...

Page 46: ...ine is only for menu title and doesn t scroll Once you have reached the line related to the parameter to change increase or decrease the value by pushing the INC and DEC keys During editing the value of the parameter is blinking When the set value is the desired one press the ENTER key to accept the value Any key different from ENTER INC DEC will escape parameter editing without changes OVEN Menu ...

Page 47: ...ys 1 Line available only if an autosampler is present To open a page menu move the cursor up to the menu of interest then press ENTER key To come back precedent page menu press the HOME key Oven Use the Oven page to set temperatures times and ramp rates You can program up to four temperature ramps per run Refer to Chapter 4 Column Oven for more information about Oven menu options FOCUS GC OVEN INL...

Page 48: ...the pressure and flow modes you select You have a choice of two flow modes Constant pressure mode which sets pressure only Constant flow mode which maintains a specific flow rate through the column Refer to Chapter 3 Gas Control for more information about Carrier menu options Detector Use this page to display the detector menu Refer to Chapter 8 Flame Ionization Detector FID or Chapter 9 Thermal C...

Page 49: ...ector in use e g FID X is added in the title line Signal Use this page to display the FID or TCD detector signal menu The first item displays a unitless digital representation of the detector output The other items help make that output more measurable and meaningful Refer to Chapter 8 Flame Ionization Detector FID or Chapter 9 Thermal Conductivity Detector TCD for more information about Signal me...

Page 50: ...more information about autosampler menu options NOTE TriPlus and HS 2000 autosamplers are controlled only by all the Thermo Fisher Scientific Data Systems referring to the instructions reported in the relevant operating manuals Sequence Use this page to display the parameters required to perform an automatic sequence of samples This page is displayed only if an AS 2000 or AI AS 3000 autosampler is...

Page 51: ...ration Info Diagnostics Configuration This paragraph describes how to configure your FOCUS GC When to Configure You need to configure the system when using the FOCUS GC for the first time changing carrier gas changing column types to set the appropriate maximum oven temperature connecting an external detector For details refer to Configuration Menu OTHERS Configuration ...

Page 52: ...Controls preliminary actions such as an automatic prep run timeout equilibration time Carrier Controls the type of carrier gas Detector Allow to select an external detector when the signal coming from an external control module is desired This line is available ONLY if the FID board is present Autosampler Controls the autosampler connected General Visualizes the Main supply frequency Keyboard and ...

Page 53: ...ines the maximum allowable oven temperature setpoint to protect the column from unintentionally high temperatures This limit must be set to the manufacturer s maximum recommended operating temperature for the column Equil time 0 00 999 99 min This parameter defines the equilibration time to stabilize the oven temperature after the run Auto prep run On Off Set On to turn on automatic Prep Run execu...

Page 54: ...elium is often used as an alternative for carrier gas You specify the type of carrier gas in the CONFIGURE CARRIER menu by using the INC and DEC key WARNING Hydrogen items is disabled unless your instrument has a hydrogen sensor See Using Hydrogen CONFIGURE CARRIER Gas Type Helium Table 2 5 Configure Carrier Menu Parameter Range Comments CONFIGURE CARRIER This line is the title bar Gas type Helium...

Page 55: ... body the gas supply and the signal analog to digital conversion for acquisition You specify the type of external detector in the CONFIGURE DETECTOR menu by using the INC and DEC key The following list determine the type of gas to use with the different external detectors CONFIG DETECTOR Use external det Y Ext det type FID x ECD x NPD x FPD x PID x PDD x Hall x Other x External Detector Type Gas A...

Page 56: ... of autosampler connected to the GC you may find the following menus AS 2000 Autosampler AI 3000 AS 3000 Hall x H2 Make up Other x H2 Air Make up CONFIG AUTOSAMPLER Status Disabled Use Internal Std Yes Table 2 6 Configure AS 2000 Autosampler Menu Parameter Range Description CONFIG AUTOSAMPLER This line is the title bar Status Not Editable It shows the status of the autosampler Use Internal STd Yes...

Page 57: ...er Menu Parameter Range Description CONFIG AUTOSAMPLER This line is the title bar Syringe volume 5 10 µL Select the parameter according to the volume of the syringe installed on the autosampler Sample tray Not Editable The system automatically recognizes the type of sample tray installed on the autosampler 105 positions tray in the case of AS 3000 Autosampler 8 position tray in the case of AI 3000...

Page 58: ... display Keyboard beep leads to a submenu where you can specify when you want the GC to alert you with a keyboard sound To move to the submenu select Keyboard beep and press ENTER GENERAL CONFIG AC mains freq 50 Table 2 8 General Config Menu Parameter Range Description GENERAL CONFIG This line is the title bar AC mains freq 50 60 Mains frequency CONFIG KEYB DISP Keyboard lock Off Keyb Beep Enter k...

Page 59: ... to select a period or comma as a decimal marker Pressure units kPa psi bar Use this option to select the pressure unit for display Brightness 3 max 0 min Use this option to adjust the brightness of the display Table 2 10 Beep Table Parameter Range Description KEYBOARD BEEP This line is the title bar All key On Off This parameter causes the GC to beep when you press any key on keypad Enter key pre...

Page 60: ...rameter Range Description CONFIG HANDSHAKE This line is the title bar Remote Start IN Pulse High to Low default Pulse Low to High This parameter allows another device to start the FOCUS GC Inhibit Ready When Low default When High This parameters delays readiness until the GC receives a signal from another device End of Run OUT Pulse High to Low default Pulse Low to High This parameter signals anot...

Page 61: ...onfigure two gas sampling valves when present and program two external events to be the default condition for an external device See also Run Time Events CONFIGURE TIME Time 18 14 11 Date Mon 11 Mar 2002 Table 2 12 Configure Time Menu Parameter Range Description CONFIGURE TIME This line is the title bar Time hhmm This option has two editing fields sequenced by pressing ENTER Date Day Month Year Th...

Page 62: ...hen press ENTER The first time you program a time event Run Time Events empty the following menu appears Table 2 13 Configure Valves Menu Parameter Range Description CONFIGURE VALVES This line is the title bar Valve 1 None Gas Sampling Select in this box Sampling only if a gas sampling valve is present and connected the GC Otherwise select none Valve 2 The same as Valve 1 EV 1 default On Off Selec...

Page 63: ...line end press ENTER to add an event EDIT EVENTS Event EV 1 Run time Pre run Setpoint 2 Next event Table 2 14 Edit Time Event Menu Parameter Range Description EDIT TIME EVENTS This line is the title bar Event Det autozero Det range Det gain 1 Det neg pol 1 EV 1 EV 2 GSValve 1 GSValve 2 Select the event you want to program Run time 0 00 to 599 99 minutes Prep run Select a time if you want to activa...

Page 64: ... the run log will record the time the run stopped and a description of the event The Run log is cleared and reset at the beginning of the next run Run log entries are shown pressing the STATUS key To see the details Run Log entries in Main Menu move the cursor until the Others page is selected then press ENTER Scroll to Run log then press ENTER An example of Run log is shown below Setpoint From 0 ...

Page 65: ...at run time 3 40 continue 2 3 Itime 200 00 220 00 at run time 0 50 ITemp 120 100 at run time 2 00 Ftime 1 00 10 00 at run time 2 50 Ramp2 50 0 120 0 at run time 3 10 Detector gain 1 10 at run time 3 50 Detector neg pol Y N at run time 3 30 Oven T is 105 110 at run time 3 40 continue 2 3 with FID with TCD Line Description 1 The number of entry X of Y e g 1 of 12 is displayed in the title line 2 The...

Page 66: ...ime remaining during the current run The flow calculator In Main Menu move the cursor until the Others page is selected then press ENTER Scroll to Time then press ENTER When the GC is not running a menu appears as follows When the GC is running a menu appears as follows OTHERS Time TIME Next runtime 15 00 Last runtime 120 00 We 13 Mar 2002 12 03 V 100 F 100 0 01 00 Flowmeter volume 100 ...

Page 67: ...a run Switch a gas sampling valve from load to inject position Activate or deactivate an external event In the Main Menu move the cursor until the Others page is selected then press ENTER Scroll to Valves then press ENTER When a gas sampling valve is not present a menu appears as follows TIME Elapsed time 5 00 Time left 110 00 We 13 Mar 2002 12 03 V 100 F 100 0 01 00 Measured volume 100 OTHERS Val...

Page 68: ... In Main Menu move the cursor until the Others page is selected then press ENTER Scroll to Info Diagnostics then press ENTER A menu appears as follows VALVES Split valve Off Sept purge valve On GSValve 1 Load EV 1 Off Table 2 15 Valves Parameter Range Description VALVES This line is the title bar Split valve On Off Switches On Off the SSL split valve Sept purge valve On Off Switches On Off the SSL...

Page 69: ...INFO DIAGNOSTICS This line is the title bar Serial T The number eight figures indicates the product code FM ver Indicates the version of the firmware DPFC ver Indicates the version of the DPFC module BOOT ver Data for Thermo Fisher Scientific authorized technical personnel only Manufact Indicates the manufacturing date of your GC Total runs The number seven figures Indicates the performed analyses...

Page 70: ...Chapter 2 The FOCUS GC User Interface Info Diagnostics 70 Instruction Manual ...

Page 71: ...and detector gas flows to the FOCUS GC Chapter at a Glance Gas Supplies 72 Carrier Gas Regulation 75 Detector Gas Regulation 75 Measuring Gas Flow 78 Carrier Gas Parameters 80 Operating Sequences Configuring the Carrier Gas 73 Configuring The Pressure Unit 74 Measuring the Detector Gas Flows with a Bubble Meter 78 ...

Page 72: ...the kilo pascal kPa WARNING Hydrogen is a dangerous gas that when mixed with air may create an explosive mixture The use of hydrogen as a carrier gas requires the operator s extreme caution Special precautions must be taken because of the risk of explosion The gas chromatograph must be equipped with a hydrogen sensor if you use hydrogen as a carrier gas Refer to Using Hydrogen for more information...

Page 73: ...d to Helium To change the configuration proceed as follows 1 In the Main Menu move the cursor until Others is selected then press ENTER 2 Scroll to Configuration then press ENTER 3 Scroll to Carrier then press ENTER 4 Select the required type of carrier gas by using INC and DEC keys 5 Press HOME to exit CONFIGURE CARRIER Gas type Helium ...

Page 74: ...e the configuration proceed as follows 1 In the Main Menu move the cursor until Others is selected then press ENTER 2 Scroll to Configuration then press ENTER 3 Scroll to Keyboard Display then press ENTER 4 Scroll to Keyboard Display then press ENTER 5 Select the required type of carrier gas by using INC and DEC keys 6 Press HOME to exit CONFIG KEYB DISP Pressure unit kPa ...

Page 75: ...sure 50 kPa higher than the maximum carrier pressure required by the application The maximum input pressure to DPFC is 1000 kPa Detector Gas Regulation The detector gases control module has conventional pneumatic regulators which and providescontrol for the detector gases WARNING Pressure of the supply gas lines should be set to a minimum of 400 kPa 60 psi to ensure the regulation of detector gase...

Page 76: ...e FID detector control menu to turn the flow on off TCD Gases The TCD detector requires the same gas whether for the measure channel carrier and make up gas when necessary and the reference channel reference gas Helium is the recommended carrier gas due to its high thermal conductivity and chemical inertness The adjustment of the detector gases flow is done in factory prior shipment Gas Flow Hydro...

Page 77: ... 3 2 TCD Detector Gases Flow Regulation The flow is measured at the exit of the detector Enter the TCD detector control menu to turn the flow on off Gas Flow Helium make up gas 27 mL min Helium reference gas 30 mL min 1 turn clockwise of the regulation screw increases the flow of about 2 5 mL min 1 turn counterclockwise of the regulation screw decreases the flow of about 2 5 mL min Ref Make up OPE...

Page 78: ...er Materials required Graduated bubble flowmeter the bulb must be half filled with a soap solution Detector base body adapter for FID only WARNING Do not measure hydrogen together with air or oxygen This can create an explosive mixture Always measure the gases separately 1 Attach the inlet line of the flowmeter to the exit of the detector base body using the adapter 2 While holding the bubble flow...

Page 79: ...00 7 When the meniscus passes the flowmeter start line marked 0 press ENTER to start the stopwatch 8 When the meniscus passes the flowmeter line corresponding to the volume set in Measured vol press ENTER to stop the stopwatch The flow rate in mL min is automatically calculated and the value is displayed ...

Page 80: ...arrier gas type Parameters change according to the selected flow mode constant flow or constant pressure In Main Menu move the cursor until Carrier is selected Press ENTER to open the CARRIER menu Flow Mode Two flow modes are available Constant Flow In constant flow mode the column flow is kept constant throughout the analysis The pressure at the column head will change with the column temperature...

Page 81: ... steps of 0 1 ml min Off It is displayed when Constant Flow is selected in Flow Mode Enter a column flow for the analytical column Pressure From 10 to 1000 kPa from 2 5 to 250 kPa in step of 1 kPa Off It is displayed when Constant Pressure is selected in Flow Mode Enter inlet pressure for the analytical run Flow Mode Constant Flow Constant Pressure Set the operating mode required Selecting Constan...

Page 82: ... the column flow with a true mass flow sensor and compares it to the calculated flow from the original column constant to see if the numbers match The instrument assumes a gas leak exists if there is a significant difference To perform a leak check refers to Chapter 6 Performing an Automatic Leak Check Column evaluation The column evaluation is an automatic measurement of the column resistance tha...

Page 83: ...es of the FOCUS GC column oven Chapter at a Glance Column Oven Overview 84 Column Oven Configuration 86 Oven Parameters 87 Operating Procedures Configuring the Column Oven 86 Setting Up a Single Ramp Temperature Program 89 Setting Up Multiple Ramp Temperature Program 90 ...

Page 84: ... of thermal stability Figure 4 1 The FOCUS GC Column Oven Opening the oven door activates a safety microswitch which automatically turns off the oven heating and the fan motor The column oven has the following capabilities maximum temperature of 350 C maximum temperature increase rate of 120 C min seven linear temperature ramps and eight levels minimum operating temperature of a few degrees above ...

Page 85: ... display shows the following safety message To return to normal operation close the oven door WARNING The oven vents at the rear of the GC discharge hot air during cooling WARNING Hydrogen is a potentially dangerous gas When hydrogen is used as a carrier gas the column oven must have a hydrogen sensor Refer to Using Hydrogen for hydrogen safety information OVEN Temp 100 door open ...

Page 86: ...s and confirm pressing ENTER 1 In Main Menu move the cursor until Others is selected Scroll to Configuration then press ENTER 2 Scroll to Oven then press ENTER 3 Scroll to Max temperature and set the maximum allowable oven temperature 4 Scroll to Equilibrium time and set the oven temperature equilibration time 5 Scroll to Auto prep run Set On to enable automatic prep run Set Off if you want the pr...

Page 87: ...on OVEN This line is the title bar Temperature On Off From 20 C to 350 C in step of 1 C Set On to display the actual and set point values Set the initial temperature in C at which the oven is set and conditioned before the GC enters the sampling phase Initial Time INF From 0 to 99 99 minutes Set the time in minutes The oven remains at the starting temperature after a programmed run has begun Setti...

Page 88: ... program the first ramp the menu adds the Ramp 2 parameter lines If you do not want an additional ramp leave this parameter set to Off To program the ramp set On The Final temp and Final time lines for the ramp will be added to the menu You can repeat this process to program up to seven temperature ramps Final temp 2 7 From 20 to 350 C in step of 1 C This parameter defines the temperature the colu...

Page 89: ...ressing ENTER Figure 4 2 Example of Single Ramp Temperature Program 1 In Main Menu move the cursor until Oven is selected Press ENTER to display the OVEN menu 2 Scroll to Temp and enter the initial the initial temperature 3 Scroll to Initial Time and enter the time you want the oven to maintain the initial temperature 4 Scroll to Ramp 1 and set it On Enter the ramp rate in C min for the oven to re...

Page 90: ...ture to a specified final temperature through up to three ramps each having a specified ramp rate time and temperature Use INC and DEC keys to increase or decrease the parameter values and confirm pressing ENTER Figure 4 3 Example of Multiple Ramp Temperature Program 1 In Main Menu move the cursor until Oven is selected Press ENTER to display the OVEN menu 2 Scroll to Temp and enter the initial th...

Page 91: ...the final temperature for the ramp 6 Scroll to Final Time 1 and enter the time the oven will maintain the Final temp 7 Scroll to Ramp 2 and set it On Enter the ramp rate in C min for the second temperature program 8 Scroll to Final Temp 2 and enter the final temperature for the second ramp 9 Scroll to Final Time 2 and enter the time the oven will maintain the Final temp 10 To end the multiple ramp...

Page 92: ...Chapter 4 Column Oven Oven Parameters 92 Instruction Manual ...

Page 93: ... operating sequences for the different split splitless operating modes Chapter at a Glance S SL Overview 94 S SL Injection Techniques 101 S SL Inlet Parameters 107 Operating Sequences Installing a Liner and a Septum 99 Programming the Split Mode 110 Programming the Splitless Mode 111 Programming the Surge Splitless Mode 112 ...

Page 94: ...either split or splitless applications to ensure effective sample transfer into the column minimizing heavy component discrimination Figure 5 1 Split Splitless Injector 1 Septum Cap 7 Graphite Column Ferrule 2 Septum 8 Capillary Column 3 Liner Seal A Carrier Gas Inlet 4 Glass Liner B Split Line 5 Fixing Nut C Septum Purge Line 6 M4 Retaining Nut ...

Page 95: ...l DPFC controls the split flow while the septum purge flow is kept constant by a calibrated flow regulator The S SL injector is also equipped with electronically actuated On Off valves for split and septum purge lines Volatile components given off by the hot septum can produce ghost peaks in a chromatogram The septum purge system can continually purge the septum with a flow of gas This prevents th...

Page 96: ...Injector Components 1 Septum Cap 9 Injector Body 2 Spring 10 Metal Ring 3 Septum Holder 11 Fixing Nut 4 Septum 12 Silver Seal 5 Septum Support 13 Terminal Fitting 6 Liner Cap 14 Fixing Nut 7 Liner 15 Graphite Column Ferrule 8 Graphite Liner Seal 16 M4 Retaining Nut 10 13 14 15 16 11 12 8 9 1 2 3 4 5 6 7 ...

Page 97: ...levant installation kit is required High pressure capability allows operation from 15 to 700 kPa 2 100 psi Longer life reduces the changes of septum leaks occurring during extended automated runs Microseal valve requires a 0 63 mm diameter 0 025 inch blunt tip syringe Liners You may choose amomg different types of glass liners depending on the injection mode used Table 5 1 shows the liner options ...

Page 98: ... SL Overview 98 Instruction Manual Packed Columns With a special adapting kit you can install packed columns in the S SL injector as shown in Figure 5 4 Figure 5 4 S SL with a Packed Column 1 Carrier Gas Inlet 3 Septum Purge Line 2 Split Line ...

Page 99: ...N Be careful not to break the graphite or to allow graphite to enter the liner 2 Hold the top of the liner with tweezers Lower it bevelled end first into the injector The liner should rest on the terminal fitting at the bottom of the injector 3 Hold the top of the liner with tweezers Lower it bevelled end first into the injector The liner should rest on the terminal fitting at the bottom of the in...

Page 100: ...mplete injector assembly CAUTION To avoid contamination do not touch the septum with your hands 7 Gently screw the septum cap onto the injector assembly until finger tight to hold the septum in place WARNING If the injector is hot use the liner cap wrench to turn the septum cap Do not overtighten the septum cap The septum will deform and may be difficult to penetrate with the syringe needle ...

Page 101: ...n of the sample goes into the column while the remainder is carried out the split line You set the column flow and the split flow in the INLET menu Narrow bore columns which have inherently low column flows can produce relatively high split ratios NOTE Hot Empty Needle Injection Technique To prevent partial sample vaporization within the hot syringe needle and avoid discrimination of higher boilin...

Page 102: ...al Figure 5 5 Split Injection Technique The major advantage of split injection is and the ability to introduce samples over a wide range of concentrations Peak shapes are very sharp due to the rapid sample introduction into the column 1 Carrier Gas Inlet 3 Septum Purge Line 2 Split Line ...

Page 103: ...ine opens to flush the vaporization chamber of any remaining solvent vapors Figure 5 6 shows the split spliless injector when used for splitless injection During splitless injection when the split valves are closed the flow of gas through the injector is relatively low It is equal to the column flow only a few mL min The injector can accept and quantitatively transfer to the column sample volumes ...

Page 104: ... column takes place slowly due to the low column flows involved With typical carrier gas flow rates of 1 4 mL min the transfer can take between 30 and 90 seconds depending on a variety of circumstances This transfer time should correspond to he splitless time You can set the splitless time in the INLET menu when you select Splitless mode 1 Carrier Gas Inlet 3 Split Line 2 Septum Purge Line ...

Page 105: ...g the injection of the sample to trap it at the column head by condensation thermal focusing or solvent effect Thermal Focussing or Phase Trapping The components are refocussed by keeping the oven temperature during injection at about 80 90 C below their elution temperature In these conditions the components are not substantially moving into the column They are then related as a sharp band when ov...

Page 106: ...olumns 0 2 mm ID are used NOTE Hot Empty Needle Injection Technique To prevent partial sample vaporization within the hot syringe needle and avoid discrimination of higher boiling components we recommed to use the Hot Empty Needle Injection Technique particularly when performing manual injection This technique consists of drawing the sample volume into the syringe barrel followed by a small air ga...

Page 107: ...nu vary depending on the operating mode you select in theINLET menu The following table shows the split splitless inlet menu for the operating modes INLET S SL Mode Split Table 5 2 Inlet Modes Mode Description Parameters to Program Split Use this injection mode when analyzing high concentration or neat samples or in instances where sensitivity is less important The split vent remains open all the ...

Page 108: ... Table 5 3 Inlet Parameters Menu Menu Range Comments INLET This line is the menu title bar Temp 50 375 C This line shows the base injector temperature Mode Split Splitless Surge Splitless This line displays the operating mode selected Total flow Not editable This line shows the total gas flow consumption which is the sum of the column flow split flow or gas saver flow and septum purge flow Split f...

Page 109: ... Surge Duration you program Surge duration 0 99 99 min in steps of 0 01 min This line indicates the duration of the surge pressure after run start Const sept purge On Off Set ON to activate a constant septum purge to continuously flush the septum with a purge flow of 5 mL min when using helium or nitrogen as a carrier gas or 10 mL min when using hydrogen as a carrier gas Stop purge for 0 99 99 min...

Page 110: ...aks Program the carrier gas flow as described in Chapter 3 Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Split 3 Scroll to Temp and set the appropriate value 4 Specify the split flow or the split ratio To set Split Flow enter the value in the...

Page 111: ...led the correct liner is in the injector and the system is free of leaks Program the carrier gas flow as described in Chapter 3 Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Splitless 3 Scroll to Temp and set the appropriate value 4 Scroll to...

Page 112: ...as described in Chapter 3 Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Surge Splitless 3 Scroll to Temp and set the appropriate value 4 Scroll to Split Flow and enter the desired value 5 Scroll to Splitless Time and enter the time the inlet ...

Page 113: ...jection techniques and operating sequences Chapter at a Glance PPKD Overview 114 PPKD Injection Techniques 116 PPKD Injector Menu 116 Operating Sequencess Replacing a Septum 119 Programming the PPKD Injector Wide bore Mode 120 Programming the PPKD Injector Surged Wide bore Mode 121 Programming the PPKD Injector Packed Mode 122 Programming the PPKD Injector Surged Packed Mode 123 ...

Page 114: ...ctor accepts wide bore capillary columns The sample vaporizes in a liner and enters the wide bore capillary column The injector temperature is controllable from 50 C to 375 C Figure 6 1 shows the PPKD injector Figure 6 1 Purged Packed Column Injector 1 Septum Cap 6 Column Ferrule 2 Septum 7 M4 Split Retaining Nut 3 Liner 8 Wide Bore Column 4 Liner Ferrule A Septum Purge Line 5 Adapter B Carrier Ga...

Page 115: ...nts Figure 6 2 PPKD Injector Components 1 Septum Cap 2 Injector Body 3 Anti rotation Plate 4 Washer 5 Retaining Nut 6 Spacer 7 Septum 8 Liner 9 Adapter for Wide bore Columns 10 Retaining Nut 11 Graphite Ferrule for 0 53 mm ID Column 12 Liner Seal 13 Fixing Nut for Column 11 Fixing Nut for Column 9 10 13 1 7 6 12 2 3 4 5 8 11 ...

Page 116: ...et temperature should be sufficiently high to guarantee the sample completely vaporizes while avoiding the possible sample component decomposition PPKD Injector Menu The INLET menu includes the operating parameters for the purged packed injector The parameters you can edit depend on the operating mode chosen Wide bore Packed Wide bore w surge or Packed w surge In Main Menu move the cursor until In...

Page 117: ...e The column flow is regulated by changing the pressure as the temperature changes Surged W bore The column flow is regulated by changing the pressure as the temperature changes A carrier gas pressure surge activates during the injection phase for a preset time Surge pressure Surge duration Packed Mode Wide bore Mode INLET PPKD INLET PPKD Temp 200 200 Mode Packed Const sept purge Off Stop purge fo...

Page 118: ... ENTER to open the INLET MODE submenu Surge pressure 10 1000 kPa 2 5 250 kPa in steps of 1 kPa This line indicates the surge pressure Only used with surged packed and surged w bore modes Surge duration 0 999 9 min This line displays the duration of surge pressure after run start Const sept purge On Off Set YES to activate a constant septum purge to continuously flush the injector with a purge flow...

Page 119: ...emperature before replacing the septum 1 Remove the septum cap from the injector 2 Using tweezers remove the septum from the septum cap 3 Place a new septum in the septum cap CAUTION To avoid contamination do not touch the septum with your hands 4 Gently tighten the septum cap onto the injector assembly until finger tight Do not overtighten the septum cap The septum will deform and may be difficul...

Page 120: ...gram the carrier gas flow as described in Chapter 3 Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Wide bore 3 Scroll to Temp and set the appropriate injector temperature 4 If constant septum purge is required scroll to Constant Septum Purge a...

Page 121: ...re and detector temperature Program the carrier gas flow as described in Chapter 3 Gas Control WARNING Hydrogen is a potentially dangerous gas Refer to Using Hydrogen for safety information Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Surged...

Page 122: ...WARNING Hydrogen is a potentially dangerous gas Refer to Using Hydrogen for safety information Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Packed and press ENTER 3 Scroll to Temp and enter the appropriate injector temperature 4 If constant ...

Page 123: ...e Program the carrier gas flow as described in Chapter 3 Gas Control WARNING Hydrogen is a potentially dangerous gas Refer to Using Hydrogen for safety information Proceed as follows Use INC and DEC keys to increase or decrease the parameter values 1 In Main Menu move the cursor until Inlet is selected Press ENTER to display the INLET menu 2 In the Mode line select Surged packed 3 Scroll to Surge ...

Page 124: ...Chapter 6 Purged Packed Column Injector PPKD PPKD Injector Menu 124 Instruction Manual ...

Page 125: ...uction 126 Capillary and Wide bore Columns 126 Packed Columns 128 Installation 132 Keeping Leaks Under Control 146 Column Conditioning 156 Operating Sequences How to Connect a Capillary Column 132 How to Connect a Packed Column 138 Manual Checking for Leaks 147 Performing a Column Evaluation 148 Performing an Automatic Leak Check 154 ...

Page 126: ...ou must use the proper column ferrules and retaining nuts Column Ferrules Graphite ferrules are used for many column connections Encapsulated graphite ferrules connect the capillary column to the detector base body and to the injector CAUTION Overtightening compression ferrules does not necessarily produce a stronger leak free joint In fact very often the reverse is true Too much pressure can caus...

Page 127: ...and removal Figure 7 1 shows how to connect capillary or wide bore column to injector and detector base body Figure 7 1 Capillary Wide Bore Column to Injector and Detector Base Body Connections Table 7 1 Ferrules Capillary Column Graphite Ferrules 0 1 mm ID 0 25 mm ID 0 25 mm ID 0 35 mm ID 0 32 mm ID 0 45 mm ID 0 53 mm ID 0 8 mm ID 1 Capillary Wide bore Column 2 Graphite Ferrule 3 M4 Split Retaini...

Page 128: ... mm OD are the metric packed columns most commonly used Using Correct Metric Fittings To connect packed columns to injector and detector base bodies you must use the correct column ferrules and retaining nuts Metric Column Ferrules Metal packed columns require double brass ferrules front and back Metric Retaining Nuts Use hexagonal 1 4 inch column retaining nuts to connect all metal packed columns...

Page 129: ...ules and retaining nuts Imperial Column Ferrules Use Swagelok ferrules front and back with a 1 4 inch hexagonal nut to connect 1 4 inch metal packed columns to injector and detector metric imperial adapters Use Swagelok ferrules front and back and Swagelok nuts to connect 1 8 inch metal packed columns to injector and detector metric imperial adapters Imperial Retaining Nuts Use Swagelok nuts to co...

Page 130: ...pter Figure shows an example of adapters Figure 7 3 Injector and Detector Base Body Adapters Table 7 3 Imperial Size Packed Column Fittings Column Type Ferrules Retaining Nut metal column 1 4 inch Swagelok 1 4 inch hexagonal 1 4 inch metal column 1 8 inch Swagelok 1 8 inch Swagelok 1 8 inch A PPKD Injector 3 Adapter for PPKD B Detector Base Body for Packed Column 4 Double Ferrule C TCD Base Body 5...

Page 131: ...lary column by using the appropriate conversion kit as shown in Figure 7 4 Figure 7 4 Convertion Kit A S SL Injector 4 Double Ferrule B Detector base Body for Capillary Column 5 Nut C TCD Base Body 6 Ferrule 1 Ferrule 7 Adapter for Detector Base Body 2 Nut 8 Adapter for TCD Detector 3 Adapter for S SL Injector 9 Double Ferrule 1 2 3 4 5 6 7 4 5 A B 8 C 2 9 ...

Page 132: ...ect a Capillary Column Operating Sequence How to Connect a Packed Column Operating Sequence OPERATING SEQUENCE How to Connect a Capillary Column To install the capillary column the following sequential steps should be performed Installing the Column Support Preparing a Capillary Column Connecting to an S SL Injector Connecting to an PPKD Injector Connecting to a FID Detector Connecting to a TCD De...

Page 133: ...ired ceramic scoring wafer 1 Hold the capillary column between your thumb and index finger with the column extending past the tip of your index finger 2 Score the column very gently Excessive force could crush the column end 3 Snap off the end of the column 4 Inspect the column end for an even flat cut Metal Capillary Column To obtain a correct cut of metal capillary column use a triangular file M...

Page 134: ... column 2 Cut at least 1 cm from the column end 3 Place the column on the column support 4 Use typewriter correction fluid or a felt tipped pen to mark the correct position of the ferrule from the end of the column depending on the injection technique The correct positions are as follows 40 mm for split injection 64 mm for splitless injection 50 mm for splitless injection when using a packed liner...

Page 135: ...ctor PPKD Materials required M4 column retaining nut graphite ferrule 6 mm wrench 1 Slide the graphite ferrule onto the wide bore column with the bevelled end facing the injector Be careful to avoid damaging the graphite ferrule when inserting the column 2 Cut 1 cm from the column end 3 Place the column on the column support 4 Insert the column into the injector and slide the ferrule up to the inj...

Page 136: ... column retaining nut graphite ferrule 6 mm wrench typewriter correction fluid or felt tipped pen 1 Slide the graphite ferrule onto the capillary column with the beveled end facing the detector base body Be careful to avoid damaging the graphite ferrule when inserting the column 2 Cut 2 3 cm from the column end 3 Use the typewriter correction fluid or felt tipped pen to mark the column 80 85 mm fr...

Page 137: ...nted on the detector base body Materials required M4 column retaining nut graphite ferrule 6 mm wrench capillary column adapter 1 Connect the capillary column adapter to the detector base body 2 Slide the graphite ferrule onto the column with the beveled end facing the injector Be careful to avoid damaging the graphite when inserting the column 3 Cut 2 3 cm from the column end 4 Insert the column ...

Page 138: ...eparing a Metal Packed Column Connecting a Packed Column to a PPKD Injector Connecting a Packed Column to the S SL Injector Connecting a Packed Column to the TCD Detector Preparing a Metal Packed Column Before you begin verify that the proper adapters are installed on the injector and detector side Slide the fittings onto the packed column injector and detector ends in the order and direction show...

Page 139: ...se the wrench to tighten the retaining nut Use no more pressure than is necessary to obtain a good seal 1 4 to 1 2 turn 5 Insert the inlet end of the column to the adapter base as far as possible 6 Slide the ferrule up to adapter base then finger tighten the column retaining nut until it starts to grip the column 7 Use the wrench to tighten the retaining nut Use no more pressure than is necessary ...

Page 140: ...reference to Figure 7 6 proceed as follows Figure 7 6 Removing the S SL Injector Top Components a Unscrew the injector cap b Remove the septum holder with septum then the septum support c Remove the liner cap by using the tool provided d Use tweezers to remove the liner with the graphite seal 1 Injector Cap 2 Septum Holder 3 Septum 4 Septum Support 5 Liner Cap Removing Tool 6 Liner Cap 7 Liner 8 G...

Page 141: ... SL Injector Bottom Components a Unscrew the retaining nut at the bottom of the injector b Remove the terminal fitting and the silver seal 3 Install the metal adapter With reference to Figure 7 8 proceed as follows Figure 7 8 Metal Adapter Installation 1 Terminal Fitting Retaining Nut 2 Terminal Fitting 3 Silver Seal 1 Ferrule 2 Retaining nut 3 Metal Adapter 1 2 3 3 2 1 ...

Page 142: ...base then finger tighten the retaining nut until it starts to grip the metal liner d Slide the appropriate graphite seal and push it onto the metal adapter from the top of the injector by using the appropriate tool as shown in Figure 7 9 Figure 7 9 Graphite Seal Installation Tool 4 Reinstall the S SL Top Components With reference to Figure 7 10 proceed as follows 1 Graphite Seal Installation Tool ...

Page 143: ...ip the graphite seal then tighten the metal adapter retaining nut b Reinstall the septum support septum septum holder then screw the injector cap 5 Connect the Packed Column With reference to Figure 7 11 proceed as follows Figure 7 11 Connecting the Packed Column 1 Liner Cap 2 Liner Cap Removing Tool 3 Septum Support 4 Septum 5 Septum Holder 6 Injector Cap 1 2 3 4 5 6 ...

Page 144: ... to reseal that particular joint when changing columns Connecting a Packed Column to the TCD Detector Materials required metric imperial retaining nut metric imperial ferrules 10 mm or 1 4 inch wrench adapter for detector 1 Insert the appropriate adapter into the bottom of the detector base then push up the adapter into the detector base as far as possible 2 Slide the ferrule up to detector base t...

Page 145: ...han is necessary to obtain a good seal 1 4 to 1 2 turn CAUTION Overtightening the compression ferrule does not necessarily produce a stronger leak free joint In fact very often the reverse is true Overtightening can cause a leak in the joint and make it very difficult to reseal that particular joint when changing columns ...

Page 146: ...nse with the K Factor values reported in K Factor Tables Refer to Performing a Column Evaluation operating sequence If the value obtained does not agree with the one reported on the card this means that the leaks have not been repaired Performing the Column Evaluation is the necessary condition for the success of any subsequent Automatic Leak Check Identifying and Removing Leaks If the Automatic L...

Page 147: ...eal it 2 Set split and purge valves Off See Controlling Valves 3 Increase the carrier gas pressure to 150 200 kPa and allow the column and injector pressure to stabilize This can take up to 30 seconds 4 Reduce the pressure to 50 kPa 5 Observe the actual pressure In a leak tight system the pressure should not drop more than 1 kPa minute 6 If your installed column is leak tight remove the septum and...

Page 148: ...o the flow and the column temperatures This operation must be carried out every time a new column is installed Before performing the column evaluation a manual checking for leaks of the system must be carried out The GC must not be performing a run and must be isothermally stable before you can perform a column evaluation 1 In Main Menu move the cursor until Carrier is selected then press ENTER 2 ...

Page 149: ...e the response with the K Factor values reported in paragraph Expected K Factor according to the carrier gas used 6 If the value obtained does not agree with the one reported on the K Factor Tables this means that the leaks have not repaired NOTE Performing the Column Evaluation is the necessary condition for the success of any subsequent Automatic Leak Check 7 In case of error the following massa...

Page 150: ...al tolerances For example a 30 m x 0 25 mm column will typically give K factors of 1 5 2 0 Large deviations from the expected values will indicate leaks in the septum or column ferrule or a plugging of the column at the inlet or exit points NOTE Porous layer open tubulat PLOT columns will exhibit actual K factor higher than the expected values depending on the particles packing K Factor Tables Hel...

Page 151: ... 15 6 58 3 17 2 08 1 42 0 852 0 318 0 042 20 8 77 4 23 2 78 1 90 1 14 0 423 0 056 25 11 0 5 29 3 47 2 37 1 42 0 529 0 070 30 13 2 6 34 4 16 2 84 1 70 0 635 0 084 35 15 3 7 40 4 86 3 32 1 99 0 741 0 098 40 17 5 8 46 5 55 3 79 2 27 0 847 0 113 45 19 7 9 52 6 24 4 26 2 56 0 953 0 127 50 21 9 10 6 6 94 4 74 2 84 1 06 0 141 55 24 1 11 6 7 63 5 21 3 13 1 16 0 155 60 12 7 8 33 5 69 3 41 1 27 0 169 65 13 ...

Page 152: ... 15 29 7 5 87 2 83 1 86 1 27 0 760 0 283 0 037 20 7 82 3 77 2 48 1 69 1 01 0 378 0 050 25 9 78 4 72 3 09 2 11 1 27 0 472 0 063 30 11 7 5 66 3 71 2 54 1 52 0 566 0 075 35 13 7 6 60 4 33 2 96 1 77 0 661 0 088 40 15 6 7 54 4 95 3 38 2 03 0 755 0 100 45 17 6 8 49 5 57 3 80 2 28 0 850 0 113 50 19 6 9 43 6 19 4 23 2 53 0 944 0 125 55 21 5 10 4 6 81 4 65 2 79 1 04 0 138 60 11 3 7 43 5 07 3 04 1 13 0 151 ...

Page 153: ...0 19 9 3 93 1 90 1 25 0 850 0 510 0 190 0 025 25 24 9 4 92 2 37 1 56 1 06 0 637 0 237 0 031 30 5 90 2 85 1 87 1 28 0 765 0 285 0 037 35 6 89 3 32 2 18 1 49 0 892 0 332 0 044 40 7 87 3 80 2 49 1 70 1 02 0 380 0 050 45 8 85 4 27 2 80 1 91 1 15 0 427 0 057 50 9 84 4 74 3 11 2 13 1 27 0 475 0 063 55 10 8 5 22 3 42 2 34 1 40 0 522 0 069 60 11 8 5 69 3 74 2 55 1 53 0 570 0 076 65 12 7 6 17 4 05 2 76 1 6...

Page 154: ...rence between the two values To start the leak check operate as follows 1 In Main Menu move the cursor until Carrier is selected then press ENTER 2 Scroll to Leak check and press ENTER to open Leak Check menu 3 To start column evaluation scroll to Run leak check and press ENTER 4 The system is automatically pressurized with carrier gas and sealed to perform leak check NOTE To exit LEAK CHECK menu ...

Page 155: ...lowing message is displayed 6 If leaks are found an error message will be displayed In this case eliminate leaks and repeat the leak check procedure Note that only a previous Column Evaluation performed in a condition of true tightness can ensure the validity of the subsequent Automatic Leak Check responses LEAK CHECK Carrier press Off LEAK CHECK GC running LEAK CHECK Packed mode LEAK CHECK Leak c...

Page 156: ...alyses provided that temperature is within the operating range of the column For detailed information on column conditioning of your specific column refer to the column manufacturer s instructions CAUTION With the column already installed before starting column conditioning disconnect the column outlet from the detector With the column not already installed connect only the column inlet to the inj...

Page 157: ...ensitivity good operational stability and wide linear response the FID remains the most popular detector for gas chromatography Chapter at a Glance FID Overview 158 FID Gas Supplies 161 FID Installation 162 FID Menu 164 Detector Signal Parameters 166 Operating Procedures Programming a FID 167 Setting the FID Signal Parameters 169 ...

Page 158: ...he ions that are generated during the combustion process of organic compounds The resulting ionization current is sensed by an electrometer amplifier and converted to a suitable output signal Figure 8 1 shows the FID Figure 8 1 Flame Ionization Detector Detector Base Body The detector FID is easily interchangeable because of base body that acts as a bridge between the detector and analytical colum...

Page 159: ...flows are pre set in the factory You may set the flows On or Off Refer also to paragraph FID Gas Supplies Figure 8 2 FID Detector Base Body and DGFC Module Jet The flame jet mounted on the detector base body for capillary wide bore or packed columns and is suitable for operating up to the max selectable detector temperature 375 C 1 Flame Ionization Detector FID 2 Detector Base Body 3 DGFC Module 1...

Page 160: ... minimally to permanent gases oxides of nitrogen sulfur compounds ammonia and water Temperature The detector base body heats the FID to prevent condensation of the water vapor formed as a result of the hydrogen combustion of the flame The FOCUS GC will not allow flame ignition to proceed at temperatures less than 150 C The base body temperature is normally set to the upper temperature limit of the...

Page 161: ... to 350 mL min for air 35 mL min for hydrogen 30 mL min for make up gas To ensure the correct regulation of detector gases a minimum line pressure of 4 bar 400 kPa 60 psi must be provided to the instrument NOTE Usually the air flow is about ten times the hydrogen flow to keep the flame lit For high sensitivity applications it is essential to exclude all traces of organic contamination from the chr...

Page 162: ...r base body housing and tighten it with the proper tool Ensure the jet is perfectly vertically aligned to avoid damaging its ceramic part Figure 8 3 Jet for FID 2 Install the FID on the detector base body and secure it by using the fixing screw on the front of the detector cell 3 Carefully connect the signal and ignition polarization cables coming from the detector control card to the detector cel...

Page 163: ...er 8 FID Installation Flame Ionization Detector FID Instruction Manual 163 Figure 8 4 Installation of the FID 1 FID 2 Fixing screw 3 Detector base body 4 Signal cable 5 Ignition polarization cable 2 1 4 3 5 ...

Page 164: ...ameters Parameter Range Description DETECTOR This line is the title bar Flame On Off This indicates the flame status On Off Igniting Waiting or Out Hydrogen and air flows are required to light the flame Set On to turn on the flame flows This happens only if the Temp is 150 C If not an error message is displayed The Out message is displayed when the flame is inadvertently extinguished Set Off to tu...

Page 165: ... current when lit This parameter defines the flame on condition The FOCUS GC uses this value to determine flame status on or off and control automatic re ignition If Flameout retry is On the flame will re ignite if the signal drops below this value This line doesn t appear at detector signal range 2 and 3 Threshold assumes 0 pA Flameout retry On Off This indicates re ignition status Set On to prog...

Page 166: ...utozero On Range 10 0 3 0 Table 8 2 FID Signal Parameters Parameter Range Description SIGNAL This line is the title bar Output Not editable This is the actual electrometer output signal expressed in gV The Autozero function forces this value to 1000 corresponding to the zero level of the baseline on a recording device You cannot enter a setpoint here Offset 0 to 100000 This is a value in counts th...

Page 167: ...afety information 1 In Main Menu move the cursor until Detector is selected Press ENTER to display the DETECTOR menu 2 Set the detector base body temperature This must be greater than 150 C to allow the flame ignition 3 Turn Hydrogen flow Air flow and Make up gas flow On 4 When the detector base body is at the set temperature scroll to Flame and set it On This turns on the air and hydrogen flows a...

Page 168: ...ector base body using the adapter Measure the gas flow and verify that the flow rate is 35 mL min By using a screwdriver adjust the gas flow with the flow regulator until the desired gas flow is achieved Turn the hydrogen flow Off WARNING Never measure air and hydrogen flow together Turn the Air supply On Measure the gas flow and verify that the flow rate is 350 mL min By using a screwdriver adjus...

Page 169: ...ge 10 0 3 and set the electrometer amplifier input range The value 0 100 is the most sensitive 3 Scroll to Run Autozero and set On 4 If offset is required scroll to Offset and enter a numeric value or set it On to recall the last offset from memory NOTE If the Range 10 is set 2 or 3 the small variation of the output signal is not detected For this reason the Signal pA Ign thresh and Flameout retry...

Page 170: ...Chapter 8 Flame Ionization Detector FID Detector Signal Parameters 170 Instruction Manual ...

Page 171: ...nces for the Thermal Conductivity Detector TCD Chapter at a Glance TCD Overview 172 TCD Gas Supplies 174 TCD Operating Modes 175 Selecting TCD Operating Parameters 177 TCD Menu 179 Detector Signal Parameters 181 Operating Sequencess Programming a TCD 182 Setting the TCD Signal Parameters 184 Shutting Down the TCD 185 ...

Page 172: ... detector when analyte concentrations are high enough The TCD typically requires only one type of gas such as helium The FID requires up to four The TCD consists of a stainless steel block containing two filaments generally tungsten rhenium filaments which have the same electrical resistance The block is housed in an aluminum case that accommodates the heating elements and the temperature sensor N...

Page 173: ...on of the filament temperature The signal polarity is a function of the thermal conductivity of the component relative to the reference gas and to the user selected polarity of the filament power supply WARNING The TCD filaments are sensitive to impurities present in the carrier reference and make up gas supplies To ensure correct detector operation you should use oxygen and water vapor traps in t...

Page 174: ...rmation Table 9 1 contains information about the thermal conductivity of several gases Detector gas flow rates are factory preset to 30 mL min for reference and to 27 mL min for make up To modify the detector flow setting refer to Chapter 3 To ensure the correct regulation of detector gases a minimum line pressure of 4 bar 400 kPa 60 psi must be provided to the instrument WARNING The TCD DGFC has ...

Page 175: ...switch to a constant current mode when the filaments reach the maximum allowable current value of 125 mA Constant Temperature In constant temperature mode the filament temperature remains constant at a set value A feedback loop circuit changes the voltage as the gas thermal conductivity changes If the required voltage reaches the maximum allowable value of 15 V the system will automatically switch...

Page 176: ...sitivity NOTE Automatic Switching to Constant Current Mode Every time the set values of filaments voltage block temperature and filaments temperature cause the filament current to reach the maximum value of 125 mA the system will automatically switch to the constant current mode and the filaments cannot be heated more than the correspondent temperature This mode has good sensitivity and a linearit...

Page 177: ...or temperature The CT mode provides the highest sensitivity and is suggested for trace analysis ppm Since the temperature remains constant this mode considerably increases the filament life compared to other operating modes For samples in concentrations not exceeding 1 use the following values detector temperature 10 C higher than the maximum temperature reached by the column oven during the analy...

Page 178: ...ure reached by the column oven during the analysis but not higher than 300 ºC filament voltage 5 V Suggested Operating Values Table 9 3 contains the suggested operating values for the detector as a function of the concentration range and detector temperature Table 9 2 Filament Temperature Values for Argon Detector Temperature 100 ºC Values Voltage V 5 6 7 8 9 10 Filament Temperature ºC 235 275 315...

Page 179: ...es Fil temp 350 Reference On Make up On Filament power Off Fil status not rdy Block temp 200 200 Trans temp 200 200 Cost fill temp No Fil volts 10 Fil temp limit 350 Reference On Make up On Table 9 4 The Detector TCD Parameters Menu Range Comments DETECTOR TCD This line is the menu title bar Filament power1 On Off Set ON to turn on the filament power Set OFF to turn off the filament Fil status Rea...

Page 180: ...yed in parentheses Fil temp 2 On Off 50 450 ºC This parameter indicates the filament temperature Fil volts 3 5 15 V This parameter indicates the filament voltage Fil temp limit3 4 50 450 ºC This parameter indicates the maximum filament temperature Ref flow On Off This parameter indicates the reference gas flow You can only turn the flow on and off Set ON to turn on the flow Set OFF to turn off the...

Page 181: ...t editable This is the actual output signal The Autozero function forces this value to 1000 corresponding to the zero level of the baseline on a recording device Offset 0 to Variable This is a value in counts that may be subtracted from the Output signal to adjust the baseline level This parameter may be manually or automatically set using the Autozero function The range of the suppression is vari...

Page 182: ...illary column in use When a wide bore or capillary column is used make sure the make up gas line is turned ON WARNING Hydrogen is a potentially dangerous gas Refer to Using Hydrogen for safety information 1 In Main Menu move the cursor until Detector is selected Press ENTER to display the DETECTOR menu 2 Adjust and measure the reference gas flow as follows a Scroll to Ref flow and set ON then adju...

Page 183: ...olumn oven temperature reached during the analysis 6 Scroll to Const fil temp to select the operating mode When constant filament temperature is required set YES otherwise set NO If Yes has been entered scroll to Fil temp and set the filament temperature This value must always be higher than the detector temperature The greater the difference between the two temperatures ΔT the higher the detector...

Page 184: ...s versus the sample 4 With all gas flows and temperatures adjusted and stable and with the filaments on and stable scroll to Offset and set OFF 5 Zeroing the Signal Every time the set condition of filaments temperature and voltage are changed an adjustment of the Zero level may be necessary in order to balance the bridge Usually this operation is performed by scrolling to Autozero function and set...

Page 185: ... Signal Parameters Thermal Conductivity Detector TCD Instruction Manual 185 Figure 9 2 Manual Zero adjustment OPERATING SEQUENCE Shutting Down the TCD At the end of the analytical cycle the filaments should be turned off ...

Page 186: ...Chapter 9 Thermal Conductivity Detector TCD Detector Signal Parameters 186 Instruction Manual ...

Page 187: ...quence with the FOCUS GC keypad when an AS 2000 or an AI 3000 AS 3000 is used and how to set up ranges of samples to run automatically NOTE TriPlus and HS 2000 autosamplers are controlled only by all the Thermo Fisher Scientific Data Systems referring to the instructions reported in the relevant operating manuals Chapter at a Glance Autosampler Overview 188 AS 2000 Autosampler Menu 190 AI 3000 AS ...

Page 188: ...s components must be done from the AS 2000 control module AI 3000 AS 3000 Thermo Data System referring to the instructions reported in the relevant operating manual FOCUS GC keypad referring to the instructions reported in this chapter NOTE TriPlus and HS 2000 autosamplers are controlled only by all the Thermo Fisher Scientific Data Systems referring to the instructions reported in the relevant op...

Page 189: ...ion According to the autosampler connected configure the instrument as described in paragraph Configuration on page 51 Autosampler Menu In Main Menu move the cursor until Autosampler is selected then press ENTER to open AUTOSAMPLER menu Refer to AS 2000 Autosampler Menu AI 3000 AS 3000 Menu ...

Page 190: ... volume 2 Pre dwell time 10 Post dwell time 10 Table 10 1 AS 2000 Autosampler Menu Parameter Range Description AUTOSAMPLER This line is the title bar Sample volume 0 0 99 9 100 500 µl This parameter specifies the amount of sample to be injected for each run Sample rinses 0 15 times This parameter specifies the number of times the syringe is pre washed with sample Rinse volume 0 0 99 9 100 500 µl T...

Page 191: ...eter specifies the volume of solvent used to clean the syringe Plunger strokes 0 15 times This parameter specifies the number of plunger strokes to eliminate bubbles Viscosity delay 0 15 times This parameter specifies how long the plunger will remain at the top of the stroke to account for viscous samples Sample draw spd 0 100 µls This parameter specifies how quickly the sample is drawn from the v...

Page 192: ...an specify an air gap in the syringe between the internal standard solution or the solvent and the sample This is the Post air gap mode To have an air gap both before and after the internal standard solution or solvent choose the Double air gap mode INT STD SETTINGS Int std vial 20 Int std volume 2 0 Air gap mode double Air gap volume Table 10 2 Internal Standard Menu Parameter Range Description I...

Page 193: ...10 Post dwell time 10 Table 10 3 AI 3000 AS 3000 Menu Parameter Range Description AUTOSAMPLER This line is the title bar Sample volume 0 to 5 µl with the 10 µl syringe 0 to 2 5 µl with the 5 µl syringe 0 to 250 nl with the 0 5 µl syringe This parameter specifies the amount of sample to be injected for each run Sample rinses 0 15 times This parameter specifies the number of times the syringe is pre...

Page 194: ...ter Set Bottom to pull up the liquid from the bottom of the sample vial Set Center from half height of the sample vial Inj Depth Standard Minimum It determines the penetration depth of the syringe needle into the vial When Standard is set default value the syringe needle penetrates into the injector up the maximum depth limit Hot Needle Technique When Minimum is set the syringe needle penetrates i...

Page 195: ...ove the cursor until Sequence is selected then press ENTER to open SEQUENCE menu SEQUENCE First sample 1 Last sample 8 Injection vial 1 When no vial Skip Start Sequence Stop sequence Table 10 4 Sequence Menu Parameter Range Description SEQUENCE This line is the title bar First sample Depends of the sample tray type Enter the position number of the first sample vial of the sequence Last sample Depe...

Page 196: ...mple table of the data system will be not affected When Abort is set the sequence will be aborted after three missing vial Start sequence This is visualized when sequence is not running To start the sequence select Start sequence then press ENTER Stop sequence This is visualized when sequence is running To stop the sequence select Stop sequence then press ENTER Table 10 4 Sequence Menu Continued P...

Page 197: ...m a Run Time Events and the instrument start up Chapter at a Glance Instrument Set up 198 Run Time Events 202 Controlling Valves 206 Instrument Start Up 208 Instrument Status Messages 211 Operating Sequences How to Set Up the Instrument 198 Editing Run Time Events 202 Deleting a Run Time Event 205 Run Time Control Gas Sampling Valve Only 206 How to Start Up the Instrument 208 ...

Page 198: ...s set at the required value as described in Chapter 1 1 Plug the power cord in the Main socket located on the GC rear panel 2 Connect the other end of the power cord to the power line 3 Turn the breaker switch on the position I 4 Wait until the initial routine is completed then the Main Menu is displayed Configure the Carrier Gas 1 In Main Menu move the cursor until Others is selected then press E...

Page 199: ...re mode then in the Pressure kPa line enter the desired value 8 Activate the Gas Saver if required In the Gas Saver Flow ml min and Gas Saver Time min lines the desired values NOTE When you install a new column you must perform a column evaluation Set Oven Parameters 9 In Main Menu move the cursor until Oven is selected Press ENTER to open OVEN menu 10 Set the oven temperature and the Oven program...

Page 200: ... 19 Observe the signal at the display This is the background offset 20 Set the electrometer amplifier input signal required Configure Autosampler If an AS 2000 or AI 3000 AS 3000 autosampler is present and properly connected to the GC proceed as follows 21 In Main Menu move the cursor until Others is selected 22 Scroll to Configuration then press ENTER 23 Scroll to Autosampler then press ENTER The...

Page 201: ...arameters 29 In Main Menu move the cursor until Sequence is selected Press ENTER to open SEQUENCE menu 30 Set the sequence parameters required 31 Press HOME to exit Set events To program time events and or to manually change the state of the inlet valves or external valves please refer to the following paragraphs Run Time Events Controlling Valves ...

Page 202: ...the PrepRun step You can program events like this shown with the RUN TIME menu and submenu Up to 16 events may be programmed OPERATING SEQUENCE Editing Run Time Events Creating a Run Time Event Use the following sequence to enter new run time events 1 In main Menu move the cursor until Others is selected then press ENTER Scroll to Run time Events then press ENTER to open RUN TIME EVENTS menu RUN T...

Page 203: ...lve 2 replaces EV 2 EV 1 4 Scroll to Run time You may choose between two conditions Select a time in minutes if you want to activate the event during the Run Time Select PrepRun if you want activates the event during the Prep run 5 Scroll to Setpoint and set the setpoint x1 or x10 according to the event you have set in the previous line Adding a New Event 6 Scroll to Next event if you want to edit...

Page 204: ...t to edit a new event NOTE The max number of events is 16 Run Table 10 If other events have not to be programmed press HOME to return RUN TABLE menu It will shows the all the Run time events programmed NOTE By pressing ENTER on an event line the relevant EDIT EVENT menu is open EDIT TIME EVENT Event 2 GSValve 1 Inject at 1 00 Inject for 0 50 Next event RUN TABLE 1 of 2 PreRun Det Azero 1 00 GSValv...

Page 205: ...r run time event and press ENTER to open CLEAR TIME EVENT menu 3 Scroll to the event line of interest and press ENTER The related event is deleted For example delete Det Autozero 4 Press HOME to return RUN TIME EVENTS menu The menu will go back to the table Run Table 1 of 1 RUN TABLE 2 of 2 Clear run time event CLEAR EVENTS 1 PreRun Det Azero 1 00 GSValve 1 Inj Add run time event Clear all events ...

Page 206: ... Gas sampling Run Time Control Gas Sampling Valve Only 1 Add a new event for GSValve 1 2 Choose the time to inject in minutes 3 Choose an injection duration in minutes 4 Press HOME to exit and check the result in the RUN TABLE Manual Control 1 In main Menu move the cursor until Others is selected then press ENTER Scroll to Valves then press ENTER to open VALVES menu 2 Two different menus may be di...

Page 207: ... change the valve condition by using INC and DEC keys The action has immediate effect 4 To exit VALVES menu press HOME VALVES VALVES Split valve Off Sept purge valve On EV 1 Off EV 2 Off Split valve Off Sept purge valve On GSValve 1 Load EV 2 Valves menu when gas sampling valve is not present Valves menu when gas sampling valve is present ...

Page 208: ...dy carried out The carrier gas supply line is correctly connected to the DPFC module and the inlet pressure is set at the required value as described in Chapter 1 The FOCUS GC is properly electrically connected and configured The carrier gas type is correctly set The analytical column is correctly installed and conditioned The correct liner is in the SSL injector The system is free of leak The aut...

Page 209: ... seconds inject the sample rapidly and rapidly remove the syringe from the injector This is the Hot Empty Needle technique 3 Press START button The GC will complete the analysis as programmed Performing Injection Using an Autosampler Before you begin an autosampler injection ensure that you have programmed the autosampler method in the AUTOSAMPLER menu and the autosampler sequence in SEQUENCE menu...

Page 210: ...then press ENTER 3 Scroll to Start Sequence and press ENTER or START button The autosampler will inject the samples according to the programmed method and sequence NOTE Pressing the STATUS key on the GC keypad the current instrument status is displayed For details refer to the paragraph Instrument Status Messages in this chapter ...

Page 211: ...isualize the instrument status According to the current GC operating phase the following messages may be displayed Not Ready Each message indicates any reasons the GC is in Not Ready condition NOT READY Oven Temperature NOT READY Equilibrium Time NOT READY Flame out NOT READY Detector temp NOT READY Carrier pressure NOT READY Inlet temp ...

Page 212: ...ver function has been selected On in the Carrier menu the following message is displayed Prep Run This message indicates that the GC performs the events at the Prep Run programmed in RUN TIME EVENTS menu NOT READY Inlet split flow NOT READY Carrier col flow NOT READY TCD filaments NOT READY TCD block temp STAND BY Waiting for Prep run STAND BY Gas saver active ...

Page 213: ...an Autosampler enabled This message indicates that autosampler is active and the GC is waiting for the Start signal Run These messages indicate the steps of the oven temperature program are currently performed PREP RUN Exec Prep run events READY TO INJECT Waiting for start READY TO INJECT Autosampler active Waiting for start RUNNING Initial temperature RUNNING Final temperature 1 ...

Page 214: ...Chapter 11 Getting Started Instrument Status Messages 214 Instruction Manual If the Run Log has entries the following message is displayed RUNNING Ramp 1 RUNNING Run log has entries ...

Page 215: ...e to check the Ionization Flame Detector FID with the Split Splitless Injector S SL Chapter at a Glance SOP number P0407 05 E 31 May 2006 216 Scope 216 Preliminary Operations 216 Parts Referenced 218 FID S SL Checkout in Splitless Mode 220 Operating Procedures FID S SL Checkout in Splitless Mode 220 ...

Page 216: ...ing a standard solution into a test column under analytical conditions set according to the injector and detector hardware provided with the GC Before starting the test checkout refer to the Parts Referenced and the Analytical Condition required NOTE Each SOP has a proper Registration and Revision Number e g PO407 01 E 27 March 2002 according to our Quality Management policy Preliminary Operations...

Page 217: ...olumn constant NOTE Column evaluation assumes there are no leaks in the column connection or gas plumbing lines Perform column evaluation following the instruction reported in the Performing a Column Evaluation operating sequence 7 Column Conditioning CAUTION When performing column conditioning the column should be connected only to the injector leaving the column outlet disconnected to avoid the ...

Page 218: ...scription Part Number Test Column Fused Silica Capillary Column TR 5 7 mt long 0 32 mm ID 0 25 μm film thickness 260 800 01 Glass Liner 3 mm ID for splitless injection 453 200 32 Liner Seal Graphite seal for glass liner 290 334 06 Graphite Ferrule Graphite ferrule for 0 32 mm ID Column 290 134 87 Septum Standard septum for S SL injector 313 032 11 Syringe 10 μl size 50 mm needle length 365 005 25 ...

Page 219: ... 30 mL min 350 kPa 50 psi Oven Program Initial Temperature 50 C Initial Time 1 minute Ramp 1 20 C minute Final Temperature 200 C Final Time 1 minute Injector Operating Mode Splitless Temperature 230 C Splitless Time 0 8 minutes Split Flow 60 ml min Constant Septum Purge Yes Detector Base Temperature 250 C Detector Signal Range 100 Injected Volume 1 μl needle of Test Mixture Analog Signal Output Ch...

Page 220: ... Others is selected then press ENTER Scroll to Configuration then press ENTER to open Configuration menu Scroll to Configure carrier submenu then press ENTER Select the carrier gas required by using the INC and DEC keys 2 Press HOME three times to return Main Menu Set Checkout Parameters 3 In Main Menu move the cursor until Carrier is selected Press ENTER to open CARRIER menu FOCUS GC Others OTHER...

Page 221: ... Main Menu 6 In Main Menu move the cursor until Oven is selected Press ENTER to open OVEN menu 7 Scroll to Temp Initial time Ramp 1 Final temp 1 Final time 1 and Ramp 2 By using the INC and DEC keys select the value or the required operating mode then press ENTER CARRIER He Flow mode Const pres CARRIER He Pressure 30 0 30 0 CARRIER He Col flow 3 00 1 CARRIER He Gas saver flow Off CARRIER He Vacuum...

Page 222: ...0 Scroll to Temp Mode Split flow Total flow Split flow Splitless time and Const Sept purge By using the INC and DEC keys select the value or the required operating mode then press ENTER 1 The values in parentheses are not editable OVEN Ramp 1 20 0 OVEN Final temp 1 200 200 OVEN Final time 1 1 00 OVEN Ramp 2 Off FOCUS GC Inlet Inlet Temp 230 230 Inlet Mode Splitless Inlet Total flow 5 0 1 ...

Page 223: ...o Flame Temp Signal pA Ign thresh Flameout retry H2 Air and Make up By using the INC and DEC keys select the value or the required operating mode then press ENTER 1 The values in parentheses are not editable Inlet Split flow 60 0 60 0 Inlet Splitless time 0 80 Inlet Const Sept purge On FOCUS GC Detector DETECTOR FID Flame On DETECTOR FID Temp 250 250 DETECTOR FID Signal pA 5 5 1 DETECTOR FID Ign t...

Page 224: ...AL menu 16 Scroll to Output Offset Run autozero and Range 10 0 3 By using the INC and DEC keys select the value or the required operating mode then press ENTER 1 The values in parentheses are not editable DETECTOR FID Flameout retry On DETECTOR FID H2 On DETECTOR FID Air On DETECTOR FID Make up On FOCUS GC Signal SIGNAL FID Output 1000 1 SIGNAL FID Offset 100 SIGNAL FID Run autozero ...

Page 225: ...n theTable 12 3 according to the data handling in use 20 Perform a blank analysis without injecting and press START on the GC to begin the checkout run 21 With the GC in Stand by Prep Run condition activate the data system for 10 minutes to evaluate your baseline in isothermal condition 22 After the baseline evaluation has been completed set up the data system to acquire a single run 23 Inject the...

Page 226: ...31 May 2006 226 Instruction Manual Figure 12 1 FID Splitless Injection 24 The following criteria indicate successful completion of FID S SL checkout 25 If these criteria are not met repeat the test 1 Dodecane 2 Tetradecane 3 Hexadecane ...

Page 227: ...nalog or 1 digital set in the Chrom Card WCC INI configuration file Computing integrator e g ChromJet When a Computing integrator e g ChromJet is used the peak area counts will result to be 5 times lower than the peak area counts obtained by using Analog Chrom Card Acceptance Values CHROMQUEST Baseline Parameters 1V Full Scale Noise μV 30 Wander μV 50 Drift μV h 100 Analytical Results 1V Full Scal...

Page 228: ...Acceptance Comments 1 When the make up gas is not used the acceptance values will result to be 2 5 times lower than the values reported in Table 12 3 2 When helium is used as make up gas the acceptance values will result to be 10 times lower than the values reported in Table 12 3 ...

Page 229: ...to check the Thermal Conductivity Detector TCD with the Split Splitless Injector S SL Chapter at a Glance SOP number P0473 04 E 02 May 2007 230 Scope 230 Preliminary Operations 230 Parts Referenced 232 TCD S SL Checkout in Splitless Mode 234 Operating Procedures TCD S SL Checkout in Splitless Mode 234 ...

Page 230: ...ing a standard solution into a test column under analytical conditions set according to the injector and detector hardware provided with the GC Before starting the test checkout refer to the Parts Referenced and the Analytical Condition required NOTE Each SOP has a proper Registration and Revision Number e g PO407 01 E 27 March 2002 according to our Quality Management policy Preliminary Operations...

Page 231: ...on assumes there are no leaks in the column connection or gas plumbing lines Perform column evaluation following the instruction reported in the Performing a Column Evaluation operating sequence 7 Column Conditioning CAUTION When performing column conditioning the column should be connected only to the injector leaving the column outlet disconnected to avoid the possibility of contamination of the...

Page 232: ...ription Part Number Test Column Fused Silica Capillary Column TR 5 7 mt long 0 32 mm ID 0 25 μm film thickness 260 800 01 Glass Liner 3 mm ID for splitless injection 453 200 32 Liner Seal Graphite seal for glass liner 290 334 06 Graphite Ferrule Graphite ferrule for 0 32 mm ID Column 290 134 87 Septum Standard septum for S SL injector 313 032 11 Syringe 10 μl size 50 mm needle length 365 001 03 Te...

Page 233: ...ial Temperature 50 C Initial Time 1 minute Ramp 1 20 C minute Final Temperature 190 C Final Time 1 minute Injector Operating Mode Splitless Temperature 200 C Splitless Time 0 8 minutes Split Flow 60 ml min Constant Septum Purge Yes Detector Block Temperature 200 C Transfer Temperature 190 C Constant Filament Temperature No Filament Voltage 10V Filament Temperature limit 350 C Gain x 10 Negative Po...

Page 234: ... Others is selected then press ENTER Scroll to Configuration then press ENTER to open Configuration menu Scroll to Configure carrier submenu then press ENTER Select the carrier gas required by using the INC and DEC keys 2 Press HOME three times to return Main Menu Set Checkout Parameters 3 In Main Menu move the cursor until Carrier is selected Press ENTER to open CARRIER menu FOCUS GC Others OTHER...

Page 235: ... Main Menu 6 In Main Menu move the cursor until Oven is selected Press ENTER to open OVEN menu 7 Scroll to Temp Initial time Ramp 1 Final temp 1 Final time 1 and Ramp 2 By using the INC and DEC keys select the value or the required operating mode then press ENTER CARRIER He Flow mode Const pres CARRIER He Pressure 30 0 30 0 CARRIER He Col flow 3 00 1 CARRIER He Gas saver flow Off CARRIER He Vacuum...

Page 236: ...0 Scroll to Temp Mode Split flow Total flow Split flow Splitless time and Const Sept purge By using the INC and DEC keys select the value or the required operating mode then press ENTER 1 The values in parentheses are not editable OVEN Ramp 1 20 0 OVEN Final temp 1 190 190 OVEN Final time 1 1 00 OVEN Ramp 2 Off FOCUS GC Inlet Inlet Temp 200 200 Inlet Mode Splitless Inlet Total flow 5 0 1 ...

Page 237: ...Block temp Transf temp Reference Make up Const fil temp Fil volts CV Fil temp limit and Filament power By using the INC and DEC keys select the value or the required operating mode then press ENTER Inlet Split flow 60 0 60 0 Inlet Splitless time 0 80 Inlet Const Sept purge On FOCUS GC Detector DETECTOR TCD Block temp 200 200 DETECTOR TCD Transf temp 190 190 DETECTOR TCD Reference On DETECTOR TCD M...

Page 238: ...nu 15 In Main Menu move the cursor until Signal is selected Press ENTER to open SIGNAL menu 16 Scroll to Output Offset Run autozero Gain and Neg polarity By using the INC and DEC keys select the value or the required operating mode then press ENTER 2 The values in parentheses are not editable DETECTOR TCD Cost fil temp N DETECTOR TCD Fil volt CV 10 DETECTOR TCD Fil temp limit 3501 DETECTOR TCD Fil...

Page 239: ...a handling in use 20 Perform a blank analysis without injecting and press START on the GC to begin the checkout run 21 With the GC in Stand by Prep Run condition activate the data system for 10 minutes to evaluate your baseline in isothermal condition 22 After the baseline evaluation has been completed set up the data system to acquire a single run 23 Inject the test mixture and press START on the...

Page 240: ...02 May 2007 240 Instruction Manual Figure 13 1 TCD Splitless Injection 24 The following criteria indicate successful completion of TCD S SL checkout 25 If these criteria are not met repeat the test 1 Dodecane 2 Tetradecane 3 Hexadecane ...

Page 241: ...omputing integrator e g ChromJet is used the peak area counts will result to be 5 times lower than the peak area counts obtained by using Analog Chrom Card Acceptance Values CHROMQUEST Baseline Parameters 1V Full Scale Noise μV 30 Wander μV 140 Drift μV h 200 Analytical Results 1V Full Scale Area Counts 0 01 μVs Components 300 000 for each component Using Chrom Quest connected to the FOCUS GC digi...

Page 242: ...Chapter 13 SOP number P0473 04 E 02 May 2007 242 Instruction Manual ...

Page 243: ...perating procedure to check the Thermal Conductivity Detector TCD with the Purged Packed Injector PPKD Chapter at a Glance SOP number P0474 05 E 02 May 2007 244 Scope 244 Preliminary Operations 244 Parts Referenced 246 TCD PPKD Checkout 249 Operating Procedures TCD PPKD Checkout 249 ...

Page 244: ...ing a standard solution into a test column under analytical conditions set according to the injector and detector hardware provided with the GC Before starting the test checkout refer to the Parts Referenced and the Analytical Condition required NOTE Each SOP has a proper Registration and Revision Number e g PO407 01 E 27 March 2002 according to our Quality Management policy Preliminary Operations...

Page 245: ...column constant NOTE Column evaluation assumes there are no leaks in the column connection or gas plumbing lines Perform column evaluation following the instruction reported in the Performing a Column Evaluation operating sequence 7 Column Conditioning CAUTION When performing column conditioning the column should be connected only to the injector leaving the column outlet disconnected to avoid the...

Page 246: ...lary Column TR 5 7 mt long 0 32 mm ID 0 25 μm film thickness 260 800 01 Glass Liner 2 mm ID tapered 453 220 50 Liner Seal Graphite seal for glass liner 290 334 05 Precolumn Fused Silica Capillary Column 0 5 mt long 0 53 mm ID 260 603 75 Press fit connections For columns 0 53 0 32 mm ID 350 438 16 Injection side adapter For Wide bore column 347 003 01 Detector side adapter For Wide bore column 347 ...

Page 247: ...ts in n Hexane Component Concentration Dodecane 200 μg ml Tetradecane 200 μg ml Hexadecane 200 μg ml 338 190 16 Gases Chromatographic grade purity Data Acquisition Chrom Card ChromQuest Atlas Xcalibur Computing integrator Table 14 1 TCD PPKD Parts Referenced Continued Part Description Part Number ...

Page 248: ...ium 30 ml min Oven Program Initial Temperature 85 C Initial Time 1 minute Ramp 1 20 C minute Final Temperature 190 C Final Time 1 minute Injector Operating Mode Wide bore Septum Purge Yes Temperature 180 C Detector Block Temperature 200 C Transfer Temperature 190 C Constant Filament Temperature No Filament Voltage 10V Filament Temperature limit 320 C Gain x 10 Negative Polarity No Injected Volume ...

Page 249: ...s selected then press ENTER Scroll to Configuration then press ENTER to open Configuration menu Scroll to Configure carrier submenu then press ENTER Select the carrier gas required by using the INC and DEC keys 2 Press HOME three times to return Main Menu Set Checkout Parameters 3 In Main Menu move the cursor until Carrier is selected Press ENTER to open CARRIER menu FOCUS GC Others OTHERS Configu...

Page 250: ... Main Menu 6 In Main Menu move the cursor until Oven is selected Press ENTER to open OVEN menu 7 Scroll to Temp Initial time Ramp 1 Final temp 1 Final time 1 and Ramp 2 By using the INC and DEC keys select the value or the required operating mode then press ENTER CARRIER He Flow mode Const pres CARRIER He Pressure 30 0 30 0 CARRIER He Col flow 3 00 1 CARRIER He Gas saver flow Off CARRIER He Vacuum...

Page 251: ...s ENTER to open INLET menu 10 Scroll to Temp Mode and Const Sept purge By using the INC and DEC keys select the value or the required operating mode then press ENTER 11 Press HOME to return Main Menu OVEN Ramp 1 20 0 OVEN Final temp 1 200 200 OVEN Final time 1 1 00 OVEN Ramp 2 Off FOCUS GC Inlet Inlet Temp 180 180 Inlet Mode Wide bore Inlet Const Sept purge On ...

Page 252: ...s CV Fil temp limit and Filament power By using the INC and DEC keys select the value or the required operating mode then press ENTER 1 In case of TCD with the polyimide coated filaments the temperature limit is 320 C FOCUS GC Detector DETECTOR TCD Block temp 200 200 DETECTOR TCD Transf temp 190 190 DETECTOR TCD Reference On DETECTOR TCD Make up On DETECTOR TCD Cost fil temp N DETECTOR TCD Fil vol...

Page 253: ...to Output Offset Run autozero Gain and Neg polarity By using the INC and DEC keys select the value or the required operating mode then press ENTER 2 The values in parentheses are not editable 17 Press HOME to return Main Menu 18 Activate your Data System and set the parameters required for the checkout DETECTOR TCD Fil status ready FOCUS GC Signal SIGNAL TCD Output 1000 2 SIGNAL TCD Offset 100 SIG...

Page 254: ...ing in use 20 Perform a blank analysis without injecting and press START on the GC to begin the checkout run 21 With the GC in Stand by Prep Run condition activate the data system for 10 minutes to evaluate your baseline in isothermal condition 22 After the baseline evaluation has been completed set up the data system to acquire a single run 23 Inject the test mixture and press START on the GC to ...

Page 255: ...E 02 May 2007 Instruction Manual 255 Figure 14 1 TCD PPKD Injection 24 The following criteria indicate successful completion of TCD PPKD checkout 25 If these criteria are not met repeat the test 1 Dodecane 2 Tetradecane 3 Hexadecane ...

Page 256: ...grator e g ChromJet is used the peak area counts will result to be 5 times lower than the peak area counts obtained by using Analog Chrom Card Acceptance Values CHROMQUEST Baseline Parameters 1V Full Scale Noise μV 30 Wander μV 140 Drift μV h 200 Analytical Results 1V Full Scale Area Counts 0 01 μVs Components 300 000 for each component Using Chrom Quest connected to the FOCUS GC digital output an...

Page 257: ...L Injector 262 Maintaining a PPKD Injector 276 Maintaining a FID 282 FID Troubleshooting 295 Maintaining a TCD 298 TCD Troubleshooting 300 Maintaning Gas Sampling Valve 304 Analytical Troubleshooting 306 Error Messages 307 Guide to Solve Analytical Problems 309 Operating Procedures Replace the S SL Standard Septum 264 Replace or Clean the Liner when a S SL Standard Septum is Installed 267 Replace ...

Page 258: ...ance and Troubleshooting 258 Instruction Manual Clean Replace the FID Jet 284 Clean Replace the FID Collecting Electrode 288 Replace the FID Ignition Assembly 292 How to Install Replace the Loop of an Automatic Valve 304 ...

Page 259: ...or must carry out a certain amount of routine maintenance on a regular basis Suggested Maintenance Schedule Preventive maintenance keeps your instruments running at peak performance The recommended maintenance schedule shown in the Maintenance Schedule Table is based on a GC running multiple samples in an 8 hour day You may need to adapt the schedule to your situation depending on The number of an...

Page 260: ...and free from dust and deposit Symptoms such as reduced sensitivity increased noise and difficulty in flame ignition indicate that detector cleaning may be necessary Make sure you not only perform each scheduled item but that you record it as well along with any observation about instrument performance Your records and notes can be invaluable when trying to trace a service problem In addition to t...

Page 261: ...orized customer support engineer for proper actions The service engineer must be fully informed on the nature of the concerned substance In the event that a hazardous material is spilled on or in the instrument clean the spill according to the procedures in the Material Data Sheet for that substance WARNING It is your responsibility to avoid that dangerous liquids and or materials seeping inside t...

Page 262: ...njections or every time a problem related to septum damage or wear occurs It is a good practice to change the septum with a new one every time the liner is replaced CAUTION Use original Thermo Fisher Scientific standard septum Septa from other manufacturers may show different rates of degradation When Cleaning or Replacing the Liner The liner must be replaced periodically depending on the number o...

Page 263: ...ing Sequences The following operating sequences help you to maintain properly the SSL injector Replace the S SL Standard Septum Replace or Clean the Liner when a S SL Standard Septum is Installed Replace the S SL Inlet Vent Line Filter NOTE To replace a standard septum with the Microseal Valve refer to the relevant Installation Guide Liner PN Split injections 3 mm 453 200 31 Split injections 5 mm ...

Page 264: ...out at low temperature to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature Preliminary Operations 1 While in Standby condition in OVEN menu set the oven temperature to 30 C 2 In INLET menu set the inlet temperature to 0 0 Off 3 When the inlet reaches the room temperature enter in CARRIER menu scroll to Pressure and set it to 0 0 Off OVEN Temp 30 3...

Page 265: ...um from the septum holder use non metallic tools See B of Figure 15 1 7 Insert a new septum into the septum holder paying attention that the center guide of the septum must be turned upward See B of Figure 15 1 CAUTION Use tweezers to avoid touching the septum with your fingers Figure 15 1 Replace the Septum Replacing the Septum 8 Clean the septum support from possible fragments left by the septum...

Page 266: ...n the top of the septum support see C of Figure 15 1 10 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance Restart the GC Conditions 11 In CARRIER OVEN and INLET menus set the normal working conditions 12 Perform an automatic leak check ...

Page 267: ...Tweezers WARNING This operation must be carrier out at low temperature to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature When handling organics solvents you must take precautions to avoid health hazards Preliminary Operations 1 While in Standby condition in OVEN menu set the oven temperature to 30 C 2 In INLET menu set the inlet temperature to 0...

Page 268: ... Septum 4 Unscrew the septum cap 5 Remove the septum holder with septum then the septum support See A of Figure 15 2 Figure 15 2 Replace and Clean the Liner 1 6 Use the liner cap wrench provided with the GC to remove the injector liner cap See B of Figure 15 2 INLET Temp 25 Off CARRIER Pressure 0 Off B A C ...

Page 269: ...ing to remove a broken liner go to step Removing a Broken Liner then continue from the step Replacing the Linerr Cleaning the liner a Put the dirty liner into an ultrasonic bath filled with a methanol acetone mixture 1 1 and sonicate it for about half an hour b Using tweezers remove the liner from the bath and dry it with compressed clean air NOTE For trace analysis you should pre treat the liner ...

Page 270: ...fitting See F of Figure 15 3 e Insert the analytical column with its ferrule into the bottom of the injector in its previous position then tighten the M4 retaining nut to hold the column in place See G of Figure 15 3 Replacing the Liner 8 Holding the new or cleaned liner with tweezers place a graphite seal over the liner making sure to leave a distance of about 10 mm between the seal and the liner...

Page 271: ...al or allow graphite to entering the liner Should this occur clean the liner with an inert gas 10 Tighten the liner cap using the liner cap wrench provided with the GC See E of Figure 15 4 11 Remove the septum from the septum holder use non metallic tools 12 Insert a new septum into the septum holder paying attention that the center guide of the septum must be turned upward See F of Figure 15 5 CA...

Page 272: ...he septum and reinsert it into the injector 14 Place the septum holder on the top of the septum support see G of Figure 15 5 15 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance Restart the GC Conditions 16 In CARRIER OVEN and INLET menus set the normal working conditions 17 Perform an automatic leak check F G ...

Page 273: ...g the FOCUS GC MUST BE SWITCHED OFF Remove the FOCUS GC Top Cover The top cover is fixed on the main unit with two front screws and two clips 1 Open the GC oven door 2 Unscrew the two front screws as shown in Figure 15 6 which remain on the main unit 3 Remove manually the top cover pulling it up from the front the two clips will be automatically unlocked Figure 15 6 Top Aluminium Cover Removal 1 R...

Page 274: ...Identify the DPFC module See B of Figure 15 7 7 Referring to Figure 15 8 replace the filter operating as follows A B REF MAKE UP CARRIER SERVO AIR max 500 kPa OUT SAMPLE EXT DET 10V 1V 0V GND AIR H2 MAKE UP IN SAMPLE WARNING HIGH TEMPERATURE OVEN EXHAUST AIR DO NOT PLACE TEMPERATURE SENSITIVE MATERIAL NEAR OPENINGS 2 2 H SENSOR 1000 kPa 120 psi Max for all inputs O O I I SIGNAL TIMED EVENTS GENERI...

Page 275: ... a Unscrew the fixing Allen screw 1 b Slightly lift the filter c Pull the filter to extract it from its seat d Replace the filter with a new one proceeding in the reverse order of its removal Reinstall the GC Panels 8 Reinstall the GC real panel and the top cover proceeding in the reverse order of their removal 1 A B D C ...

Page 276: ...ery time a problem occurs related to a septum damage or wear It is good practice to replace the septum every time the liner is replaced When replacing the liner The liner must be replaced periodically depending on the number of injections performed and on the characteristics of the samples injected The most common symptom indicating that the liner should be replaced is the appearance of tailing pe...

Page 277: ...at low temperature to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature Preliminary Operations 1 While in Standby condition in OVEN menu set the oven temperature to 30 C 2 In INLET menu set the inlet temperature to 0 0 Off 3 When the inlet reaches the room temperature enter in CARRIER menu scroll to Pressure and set it to 0 0 Off OVEN Temp 30 30 IN...

Page 278: ...tum into the septum cap See B of Figure 15 9 CAUTION Use tweezers to avoid touching the septum with your fingers Figure 15 9 PPKD Injector Septum Replacement 7 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance Restart the GC Conditions 8 In CARRIER OVEN and INLET menus set the normal working conditions 9 Perform ...

Page 279: ...oid burns Therefore before beginning the sequence the injector must be cooled to room temperature When handling organics solvents you must take precautions to avoid health hazards Preliminary Operations 1 While in Standby condition in OVEN menu set the oven temperature to 30 C 2 In INLET menu set the inlet temperature to 0 0 Off 3 When the inlet reaches the room temperature enter in CARRIER menu s...

Page 280: ...ut at the bottom of the injector Remove the adapter and the liner then remove the ferrule See B of Figure 15 10 Figure 15 10 PPKD Injector Replace Clean the Liner 6 If you are using a new liner go to step 8 If you are cleaning the liner put the dirty liner into an ultrasonic bath filled with a methanol acetone mixture 1 1 and clean it for about half an hour 7 Using tweezers remove the liner from t...

Page 281: ...tor and push it gently upwards Tighten the retaining nut with the adapter to close the bottom of the injector See C of Figure 15 10 NOTE For trace analysis you should pre treat the liner with a suitable silylating reagent prior to inserting it into the injector 10 Insert the analytical column with its ferrule into the bottom of the injector in its previous position then tighten the M4 nut that ret...

Page 282: ... of dust and deposits Symptoms such as reduced sensitivity and increased noise indicate that detector needs cleaning To properly maintain the FID you should perform the following cleaning or replacement sequences Clean Replace the FID Jet Clean Replace the FID Collecting Electrode Replace the FID Ignition Assembly Figure 15 11 shows the Flame Ionization Detector components ...

Page 283: ... 283 Figure 15 11 FID Parts Identification 1 Detector Body 2 Chimney 3 Electrical Connection Assembly 4 Collecting Electrode 5 Retaining Nut 6 Jet 7 Collecting Electrode Pin 8 Flame Ignition Coil Polarization Assembly 9 Ceramic Insulator 10 Jet Removing Tool 11 Detector Base Body ...

Page 284: ...h Liquid detergent Clean compressed air GC grade methanol Clean paper towel Jet for FID WARNING This operation must be carried out at low temperature to avoid burns Therefore before beginning the sequence the detector must be cooled to room temperature When handling organics solvents you must take precautions to avoid health hazards 1 In DETECTOR menu scroll to Flame and set OFF 2 Scroll to Temp a...

Page 285: ...s from the detector See Figure 15 12 5 Loosen the fixing screw on the front of the detector cell and remove it See Figure 15 12 Figure 15 12 Clean Replace the Jet 1 6 Using the tool provided with the GC unscrew the jet See Figure 15 13 DETECTOR Flame Off Temp 25 Off Signal pA 0 0 Ing Thresh 2 0 Flameout retry Off H2 Off Air Off Make up Off ...

Page 286: ...rgent and clean it for about five minutes b Handling the jet with forceps or tweezers rinse the jet with distilled water then with methanol c Place the jet on a paper towel and let it air dry When the jet is dry place the jet into the housing and tighten it with the proper tool Ensure the jet is perfectly vertically aligned to avoid damaging its ceramic part Replace the Jet a Place a new jet into ...

Page 287: ...ean Replace the Jet 3 7 Place the detector cell on the detector base body and tighten the fixing screw on front of the detector cell Reconnect the signal and ignition cables to the detector See Figure 15 15 Figure 15 15 Clean Replace the Jet 4 8 Reset the detector to the required operating conditions ...

Page 288: ...gent Clean compressed air GC grade methanol Clean paper towel Collecting electrode WARNING This operation must be carried out at low temperature to avoid burns Therefore before beginning the sequence the detector must be cooled to room temperature When handling organics solvents you must take precautions to avoid health hazards 1 In DETECTOR menu scroll to Flame and set OFF 2 Scroll to Temp and se...

Page 289: ...r cell and remove it See Figure 15 16 6 Unscrew and remove the cap of the detector cell See Figure 15 16 Figure 15 16 Clean Replace the Collecting Electrode 1 7 Remove the holder assembly of the signal cable by unscrewing the two screws that fix it on the detector cell 8 Using forceps unscrew and remove the gold contact pin DETECTOR Flame Off Temp 25 Off Signal pA 0 0 Ing Thresh 2 0 Flameout retry...

Page 290: ...electrode in the ultrasonic bath filled with liquid detergent and clean it for about five minutes b Handle the collecting electrode with forceps or tweezers rinse it using distilled water then methanol c Place the collecting electrode on a paper towel and let it air dry d When the electrode is dry place it in its housing Ensure the insert hole is perfectly vertically aligned with the hole on the c...

Page 291: ... verifying the contact efficiency See Figure 15 17 12 Screw the detector cap into its housing See Figure 15 17 13 Place the detector cell on the base body and tighten the fixing screw See Figure 15 18 Figure 15 18 Clean Replace the Collecting Electrode 3 14 Reconnect the signal and ignition cables to the detector See Figure 15 18 15 Reset the detector to the required operating conditions ...

Page 292: ...or must be cooled to room temperature When handling organics solvents you must take precautions to avoid health hazards 1 In DETECTOR menu scroll to Flame and set OFF 2 Scroll to Temp and set OFF 3 Scroll to H2 and Air and set OFF 4 Disconnect the signal and ignition polarization cables from the detector See Figure 15 19 5 Loosen the fixing screw on the front of the detector cell and remove it See...

Page 293: ...ing screws and remove the lower connector holder assembly from the detector cell See Figure 15 19 7 Remount the new connector holder assembly and fix it to the detector cell using the two screws 8 Make sure the connecting fork is placed downwards to achieve the correct contact with the jet See Figure 15 20 Figure 15 20 Replace the Ignition Assembly 2 ...

Page 294: ...truction Manual 9 Place the detector cell on the detector base body and tighten the retaining screw See Figure 15 20 10 Reconnect the signal and ignition cables to the detector See Figure 15 20 11 Reset the detector to the required operating conditions See Figure 15 20 ...

Page 295: ...ble 15 3 Because to gain optimum analytical performance from the FID the hydrogen flow rate has been experimentally optimized To obtain the maximum signal intensity for the components of interest the carrier and air flows must be maintained constant An incorrect hydrogen flow rate reduces the FID sensitivity The flow rate of the air is less critical than the hydrogen one An excessive amount of air...

Page 296: ...hydrogen requires the operator s extreme caution due to the risks involved For further details concerning hydrogen please refer to Using Hydrogen on page xxiii Flame Ignition You can ignite the flame as soon as the detector temperature has reached 150 C After the flame appears to have ignited check for water vapor condensed on a mirror or on the polished end of a wrench directly over the FID exit ...

Page 297: ...ating Sequence on page 78 for instructions If required remove and clean the jet following the Clean Replace the FID Jet Operating Sequence on page 284 Faulty electronics Contact your customer support organization Appendix B Customer Communication contains contact information for Thermo Fisher Scientific offices and affiliates worldwide Contamination Contact your customer support organization Appen...

Page 298: ...ain halogenated or acid compounds at high concentrations Ensure that oxygen air could not enter into the filaments cells Oxidation would irreversibly damage the filaments Install traps for moisture and oxy gen on the gas lines to reduce the hazard WARNING Set Filament power to Off before disconnecting the column from the detector When the column is disconnected air will enter into the cell and the...

Page 299: ...or Insulated Box 2 Reference Gas Line 3 Make up Gas Line 4 Reference Gas Exhaust 5 Carrier Make up Gas Exhaust 6 Transfer Line Heater 7 Column Fitting 8 Fixing Nut 9 Kit for Connecting Capillary Column 10 Retaining Nut for 6 mm OD Column and Ferrule 11 Retaining Nut for 4 mm OD Column and Ferrule 10 9 1 4 3 2 6 7 8 5 11 ...

Page 300: ...eight compounds inside the cell or to contaminated gases Low temperatures of the detector block may cause high boiling compounds condensate on the filaments reducing sensitivity Baseline drift A small baseline drift normally occurs during a temperature program and does not indicate a trouble This effect is due to the decrease of the carrier gas flow rate as temperature increases A baseline that su...

Page 301: ...o a proper value Trans temp set too high Set Trans temp to a proper value about 10 to 20 C below the Block temp value Faulty temperature regulation Contact your customer support organization Refer to Appendix A Customer Communication for contact information Baseline drift Unstable regulation of the flow rate of the gases Check the controllers of the carrier reference and make up gases work well Le...

Page 302: ... to the actual operating mode Constant Voltage Constant Temperature Thermal conductivity of the carrier gas is too close to the one of the compound to be analyzed Use a different carrier gas Contaminated filaments Remove contamination by baking the filaments for one hour at a temperature higher than the boiling point of the most high boiling compound Perform baking twice if necessary If the sympto...

Page 303: ...vity Oxidized filaments Contact your customer support organization Refer to Appendix A Customer Communication for contact information The detector does not work Message Filament power Off Lack of carrier make up or reference gas or pressure too low Check the feed of the carrier make up and reference gas Filament burnt Contact your customer support organization Refer to Appendix A Customer Communic...

Page 304: ...rating sequence OPERATING SEQUENCE How to Install Replace the Loop of an Automatic Valve WARNING Before starting the FOCUS GC MUST BE SWITCHED OFF Operate as follows Remove the FOCUS GC Top Cover The top cover is fixed on the main unit with two front screws and two clips 1 Open the GC oven door 2 Unscrew the two front screws as shown in Figure 15 22 which remain on the main unit 3 Remove manually ...

Page 305: ... 4 By using the 1 4 inch wrench loosen the two fittings of the sampling loop and remove it See A and B of Figure 15 24 Figure 15 24 Sampling Loop Installation Replacing 5 Insert the new sampling loop then screw the two fittings by using the 1 4 inch wrench avoiding to overtighten them See B and C of Figure 15 3 6 5 4 3 2 1 Carrier Column Sample IN Sample OUT Sampling Loop 6 5 4 3 2 1 Carrier Colum...

Page 306: ... eventual subsidiary units are correct Gases Verify that the carrier gas line is turned on Verify that the detector gases are set to the correct flow rate Check that leaks are not present in the system Injection Use syringe for gas chromatography having appropriate volume The sample must be prepared and diluted correctly Always inject the same sample volume The split ratio must remain constant If ...

Page 307: ...fied by the red lighting of the Not Ready Error LED located on the GC Status Panel When lit this LED indicates that the injector and oven power has been cut off for safety reasons and an error message indicating the possible cause of error appears on the display See Error Messages Error Messages The following table reports the error messages and the explanation of the relevant correlated problem T...

Page 308: ...ine detector temperature exceeds the temperature limits Refer to the relevant MS detector manual TEMP SHUTDOWN Oven not heating The oven is not heating Contact local TE Customer Support TEMP SHUTDOWN Inlet not heating The inlet not heating Contact local TE Customer Support TEMP SHUTDOWN Det not heating The detector is not heating Contact local TE Customer Support TEMP SHUTDOWN X line not heating T...

Page 309: ...heir protection This message appears When trying to switch the TCD filaments to ON with Reference gas Off When trying to switch the TCD filaments to ON with Carrier gas Off When the Carrier gas is switched to Off with the filaments On When the Reference gas is switched to Off with the filaments On HW signal of pressure switch from the TCD control board With any key the message page is exit but the...

Page 310: ...Solve Analytical Problems 310 Instruction Manual Additionally a leak must be performed should any part of the system be disturbed Finally routine cleaning of injector and detector units will help to avoid problems occurring in the chromatographic system ...

Page 311: ...evels in the gas source Use correct gas purity Falling Carrier gas leak in the system Perform a leak test and ensure the tightness of the connections on the carrier gas line Column is baking out Allow enough time for the column to stabilize Rising Accumulation of impurities in column Check impurity levels in the gas source Use correct gas purity Contaminated detector Check the detector and clean i...

Page 312: ...g Reduce the upper column temperature Bake out the column Install a high temperature column Oxygen contamination is decomposing the stationary phase Install oxygen filters in carrier gas line Check pneumatic and inlet systems for leaks Use correct gas purity with low oxygen content Square waves Large AC power fluctuations heavy equipment on same line Use a dedicated clean AC line of sufficient amp...

Page 313: ...y Loose column fittings Tighten fittings accordingly Loose detector electrical connections Make sure the leads are properly connected Spiking Defective electrometer or amplifier Replace the electrometer or amplifier F s column too close to flame FID Lower the column to the correct position 2 3 mm below the tip of the jet Dirty jet or detector Isolate the detector from the electronics If noise disa...

Page 314: ... phase accumulated in the outlet Remove the last two coils from the column Detector base body temperature too low Increase the temperature to 5 C below the column maximum Clipping at bottom Detector or integrator zero set too low Set the zero correctly at top Data system zoomed in too close Zoom out to view the entire chromatogram Detector or integrator attenuation set too low Set the attenuation ...

Page 315: ...ee Decomposition of injected sample Decrease the injection port temperature Dirty injection solution Carry out adequate clean up of sample prior to injection Ghost peaks Broad ghost peaks Contaminated inlet or pneumatics Remove the column and bake out the inlet Use a high quality septum Replace the split vent filter Install an in line filter between the pneumatics and the inlet Incomplete elution ...

Page 316: ...igh Check the column position at all Clogged syringe needle Replace or repair the syringe Column broken or disconnected Check the column and connections Defective electrometer or amplifier Replace the electrometer or amplifier Defective recording device Replace the recording device FID flame is out Light the flame Poor or missing electrical connection Check the cable connections Incorrect column p...

Page 317: ...lumn manufacturer literature Incorrect column position in inlet Reinstall the column Initial oven temperature too high On Column Reduce the initial oven temperature Septum purge flow too low and or split splitless vent flow too low Check and adjust the septum purge and vent flows Too large injection size Reduce the injection size Unresolved peaks Carrier gas flow rate too high Reduce the carrier g...

Page 318: ...Non reproducible sample injection technique Evaluate the sample preparation sequences Compare the results with a series of standard injections Leaking syringe or septum Check and replace the syringe and or septum at regular intervals Leaks at the injection Check the column connections Run a leak check Poor injection technique Carefully meter the injected amount Use a clean good quality syringe Poo...

Page 319: ...eriorated by oxygen and or water Use a carrier gas free of oxygen and water Stationary phase loss due to column bleeding Reduce the column temperature Increasing Increasing carrier leakage Check the septum and column connections Carrier gas supply running out Replace the bottle Low reproducibility Drifting or unstable pneumatic controller Monitor the column pressure or flow Check and replace the c...

Page 320: ...Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems 320 Instruction Manual ...

Page 321: ... Option Set up This chapter contains notes on how to set up and start using the FOCUS GC with the LAN Local Area Network option Chapter at a Glance Introduction 322 Set Up 324 Operating Sequences How to Set up the FOCUS GC LAN 324 ...

Page 322: ...fault IP address To change the default values contact your LAN administrator and ask for the IP address to be assigned the netmask and eventually the port The IP address is a 3 digits x 4 fields number given by the network administrator e g 192 168 127 10 The netmask is a 3 digits x 4 fields number given by the network administrator e g 255 255 255 0 The port is a 4 digits number given by the netw...

Page 323: ...on located on the rear panel of the FOCUS GC for at least 5 seconds Network Cables Two network cables are included in the standard outfit of the FOCUS GC LAN a reversed RED patch for computer to FOCUS GC direct connection This is used for the initial set up operation a standard GREY patch for FOCUS GC to local area network connection This is used for normal use ...

Page 324: ...twork connecting RED cable Network connecting GREY cable Proceed as follows Verify that the GC and the PC are switched off 1 By using the LAN reversed RED patch included in the standard outfit connect a PC desktop or portable directly to the RJ45 connector marked LAN located on the rear panel of the FOCUS GC power module 2 Switch on the GC as well as the PC 3 Make sure your PC communicates with th...

Page 325: ...o communicate with the default IP address it is necessary to set your computer to a different IP address following the instruction reported in paragraph How to operate when the IP address is not reachable How to operate when the IP address is not reachable 1 Select the Local Area Network connection properties of your computer please refer to specific operating system instructions to access this co...

Page 326: ...ocol TCP IP and then click on Properties 3 Make sure the IP address of the computer you are using is set for same subnet of the default IP address of the FOCUS GC LAN It may be any IP in the range 192 168 127 1 to 192 168 127 253 Please also set the subnet as reported in the next figure ...

Page 327: ... address It may happen that for some reason the IP address has been previously changed from default to another IP address and therefore a reset procedure is advisable Refer to Reset Button on pagina 323 5 Proceed following the instructions reported in paragraph How to operate when the IP address is reachable How to operate when the IP address is reachable When the IP is reachable it means that the...

Page 328: ...am connects to the IP 192 168 127 254 and shows the following page 3 Confirm the default selection 1 by pressing ENTER The following page will be visualized With ARROWS ENTER and ESC keys you ll navigate the program 4 Select server Config to enter the new IP address and netmask ...

Page 329: ...N environment where the FOCUS GC LAN is installed Also the netmask is entered in the same menu section In this example the IP set is 192 168 0 101 so when the setup procedure is completed the FOCUS GC LAN will be communicating with a new IP Press ESC when the settings of this menu is over to return to upper level menu Press the right arrow key to select OP_mode and then press ENTER ...

Page 330: ...lect Raw connection TCP Server and then confirm with ENTER Press ESC when done to return to upper level menu After selecting Raw connection TCP server it will be possible to enter the Select for more setting menu and to enter a different TCP port rather than the default 4001 6 Use the arrow key to select Serial Port ...

Page 331: ...o the newly assigned IP Address 8 Disconnect the FOCUS GC from direct RED patch and connect it to its final destination LAN environment At this point as a final check start from the computer that should be used for controlling the newly installed FOCUS GC and run Command Prompt Then type ping xxx xxx xxx xxx where the xxx xxx xxx xxx is the new IP you just configured The FOCUS GC LAN should answer...

Page 332: ...ink Xcalibur ChromQuest ChemStation Data System Configuration It is advisable to use the tags you find in the standard outfit of the FOCUS GC LAN A couple of self adhesive labels are available to annotate the IP address and the TCP Port that have been set in the FOCUS GC LAN Please write on one of the label the two set parameters and stick the label in a place that can be easily referenced when it...

Page 333: ...munication port used by the TCP IP protocol and the timeout The parameters set by default are those necessary for standard operations however your LAN may be provided with Firewall services that may prevent the Port 4001 to be used For this reason you have here the possibility to set an alternative port number However the number of the port entered in this box must correspond to the port assigned ...

Page 334: ...rogram must be installed and used to monitor setup or update each of the instruments connected The program to be installed is named DSSETUP EXE and available in the CD of the Chrom Card data system as well as in the CD of this manual 1 Run the installation setup program DSSETUP EXE 2 Deselect the check box COM Port Mapping Tools since it is not required in the management of FOCUS GCs Please just f...

Page 335: ...acement of the step to step set up previously described in the document By double clicking on any of the found FOCUS GC you can also setup it directly Any change can be entered individually for a certain parameter and when OK is pressed the parameter is updated to the instrument on edit ...

Page 336: ...Chapter 16 LAN Option Set up Set Up 336 Instruction Manual ...

Page 337: ... reported in Customer Communication to contact your local Thermo Fisher Scientific office or affiliate This appendix also contains a one page Reader Survey Use this survey to give us feedback on this manual and help us improve the quality of our documentation Thermo Electron S p A INTERNATIONAL SALES DEPARTMENT Strada Rivoltana 20090 Rodano Milano Tel 39 02 95059 226 Fax 39 02 95059 256 Thermo Ele...

Page 338: ..._____________________________________________________________________________ ________________________________________________________________________________________ Fax or mail this form to Thermo Electron S p A Strada Rivoltana km 4 20090 Rodano MI ITALY Fax 39 02 95059388 Strongly Agree Agree Neutral Disagree Strongly Disagree The manual is well organized 1 2 3 4 5 The manual is clearly writte...

Page 339: ...s and symbols A A ampere ac alternating current ADC analog to digital converter B b bit B byte 8 b baud rate data transmission speed in events per second C ºC Celsius CIP Carriage and Insurance Paid To cm centimeter CPU central processing unit of a computer CSE Customer Service Engineer D d depth DAC digital to analog converter dc direct current DS data system E EMC electromagnetic compatibility ...

Page 340: ...ctronic circuit or device to increase the magnitude of an electronic input parameter GC gas chromatograph GND electrical ground H h height h hour harmonic distortion A high frequency disturbance that appears as distortion of the fundamental sine wave HV high voltage Hz hertz cycles per second I ID inside diameter IEC International Electrotechnical Commission impulse See transient ...

Page 341: ...lvin kg kilogram kPa kilopascal L l length l liter LAN Local Area Network lb pound LED light emitting diode M m meter or milli 10 3 M mega 106 µ micro 10 6 MBq megabecquerel mCi millicurie meniscus The curved upper surface of a column of liquid min minute mL milliliter mm millimeter ...

Page 342: ...ctor signal polarity nm nanometer O OD outside diameter Ω ohm P p pico 10 12 Pa pascal PCB printed circuit board PN part number PPKD Purged Packed Injector psi pounds per square inch R RAM random access memory RF radio frequency ROM read only memory RS 232 industry standard for serial communications S s second ...

Page 343: ...rage RMS voltage level with typical durations greater than 2 s source current The current needed to ignite a source such as a detector lamp surge A sudden change in average RMS voltage level with typical duration between 50 µs and 2 s T TCD Thermal Conductivity Detector TFS Thermo Fisher Scientific transient A brief voltage surge of up to several thousand volts with a duration of less than 50 µs V...

Page 344: ...Glossary 344 Instruction Manual C min 1 instead of C min g L 1 instead of g L ...

Page 345: ...ns Required for Splitless Injection 233 Parts Referenced 232 ChromQuest 218 Cleaning xxiv 261 Cleaning the unit 27 Collecting Electrode Cleaning 288 Replacement 288 Column Conditioning 217 231 245 Column Evaluation 217 231 245 Column Installation 217 231 245 Column Leak Check 217 231 245 Column Oven 26 28 Columns 29 Fittings 126 Ferrules 126 Retaining Nuts 127 Constant Filament Temperature 233 248...

Page 346: ...s Sampling Valve Maintenance 304 Overview 40 Sample In Out Ports 37 Servo air 36 Gas Supply Connections 216 230 244 Gases 218 219 232 233 247 248 Getting Started 197 Glass Liner 218 232 246 Breakage 263 Glass Liner Installation 216 230 244 gnition polarization cable 163 Graphite ferrule for 0 32 mm ID Column 218 232 246 Graphite seal for glass liner 218 232 246 Guide to Solve Analytical Problems 3...

Page 347: ...p 233 248 Make up Gas 219 Markings xviii Material Safety Data Sheets xxiv Messages 211 Methods and Sequences 31 N Negative Polarity 233 248 Network Cables 323 Nitrogen 219 233 248 Noise 227 241 256 Not Ready Error LED 44 O Operating Mode 219 233 248 Operating Procedure 217 231 245 Oven Program 219 233 248 P Packed Column Injector Septum 119 Pneumatic Compartment 26 Pneumatic compartment 26 PPKD Li...

Page 348: ... Status Panel 27 Surge Splitless Mode 112 Symbols xviii Syringe 218 232 246 T TCD Detector Gases Flow Regulation 77 Troubleshooting 300 TCD See Thermal Conductivity Detector TCD PPKD Acceptance Criteria 256 CHROM CARD 256 CHROMQUEST 256 Computing integrator e g ChromJet 256 TCD S SL Acceptance Criteria 241 CHROM CARD 241 CHROMQUEST 241 Computing integrator e g ChromJet 241 TCD S SL Analytical Cond...

Page 349: ...Index Instruction Manual 349 Troubleshooting the TCD 301 U Use of Gases xxii User Interface 27 41 42 Using Hydrogen xxiii Using the Hydrogen Sensor xxiv W Wander 227 241 256 X Xcalibur 218 ...

Page 350: ...Index 350 Instruction Manual ...

Page 351: ...Programming the PPKD Injector Surged Packed Mode 123 How to Connect a Capillary Column 132 How to Connect a Packed Column 138 Manual Checking for Leaks 147 Performing a Column Evaluation 148 Performing an Automatic Leak Check 154 Programming a FID 167 Setting the FID Signal Parameters 169 Programming a TCD 182 Setting the TCD Signal Parameters 184 Shutting Down the TCD 185 How to Set Up the Instru...

Page 352: ...lace or Clean the PPKD Liner 279 Clean Replace the FID Jet 284 Clean Replace the FID Collecting Electrode 288 Replace the FID Ignition Assembly 292 How to Install Replace the Loop of an Automatic Valve 304 ...

Page 353: ...eptum Purge System 95 Split Splitless Injector Components 96 S SL with a Packed Column 98 Split Injection Technique 102 Splitless Injection Technique 104 Purged Packed Column Injector 114 PPKD Injector Components 115 Capillary Wide Bore Column to Injector and Detector Base Body Connections 127 Metric Packed Column Fittings 129 Injector and Detector Base Body Adapters 130 Convertion Kit 131 Metal P...

Page 354: ... Rear Panel 274 Filter Replacing 275 PPKD Injector Septum Replacement 278 PPKD Injector Replace Clean the Liner 280 FID Parts Identification 283 Clean Replace the Jet 1 285 Clean Replace the Jet 2 286 Clean Replace the Jet 3 287 Clean Replace the Jet 4 287 Clean Replace the Collecting Electrode 1 289 Clean Replace the Collecting Electrode 2 290 Clean Replace the Collecting Electrode 3 291 Replace ...

Page 355: ...s 68 Info Diagnostics 69 Carrier Gas Parameters Menu 81 Oven Parameters Menu 87 Liner Sizes and Applications 97 Inlet Modes 107 Inlet Parameters Menu 108 Inlet PPKD Menu 118 Ferrules 127 Metric Packed Column Fittings 128 Imperial Size Packed Column Fittings 130 FID Parameters 164 FID Signal Parameters 166 Thermal Conductivity of Gases 174 Filament Temperature Values for Argon 178 Selectable TCD Pa...

Page 356: ...l Conditions 233 TCD S SL Acceptance Criteria 241 TCD PPKD Parts Referenced 246 TCD PPKD Analytical Conditions 248 TCD PPKD Acceptance Criteria 256 Standard Maintenance Schedule 260 Gases used for FID 295 Gas for FID Flow Rates 295 Difficulty in Igniting the Flame 296 TCD Troubleshooting Table 301 Error Messages 307 ...

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