Page 1 Thermo Scientific FOCUS GC Gas Chromatograph Instruction Manual PN 31709412, Revision May 2007 HOME...
Page 2 Reference to System Configurations and Specifications supercede all previous information and are subject to change without notice. Trademarks FOCUS™ GC is a trademark of Thermo Thermo Scientific Inc., and its subsidiaries. Other brand and product names may be trademarks or registered trademarks of their respective companies.
Page 3 Declaration Manufacturer: Thermo Electron S.p.A. Thermo Electron S.p.A. is the manufacturer of the instrument described in this manual and, as such, is responsible for the instrument safety, reliability and performance only if: • installation • re-calibration • changes and repairs have been carried out by authorized personnel and if: •...
Page 4 Instruction Manual...
Page 5: Table Of Contents
Contents About This Manual..........................xiii Overview ..........................xiii Conventions Used in This Manual................... xv Instrument Markings and Symbols ..................xviii Using the FOCUS GC Document Set ..................xx Classification of the Instrument ....................xxi Technical Features ........................xxi Safety Information .........................xxii Use of Gases......................xxii Using Hydrogen ........................xxiii...
Page 6 Electrical Connections................... 37 Oven Exhaust Vent..................38 Top Panel........................39 Gas Sampling 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 ...................
Page 7 Contents AS 2000 Autosampler..................56 AI 3000/AS 3000 ................... 56 Messages ......................57 General Configuration Menu ..................58 Keyboard & Display Configuration Menu..............58 Beep Table ..................... 59 Handshake Configuration Menu ................. 60 Time Configuration Menu ..................61 Valves Configuration Menu..................61 Run Time Events........................
Page 8 Contents Packed Columns .................... 98 S/SL Injection Techniques..................... 101 Split Injection Technique..................101 Splitless Injection Technique..................103 Refocusing the Sample ................105 Flooding....................... 106 S/SL Inlet Parameters ......................107 Chapter 6 Purged Packed Column Injector (PPKD) ..................113 PPKD Overview ........................114 Septa .........................
Page 9 Contents Chapter 8 Flame Ionization Detector (FID) ....................... 157 FID Overview......................... 158 Detector Base Body ....................158 Detector Gas......................159 Jet ..........................159 Selectivity........................160 Temperature ......................160 FID Gas Supplies ........................161 FID Installation ........................162 FID Menu ..........................164 Flame Out Conditions ....................
Page 10 Contents Sequence Programming ......................195 Chapter 11 Getting Started ..........................197 Instrument Set-up........................198 Run Time Events ........................202 Controlling Valves......................... 206 Run Time Control (Gas Sampling Valve Only) ............206 Manual Control......................206 Instrument Start-Up ....................... 208 Instrument Status Messages....................211 Not Ready .........................
Page 11 Contents Parts Referenced ....................... 246 Analytical Conditions Required for Splitless Injection ..........248 Chapter 15 Maintenance and Troubleshooting 257 Maintenance ........................... 259 How To Perform Maintenance.................. 259 Suggested Maintenance Schedule................259 Septa......................259 Ferrules and Seals ..................260 Traps ......................260 Detector Unit....................
Page 12 Contents Chapter 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 ..............................
Page 13: About This Manual
Overview This Operating Manual contains descriptions of the features and components of the FOCUS GC gas chromatograph. Inside, you will find all of the information necessary for routine operation of your GC, including operating sequences, sample injection techniques, and diagrams and descriptions of the major components.
Page 14 AI 3000/AS 3000 by using the FOCUS GC keypad. This chapter contains also the instructions to programming a sample sequence with the FOCUS GC keypad when an AS 2000 or an AI 3000/AS3000 is used and how to set up ranges of samples to run automatically.
Page 15: Conventions Used In This Manual
Conventions Used in This Manual About This Manual Conventions Used in This Manual The following symbols and typographical conventions are used throughout this manual. Bold Bold text indicates names of windows, dialog boxes, and fields. Italic Italic indicates cross references, first references to important terms defined in the glossary, and special emphasis.
Page 16 About This Manual Conventions Used in This Manual This symbol indicates danger from hazardous chemicals. This symbol indicates danger from high temperature surfaces or substances. This symbol indicates a fire hazard. This symbol indicates an explosion hazard. This symbol indicates a toxic hazard. This symbol indicates the presence of flammable materials.
Page 17 Conventions Used in This Manual About This Manual 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: Instrument Markings And Symbols
About This Manual Instrument Markings and Symbols Instrument Markings and Symbols The following table explains the symbols used on Thermo Fisher Scientific instruments. Only a few of them are used on the FOCUS GC gas chromatograph. Symbol Description Direct Current...
Page 19 Instrument Markings and Symbols About This Manual Symbol Description Equipment protected throughout by DOUBLE INSULATION or REINFORCED INSULATION (Equivalent to Class II of IEC 536) Indicates that the user must refer to the manual for specific Warning or Caution information to avoid personal injury or damage to the product.
Page 20: Using The Focus Gc Document Set
FOCUS hardware and software. The FOCUS GC Document Set (PN 317 094 10) as paper copy is also available Furthermore,Thermo Fisher Scientific part numbers (PN) for the paper copy manuals are provided for each book title.
Page 21: Classification Of The Instrument
• 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 —...
Page 22: Safety Information
About This Manual Safety Information Safety Information WARNING! The instrument must be used according to the specifications of this guide. Improper use can adversely affect the instrument protection. The analytical operation requires the use of chemical substances having different hazard specifications. 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.
Page 23: Using Hydrogen
Perform this test after the pressure test described in the instrument. Testing for Leaks paragraph in FOCUS GC Site Preparation and Installa- tion Guide Manual. Repeat this test to eliminate all leaks. • Ensure your GC column oven has a Thermo Fisher Scientific hydrogen sen- sor.
Page 24: Using The Hydrogen Sensor
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 CSEs are not authorized to install or repair any instrument using hydrogen as a carrier gas unless the instrument is equipped with the appro- priate sensor.
Page 25: Focus Gc Description
FOCUS GC Description This chapter provides a basic overview 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.
Page 26: Instrument Overview
Chapter 1 FOCUS GC Description Instrument Overview Instrument Overview The FOCUS GC consists of four major components, as shown in Figure 1-1. FOCUS GC Components 1. Pneumatic Compartment 3. Electronic Compartment 2. Analytical Unit 4. Status Panel and Keyboard Figure 1-1. FOCUS GC Components Pneumatic Compartment The pneumatic compartment contains the pneumatic gas control circuits.
Page 27: Electronic Compartment
• the low voltage compartment Status Panel and Keypad The status panel and the keypad make up the FOCUS GC user interface. Gas Control The GC is equipped with digital pneumatics for carrier gas control and conventional pneumatics for detector gases control.
Page 28: Detector Gas Control
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 precise analytical performance and helps prevent chromatogram peak distortion.
Page 29: Purged Packed Column (Ppkd) Injector
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 GC because of its high sensitivity, good stability and wide range of linearity of response. The FID ensures stable, reproducible, and long-term trouble-free performance.
Page 30: Thermal Conductivity Detector (Tcd)
Thermal Conductivity Detector (TCD) External Detectors FOCUS GC may also operate with external detectors. An external detector is a detector controlled by an external control module. The FOCUS GC only provides the heating through the base body, the gas supply and the signal analog to digital conversion for acquisition.
Page 31: Gc Parts Description
This paragraph gives you a detailed description of the instrument components. Front Panel 1. Column Oven Door 3. Status Panel and Keypad 2. Column Oven Door Push Button 4. Electronic Compartment Figure 1-2. FOCUS GC Front Panel It comprises: • Column Oven • Status Panel and keypad •...
Page 32: Column Oven
Chapter 1 FOCUS GC Description GC Parts Description Column Oven The FOCUS GC column oven, shown in Figure 1-3, is accessible opening the column oven door by pushing the relevant button. Figure 1-3. Column Oven Internal View Refer To...Chapter 4,...
Page 33: Electronic Compartment
Chapter 1 GC Parts Description FOCUS GC Description Electronic Compartment It is located on the bottom part of the GC, and it is accessible only by authorized Thermo Fisher Scientific technical personnel. WARNING! Before opening the electrical compartment, cut off power supply to the instrument and disconnect the power cord.
Page 34 Chapter 1 FOCUS GC Description GC Parts Description factory set, located on the Main Board. According to the instrument power supply configuration, the breaker ON/OFF main switch changes as follows: Power Supply Breaker 120 Vac 230 Vac The high voltage section is provided of a series of protection fuses as reported in...
Page 35: Rear Panel
Chapter 1 GC Parts Description FOCUS GC Description Rear Panel The FOCUS GC Rear Panel is shown in Figure 1-6. 1000 kPa/120 psi CARRIER Max for all inputs H SENSOR SERVO AIR max 500 kPa MAKE UP MAKE-UP REF. SAMPLE...
Page 36: Carrier Gas Inlet Port
WARNING! Pressure of the supply gas lines should be set to a minimum of 400 kPa (60 psi) to ensure the regulation of detector gases. Maximum input pressure to FOCUS GC (from supply gas lines) is 1000 kPa (145 psi). Servo Air for Gas Sampling Valve Inlet Port It is located on the left upper part of the instrument rear panel.
Page 37: Gas Sampling Valve Sample In/Out Ports
Chapter 1 GC Parts Description FOCUS GC Description WARNING! Pressure of the servo air supply line should be set to a maximum of 500 kPa (72 psi). Gas Sampling Valve Sample In/Out Ports They are located on the middle upper part of the instrument rear panel.
Page 38: Oven Exhaust Vent
The IP address and communication port may be reset to default value by pushing the reset button, accessible from the rear panel of the FOCUS GC, for at least 5 seconds. CAUTION The reset button is accessible introducing a little screwdriver into the relevant passing hole.
Page 39: Top Panel
Chapter 1 GC Parts Description FOCUS GC Description Any material exposed to the oven exhaust must be able to withstand repeated exposure to temperatures of up to 350°C (660 °F). WARNING! Oven exhaust can cause severe burns. Avoid working behind the instrument when the oven vents during cooling-down cycles.
Page 40: Gas Sampling Valve Overview
FOCUS GC Description GC Parts Description Gas Sampling Valve Overview A valve for the automatic sampling of gas is available with the FOCUS GC. The valve is installed behind the injector/detector compartment of the GC. The valve is not heated.
Page 41: The Focus Gc User Interface
The FOCUS GC User Interface FOCUS GC user interface, provides basic information about key functions 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.
Page 42: Overview
LEDs showing the instrument’s status • 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.
Page 43: The Focus Gc User Interface
Scroll Indicator Parameter Line Actual Value Figure 2-2. Components of the FOCUS GC Menu Display The following are the menu display components: Menu Title—This is the first line of each menu. The menu title is always visible when scrolling through the menu items.
Page 44: The Display Leds
Chapter 2 The FOCUS GC User Interface Overview The Display LEDs The LEDs (Light Emitting Diodes) on the left side of the display screen indicate the FOCUS GC’s operating status. The status LEDs indicate the current operating mode and special settings activated by the operator.
Page 45: The Focus Gc Keypad
Overview The FOCUS GC User Interface The FOCUS GC Keypad The following Table lists and describe the keys on the FOCUS GC Keypad. Table 2-2. Keypad Descriptions Description The blue START key is a double function key. When pressed a first time it starts the PREP RUN function.
Page 46: Parameters Entry
Chapter 2 The FOCUS GC User Interface Overview Parameters Entry The user points to any of the parameter navigating with the keys HOME, SCROLL UP and SCROLL DOWN. Only the bottom line is dedicated to parameters editing, first line is only for menu title and doesn’t scroll.
Page 47: User Interface Main Menu
Chapter 2 User Interface Main Menu The FOCUS GC User Interface User Interface Main Menu To open the main menu, press the HOME key. The Main menu contains the following page menus available sequentially by pressing the SCROLL UP and SCROLL DOWN arrow keys.
Page 48: Inlet
Chapter 2 The FOCUS GC User Interface User Interface Main Menu Inlet INLET Temp 200 200 Use this page to set inlet parameters such as temperature and split flow. Refer to Chapter 5 Split/Splitless Injector (S/SL) or Chapter 6 Purged Packed Column Injector (PPKD)for more information about Inlet menu options.
Page 49: No Detector
Chapter 2 User Interface Main Menu The FOCUS GC User Interface No Detector ATTENTION! If the detector is not present but the detector zone is enabled, the following page is displayed: DETECTOR (MS) MS X-line External Detector In the case of external detector the following page will be displayed:...
Page 50: External Detector
Chapter 2 The FOCUS GC User Interface User Interface Main Menu External Detector In case of external detector the following page will be displayed: SIGNAL (FID-X) Output (1000000) The name of the external detector in use, e.g. FID-X, is added to the title line.
Page 51: Others
• Run-Log • Configuration • 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 •...
Page 52: Configuration Menu
Chapter 2 The FOCUS GC User Interface Configuration Menu Configuration Menu In Main Menu press the SCROLL DOWN key until the page appears, then Others press ENTER. OTHERS Configuration and press ENTER. The following table describes the Scroll to Configuration items in the menu.
Page 53: Oven Configuration Menu
Chapter 2 Configuration Menu The FOCUS GC User Interface Oven Configuration Menu The FOCUS GC oven provides great flexibility in controlling and programming temperatures. In the menu you can set various preparatory CONFIGURE OVEN parameters. CONFIGURE OVEN Max temperature Equilib. Time 10.00...
Page 54: Carrier Configuration Menu
Chapter 2 The FOCUS GC User Interface Configuration Menu Carrier Configuration Menu Commonly used gases are Helium, Hydrogen and Nitrogen. Hydrogen offers the best chromatography properties (optimum resolution at the highest flow rates). However, because Hydrogen is flammable, Helium is often used as an alternative for carrier gas.
Page 55: Detector Configuration Menu
This line is available ONLY if the detector board is present and detected at GC power An external detector is a detector controlled by an external control module. The FOCUS GC only provides the heating through the base body, the gas supply and the signal analog to digital conversion for acquisition.
Page 56: Autosampler Configuration Menu
, Make-up Other-x , Air, Make-up Autosampler Configuration Menu The autosampler method can be controlled from the FOCUS GC or the data system. ATTENTION! Only with the AS 2000 the alignment must be programmed with control module. You specify the information required in the...
Page 57: Messages
Chapter 2 Configuration Menu The FOCUS GC User Interface Table 2-7. Configure AI 3000/AS 3000 Autosampler Menu Parameter Range Description This line is the title bar. CONFIG AUTOSAMPLER 5 – 10 µL Select the parameter according to the volume of the Syringe volume syringe installed on the autosampler.
Page 58: General Configuration Menu
Chapter 2 The FOCUS GC User Interface Configuration Menu General Configuration Menu Use this item to visualize the mains supply frequency. GENERAL CONFIG AC mains freq. Table 2-8. General Config Menu Parameter Range Description This line is the title bar.
Page 59: Beep Table
Chapter 2 Configuration Menu The FOCUS GC User Interface Table 2-9. Configure Keyboard & Display Menu Parameter Range Description This line is the title bar. CONFIG KEYB. & DISP: On – Off This parameter locks the keypad from editing. Keyboard lock...
Page 60: Handshake Configuration Menu
Configuration Menu Handshake Configuration Menu The FOCUS GC can be coupled to other instruments, such as an autosampler or a mass spectrometer. To allow other devices to run properly, you must indicate how the signal will change. For example, the menu line specifies that another device will start the GC when the remote start signal changes from high to low.
Page 61: Time Configuration Menu
Chapter 2 Configuration Menu The FOCUS GC User Interface Time Configuration Menu FOCUS GC displays the current date and time. You can set this time from the menu. When you open the menu, the following CONFIGURE CONFIGURE TIME items appear:...
Page 62: Run Time Events
Chapter 2 The FOCUS GC User Interface Run Time Events Table 2-13. Configure Valves Menu Parameter Range Description This line is the title bar. CONFIGURE VALVES None Select in this box Sampling only if a gas sampling valve Valve #1 Gas Sampling is present and connected the GC.
Page 63 Chapter 2 Run Time Events The FOCUS GC User Interface RUN TIME EVENTS <None> Add run time event Option Description No events are programmed <none> Scroll to this line end press ENTER to add an event Add run time event...
Page 64: Run-Log
Chapter 2 The FOCUS GC User Interface Run-Log Table 2-14. Edit Time Event Menu (Continued) Parameter Range Description From 0 to 3 for Det range Select the correct setpoint according to the event Setpoint On/Off for EV you have set in the previous line. This line doesn’t appear for Det autozero.
Page 65 Chapter 2 Run-Log The FOCUS GC User Interface RUN LOG (XofY) RUN LOG (XofY) ’ ’ Itime 200.00 220.00 Itime 200.00 220.00 at run time 0.50 at run time 0.50 ’ ’ ITemp 120 ITemp 120 at run time 2.00 at run time 2.00...
Page 66: Time
Chapter 2 The FOCUS GC User Interface Time Time This option allows you to visualize the following parameter • Time • Date • Last run time • Next run time • Elapsed time and time remaining during the current run •...
Page 67: Valves
Chapter 2 Valves The FOCUS GC User Interface TIME Elapsed time 5.00 Time left 110.00 We 13 Mar 2002 12:03 V=100 F=100.0 01:00 Measured volume Valves Use this feature to specify and control up to four valves, or to manually change the state of inlet valves.
Page 68: Info/Diagnostics
Chapter 2 The FOCUS GC User Interface Info/Diagnostics When a gas sampling valve is present and configured (refer to Valves Configuration Menu in paragraph Configuration) a menu appears it follows: VALVES Split valve Sept purge valve GSValve#1 Load EV#1 Table 2-15. Valves...
Page 69 Chapter 2 Info/Diagnostics The FOCUS GC User Interface INFO/DIAGNOSTICS Serial #: 12345678 FW ver: 2.00.31 DPFC ver: 0.27 BOOT ver: 1 B.0 Manufact.: 1/Jan/02 Total runs 1234567 Ambient press 103.0 Table 2-16. Info/Diagnostics Parameter Description This line is the title bar.
Page 70 Chapter 2 The FOCUS GC User Interface Info/Diagnostics Instruction Manual...
Page 71: Chapter 3 Gas Control
Gas Control This chapter contains information on controlling and programming the carrier 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..................
Page 72: Gas Supplies
Contact a Thermo Fisher Scientific sales representative if you plan to use hydrogen as the carrier gas in FOCUS GC. If you don’t have the hydrogen sensor, you must use an inert carrier gas.
Page 73: Configuring The Carrier Gas
Chapter 3 Gas Supplies Gas Control OPERATING SEQUENCE Configuring the Carrier Gas Carrier gas is already configured to Helium. To change the configuration, proceed as follows: 1. In the Main Menu move the cursor until is selected, then press Others ENTER.
Page 74: Configuring The Pressure Unit
Chapter 3 Gas Control Gas Supplies OPERATING SEQUENCE Configuring The Pressure Unit The pressure Unit is already configured to kPa (kilo pascal). To change the configuration proceed as follows: 1. In the Main Menu move the cursor until is selected, then press Others ENTER.
Page 75: Carrier Gas Regulation
WARNING! Pressure of the supply gas lines should be set to a minimum of 400 kPa (60 psi) to ensure the regulation of detector gases. Maximum input pressure to FOCUS GC (from supply gas lines) is 1000 kPa (145 psi). The pressure regulation is accessible from outside the instrument. The adjustment of the detector gases is done in factory prior shipment.
Page 76: Fid-External Detector Gases Flow Regulation
Chapter 3 Gas Control Detector Gas Regulation FID Gases The FID requires hydrogen and air as fuel gas and nitrogen as make-up gas. The adjustment of the detector gases flow is done in factory prior shipment. Flow Hydrogen (fuel gas) 35 mL/min Air (fuel gas) 350 mL/min...
Page 77 Chapter 3 Detector Gas Regulation Gas Control Flow Helium (make-up gas) 27 mL/min Helium (reference gas) 30 mL/min Verify that the corresponding gases flows are correct. If not adjust the value turning the relevant regulation screw as shown in Figure 3-2. Make-up Ref.
Page 78: Measuring Gas Flow
Chapter 3 Gas Control Measuring Gas Flow Measuring Gas Flow The septum purge and split flows can be measured at the relevant vents located on the top of the instrument. Detector gas flows can be measured at the detector vent. Use a bubble flow meter or a calibrated electronic flow meter to check flows.
Page 79 Chapter 3 Measuring Gas Flow Gas Control 6. Scroll to the stopwatch line ( F= 000 00:00 , press ENTER to 7. When the meniscus passes the flowmeter start line, marked start the stopwatch. 8. When the meniscus passes the flowmeter line corresponding to the volume set , press ENTER to stop the stopwatch.
Page 80: Carrier Gas Parameters
Chapter 3 Gas Control Carrier Gas Parameters Carrier Gas Parameters This paragraph explains the electronic programming and control of the GC carrier gases. The Digital Pressure Flow Control (DPFC) module regulates carrier gas electronically. You control the gas flow by programming parameters in the carrier gas menu.
Page 81: Carrier Gas Parameters Menu
Chapter 3 Carrier Gas Parameters Gas Control CARRIER (He) CARRIER (He) Pressure (100) Pressure 100 100 Col.Flow 12.0 12.0 Col.Flow (10.0) Flow mode Const flow Flow mode Const Pres Gas saver flow Gas saver flow Saver time 1.00 Saver time 1.00 Vacuum comp.
Page 82 Chapter 3 Gas Control Carrier Gas Parameters Table 3-1. Carrier Gas Parameters Menu Parameter Range Description From 10 to 500 ml/min Activates gas saver control to reduces carrier gas Gas Saver Flow in step of 1 ml/min; consumption after the injection or in Standby (suggested at high split mode).
Page 83: Chapter 4 Column Oven
Column Oven This chapter describes the features 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 ..........
Page 84: Column Oven Overview
Column Oven Overview Column Oven Overview The FOCUS GC column oven, shown in Figure 4-1, provides a stable heating environment for the analytical column. The oven heats and cools quickly. Efficient air circulation ensures a high degree of thermal stability.
Page 85: Oven Safety
Chapter 4 Column Oven Overview Column Oven Oven Safety Opening the oven door cuts off the power to the oven heater and fan. The setpoints are kept in memory. The display shows the following safety message: OVEN Temp 100 door open To return to normal operation, close the oven door.
Page 86: Column Oven Configuration
Chapter 4 Column Oven Column Oven Configuration Column Oven Configuration menu contains the control parameters for the column CONFIGURE OVEN oven. Refer to Oven Configuration Menu in Chapter 2 for more information about the menu. CONFIGURE OVEN CONFIGURE OVEN Max temperature Equilib.
Page 87: Oven Parameters
Chapter 4 Oven Parameters Column Oven Oven Parameters menu contains the parameters for programming the oven temperature, OVEN from an initial temperature to a final temperature, using up to three ramps during the analytical run. It is possible to set a single (isothermal) or multiple ramp program.
Page 88 Chapter 4 Column Oven Oven Parameters Table 4-1. Oven Parameters Menu (Continued) Parameter Range Description From 30 to 350 °C In This parameter defines the temperature the column Final temp 1 step of 1 °C oven will reach at the end of the heating or cooling ramp.
Page 89: Setting Up A Single Ramp Temperature Program
Chapter 4 Oven Parameters Column Oven OPERATING SEQUENCE Setting Up a Single Ramp Temperature Program This program raises the initial oven temperature to a specified final temperature at a specified rate and maintains the final temperature for a specified time. Use INC and DEC keys to increase or decrease the parameter values and confirm pressing ENTER.
Page 90: Setting Up Multiple Ramp Temperature Program
Chapter 4 Column Oven Oven Parameters 5. Scroll to and enter the final temperature for the ramp. Final Temp 1 6. Scroll to and enter the time the oven will maintain the Final Final Time 1 temp. 7. To end the single ramp program, must be Ramp 2 OPERATING SEQUENCE...
Page 91 Chapter 4 Oven Parameters Column Oven 3. Scroll to and enter the time you want the oven to maintain Initial Time the initial temperature. 4. Scroll to and set it . Enter the ramp rate in °C/min for the oven to Ramp 1 reach the ramp’s Final Temp.
Page 92 Chapter 4 Column Oven Oven Parameters Instruction Manual...
Page 93: Split/Splitless Injector (S/Sl)
Split/Splitless Injector (S/SL) This chapter describes the Split/Splitless (S/SL) injector and contains 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................
Page 94: S/Sl Overview
Chapter 5 Split/Splitless Injector (S/SL) S/SL Overview S/SL Overview The S/SL injector, shown in Figure 5-1, is optimized for either split or splitless applications to ensure effective sample transfer into the column, minimizing heavy component discrimination. 1. Septum Cap 7. Graphite Column Ferrule 2.
Page 95 Chapter 5 S/SL Overview Split/Splitless Injector (S/SL) For both split and splitless applications, the sample is injected through a septum into a glass liner in the vaporization chamber. The technique used, either split or splitless, determines the choice of the glass liner and the length of the syringe needle.
Page 96 Chapter 5 Split/Splitless Injector (S/SL) S/SL Overview 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.
Page 97: Septum
Septum Standard Septum You should always use good quality septa, such as the BTO septa supplied with the FOCUS GC. Such septa resist deformation, have longer life expectancy, and have a low bleed level, even at high temperatures. Microseal™ Valve S/SL injector is compatible to use Merlin Microseal™...
Page 98: Packed Columns
Chapter 5 Split/Splitless Injector (S/SL) S/SL Overview Packed Columns With a special adapting kit, you can install packed columns in the S/SL injector, as shown in Figure 5-4. 1. Carrier Gas Inlet 3. Septum Purge Line 2. Split Line Figure 5-4. S/SL with a Packed Column Instruction Manual...
Page 99: Septum
Chapter 5 S/SL Overview Split/Splitless Injector (S/SL) OPERATING SEQUENCE Installing a Liner and a Septum Materials required: • liner • septum • tweezers • graphite seal • liner cap wrench (included with the GC) NOTE he injector fittings may be hot. This sequence must be performed with the injector at working temperature.
Page 100 Chapter 5 Split/Splitless Injector (S/SL) S/SL Overview 6. Use tweezers to pick up the septum. Place the septum into the septum holder, then place the holder on top of the complete injector assembly. CAUTION To avoid contamination, do not touch the septum with your hands. 7.
Page 101: S/Sl Injection Techniques
Chapter 5 S/SL Injection Techniques Split/Splitless Injector (S/SL) S/SL Injection Techniques You use different sample injection techniques for split and splitless applications. Split Injection Technique In split injection, only a part of the sample transfers into the column. The rest discharges through the split line.
Page 102: Split Injection Technique
Chapter 5 Split/Splitless Injector (S/SL) S/SL Injection Techniques 1. Carrier Gas Inlet 3. Septum Purge Line 2. Split Line 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.
Page 103: Splitless Injection Technique
Chapter 5 S/SL Injection Techniques Split/Splitless Injector (S/SL) Splitless Injection Technique Splitless injection is suitable for the analysis of compounds present in very low concentrations. The splitless technique allows the entire sample to enter the column without splitting. This offers better sensitivity than the split technique. With splitless injection, the split line is closed during the sample injection and transfer to the column.
Page 104: Splitless Injection Technique
Chapter 5 Split/Splitless Injector (S/SL) S/SL Injection Techniques 1. Carrier Gas Inlet 3. Split Line 2. Septum Purge Line Figure 5-6. Splitless Injection Technique The transfer of the vaporized sample from the injector to the 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.
Page 105: Refocusing The Sample
Chapter 5 S/SL Injection Techniques Split/Splitless Injector (S/SL) For narrow bore columns (< 0.20 mm ID) with inherently lower flows (< 1.0 mL/ min), the transfer is even longer. You can counter this by using the splitless surge pressure mode. In this mode, the pressure in the injector temporarily increases during the splitless period to increase the flow into the column.
Page 106: Flooding
Chapter 5 Split/Splitless Injector (S/SL) S/SL Injection Techniques Flooding Splitless injections may occasionally exhibit an effect known as flooding, which can results in peak distortion. Peak distortion due to flooding is generally critical only when sample volume exceed 3-4 μL or when a very polar solvent is used (as methanol) or a narrow bore columns (<0.2 mm ID) are used.
Page 107: S/Sl Inlet Parameters
Chapter 5 S/SL Inlet Parameters Split/Splitless Injector (S/SL) S/SL Inlet Parameters menu includes the operating parameters for the split/splitless INLET injector. The parameters you can edit depend on the operating mode chosen: split, splitless, or splitless with surge. is selected. Press ENTER to open In Main Menu move the cursor until Inlet menu...
Page 108 Chapter 5 Split/Splitless Injector (S/SL) S/SL Inlet Parameters Split Mode Splitless Mode Surge Splitless Mode INLET (S/SL) INLET (S/SL) INLET (S/SL) Temp 200.. 200 Temp 200..200 Temp 200..200 Mode Split Mode Splitless Mode Surge Splitless Total flow (150.0) Total flow (150.0) Total flow (150.0)
Page 109 Chapter 5 S/SL Inlet Parameters Split/Splitless Injector (S/SL) Table 5-3. Inlet Parameters Menu (Continued) Menu Range Comments 0–99.99 min This line shows the splitless time, which is the duration Splitless time in steps of 0.01 min of split valve closure. 10–1000 kPa Specify the surge pressure to accelerate the transfer Surge...
Page 110: Programming The Split Mode
Chapter 5 Split/Splitless Injector (S/SL) S/SL Inlet Parameters OPERATING SEQUENCE Programming the Split Mode In split injection, only a portion of the sample transfers to the column. Most of it discharges through the splitting line. The ratio between the split flow and the column flow defines the amount of sample that enters the chromatographic system.
Page 111: Programming The Splitless Mode
Chapter 5 S/SL Inlet Parameters Split/Splitless Injector (S/SL) OPERATING SEQUENCE Programming the Splitless Mode In splitless analyses, the splitting line is closed during the sample transfer onto the column. The time during which the splitting valve remains closed is called the splitless time.
Page 112: Programming The Surge Splitless Mode
Chapter 5 Split/Splitless Injector (S/SL) S/SL Inlet Parameters OPERATING SEQUENCE Programming the Surge Splitless Mode In surge splitless mode, a carrier gas pressure surge activates during the injection phase for a preset time. This surge accelerates the transfer process of the substances from the injector to the column.
Page 113: Purged Packed Column Injector (Ppkd)
Purged Packed Column Injector (PPKD) This chapter describes Purged Packed (PPKD) column injector, which has a septum purge. Included in this chapter are PPKD injection techniques and operating sequences. Chapter at a Glance… PPKD Overview ....................114 PPKD Injection Techniques ................
Page 114: Ppkd Overview
Chapter 6 Purged Packed Column Injector (PPKD) PPKD Overview PPKD Overview The Purged Packed (PPKD) column injector is a packed column injector with a septum purge. The PPKD standard injector 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.
Page 115 Chapter 6 PPKD Overview Purged Packed Column Injector (PPKD) Figure 6-2 shows the 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.
Page 116: Septa
Chapter 6 Purged Packed Column Injector (PPKD) PPKD Injection Techniques Septa You should use high temperature septa with a longer life expectancy, good resistance to deformation, and a low bleed level, even at high temperatures. Use high temperature septa for both manual and automatic injections. Liners Two different glass liners can be used for wide-bore capillary columns: •...
Page 117 Chapter 6 PPKD Injector Menu Purged Packed Column Injector (PPKD) Mode Description Parameters to set The column flow is controlled through true mass flow Packed control. The column flow is controlled through true mass flow Surged Packed Surge pressure control. A carrier gas pressure surge activates during the Surge duration injection phase for a preset time.
Page 118: Inlet (Ppkd) Menu
Chapter 6 Purged Packed Column Injector (PPKD) PPKD Injector Menu Table 6-1. Inlet (PPKD) Menu Menu Range Comments This line is the menu title bar. INLET(PPKD) ° 50–375 This line shows the base injector temperature. Temp Packed, This line displays the currently selected operating Mode: mode.
Page 119: Replacing A Septum
Chapter 6 PPKD Injector Menu Purged Packed Column Injector (PPKD) OPERATING SEQUENCE Replacing a Septum Materials required: • septum • tweezers WARNING! he injector fittings may be hot. Make sure the injector is at room temperature before replacing the septum. 1.
Page 120: Programming The Ppkd Injector Wide Bore Mode
Chapter 6 Purged Packed Column Injector (PPKD) PPKD Injector Menu OPERATING SEQUENCE Programming the PPKD Injector Wide bore Mode Before programming the purged packed column injector, do the following: • Verify that a wide-bore column is correctly installed, the correct liner is in the injector and the system is free of leaks.
Page 121 Chapter 6 PPKD Injector Menu Purged Packed Column Injector (PPKD) OPERATING SEQUENCE Programming the PPKD Injector Surged Wide bore Mode In the mode, a carrier gas pressure surge activates during Wide bore w/surge the injection phase for a preset time. This surge accelerates the transfer process of the substances from the injector to the column.
Page 122: Mode
Chapter 6 Purged Packed Column Injector (PPKD) PPKD Injector Menu OPERATING SEQUENCE Programming the PPKD Injector Packed Mode Before programming the purged packed column injector, do the following: • Verify that a column is correctly installed, the correct liner is in the injector, if used, and the system is free of leaks.
Page 123 Chapter 6 PPKD Injector Menu Purged Packed Column Injector (PPKD) OPERATING SEQUENCE Programming the PPKD Injector Surged Packed Mode In the mode, a carrier gas pressure surge activates during the Packed w/surge injection phase for a preset time. This surge accelerates the transfer process of the substances from the injector to the column.
Page 124 Chapter 6 Purged Packed Column Injector (PPKD) PPKD Injector Menu Instruction Manual...
Page 125: Chapter 7 Column
Column This chapter describes the analytical column installed in the FOCUS GC oven. Chapter at a Glance… Introduction ......................126 Capillary and Wide-bore Columns ..............126 Packed Columns ....................128 Installation ......................132 Keeping Leaks Under Control................146 Column Conditioning ..................
Page 126: Introduction
Chapter 7 Column Introduction Introduction The analytical column should be positioned inside the oven. The column ends should align correctly with the injector and detector base body. Refer to: • Capillary and Wide-bore Columns • Packed Columns Capillary and Wide-bore Columns The capillary column should be positioned inside the oven on the column support.
Page 127: Capillary/Wide Bore Column To Injector And Detector Base Body Connections
Chapter 7 Capillary and Wide-bore Columns Column 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 Retaining Nuts M4 split retaining nuts are used to connect capillary columns to injector and detector base bodies.
Page 128: Packed Columns
Chapter 7 Column Packed Columns Packed Columns There are different sizes of packed columns with both metric and imperial dimensions with dedicated adapters. The FOCUS accepts 1/4 inch OD, 1/8 inch OD imperial metal packed columns, 6 mm OD metric metal packed columns. The metal packed columns can be installed into the S/SL injector by using the appropriate conversion kit.
Page 129: Imperial Packed Columns
Chapter 7 Packed Columns Column A. 6 mm OD Metal Column 1. Hexagonal 1/4 Inch Nut 2. Double Brass Ferrules Figure 7-2. Metric Packed Column Fittings Imperial Packed Columns The following types of imperial packed columns are commonly used. • 1/4 inch OD metal packed column •...
Page 130 Chapter 7 Column Packed Columns 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 The adapters size depends on the type of column that has to be use: 6-mm, 1/4-inch, 1/8-inch OD.
Page 131: Convertion Kit
Chapter 7 Packed Columns Column NOTE Metal Packed Column may be installed into the S/SL injector and the detector base body for capillary column by using the appropriate conversion kit as shown in Figure 7-4. A. S/SL Injector 4. Double Ferrule B.
Page 132: Installation
Chapter 7 Column Installation Installation CAUTION Each column has a maximum recommended operating temperature. To protect the column from excessively high temperatures, remember to set the Max temp parameter for the column oven in the Oven Configuration Menu as described in Chapter 2.
Page 133 Chapter 7 Installation Column Preparing a Capillary Column To prepare metal or fused silica capillary column operate as follows: CAUTION Wear safety glasses to protect your eyes from flying particles while handling, cutting, or installing columns. Be careful handling columns to avoid accidental hand injuries.
Page 134 5. Insert the column about 2 cm into the injector and slide the ferrule on the column up to the injector base, then slide the retaining nut onto the column through the side cut. The FOCUS GC. retaining nuts have a slotted design that makes them easy to add and remove.
Page 135 Chapter 7 Installation Column 8. Use the 6 mm wrench to tighten the retaining nut using no more pressure than is necessary to obtain a good seal (1/4 to 1/2 turn). 9. Conduct a leak check of the column installation, as described in the paragraph Keeping Leaks Under Control on page 146.
Page 136 Chapter 7 Column Installation 9. Conduct a leak check of the column installation, as described in the paragraph Keeping Leaks Under Control on page 146. Connecting to a FID Detector It is a good practice, before connecting the column to the detector, to perform a manual leak check as described in the Manual Checking for Leaks operating...
Page 137 Chapter 7 Installation Column 6. Use the 6 mm wrench to tighten the retaining nut. Use no more pressure than is necessary to obtain a good seal (1/4 to 1/2 turn). Connecting to a TCD Detector It is a good practice, before connecting the column to the detector, to perform a manual leak check as described in the Manual Checking for Leaks.operating...
Page 138: How To Connect A Packed Column
Chapter 7 Column Installation 8. Tighten the M4 retaining nut using the 6 mm wrench. Use no more pressure than is necessary to achieve a good seal (1/4 to 1/2 turn). OPERATING SEQUENCE How to Connect a Packed Column To install the packed column, the following sequential steps should be performed: •...
Page 139 Chapter 7 Installation Column Connecting a Packed Column to a PPKD Injector Materials required: • retaining nut • ferrules • 10 mm or 1/4 inch wrench • adapter for injector 1. Make sure that your packed column has been correctly prepared. 2.
Page 140: Removing The S/Sl Injector Top Components
Chapter 7 Column Installation Connecting a Packed Column to the S/SL Injector Materials required: • liner cap removal tool • retaining nut • ferrules • metal adapter 1. Remove the S/SL Injector Top Components. With reference to Figure 7-6 proceed as follows: 1.
Page 141: Removing The S/Sl Injector Bottom Components
Chapter 7 Installation Column 2. Remove the S/SL Injector Bottom Components. With reference to Figure 7-7 proceed as follows: 1. Terminal Fitting Retaining Nut 2. Terminal Fitting 3. Silver Seal Figure 7-7. Removing the S/SL Injector Bottom Components a. Unscrew the retaining nut at the bottom of the injector. b.
Page 142: Graphite Seal Installation Tool
Chapter 7 Column Installation a. Slide the appropriate nut and ferrule onto the metal adapter, then insert it into the bottom of the injector. b. Push the metal adapter into the injector as far as possible. c. Slide the ferrule up the injector base then finger-tighten the retaining nut until it starts to grip the metal liner.
Page 143 Chapter 7 Installation Column 1. Liner Cap 2. Liner Cap Removing Tool 3. Septum Support 4. Septum 5. Septum Holder 6. Injector Cap Figure 7-10. Reinstalling the S/SL Injector Top Components a. Reinstall and tighten the liner cap until it start to grip the graphite seal then tighten the metal adapter retaining nut.
Page 144 Chapter 7 Column Installation a. Make sure that your packed column has been correctly prepared as described in the Preparing a Metal Packed Column. b. Insert the column end to the metal adapter paying attention that the column end touches the bottom c.
Page 145 Chapter 7 Installation Column 6. Use 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). CAUTION Overtightening the compression ferrule does not necessarily produce a stronger, leak-free joint.
Page 146: Keeping Leaks Under Control
Keeping Leaks Under Control Keeping Leaks Under Control FOCUS GC features a series of automatized operations that make easier the task of keeping under control the tightness of your system. The sequence Manual Check for Leaks - Column Evaluation - Automatic Leak Check is the key for minimizing troubles related to leaks.
Page 147: Manual Checking For Leaks
Chapter 7 Keeping Leaks Under Control Column OPERATING SEQUENCE Manual Checking for Leaks Before you begin this sequence, you must install the column into the injector, but not into the detector base body. Materials needed: • silicon rubber septum of any dimension 1.
Page 148: Performing A Column Evaluation
OPERATING SEQUENCE Performing a Column Evaluation The column flow control in the FOCUS GC is indirect. This means that the GC regulates pressure to control the flow of gas through the column. To do this, the GC relies on a column constant. The column constant is a measure of the columns pneumatic resistance.
Page 149 Chapter 7 Keeping Leaks Under Control Column Column evaluation cannot be started in the following cases: COLUMN EVALUATION Oven not ready COLUMN EVALUATION Carrier press. Off! COLUMN EVALUATION GC running COLUMN EVALUATION Packed mode! 4. The GC automatically performs column evaluation. NOTE To abort column evaluation, scroll to Abort column eval.
Page 150: Expected K Factor
Chapter 7 Column Keeping Leaks Under Control COLUMN EVALUATION Err! Too low P drop COLUMN EVALUATION Err! Too High P drop. Expected K Factor The following tables indicate the expected K factors for columns of ideal dimensions when using helium, hydrogen, or nitrogen as a carrier gas. Use this information when interpreting results from a Column Evaluation.
Page 151: Helium Carrier Gas Theoretical K Factor
Chapter 7 Keeping Leaks Under Control Column Helium Carrier Gas Theoretical K Factor COLUMN ID (mm) 0.10 0.15 0.18 0.20 0.22 0.25 0.32 0.53 5.55 1.095 0.53 0.347 0.237 0.142 0.053 11.1 2.19 1.06 0.694 0.474 0.284 0.106 0.014 13.3 2.63 1.27 0.833...
Page 152: Nitrogen Carrier Gas Theoretical K Factor
Chapter 7 Column Keeping Leaks Under Control Nitrogen Carrier Gas Theoretical K Factor COLUMN ID (mm) 0.10 0.15 0.18 0.20 0.22 0.25 0.32 0.53 4.95 0.98 0.471 0.309 0.2155 0.126 0.047 9.90 1.96 0.943 0.619 0.423 0.253 0.094 0.012 11.9 2.35 1.13 0.743...
Page 153: Hydrogen Carrier Gas Theoretical K Factor
Chapter 7 Keeping Leaks Under Control Column Hydrogen Carrier Gas Theoretical K Factor COLUMN ID (mm) 0.10 0.15 0.18 0.20 0.22 0.25 0.32 0.53 2.49 0.492 0.237 0.155 0.106 0.063 0.023 4.98 0.984 0.474 0.311 0.213 0.127 0.047 5.98 1.18 0.569 0.374 0.255...
Page 154: Performing An Automatic Leak Check
OPERATING SEQUENCE Performing an Automatic Leak Check When you perform an automatic leak check of the FOCUS GC system, the GC measures the column flow with a true mass flow sensor and compares it to a calculated flow value obtained from the original column constant to see if the numbers match.
Page 155 Chapter 7 Keeping Leaks Under Control Column LEAK CHECK Carrier press. Off! LEAK CHECK GC running LEAK CHECK Packed mode! NOTE To abort leak check, scroll to Abort leak check. and press ENTER. The message Aborted by operator will be displayed. 5.
Page 156: Column Conditioning
Chapter 7 Column Column Conditioning Column Conditioning To ensure optimum analytical performance, a new column must be conditioned to remove contaminants and unwanted volatile compounds. Column conditioning is required to remove volatile contaminants adsorbed from the air. Column conditioning consists of passing a carrier gas flow through the column and heating the column to a temperature 20–50 °C above the maximum temperature that will be used for running analyses, provided that temperature is within the operating range of the column.
Page 157: Flame Ionization Detector (Fid)
Flame Ionization Detector (FID) This chapter describes the Flame Ionization Detector (FID). Due to its high sensitivity, good operational stability, and wide linear response, the FID remains the most popular detector for gas chromatography. Chapter at a Glance… Overview..................... 158 FID Gas Supplies....................
Page 158: Fid Overview
Chapter 8 Flame Ionization Detector (FID) FID Overview FID Overview In the FID, the effluent from the column is mixed with hydrogen and burned in a stream of air as it emerges from the jet. The jet acts as a polarizing electrode, while the metal collar surrounding the flame forms the collecting electrode.
Page 159: Detector Gas
FID Overview Flame Ionization Detector (FID) Detector Gas FOCUS GC is equipped with a conventional detector gas flow control module (DGFC). See Figure 8-2. The detector gases flows are pre-set in the factory. You may set the flows On or Off.
Page 160: Selectivity
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 column in use.
Page 161: Fid Gas Supplies
Chapter 8 FID Gas Supplies Flame Ionization Detector (FID) FID Gas Supplies The performance of the FID is affected by the flow of the various gases through the detector. The fuel and make-up gases used for the FID are: • fuel gas: hydrogen and air •...
Page 162: Fid Installation
Chapter 8 Flame Ionization Detector (FID) FID Installation FID Installation This operation allows the correct installation of the FID on your FOCUS GC. Material required • Jet for FID • Tool for jet 1. Place the jet into the detector base body housing and tighten it with the proper tool.
Page 163 Chapter 8 FID Installation Flame Ionization Detector (FID) 1. FID 2. Fixing screw 3. Detector base body 4. Signal cable 5. Ignition polarization cable Figure 8-4. Installation of the FID Instruction Manual...
Page 164: Fid Menu
Chapter 8 Flame Ionization Detector (FID) FID Menu FID Menu menu contains the detector control parameters. DETECTOR In Main Menu, move the cursor until is selected. Press ENTER to Detector display the menu. DETECTOR DETECTOR (FID) Flame Temp 200 200 Signal pA (10.0) Ing.
Page 165: Flame Out Conditions
Chapter 8 FID Menu Flame Ionization Detector (FID) Table 8-1. FID Parameters (Continued) Parameter Range Description 0 - 1000.00 pA This parameter shows the collector current in pico Signal pA Not editable amperes (standing current level). The displayed value is also used to indicate the flame status.
Page 166: Detector Signal Parameters
Chapter 8 Flame Ionization Detector (FID) Detector Signal Parameters Detector Signal Parameters The detector menu contains the parameters that control the detector SIGNAL signal. As compounds elute from the column and enter the detector, an electrical signal is generated. The size of the signal is related to the amount of the corresponding compounds.
Page 167: Programming A Fid
Chapter 8 Detector Signal Parameters Flame Ionization Detector (FID) OPERATING SEQUENCE Programming a FID Materials required: • bubble flow or electronic flow meter • detector base body/flow meter adapter Before you begin this sequence, do the following: • Verify that all detector gases are connected, a column is correctly installed, and the system is free of leaks.
Page 168 Chapter 8 Flame Ionization Detector (FID) Detector Signal Parameters 6. Refer to Setting the FID Signal Parameters operating sequence for instructions on setting the signal parameters. If you desired to check or modify the detector gas flows operate as follows: •...
Page 169: Setting The Fid Signal Parameters
Chapter 8 Detector Signal Parameters Flame Ionization Detector (FID) OPERATING SEQUENCE Setting the FID Signal Parameters is selected. Press ENTER to 1. In Main Menu move the cursor until Signal display the menu. SIGNAL 2. Scroll to and set the electrometer amplifier input Range 10^ (0...3) range.
Page 170 Chapter 8 Flame Ionization Detector (FID) Detector Signal Parameters Instruction Manual...
Page 171: Thermal Conductivity Detector (Tcd)
Thermal Conductivity Detector (TCD) This chapter describes the operating principles and sequences 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 ..............
Page 172: Tcd Overview
Chapter 9 Thermal Conductivity Detector (TCD) TCD Overview TCD Overview The TCD is sensitive to any compound having thermal conductivity other than that of the carrier gas used. The TCD is a universal type detector. It has a broad range of uses in the analysis of permanent gases and other organic or inorganic compounds for which the Flame Ionization Detector (FID) is practically non- sensitive, such as CO , CS...
Page 173 Chapter 9 TCD Overview Thermal Conductivity Detector (TCD) 1.Measure Cell A.Reference Gas 2.Reference Cell B.Make-up Gas 3.Column Figure 9-1. TCD Filaments and Gas Flows When the filaments are properly powered, they heat at a temperature (resistance) that is a function of the thermal conductivity of the gas flowing through the filaments.
Page 174: Tcd Gas Supplies
Chapter 9 Thermal Conductivity Detector (TCD) TCD Gas Supplies TCD Gas Supplies The TCD detector requires the same gas whether for the measure channel (carrier plus make-up gas) and the reference channel (reference gas). Helium is the recommended carrier gas due to its high thermal conductivity and chemical inertness.
Page 175: Columns
Chapter 9 TCD Operating Modes Thermal Conductivity Detector (TCD) Columns The TCD use two separate gas lines. One connects to the analytical column and the other connects to the reference channel. The column effluent connects to the analytical cell along with the make-up gas, from the DGFC pneumatic detector module.
Page 176 Chapter 9 Thermal Conductivity Detector (TCD) TCD Operating Modes temperature limit in the TCD detector menu (Table 9-4). If this value is reached, the system will automatically switch to the constant temperature mode. The CV mode extends the linearity range to higher values, but with a negative impact on sensitivity.
Page 177: Selecting Tcd Operating Parameters
Chapter 9 Selecting TCD Operating Parameters Thermal Conductivity Detector (TCD) Selecting TCD Operating Parameters The TCD can be set to operate in constant temperature (CT) and constant voltage (CV) modes. WARNING! In case of TCD with the polyimide coated filaments, the maximum operating temperature is 300 °C for the TCD cell and 320 °C for the filaments.
Page 178: Suggested Operating Values
Chapter 9 Thermal Conductivity Detector (TCD) Selecting TCD Operating Parameters When using low thermal conductivity gases, the temperatures reached by the filaments are very high. Table 9-2 contains the experimental filament temperature values corresponding to the applied voltages when using argon. Table 9-2.
Page 179: Tcd Menu
Chapter 9 TCD Menu Thermal Conductivity Detector (TCD) TCD Menu menu contains the detector control parameters. DETECTOR In Main Menu, move the cursor until is selected. Press ENTER to Detector display the menu. DETECTOR DETECTOR (TCD) DETECTOR (TCD) Filament power Filament power Fil status (not rdy) Fil status...
Page 180 Chapter 9 Thermal Conductivity Detector (TCD) TCD Menu Table 9-4. The Detector (TCD) Parameters (Continued) Menu Range Comments 50–375 ºC This is the transfer line temperature for the heated Transf temp zone between the oven and the detector cell. Set ON to turn on the heater and display the actual and setpoint values.
Page 181: Detector Signal Parameters
Chapter 9 Detector Signal Parameters Thermal Conductivity Detector (TCD) Detector Signal Parameters The detector menu contains the parameters that control the detector SIGNAL signal. In Main Menu move the cursor until is selected. Press ENTER to Signal display the menu. SIGNAL SIGNAL (TCD) Output...
Page 182: Programming A Tcd
Chapter 9 Thermal Conductivity Detector (TCD) Detector Signal Parameters OPERATING SEQUENCE Programming a TCD When a wide-bore or capillary column is used, the make-up gas line is required. Materials required: • bubble flow or electronic flow meter Before you begin, do the following: •...
Page 183 Chapter 9 Detector Signal Parameters Thermal Conductivity Detector (TCD) b. Adjust the make-up flow by operating on the relevant flow regulator. c. Measure the flow after stabilization. If necessary, repeat this step until the make-up gas flow rate is correct. 4.
Page 184: Setting The Tcd Signal Parameters
Chapter 9 Thermal Conductivity Detector (TCD) Detector Signal Parameters OPERATING SEQUENCE Setting the TCD Signal Parameters is selected. Press ENTER to 1. In Main Menu move the cursor until Signal display the menu. SIGNAL 2. Scroll to and set the desired value. When the gain is x10, the system Gain sensitivity is higher.
Page 185: Shutting Down The Tcd
Chapter 9 Detector Signal Parameters Thermal Conductivity Detector (TCD) 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. Instruction Manual...
Page 186 Chapter 9 Thermal Conductivity Detector (TCD) Detector Signal Parameters Instruction Manual...
Page 187: Autosamplers
Autosamplers This chapter describes how to program and control the AS 2000 autosampler and the AI 3000/AS 3000 by using the FOCUS GC keypad. This chapter contains also the instructions to programming a sample sequence 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.
Page 188: Autosampler Overview
Thermo Data Systems referring to the instructions reported in the relevant operating manual. • FOCUS GC keypad, referring to the instructions reported in this chapter. CAUTION The autosampler setup involving alignment of the various components must be done from the AS 2000 control module.
Page 189: Autosampler Configuration
Chapter 10 Autosampler Overview Autosamplers Autosampler Configuration According to the autosampler connected, configure the instrument as described in paragraph Configuration on page 51. Autosampler Menu is selected, then press ENTER In Main Menu move the cursor until Autosampler to open menu.
Page 190: As 2000 Autosampler Menu
Chapter 10 Autosamplers AS 2000 Autosampler Menu AS 2000 Autosampler Menu This paragraph describes the AS 2000 Autosampler menu. AUTOSAMPLER Sample volume Sample rinses Rinse volume Injection speed Pre wash solv Pre wash cycles Post wash solv Post wash cycles Solvent wash vol Plunger strokes Viscosity delay...
Page 191 Chapter 10 AS 2000 Autosampler Menu Autosamplers Table 10-1. AS 2000 Autosampler Menu (Continued) Parameter Range Description A, B, C, D, This parameter specifies the solvent vial used for Pre wash solv washing prior the injection. 0–15 times This parameter specifies the number of times the syringe Pre wash cycles is pre-washed with solvent.
Page 192: Internal Standard Use
Chapter 10 Autosamplers AS 2000 Autosampler Menu When you scroll to in the menu and press Int Std Settings AUTOSAMPLER ENTER, the menu is displayed: INTERNAL STANDARD INT STD SETTINGS Int std vial# 20 Int std volume 2.0 Air gap mode double Air gap volume Table 10-2.
Page 193: Ai 3000/As 3000 Menu
Chapter 10 AI 3000/AS 3000 Menu Autosamplers AI 3000/AS 3000 Menu This paragraph describes the AI 3000/AS 3000 menu. AUTOSAMPLER Sample volume Sample rinses Plunger strokes Pre wash solv Pre wash cycles Post wash solv Post wash cycles Viscous sample Sampl.depth Bottom Inj.
Page 194 Chapter 10 Autosamplers AI 3000/AS 3000 Menu Table 10-3. AI 3000/AS 3000 Menu (Continued) Parameter Range Description A, B, C, D, AB, This parameter specifies the solvent vial used for Pre wash solv washing prior the injection. 0–15 times This parameter specifies the number of times the Pre wash cycles syringe is pre-washed with solvent.
Page 195: Sequence Programming
Autosamplers Sequence Programming This paragraph contains the instructions to programming a samples sequence with the FOCUS GC keypad when an AS 2000 or an AI 3000/AS 3000 is used and how to set up. CAUTION The Sequence menu is available in Main Menu only when an autosampler is present.
Page 196 Chapter 10 Autosamplers Sequence Programming Table 10-4. Sequence Menu (Continued) Parameter Range Description Skip - Abort When Skip is set, the autosampler skips an eventual When no vial missing sample vial and moves to find the next vial. The sample sequence and the sample table of the data system will be not affected.
Page 197: Chapter 11 Getting Started
Getting Started This chapter contains instructions to operate with your FOCUS GC through the instrument keypad. We also included instructions to program a Run Time Events and the instrument start-up. Chapter at a Glance… Instrument Set-up ....................198 Run Time Events ....................
Page 198: Instrument Set-Up
How to Set Up the Instrument FOCUS GC Switching On Before switching the FOCUS GC On, verify that: 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.
Page 199 Chapter 11 Instrument Set-up Getting Started Set Carrier parameters 6. Check that the carrier gas type is correct for the analysis. In Main Menu move the cursor until is selected. Press ENTER to Carrier open menu. CARRIER 7. Select the Carrier Constant Flow or Constant Pressure Mode. Enter the initial Flow or Pressure.
Page 200 Chapter 11 Getting Started Instrument Set-up Set Detector Parameters is selected. Press ENTER to 15. In Main Menu move the cursor until Detector open menu. DETECTOR 16. Set the required temperature and open (On) the detector gases setting the relevant inlet pressure as indicated in Chapter 3. 17.
Page 201 Chapter 11 Instrument Set-up Getting Started 27. Set the autosampler parameters required. 28. Press HOME to exit. Set Sequence Parameters is selected. Press ENTER to 29. In Main Menu move the cursor until Sequence open menu. SEQUENCE 30. Set the sequence parameters required. 31.
Page 202: Run Time Events
Chapter 11 Getting Started Run Time Events Run Time Events This option allows you to program events to happen prior to or during a run. The following tables are showing two menus, one without RUN TIME EVENTS entries and one with one entry. RUN TIME EVENTS RUN TABLE (1 of 1) <none>...
Page 203 Chapter 11 Run Time Events Getting Started RUN TIME EVENTS <none> Add run time event and press ENTER to open 2. Scroll to Add run time event EDIT EVENT submenu. EDIT TIME EVENT Event#1 <none> Run Time 0.00 Setpoint Next event .
Page 204 Chapter 11 Getting Started Run Time Events 8. To program a new event repeat the steps 3, 4 and 5. For example, If event is selected, the GSValve #1 GSValve #2 EDIT menu change as follows: EVENTS EDIT TIME EVENT Event#2 GSValve#1 Inject at...
Page 205: Deleting A Run Time Event
Chapter 11 Run Time Events Getting Started OPERATING SEQUENCE Deleting a Run Time Event is selected, then press ENTER. 1. In Main Menu move the cursor until Others Scroll to , then press ENTER to open Run time Events RUN TIME EVENTS menu.
Page 206: Controlling Valves
You can manually open or close valves before a run. You can affect the inlet valves and up to two external valves Possible valves types for the FOCUS GC and external device are: Septum purge, Split, External event or Gas sampling Run Time Control (Gas Sampling Valve Only) 1.
Page 207 Chapter 11 Controlling Valves Getting Started VALVES VALVES Split valve Split valve Sept purge valve Sept purge valve EV#1 GSValve#1 Load EV#2 EV#2 Valves menu when gas Valves menu when gas sampling valve is not present sampling valve is present 3.
Page 208: Instrument Start-Up
Instrument Start-Up Instrument Start-Up This start-up sequence contains the instructions, which combines the analytical procedure with the use of the FOCUS GC program. OPERATING SEQUENCE How to Start Up the Instrument The sequence of instructions begins with the assumption that all the instruments of the system are ON, set and ready to initiate the analyses.
Page 209 Getting Started Performing a Manual Injection 1. Perform the Prep Run. by pressing the START button a first time. Depending on the mode you have programmed, the FOCUS GC will perform the following operation. • When the gas saver function is programmed, Prep Run ends the gas saver mode and resets the split flow to the flow used during the injection.
Page 210 Chapter 11 Getting Started Instrument Start-Up 2. In Main Menu, move the cursor until is selected, then press Sequence 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.
Page 211: Instrument Status Messages
Chapter 11 Instrument Status Messages Getting Started Instrument Status Messages By pressing STATUS key, you can visualize 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...
Page 212: Stand-By
Chapter 11 Getting Started Instrument Status Messages NOT READY Inlet split flow NOT READY Carrier col. flow NOT READY TCD filaments NOT READY TCD block temp Stand-By The message indicates that the GC is waiting for the Prep run. STAND-BY Waiting for Prep run If the gas saver function has been selected On in the Carrier menu, the following message is displayed.
Page 213: Ready To Inject
Chapter 11 Instrument Status Messages Getting Started PREP-RUN Exec Prep-run events Ready to Inject This message indicates that the GC is waiting for the Start signal. READY TO INJECT Waiting for start Ready to Inject with an Autosampler enabled This message indicates that autosampler is active and the GC is waiting for the Start signal.
Page 214 Chapter 11 Getting Started Instrument Status Messages RUNNING Ramp If the Run Log has entries the following message is displayed. RUNNING Run log has entries Instruction Manual...
Page 215: Checkout Using Fid With S/Sl
Checkout Using FID with S/SL This chapter contains the operating procedure 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....................
Page 216: Sop Number: P0407/05/E - 31 May 2006
The SOP has been developed to test and verify instrument complete analytical performance after the installation has been completed. This will help you as a guideline, to check if your FOCUS GC continues to perform according to the original checkout testing specifications carried out in the factory premises.
Page 217 Chapter 12 SOP number: P0407/05/E - 31 May 2006 4. Column Installation Install the test column as described in the How to Connect a Capillary Column operating sequence following the instructions reported in: • Preparing a Capillary Column • Connecting to an S/SL Injector 5.
Page 218: Parts Referenced
Chapter 12 SOP number: P0407/05/E - 31 May 2006 • Connecting to a FID Detector 9. Leak Test This operation should be performed on the system each time the column installation is disturbed, to ensure a good seal throughout the system. Perform the leak test following the instruction reported in the Performing an Automatic Leak Check...
Page 219: Analytical Conditions Required For Fid-S/Sl
Chapter 12 SOP number: P0407/05/E - 31 May 2006 Analytical Conditions Required for FID-S/SL Table 12-2. FID-S/SL Analytical Conditions Parameters Setting Gases Carrier Gas: Helium = 30 kPa Constant Pressure Hydrogen = 35 mL/min (350 kPa; 50 psi) Air = 350 mL/min (350 kPa; 50 psi) Make-up Gas: Nitrogen = 30 mL/min (350 kPa;...
Page 220: Fid-S/Sl Checkout In Splitless Mode
, then press ENTER to open Configuration menu Scroll to Configuration Scroll to submenu then press ENTER. Configure carrier Select the carrier gas required by using the INC and DEC keys. FOCUS GC Others OTHERS Configuration CONFIGURATION Carrier CONFIGURE CARRIER...
Page 221 Press ENTER to open 6. In Main Menu move the cursor until Oven menu. OVEN FOCUS GC Oven 7. Scroll to Temp Initial time, Ramp 1, Final temp 1, Final By using the INC and DEC keys select the value or the time 1 Ramp 2.
Page 222 8. Press HOME to return Main Menu. 9. In Main Menu move the cursor until is selected. Press ENTER to open Inlet menu. INLET FOCUS GC Inlet 10. Scroll to Temp Mode, Split flow, Total flow, Split flow, . By using the INC and DEC Splitless time Const.
Page 223 Press ENTER to 12. In Main Menu move the cursor until Detector open menu. DETECTOR FOCUS GC Detector 13. Scroll to Flame, Temp, Signal pA, Ign. thresh., Flameout . By using the INC and DEC keys select the retry, H2, Air Make-up value or the required operating mode, then press ENTER.
Page 224 15. In Main Menu move the cursor until is selected. Press ENTER to Signal open menu. SIGNAL FOCUS GC Signal 16. Scroll to Output, Offset, Run autozero Range=10^(0..3) By using the INC and DEC keys select the value or the required operating mode, then press ENTER.
Page 225 Chapter 12 SOP number: P0407/05/E - 31 May 2006 SIGNAL (FID) Range=10^(0..3) 17. Press HOME to return Main Menu. 18. Activate your Data System and set the parameters required for the checkout. . 19. In menu , then press ENTER to perform SIGNAL select Run auto zero the automatic zeroing of the system.
Page 226 Chapter 12 SOP number: P0407/05/E - 31 May 2006 1. Dodecane 2. Tetradecane 3. Hexadecane 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. Instruction Manual...
Page 227: Fid-S/Sl Acceptance Criteria
> 34 000 000 for each component Area Count Ratio Calculated as C12/C16 1 + 0.1 Using ChromQuest, connected to the FOCUS GC digital output, and using a range of zero, set in the ChromQuest configuration page, a multiplier of 10 in V scale (or 10 in mV scale) in order to have equivalency with FOCUS GC displayed signal output.
Page 228: Analytical Acceptance Comments
Chapter 12 SOP number: P0407/05/E - 31 May 2006 Analytical Acceptance Comments 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. 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: Checkout Using Tcd With S/Sl
Checkout Using TCD with S/SL This chapter contains the operating procedure 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....................
Page 230: Sop Number: P0473/04/E - 02 May 2007
The SOP has been developed to test and verify instrument complete analytical performance after the installation has been completed. This will help you as a guideline, to check if your FOCUS GC continues to perform according to the original checkout testing specifications carried out in the factory premises.
Page 231 Chapter 13 SOP number: P0473/04/E - 02 May 2007 4. Column Installation Install the test column as described in the How to Connect a Capillary Column operating sequence following the instructions reported in: • Preparing a Capillary Column • Connecting to an S/SL Injector 5.
Page 232: Parts Referenced
Chapter 13 SOP number: P0473/04/E - 02 May 2007 • Connecting to a TCD Detector 9. Leak Test This operation should be performed on the system each time the column installation is disturbed, to ensure a good seal throughout the system. Perform the leak test following the instruction reported in the Performing an Automatic Leak Check...
Page 233: Analytical Conditions Required For Tcd-S/Sl
Chapter 13 SOP number: P0473/04/E - 02 May 2007 Analytical Conditions Required for TCD-S/SL Table 13-2. TCD-S/SL Analytical Conditions Parameters Setting Gases Carrier Gas: Helium = 30 kPa Constant Pressure Make-up: Helium = 27.5 ml/min Reference Gas: Helium = 30 ml/min Oven Program Initial Temperature = 50 °C Initial Time = 1 minute...
Page 234: Tcd-S/Sl Checkout In Splitless Mode
, then press ENTER to open Configuration menu Scroll to Configuration Scroll to submenu then press ENTER. Configure carrier Select the carrier gas required by using the INC and DEC keys. FOCUS GC Others OTHERS Configuration CONFIGURATION Carrier CONFIGURE CARRIER...
Page 235 Press ENTER to open 6. In Main Menu move the cursor until Oven menu. OVEN FOCUS GC Oven 7. Scroll to Temp Initial time, Ramp 1, Final temp 1, Final By using the INC and DEC keys select the value or the time 1 Ramp 2.
Page 236 8. Press HOME to return Main Menu. 9. In Main Menu move the cursor until is selected. Press ENTER to open Inlet menu. INLET FOCUS GC Inlet 10. Scroll to Temp Mode, Split flow, Total flow, Split flow, . By using the INC and DEC Splitless time Const.
Page 237 11. Press HOME to return Main Menu. is selected. Press ENTER to 12. In Main Menu move the cursor until Detector open menu. DETECTOR FOCUS GC Detector 13. Scroll to Block temp, Transf temp, Reference Make-up, Const fil temp, Fil volts (CV), Fil temp limit Filament .
Page 238 Press ENTER to 15. In Main Menu move the cursor until Signal open menu. SIGNAL FOCUS GC Signal 16. Scroll to Output, Offset, Run autozero, Gain Neg polarity By using the INC and DEC keys select the value or the required operating mode, then press ENTER.
Page 239 Chapter 13 SOP number: P0473/04/E - 02 May 2007 SIGNAL (TCD) Offset SIGNAL (TCD) Run autozero SIGNAL (TCD) Gain (x1..x10) SIGNAL (TCD) Neg polarity 17. Press HOME to return Main Menu. 18. Activate your Data System and set the parameters required for the checkout. . , then press ENTER to perform 19.
Page 240 Chapter 13 SOP number: P0473/04/E - 02 May 2007 1. Dodecane 2. Tetradecane 3. Hexadecane 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. Instruction Manual...
Page 241: Tcd-S/Sl Acceptance Criteria
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, and using a range of zero, set in the ChromQuest configuration page, a multiplier of 10 in V scale (or 10 in mV scale) in order to have equivalency with FOCUS GC displayed signal output.
Page 242 Chapter 13 SOP number: P0473/04/E - 02 May 2007 Instruction Manual...
Page 243: Checkout Using Tcd With Ppkd
Checkout Using TCD with PPKD This chapter contains the operating 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..................
Page 244: Sop Number: P0474/05/E - 02 May 2007
The SOP has been developed to test and verify instrument complete analytical performance after the installation has been completed. This will help you as a guideline, to check if your FOCUS GC continues to perform according to the original checkout testing specifications carried out in the factory premises.
Page 245 Chapter 14 SOP number: P0474/05/E - 02 May 2007 4. Column Installation Install the test column as described in the How to Connect a Capillary Column operating sequence following the instructions reported in: • Preparing a Capillary Column • Connecting to an PPKD Injector 5.
Page 246: Parts Referenced
Chapter 14 SOP number: P0474/05/E - 02 May 2007 • How to Connect a Capillary Column • Connecting to a TCD Detector 9. Leak Test This operation should be performed on the system each time the column installation is disturbed, to ensure a good seal throughout the system. Perform the leak test following the instruction reported in the Performing an Automatic Leak Check...
Page 247 Chapter 14 SOP number: P0474/05/E - 02 May 2007 Table 14-1. TCD-PPKD Parts Referenced (Continued) Part Description Part Number Test Mixture Three components in n-Hexane: 338 190 16 Component Concentration 200 μg/ml Dodecane 200 μg/ml Tetradecane 200 μg/ml Hexadecane Gases Chromatographic-grade purity Data Acquisition Chrom-Card, ChromQuest, Atlas, Xcalibur,...
Page 248: Analytical Conditions Required For Splitless Injection
Chapter 14 SOP number: P0474/05/E - 02 May 2007 Analytical Conditions Required for Splitless Injection Table 14-2. TCD-PPKD Analytical Conditions Parameters Setting Gases Carrier Gas: Helium = 30 kPa Constant Pressure Make-up: Helium = 27.5 ml/min Reference Gas: Helium = 30 ml/min Oven Program Initial Temperature = 85 °C Initial Time = 1 minute...
Page 249: Tcd-Ppkd Checkout
, then press ENTER to open Configuration menu Scroll to Configuration Scroll to submenu then press ENTER. Configure carrier Select the carrier gas required by using the INC and DEC keys. FOCUS GC Others OTHERS Configuration CONFIGURATION Carrier CONFIGURE CARRIER...
Page 250 Press ENTER to open 6. In Main Menu move the cursor until Oven menu. OVEN FOCUS GC Oven 7. Scroll to Temp Initial time, Ramp 1, Final temp 1, Final By using the INC and DEC keys select the value or the time 1 Ramp 2.
Page 251 8. Press HOME to return Main Menu. 9. In Main Menu move the cursor until is selected. Press ENTER to open Inlet menu. INLET FOCUS GC Inlet . By using the INC and DEC 10. Scroll to Temp Mode Const. Sept purge keys select the value or the required operating mode, then press ENTER.
Page 252 SOP number: P0474/05/E - 02 May 2007 12. In Main Menu move the cursor until is selected. Press ENTER to Detector open menu. DETECTOR FOCUS GC Detector 13. Scroll to Block temp, Transf temp, Reference Make-up, Const fil temp, Fil volts (CV), Fil temp limit Filament .
Page 253 Press ENTER to 15. In Main Menu move the cursor until Signal open menu. SIGNAL FOCUS GC Signal 16. Scroll to Output, Offset, Run autozero, Gain Neg polarity By using the INC and DEC keys select the value or the required operating mode, then press ENTER.
Page 254 Chapter 14 SOP number: P0474/05/E - 02 May 2007 19. In menu , then press ENTER to perform SIGNAL select Run auto zero the automatic zeroing of the system. Baseline acquisition and Analysis NOTE Refer to the Acceptance Values reported in theTable 14-3 according to the data handling in use.
Page 255 Chapter 14 SOP number: P0474/05/E - 02 May 2007 1. Dodecane 2. Tetradecane 3. Hexadecane 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. Instruction Manual...
Page 256: Tcd-Ppkd Acceptance Criteria
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, and using a range of zero, set in the ChromQuest configuration page, a multiplier of 10 in V scale (or 10 in mV scale) in order to have equivalency with FOCUS GC displayed signal output.
Page 257: Maintenance And Troubleshooting
Maintenance and Troubleshooting This chapter contains information and operating sequences to perform the necessary maintenance of the instrument and also information concerning troubleshooting in case of malfunctioning. Chapter at a Glance… Maintenance ....................... 259 Maintaining a SSL Injector ................262 Maintaining a PPKD Injector ................
Page 258 Chapter 15 Maintenance and Troubleshooting 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 Instruction Manual...
Page 259: Maintenance
Service Contract Program will normally perform full instrument servicing. To ensure that your FOCUS GC always performs to its full potential, the operator must carry out a certain amount of routine maintenance on a regular basis.
Page 260: Ferrules And Seals
Unless required applications necessitate frequent dismantling and replacement of columns and accessories, seals and ferrules normally need to be disturbed only when dismantling is required. However, the FOCUS GC should be periodically leak-tested and the seal tightened or replaced as necessary.
Page 261: Instrument Cleaning
WARNING! Cleaning must be performed with the instrument off and the power cord discon- nected. Normal usage of the FOCUS GC can cause the exterior to get dirty. Externally clean the instrument with a cloth dampened with soap and water solution, or with a household non-abrasive product, carefully avoid seeping of the products used inside the instrument.
Page 262: Maintaining A Ssl Injector
Chapter 15 Maintenance and Troubleshooting Maintaining a SSL Injector Maintaining a SSL Injector The S/SL (Split/Splitless) injector will normally be serviced by Thermo Fisher Scientific authorized technical personnel. In order to operate at peak performances, the injector requires periodic maintenance from the user. This maintenance includes: •...
Page 263: If The Glass Liner Breaks Inside The Injector
Chapter 15 Maintaining a SSL Injector Maintenance and Troubleshooting Liner Split injections, 3 mm 453 200 31 Split injections, 5 mm 453 200 30 Splitless injections, 3 mm 453 200 32 Splitless injections, 5 mm 453 200 33 Liner for direct injections into wide bore column 453 003 10 Laminar cup liner for split injections at high split flow rates or 453 003 20...
Page 264: Operating Procedures Replace The S/Sl Standard Septum
Chapter 15 Maintenance and Troubleshooting Maintaining a SSL Injector OPERATING SEQUENCE Replace the S/SL Standard Septum Material needed • Non metallic sharp tool • Septum • 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.
Page 265 Chapter 15 Maintaining a SSL Injector Maintenance and Troubleshooting Removing the Septum 4. Unscrew the septum cap. 5. Remove the septum holder with septum, then the septum support. See A of Figure 15-1. 6. Remove the septum from the septum holder (use non-metallic tools). See B of Figure 15-1.
Page 266 Chapter 15 Maintenance and Troubleshooting Maintaining a SSL Injector 9. Place the septum holder on 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.
Page 267: Replace Or Clean The Liner When A S/Sl Standard Septum Is
Chapter 15 Maintaining a SSL Injector Maintenance and Troubleshooting OPERATING SEQUENCE Replace or Clean the Liner when a S/SL Standard Septum is Installed Material needed • Liner cap removal tool • Glass liner • Graphite seal • Ultrasonic bath • Methanol/acetone mixture (1:1) •...
Page 268 Chapter 15 Maintenance and Troubleshooting Maintaining a SSL Injector INLET Temp CARRIER Pressure Removing the 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.
Page 269 Chapter 15 Maintaining a SSL Injector Maintenance and Troubleshooting 7. Use tweezers to remove the liner with the graphite seal. See C of Figure 15-2. CAUTION Be careful not to break the glass liner inside the injector when removing it. Glass splinters might fall into the lower part of the vaporization chamber.
Page 270 Chapter 15 Maintenance and Troubleshooting Maintaining a SSL Injector Figure 15-3. Replace a Broken Liner c. With the aid of a pipe cleaner, remove the possible glass fragments from the vaporization chamber. d. Reinsert the silver seal and the terminal fitting, and then tighten the nut that retains the terminal fitting.
Page 271 Chapter 15 Maintaining a SSL Injector Maintenance and Troubleshooting Figure 15-4. Replace and Clean the Liner (2) CAUTION Make sure you insert the beveled end of the liner towards the bottom of the injector. Be careful not to damage the graphite seal or allow graphite to entering the liner. Should this occur, clean the liner with an inert gas.
Page 272 Chapter 15 Maintenance and Troubleshooting Maintaining a SSL Injector Figure 15-5. Replace and Clean the Liner (3) 13. Clean the septum support from possible fragments left by the 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).
Page 273: Replace The S/Sl Inlet Vent Line Filter
This carbon filter is mounted on the DPFC module located on the rear of the GC. To replace the filter operate as follows: WARNING! Before operating 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.
Page 274 GENERIC SAMPLER HANDSHAKE SIGNAL SIGNAL Figure 15-7. FOCUS GC Rear Panel 5. Lift the panel pulling it upward. CAUTION To remove completely the rear cover, its GND cable must be also disconnected. Replace the Carbon Filter 6. Identify the DPFC module. See B of Figure 15-7.
Page 275 Chapter 15 Maintaining a SSL Injector Maintenance and Troubleshooting Figure 15-8. Filter Replacing 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.
Page 276: Maintaining A Ppkd Injector
Chapter 15 Maintenance and Troubleshooting Maintaining a PPKD Injector Maintaining a PPKD Injector The Purged Packed Column injector and its interface module will normally be serviced by Thermo Fisher Scientific authorized technical personnel. In order to operate at peak performances, the injector requires periodic maintenance from the user.
Page 277: Replace The Ppkd Septum
Chapter 15 Maintaining a PPKD Injector Maintenance and Troubleshooting OPERATING SEQUENCE Replace the PPKD Septum Material needed • Non metallic sharp tool • Septum • 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.
Page 278 Chapter 15 Maintenance and Troubleshooting Maintaining a PPKD Injector Removing the Septum 4. Unscrew the septum cap. 5. Remove the septum using a non metallic sharp. See A of Figure 15-9 6. Insert a new septum into the septum cap. See B of Figure 15-9. CAUTION Use tweezers to avoid touching the septum with your fingers.
Page 279: Replace Or Clean The Ppkd Liner
Chapter 15 Maintaining a PPKD Injector Maintenance and Troubleshooting OPERATING SEQUENCE Replace or Clean the PPKD Liner Material needed • Glass liner • Ultrasonic bath • Methanol/acetone mixture (1:1) • 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.
Page 280 Chapter 15 Maintenance and Troubleshooting Maintaining a PPKD Injector Removing the Liner 4. Unscrew the nut that retains the analytical column, then remove the column with the inserted ferrule. See A of Figure 15-10 5. Unscrew the retaining nut at the bottom of the injector. Remove the adapter and the liner then remove the ferrule.
Page 281 Chapter 15 Maintaining a PPKD Injector Maintenance and Troubleshooting 8. Insert a ferrule on the new (or cleaned) liner, using tweezers to hold it. See C of Figure 15-10. CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner. Should this occur, clean the liner with an inert gas.
Page 282: Maintaining A Fid
Chapter 15 Maintenance and Troubleshooting Maintaining a FID Maintaining a FID To ensure optimum performance of the FID, you must keep it clean and free 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: •...
Page 283 Chapter 15 Maintaining a FID Maintenance and Troubleshooting 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.
Page 284: Clean/Replace The Fid Jet
Chapter 15 Maintenance and Troubleshooting Maintaining a FID OPERATING SEQUENCE Clean/Replace the FID Jet Material needed • Screwdriver • Tool for extracting the jet (P/N 205 019 00) • Forceps or tweezers • Ultrasonic cleaning bath • Liquid detergent • Clean compressed air •...
Page 285 Chapter 15 Maintaining a FID Maintenance and Troubleshooting DETECTOR Flame Temp Signal pA (0.0) Ing. Thresh. Flameout retry Make-up Disconnect the signal and ignition polarization cables 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.
Page 286 Chapter 15 Maintenance and Troubleshooting Maintaining a FID Figure 15-13. Clean/Replace the Jet (2) • To clean the jet refer to Clean the Jet then continue from the point 7. • To replace the jet refer to Replace the Jet then continue from the point 7.
Page 287 Chapter 15 Maintaining a FID Maintenance and Troubleshooting Figure 15-14. Clean/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.
Page 288: Clean/Replace The Fid Collecting Electrode
Chapter 15 Maintenance and Troubleshooting Maintaining a FID OPERATING SEQUENCE Clean/Replace the FID Collecting Electrode Material needed • Screwdriver • Pliers • Forceps or tweezers • Ultrasonic cleaning bath • Liquid detergent • Clean compressed air • GC-grade methanol • Clean paper towel •...
Page 289 Chapter 15 Maintaining a FID Maintenance and Troubleshooting DETECTOR Flame Temp Signal pA (0.0) Ing. Thresh. Flameout retry Make-up Disconnect the signal and ignition polarization cables from the detector. See Figure 15-16. 5. Loosen the fixing screw on the front of the detector cell and remove it. See Figure 15-16.
Page 290 Chapter 15 Maintenance and Troubleshooting Maintaining a FID 9. Using tweezers, extract the collecting electrode through the top of the detector cell. • To clean the collecting electrode refer to Clean the Collecting Electrode then continue from the point 10. •...
Page 291 Chapter 15 Maintaining a FID Maintenance and Troubleshooting 10. Using forceps, reconnect the gold contact pin. See Figure 15-17. 11. Remount the connector holder assembly, verifying the contact efficiency. See Figure 15-17. 12. Screw the detector cap into its housing. See Figure 15-17. 13.
Page 292: Replace The Fid Ignition Assembly
Chapter 15 Maintenance and Troubleshooting Maintaining a FID OPERATING SEQUENCE Replace the FID Ignition Assembly Material needed • Screwdriver • Connector Holder Assembly 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.
Page 293 Chapter 15 Maintaining a FID Maintenance and Troubleshooting Figure 15-19. Replace the Ignition Assembly (1). 6. Unscrew the two fixing 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.
Page 294 Chapter 15 Maintenance and Troubleshooting Maintaining a FID 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. Instruction Manual...
Page 295: Fid Troubleshooting
Chapter 15 FID Troubleshooting Maintenance and Troubleshooting FID Troubleshooting Change in Sensitivity The sensitivity of the Flame Ionization Detector depends on the carrier and detector gases flow rates and to the detector temperature. Gases The carrier gas flow range depends on the type of the gas used and on the type and diameter of the capillary column installed.
Page 296: Flame Ignition
Chapter 15 Maintenance and Troubleshooting FID Troubleshooting NOTE Generally the air flow rate must be set to about 10 times the hydrogen flow rate to keep the flame lit. For high sensitivity applications, it is essential that you exclude all traces of organic contamination from the chromatographic system and/or from the gas lines of the detector.
Page 297 Chapter 15 FID Troubleshooting Maintenance and Troubleshooting Table 15-4. Difficulty in Igniting the Flame (Continued) Broken or Replace jet. Refer to the Clean/Replace the FID Jet cracked flame Operating Sequence on page 284 for instructions. Check for a blocked jet by measuring the hydrogen flow with a flowmeter.
Page 298: Maintaining A Tcd
Chapter 15 Maintenance and Troubleshooting Maintaining a TCD Maintaining a TCD The TCD detector does not usually need current maintenance. Nevertheless, if you follow a few simple sequences, you will prolong the detector’s lifetime. Pay a special attention to avoid contamination or damage of the filaments. Follow these simple rules: •...
Page 299 Chapter 15 Maintaining a TCD Maintenance and Troubleshooting 1. Detector 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.
Page 300: Tcd Troubleshooting
Chapter 15 Maintenance and Troubleshooting TCD Troubleshooting TCD Troubleshooting Sensitivity Sensitivity is related to the detector temperature (increasing temperature reduce sensitivity) and to the flow rate of the carrier, reference and make-up gas. A gain in sensitivity can be obtained increasing the gap between the temperature of the block and that of the filaments or increasing the filaments voltage.
Page 301: Troubleshooting The Tcd
Chapter 15 TCD Troubleshooting Maintenance and Troubleshooting Troubleshooting the TCD Table 15-5. TCD Troubleshooting Table Symptom Diagnosis Remedy Unstable regulation of the Check the controllers of the carrier, flow rate of the gases reference and make-up gases work well. Leaks on the gas lines Check the connections of the carrier, reference and make-up gas are tight.
Page 302 Chapter 15 Maintenance and Troubleshooting TCD Troubleshooting Table 15-5. TCD Troubleshooting Table (Continued) Symptom Diagnosis Remedy Leaks on the gas lines Check the connections of the carrier, reference and make-up gas are tight. Leak due to septum wearing Replace the septum. Operating conditions of the Optimize working parameters of the detector not properly set...
Page 303 Chapter 15 TCD Troubleshooting Maintenance and Troubleshooting Table 15-5. TCD Troubleshooting Table (Continued) Symptom Diagnosis Remedy Faulty temperature control Contact your customer support organization. Baseline drift Refer to Appendix A, Customer Communication, for contact information. Oxidized filaments Contact your customer support organization.
Page 304: Maintaning Gas Sampling Valve
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.
Page 305 Chapter 15 Maintaning Gas Sampling Valve Maintenance and Troubleshooting Remove the sampling loop The sampling loop is connected between the valve ports 1 and 4 as shown in the scheme of Figure 15-23. Sampling Loop Sampling Loop Column Column Carrier Carrier INJECT LOAD...
Page 306: Analytical Troubleshooting
Chapter 15 Maintenance and Troubleshooting Analytical Troubleshooting Analytical Troubleshooting This paragraph contains instructions for the instrument troubleshooting and a brief guide for the analytical troubleshooting. Systematic approach is required to cause identification and problem solving. For this is purpose, a method as the following one is suggested. Electrical Connections •...
Page 307: Instrument Troubleshooting
Chapter 15 Error Messages Maintenance and Troubleshooting • Check the column efficiency periodically. Detector • Ensure that the detector parameters are correctly set. • Check for eventual detector contamination. Data System • Check that the Data System in use is properly connected. Instrument Troubleshooting The control unit of the GC performs a number of test routines to monitor and report on the status of the major chromatographic and control functions.
Page 308 Chapter 15 Maintenance and Troubleshooting Error Messages Table 15-6. Error Messages (Continued) Message Description The inlet temperature exceeds the temperature limits (375 °C). Error HARDWARE SHUTDOWN Inlet T over limits may be due to a probe malfunctioning. The detector temperature exceeds the temperature limits HARDWARE SHUTDOWN Det T over limits (375 °C).
Page 309: Guide To Solve Analytical Problems
Chapter 15 Guide to Solve Analytical Problems Maintenance and Troubleshooting Table 15-6. Error Messages (Continued) Message Description The TCD filaments are set to Off for their protection. TCD fil switched This message appears: Required flow not - When trying to switch the TCD filaments to ON with Reference gas Off.
Page 310 Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems 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. Instruction Manual...
Page 311 Chapter 15 Guide to Solve Analytical Problems Maintenance and Troubleshooting Baseline Behavior Characteristics Cause Remedy Accumulation of stationary Replace the end section of the phase column. Carrier gas cylinder Replace the carrier gas cylinder pressure too low to allow or increase the pressure. control Drifting carrier gas or Check the gas controllers.
Page 312 Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems Behavior Characteristics Cause Remedy Excessive column Check the oven temperature, stationary phase bleeding ensuring it doesn't exceed the column upper limit. High-standing current Recondition the column. (continued) Replace the column. Loose connections Ensure all interconnections and screw connections are tight.
Page 313 Chapter 15 Guide to Solve Analytical Problems Maintenance and Troubleshooting Behavior Characteristics Cause Remedy Detector temperature higher Reduce the detector temperature than column maximum to the column temperature upper temperature limit. Noise External electrical Attach an AC line monitor and High-frequency interference check purity of the AC supply...
Page 314 Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems Peaks Behavior Characteristics Cause Remedy Column flow too high Reduce the flow to slightly above optimum. Column flow too low Increase the flow to slightly above optimum. Split flow too low in split Increase the flow to 40-50 injection ml/min.
Page 315 Chapter 15 Guide to Solve Analytical Problems Maintenance and Troubleshooting Behavior Characteristics Cause Remedy Column or detector Decrease the injected amount overloaded and/or analyte concentrations. Increase the split ratio. Fronting Column temperature too Increase the temperature. Stationary phase too thin Use a thicker-film column.
Page 316 Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems Behavior Characteristics Cause Remedy Negative Some Symptom can be normal peaks Carrier gas flow too high Reduce the carrier gas flow rate. Combustion gas flow Check the combustion gas flow. incorrect Detector contaminated Bake out or clean the detector.
Page 317 Chapter 15 Guide to Solve Analytical Problems Maintenance and Troubleshooting Behavior Characteristics Cause Remedy Glass wool or inlet liner Replace with fresh silanized causing activity wool and a clean inlet liner. Inlet temperature too low Increase the inlet temperature Poor or obstructed column Remake the column inlet connections connection.
Page 318 Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems Results Behavior Characteristics Cause Remedy Concentration not Ensure that the sample compatible with the concentration is suitable for the dynamic range of the detection system. detection system Inappropriate injection Try a different injection technique technique.
Page 319 Chapter 15 Guide to Solve Analytical Problems Maintenance and Troubleshooting Behavior Characteristics Cause Remedy Leaks in the GC carrier gas Run a leak test and correct leaks. line. Poor with normal Syringe leaks during Replace syringe or piston seals, sensitivity retention time injection if applicable.
Page 320 Chapter 15 Maintenance and Troubleshooting Guide to Solve Analytical Problems Instruction Manual...
Page 321: Chapter 16 Lan Option Set-Up
LAN 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: Introduction
Introduction Introduction The FOCUS GC LAN version is basically an instrument equipped with a CPU featuring LAN (Local Area Network) capabilities. The FOCUS GC LAN is easily recognizable by the presence on the rear panel of a RJ45 connector, 2 LEDs for LAN activity and a reset button.
Page 323: Reset Button
Reset Button To reset the IP address and communication port to default values, push the reset button, 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: •...
Page 324: Set-Up
LAN Option Set-up Set-Up Set-Up To set the desired IP and set up the LAN communication port of the FOCUS GC then to configure the data system, please follow the instruction reported in How to Set up the FOCUS GC LAN operating sequence.
Page 325 Chapter 16 Set-Up LAN Option Set-up • If the default IP address 192.168.127.254 is reachable, please go to paragraph How to operate when the IP address is reachable. • If your PC is not able to 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...
Page 326 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 Should you still have problems, please check the cable connection, and go through the reset procedure of the FOCUS GC CPU. The CPU/LAN is hence reset to the default IP 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.
Page 328 Chapter 16 LAN Option Set-up Set-Up 2. The telnet program 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.
Page 329 Use the ARROWS and ENTER keys to navigate the menus. In this page you’ll need to enter the new IP assigned needed for the LAN environment where the FOCUS GC LAN is installed. Also the netmask is entered in the same menu section.
Page 330 Chapter 16 LAN Option Set-up Set-Up 5. By moving the selection with the up/down arrow keys, select 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.
Page 331 Please confirm to make the changes effective, and remember that from now on, the FOCUS GC LAN will respond to the newly assigned IP Address. 8. Disconnect the FOCUS GC from direct RED patch, and connect it to its final destination LAN environment.
Page 332 • 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.
Page 333 GC through the COM ports and to specify a direct TCP/IP address. 10. Enter the IP address of the FOCUS GC and complete the configuration in the usual way. When the ADVANCED button is pressed, it is possible to set the communication port used by the TCP/IP protocol and the timeout.
Page 334 In the case of switched network, this warning can be ignored. Alternative Configuration An alternative to the direct setup of the FOCUS GC LAN, it is also possible to use a management program designed for sites where multiple FOCUS GCs with LAN option are available.In this case a specific program must be installed and used to...
Page 335 LAN Option Set-up The program is a valid replacement 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 Instruction Manual...
Page 337: Customer Communication
Customer Communication Thermo Fisher Scientific provides comprehensive technical assistance worldwide and is dedicated to the quality of our customer relationships and services. How To Contact Us This appendix contains contact information for Thermo Fisher Scientific S.p.A office. Use the list reported in Customer Communication to contact your local Thermo Fisher Scientific office or affiliate.
Page 338: Reader Survey
Appendix A How To Contact Us Reader Survey Product: FOCUS GC Manual: Instruction Manual Part No.: 317 094 12 Please help us improve the quality of our documentation by completing and returning this survey. Circle one number for each of the statements below.
Page 339: Glossary
Glossary This section contains an alphabetical list and descriptions of terms used in this guide and the help diskette. It also includes abbreviations, acronyms, metric prefixes, and symbols. ampere alternating current analog-to-digital converter byte (8 b) baud rate data transmission speed in events per second ºC Celsius Carriage and Insurance Paid To...
Page 340 Glossary electrostatic discharge ºF Fahrenheit Flame Ionization Detector Free on Board foot gram gain A measure of the ability of an electronic circuit or device to increase the magnitude of an electronic input parameter. gas chromatograph electrical ground height hour harmonic A high-frequency disturbance that appears as distortion of the distortion...
Page 341 Glossary inch input/output kilo (10 or 1024) Kelvin kilogram kilopascal length liter Local Area Network pound light-emitting diode meter (or milli [10 mega (10 µ micro (10 megabecquerel millicurie meniscus The curved upper surface of a column of liquid. minute milliliter millimeter Instruction Manual...
Page 342 Glossary mass-to-charge ratio nano (10 negative polarity The inverse of a detector signal polarity. nanometer outside diameter Ω pico (10 pascal printed circuit board part number PPKD Purged Packed Injector pounds per square inch random access memory radio frequency read-only memory RS-232 industry standard for serial communications second...
Page 343 Glossary S/SL Split/Splitless Injector surge slow average A gradual, long-term change in average 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.
Page 344 Glossary ° C min instead of ° C/min instead of g/L Instruction Manual...
Page 345: Index
Index Cleaning About This Manual xiii Replacement 288 Conventions Used xv Column Conditioning 217, 231, 245 Overview xiii Column Evaluation 217, 231, 245 Acceptance Criteria Column Installation 217, 231, 245 CHROM-CARD 256 Column Leak Check 217, 231, 245 CHROMQUEST 241, 256 Column Oven 26, 28 Computing-integrator (e.g.
Page 346 How to Starting Up the Instrument 208 Jet 159 Hydrogen 219 Menu 164 Sensor Selectivity 160 xxiv Temperature 160 Use xxiii FOCUS GC Hydrogen Sensor xxiv Components 26 Description 25 Ignition Assembly Document Set xx Replacement 292 Instrument Initial Temperature 219, 233, 248...
Page 347 Index Instrument Cleaning 261 Material Safety Data Sheets xxiv Instrument Set-up 198 Messages 211 Instrument Start-Up 208 Methods and Sequences 31 Instrument Troubleshooting 307 Negative Polarity 233, 248 Jet 162 Network Cables 323 Cleaning 284 Nitrogen 219, 233, 248 Replacement 284 Noise 227, 241, 256 jet 162 Not Ready/Error LED 44...
Page 348 Index S/SL. See Split/Splitless Injector Safety Information xxii Detector Gases Flow Regulation 77 Use of Gases xxii Troubleshooting 300 safety symbols xv–xix TCD. See Thermal Conductivity Detector Septum 99, 218, 232, 246 TCD-PPKD Acceptance Criteria 256 Septum Installation 216, 230, 244 CHROM-CARD 256 Servo Air 36 CHROMQUEST 256...
Page 349 Index Troubleshooting the TCD 301 Use of Gases xxii User Interface 27, 41, 42 Using Hydrogen xxiii Using the Hydrogen Sensor xxiv Wander 227, 241, 256 Xcalibur 218 Instruction Manual...
Page 350 Index Instruction Manual...
Page 351 Operating Sequences Configuring the Carrier Gas ......................73 Configuring The Pressure Unit ......................74 Measuring the Detector Gas Flows with a Bubble Meter ..............78 Configuring the Column Oven ......................86 Setting Up a Single Ramp Temperature Program ................89 Setting Up Multiple Ramp Temperature Program ................90 Installing a Liner and a Septum ......................
Page 352 Replace 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 ............................39 Gas Sampling Valve ..........................40 The FOCUS GC User Interface ......................42 Components of the FOCUS GC Menu Display ................. 43 FID-External Detector Gases Flow Regulation................. 76 TCD Detector Gases Flow Regulation ....................77 The FOCUS GC Column Oven ......................84 Example of Single Ramp Temperature Program ................
Page 354 Replace and Clean the Liner (2) ......................271 Replace and Clean the Liner (3) ......................272 Top Aluminium Cover Removal (1) ....................273 FOCUS GC Rear Panel ........................274 Filter Replacing ..........................275 PPKD Injector Septum Replacement ....................278 PPKD Injector Replace/Clean the Liner .................... 280 FID Parts Identification ........................
Page 355 List of Tables Status LED Descriptions ........................44 Keypad Descriptions ..........................45 Configuration Menu ........................... 52 Configure Oven Menu ........................53 Configure Carrier Menu ........................54 Configure AS 2000 Autosampler Menu ....................56 Configure AI 3000/AS 3000 Autosampler Menu ................57 General Config Menu ........................58 Configure Keyboard &...
Page 356 FID-S/SL Analytical Conditions ....................... 219 FID-S/SL Acceptance Criteria ......................227 TCD-S/SL Parts Referenced ......................232 TCD-S/SL Analytical 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 ..........................

Thermo Scientific FOCUS GC Instruction Manual

Table of Contents

Chapter 1 FOCUS GC Description

Interface

Chapter 2 The FOCUS GC User Interface

3 Gas Control

Chapter 3 Gas Control

4 Column Oven

Chapter 4 Column Oven

5 Split/Splitless Injector

Chapter 5 Split/Splitless Injector (S/SL)

6 Purged Packed Column

Chapter 6 Purged Packed Column Injector (PPKD)

7 Column

Chapter 7 Column

8 Flame Ionization

Chapter 8 Flame Ionization Detector (FID)

9 Thermal Conductivity

Chapter 9 Thermal Conductivity Detector (TCD)

10 Autosamplers

Chapter 10 Autosamplers

11 Getting Started

Chapter 11 Getting Started

12 Checkout Using Fid

Chapter 12 Checkout Using FID with S/SL

13 Checkout Using Tcd

Chapter 13 Checkout Using TCD with S/SL

14 Checkout Using Tcd

Chapter 14 Checkout Using TCD with PPKD

15 Maintenance and

Chapter 15 Maintenance and Troubleshooting

Chapter 16 LAN Option Set-Up

Appendix A Customer Communication

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