Thermo Scientific. TRACE GC Ultra UFM. Ultra Fast Module Device Instruction Manual. PN , Revision May 2010

Transcription

1 Thermo Scientific TRACE GC Ultra UFM Ultra Fast Module Device Instruction Manual PN , Revision May 2010

2 UFM Ultra Fast Module Device for TRACE GC Ultra Instruction Manual May 2010 Edition Part Number Thermo Fisher Scientific Inc. All rights reserved. Printed in Italy Published by Thermo Fisher Scientific S.p.A., Strada Rivoltana, Rodano - Milan - Italy Tel: Fax: Printing History: First Edition, released February 2002 Second Edition, released December 2002 Third Edition, released May 2003 Fourth Edition, released April 2004 Fifth Edition, released January 2005 Sixth Edition, released September 2005 Seventh Edition, released May 2006 Eight Edition, released December 2006 Ninth Edition, released May 2007 Tenth Edition, released April 2009 Eleventh Edition, released May 2010 Disclaimer Technical Information contained in this publication is for reference purposes only and is subject to change without notice. Every effort has been made to supply complete and accurate information; however, Thermo Fisher Scientific assumes no responsibility and will not be liable for any errors, omissions, damage, or loss that might result from any use of this manual or the information contained therein (even if this information is properly followed and problems still arise). This publication is not part of the Agreement of Sale between Thermo Fisher Scientific and the purchaser of a TRACE GC Ultra system. In the event of any conflict between the provisions of this document and those contained in Thermo Fisher Scientific s Terms and Conditions, the provisions of the Terms and Conditions shall govern. Reference to System Configurations and Specifications supercede all previous information and are subject to change without notice. Trademarks TRACE GC Ultra is a trademark of Thermo Fisher Scientific Inc., and its subsidiaries. Other brand and product names may be trademarks or registered trademarks of their respective companies.

3 Declaration Manufacturer: Thermo Fisher Scientific Thermo Fisher Scientific 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: the local installation complies with local law regulations the instrument is used according to the instructions provided and if its operation is only entrusted to qualified trained personnel Thermo Fisher Scientific is not liable for any damages derived from the non-compliance with the aforementioned recommendations. Instruction Manual 3

4 4 Instruction Manual

5 Contents About This Manual...9 Overview...9 Conventions Used in This Manual Instrument Markings and Symbols Classification of the Instrument...14 Environmental Conditions Using the TRACE GC Ultra Document Set Using Hydrogen...16 Using the Hydrogen Sensor Chapter 1 UFM Device Overview The UFM Device General Information GC Installation Note Carrier Gas Requirements Detector Gases Requirements When FID/FPD detector is used When TEMPUS TOF MS detector is used Columns Chapter 2 UFM Device Set-Up Introduction...26 Menus Description Column Oven Configuration Menu Oven (UFM) Menu...27 UFM Calibration UFM Calibration Menu Set-Up Getting Started UFM Column Installation...31 System Power Up Configure Column Oven for UFM UFM Calibration Column Evaluation and Leak Check Automatic Leak Check Column Evaluation Parameters Programming Instruction Manual 5

6 Contents Column Oven Parameters Programming Split/Spliless Injector Parameters Programming Programmable Temperature Vaporizing Injector Parameters Programming FID/FPD Detector Parameters Programming TEMPUS TOF MS Parameters Programming Chapter 3 Analysis...51 Performing an Analysis Chapter 4 Maintenance and Troubleshooting...57 Maintenance Maintaining the UFM Device Messages Calibration Routine Error Messages Calibration Verify Routine Error Messages General Messages Chapter 5 UFM Device Installation...65 Introduction Who Performs the Installation of the Device Getting Started S/SL - FID/FPD Configuration Removing the GC Panels Preparing the Injector and Detector Base Installing the Heating Block Installing the Column Fixing Bracket Installing the UFM Control Card Installing the External Power Module Connecting the Cables Reinstalling the GC panels Powering on the GC Configuring the UFM Device S/SL - MS Configuration...94 Removing the GC Panels Preparing the Injector and Detector Transfer Line Instruction Manual

7 Contents Installing the Heating Block Installing the UFM Control Card Installing the External Power Module Connecting the Cables Reinstalling the GC panels Powering On the GC Configuring the UFM Device PTV - FID/FPD Configuration Removing the GC Panels Preparing the Injector and Detector Base Installing the Heating Block Installing the Column Fixing Bracket Installing the UFM Control Card Installing the External Power Module Connecting the Cables Reinstalling the GC panels Powering on the GC Configuring the UFM Device UFM Device Removal Customer Communication How To Contact Us Reader Survey Glossary Index Instruction Manual 7

8 Contents 8 Instruction Manual

9 Overview About This Manual This Instruction Manual contains descriptions of the features and components of the UFM device. Inside, you will find all of the information necessary for routine operation of your GC, including operating sequences to install and remove the UFM device on your GC, and diagrams and descriptions of the major components. This manual is organized as follows: Chapter 1, UFM Device Overview, contains a description of the features and components of the UFM Device. Information about the configuration options, menus for the UFM and procedures for using UFM capillary column are also included. Chapter 2, UFM Device Set-Up, describes configuration options, menus and instrument set-up operating sequences for the correct use of the UFM device. Chapter 3, Analysis, This chapter provides information to run analyses with your TRACE GC Ultra equipped with the UFM device. Chapter 4, Maintenance and Troubleshooting, provides maintenance guidelines and troubleshooting suggestions for the UFM device. Chapter 5, UFM Device Installation, provides the instructions to properly install the UFM device on your TRACE GC Ultra. It also contains operating sequences to remove the device from your GC when normal gas chromatography conditions are required. Appendix A, Customer Communication, contains contact information for Thermo Fisher Scientific offices worldwide. This appendix also contains a one-page Reader Survey. The Glossary contains definitions of terms used in this guide and the help diskette. It also includes abbreviations, acronyms, metric prefixes, and symbols. The Index contains an alphabetical list of key terms and topics in this guide, including cross references and the corresponding page numbers. Instruction Manual 9

10 About This Manual Conventions Used in This Manual Conventions Used in This Manual The following symbols and typographical conventions are used throughout this manual. Bold Italic Monospace Monospace Bold Bold text indicates names of windows, dialog boxes, and fields. Italic indicates cross references, first references to important terms defined in the glossary, and special emphasis. Monospace, or Courier, indicates filenames and filepaths or text the user should enter with the keyboard. Monospace Bold indicates messages, prompts, or menu titles displayed on the computer screen or on a digital display.» This symbol illustrates menu paths to select, such as File»Open. KEY NAME CAUTION Bold, uppercase sans serif font indicates the name of a key on a keyboard or keypad, such as ENTER. This symbol alerts you to an action or sequence that, if performed improperly, could damage the instrument. NOTE WARNING! This symbol alerts you to important information related to the text in the previous paragraph. This symbol alerts you to an action or sequence that, if improperly performed, could result in damage to the instrument or possible physical harm to the user. This symbol may be followed by icons indicating special precautions that should be taken to avoid injury. This symbol indicates an electric shock hazard. 10 Instruction Manual

11 Conventions Used in This Manual About 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. This symbol indicates the presence of radioactive material. This symbol indicates an operation or sequence that must not be performed by the user. A Thermo Fisher Scientific authorized Customer Support Engineer must perform this sequence. This symbol indicates all metal objects, such as watches and jewelry, must be taken off. This symbol indicates an eye hazard. Eye protection must be worn. This symbol indicates the user must wear a protective screen when performing the sequence. Instruction Manual 11

12 About This Manual Instrument Markings and Symbols 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. 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 TRACE GC Ultra gas chromatograph. Symbol Direct Current Description Alternating Current Both direct and alternating current 3 Three-phase alternating current Earth (ground) terminal Protective conductor terminal Frame or chassis terminal 12 Instruction Manual

13 Instrument Markings and Symbols About This Manual Symbol Equipotentiality Description On (Supply) Off (Supply) 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. Caution, risk of electric shock Caution, hot surface Caution (refer to accompanying documents) In-position of a bistable push control Out-position of a bistable push control Symbol in compliance to the Directive 2002/96/EC on Waste Electrical and Electronic Equipment (WEEE) placed on the european market after August, 13, Instruction Manual 13

14 About This Manual Classification of the Instrument Classification of the Instrument Environmental Conditions Internal use Up to 2000 meters altitude Temperature 18 to 30 C Maximum relative humidity between 30% and 85% Voltage variations must not exceed the nominal voltage by ± 10% Transient overloads in compliance with installation categories II Pollution degree according to IEC 664 (3.7.3) 2 Protection degree IP00 14 Instruction Manual

15 Using the TRACE GC Ultra Document Set About This Manual Using the TRACE GC Ultra Document Set The TRACE GC Ultra Document Set (CD-Rom PN ) includes all manuals in electronic format, and serves as your library for information about the TRACE hardware and software. The TRACE GC Ultra Document Set (PN ) as paper copy is also available. Furthermore, Thermo Fisher Scientific part numbers (PN) for the paper copy manuals are provided for each book title. Site Preparation and Installation Manual (PN ) This manual and diskette describes how to set up a workspace for the TRACE GC and how to connect the TRACE GC Ultra to the gas supplies and peripheral devices. Acceptance Package (PN ) This folder contains required shipping documents and quality report forms. Getting Started (PN ) This guide contains sequences for checking configuration, installing detectors, and making a first analysis with the TRACE GC Ultra. Operating Manual (PN ) This manual provides descriptions of the TRACE GC Ultra hardware and software and instructions for their use. UFM Ultra Fast Module Device (PN ) This manual provides descriptions of the TRACE GC Ultra equipped with the UFM device. and instructions for it use. The relevant Standard Operating Procedure is provided in a separated document PN Quick Reference Card (PN ) This reference card contains guidelines for carrier gas use and injection sequences. K-Factor Quick Reference (P/N ) This reference card contains information to interpretate results from a Column Evaluation. Instruction Manual 15

16 About This Manual Using Hydrogen Using Hydrogen Preventive Maintenance Schedule (PN ) This document provides a list of recommended scheduled maintenance and a year-long log book to record maintenance, observations, supply lists, and service records. Maintenance and Troubleshooting Guide (PN ) This manual contains instructions for diagnosing and resolving operational problems. Standard Operating Procedures (PN ) This manual contains instructions, operating sequences, and test criteria for final testing of the TRACE GC Ultra. Spare Parts Catalog (PN ) This catalog contains a list of spare parts for the TRACE GC Ultra. The use of hydrogen as a carrier gas or as fuel for certain flame detectors requires the operator s strict attention and compliance with special precautions due to the hazards involved. Hydrogen is a dangerous gas, particularly in an enclosed area when it reaches a concentration corresponding to its lower explosion level (4% in volume). When mixed with air it can create an explosive mixture. An explosion hazard could develop in the GC oven when hydrogen is used as a carrier gas if oven elements are not perfectly connected to each other, or if the connection materials are worn out, broken, or otherwise faulty. Use the following safety precautions when using hydrogen: Ensure that all hydrogen cylinders comply with the safety requirements for proper use and storage. Hydrogen cylinders and delivery systems must comply with local regulations. Make sure the gas supply is turned completely off when connecting hydrogen lines. 16 Instruction Manual

17 Using Hydrogen About This Manual Perform a bubble test to ensure that the hydrogen lines are leak-tight before using the instrument. Perform the bubble test after performing the pressure test described in the TRACE GC Ultra Maintenance and Troubleshooting Manual. Avoid spraying any electrical components during the bubble test. Continue checking each section of the pneumatic circuit until you identify the leak. If you need to perform a leak check inside the pneumatic compartment, first perform the bubble test with all circuits pressurized, then disconnect the GC from the main gas supply and remove the pneumatic circuit panel. Repeat this sequence until you eliminate all leaks. Ensure your GC column oven has a hydrogen sensor. A hydrogen sensor continuously monitors the hydrogen level in the GC column oven. Using the Hydrogen Sensor If your GC oven does not have a hydrogen sensor already installed, contact your Thermo Fisher Scientific sales representative. To comply with instrument safety requirements, a Thermo Fisher Scientific CSE or authorized service technician should install the sensor. If you plan to use a sensor other than the sensor recommended by Thermo Fisher Scientific, you must verify its ability to perform the functions listed above before installing it. It must comply with your local safety regulations, or with the IEC regulations if local regulations do not exist. The lower limit of the hydrogen sensor is 0.5% in volume. You should adjust the detection threshold to 1% in volume, which is 25% of the hydrogen lower limit of explosion (4% in volume). In cases where the connections begin to leak or the column breaks, the sensor alerts the operator. It then automatically cuts off the gas supply and heating to the active zones, and sweeps the column oven with forced air ventilation. If the sensor detects anomalies or leaks during GC operation due to instrument malfunction, the operator must immediately: 1. IEC , First Edition, September 1990; IEC , Amendment 1, September 1992; IEC , Amendment 2, June Instruction Manual 17

18 About This Manual Using Hydrogen close the hydrogen supply switch off the gas chromatograph air out the room The reliability of the sensor depends on careful maintenance. After the sensor is in use, you must periodically check its operating performance and calibration as recommended by the manufacturer. Refer to your hydrogen sensor s instruction manual for maintenance guidelines. WARNING! NOTE Never use hydrogen in your TRACE GC Ultra system 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 appropriate sensor. 18 Instruction Manual

19 1 UFM Device Overview This chapter contains a description of the features and components of the UFM Device. Information about the configuration options, menus for the UFM and procedures for using UFM capillary column are also included. Chapter at a Glance The UFM Device...20 General Information...22 Instruction Manual 19

20 Chapter 1 UFM Device Overview The UFM Device The UFM Device The Ultra Fast Module (UFM) device, shown in Figures 1-1 and 1-2, is a GC device that integrates a GC capillary column with the components for its temperature control. Figure 1-1. The UFM Device (S/SL or PTV - FID/FPD Configuration) Figure 1-2. The UFM Device (S/SL - MS Configuration) 20 Instruction Manual

21 The UFM Device Chapter 1 UFM Device Overview Compared to conventional air circulating GC oven UFM Device features faster temperature programming and it allows heating rates up to 1200 C/min while maintaining low power consumption. The UFM device includes a column module where a capillary column, a heating wire and a temperature sensing wire are combined in a tight package using a ceramic fiber insulation. The column module may be operated at programmable temperatures ranging from ambient to 370 C or to the maximum operating temperature of the related stationary phase. The power required by the capillary column module to operate is furnished by the external Power Module. Additionally the UFM Device includes a heated block and the relevant cover. This heated block allows the proper connection of the column module to the inlet and to the detector. The heating block is maintained at constant temperature choosing in the range from ambient to 400 C. The device control is performed by a dedicated control card installed in the GC electronic compartment. Instruction Manual 21

22 Chapter 1 UFM Device Overview General Information General Information The Ultra Fast Module (UFM) Device allows the direct heating of the analytical capillary column properly installed inside the GC oven. To operate with the UFM device the GC must be equipped with: Gas Control DPFC and DGFC modules for the digital control of the injector and detector gases. Injector According to the UFM Device configuration, the following injectors may be used: Split/Splitless (S/SL) Programmable Temperature Vaporizing (PTV) Detector According to the UFM Device configuration, the following detectors may be used: Flame Ionization Detector (FID), Flame Photometric Detector (FPD) TEMPUS TOF MS detector CAUTION NOTE FPD requires the use of the silcosteeled jet PN to avoid interaction with steel. PTV-MS configuration is not currently available. GC Installation Note Install the GC equipped with the UFM device such as a standard TRACE GC Ultra. To properly install the GC in your lab, please refer to the instructions reported in the TRACE GC Ultra Site Preparation and Installation Manual. The GC also requires the use of an external Power Module to supply the UFM device. 22 Instruction Manual

23 General Information Chapter 1 UFM Device Overview To properly install and connect this module, please refer to Installing the External Power Module in Chapter 5 of this manual. WARNING! The PTV Backflush option, if present, must be removed, due to its interference with the installation of the UFM device in the configuration with the PTV injector. Carrier Gas Requirements The GC may require helium, nitrogen or hydrogen as carrier gas. WARNING! Hydrogen is a potentially dangerous gas that requires the operator s strict attention and compliance with special precautions due to the hazards involved. Refer to Using Hydrogen on page 16 for safety informations. Detector Gases Requirements Verify the detector gases requirements according to the detector in use. When FID/FPD detector is used FID/FPD requires air and hydrogen as fuel gases. The use of the make-up gas is optional. According to the required gases, the DGFC module may be: Type AB for the control of air and hydrogen. Type AD for the control of air and hydrogen. Type AC for the control of air, hydrogen and make-up gas. 1. Verify that the detector gas control module installed on your GC is compatible with the detector gas requirements. 2. The connections of the FID/FPD detector gases must be performed as described in the following table: Instruction Manual 23

24 Chapter 1 UFM Device Overview General Information Installed Module Connect Hydrogen to Connect Air to Connect Make-up Gas to AB Gas 2 Gas 1 AC Gas 2 Gas 1 Gas 3 (*) AD Gas 3 Gas 1 (*) FPD applications typically do not require Make-up gas. For further details, refer to the TRACE GC Ultra Operating Manual. When TEMPUS TOF MS detector is used To verify MS detector gas requirements please refer to the relevant instruction manual. Columns Several UFM capillary columns are available. The column is placed in a proper cage according to the instrument configuration. No preventive column preparation is required; the fittings required for the installation are already present. To install the UFM column refer to UFM Column Installation on page Instruction Manual

25 2 UFM Device Set-Up This chapter describes configuration options, menus and instrument set-up operating sequences for the correct use of the UFM device. Chapter at a Glance Introduction...26 Menus Description...26 Set-Up Getting Started...30 UFM Column Installation...31 System Power Up...31 Configure Column Oven for UFM...32 UFM Calibration...33 Column Evaluation and Leak Check...37 Parameters Programming...43 Operating Sequences How to Configure Column Oven for UFM...32 How to Perform an UFM Calibration...33 How to Perform a Manual Calibration Verify...35 How to Perform a Column Evaluation...39 How to Perform an Automatic (DPFC) Leak Check...41 Setting Up a Single Ramp Temperature Program...43 Setting Up a Multiple Ramp Temperature Program...44 Setting Up the Split/Splitless Injector...45 Setting Up the Programmable Temperature Vaporizing Injector...47 Programming an FID/FPD...49 Instruction Manual 25

26 Chapter 2 UFM Device Set-Up Introduction Introduction This manual will give you additional information to the TRACE GC Ultra Document Set also delivered with the unit, due to specific features of the UFM device. To properly install the instrument refer to the TRACE GC Ultra Site Preparation and Installation Manual. Menus Description This paragraph details the TRACE GC Ultra menus dedicated to the UFM device. Column Oven Configuration Menu The CONFIGURE OVEN menu contains the configuration parameters for the column oven. NOTE The UFM Device is automatically recognized when the GC is turned on. The following message will be displayed during the GC start-up routine.. Thermo Fisher Scientific Trace GC Ultra ULTRA FAST MOD. found 1. Press CONFIG. Then press OVEN or scroll to Oven and press ENTER to open the menu shown in Table 2-1. Table 2-1. Configure Oven Menu Menu Range Comments CONFIGURE OVEN This line is the menu title bar. Auto prep run On/Off Press ON to turn on automatic Prep Run execution without pressing PREP RUN. This feature is useful when you use the autosampler. When this item is set to Off, you must press PREP RUN to activate the Prep Run. 26 Instruction Manual

27 Menus Description Chapter 2 UFM Device Set-Up Table 2-1. Configure Oven Menu (Continued) Menu Range Comments Auto Start On/Off Allows an automatic Start signal. PR timeout min, Enter the duration of the prep run. The injection must occur within this time or the timeout will return the GC to the Standby condition. Enable UFM? 1 Yes/No This function enables the UFM system. Press YES to activate the UFM system. Press NO to deactivate it. Equil time min This is the time required for equilibrating the oven temperature after the temperature is set or modified. Ready delay min This parameter delays the Ready to Inject condition. This function is useful for on-column injectors. It allows the secondary cooling to cool the injector before the injection. This time must not exceed the PR timeout value. Max temp (UFM) C This parameter defines the maximum allowable column temperature setpoint to protect the column from unintentionally high temperatures. UFM Calibration 2 This function allows the calibration of the heating element of the column. 1. When UFM system is present. 2. When UFM system is present and enabled, its parameters are included in the menu. Oven (UFM) Menu The OVEN (UFM) menu contains the parameters for programming the UFM Column temperature, 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. Press OVEN to open the OVEN (UFM) menu, shown in Table 2-2. Instruction Manual 27

28 Chapter 2 UFM Device Set-Up Menus Description Table 2-2. Oven (UFM) Menu Menu Range Comments OVEN (UFM) This line is the menu title bar. Col.temp On/Off, C Press ON to display the actual and setpoint values. This value is the column initial temperature. Initial time min This parameter defines the time the column remains at the starting temperature after a programmed run has begun. Ramp 1 On/Off, C/min This is the temperature ramp rate in C/min to reach the final temperature. Press ON to enable a temperature ramp. Final temp C This parameter defines the temperature the column will reach at the end of the heating or cooling ramp. This line only appears if Ramp 1 is On. Final time 1 Ramp min, On/Off, C/min This parameter defines how long (in minutes) the column will maintain the final temperature of the ramp. After you program the first ramp, the menu adds the Ramp 2 parameter lines. If you do not want an additional ramp, leave this parameter set to OFF. To program the ramp, press ON. The Final temp and Final time lines for the ramp will be added to the menu. You can repeat this process to program up to three temperature ramps. Final temp C This parameter defines the temperature the column will reach at the end of the relevant ramp. Final time 2-3 Block Temp min, C, On, Off This parameter defines how long (in minutes) the oven will maintain the final temperature of the ramp. This parameter defines the temperature of the heating block. 28 Instruction Manual

29 Menus Description Chapter 2 UFM Device Set-Up UFM Calibration UFM Calibration Menu This paragraph describes the operations needed to perform the calibration of the UFM column temperature sensor. This operation must be carried out every time a new column is installed and when required by the system. UFM calibration is automatically verified every time the GC is powered on. Press CONFIG, then scroll to Oven and press ENTER to open the OVEN CONFIGURE menu. Scroll to UFM Calibration and press ENTER to open the UFM CALIBRATION menu, shown in Table 2-3: Table 2-3. UFM Calibration Menu Menu Comments Exit w/o calibrate To exit UFM Calibration menu without performing calibration Start calibration To start calibration Verify calibration To verify calibration when needed. Every time the GC is powered on the system performs automatically a Calibration Verify routine to check the UFM calibration status. No messages are displayed during this routine. At the end of the routine if calibration status is correct, the GC goes to READY condition. If not, you need manually perform a calibration verify selecting the relevant option in UFM calibration menu and following the instructions reported in How to Perform a Manual Calibration Verify operating sequence. CAUTION If calibration or verify calibration routine are not successfully passed, the system automatically turns off power supply to the column. This avoids to damage the column. A relevant status message will be displayed in the status window. Instruction Manual 29

30 Chapter 2 UFM Device Set-Up Set-Up Getting Started Set-Up Getting Started The set-up and the programming of the TRACE GC Ultra equipped with the UFM involve the following operations: Column Installation UFM Calibration Column Evaluation and Leak Check TRACE GC Ultra parameters programming. Column Oven (configuration and parameters programming). Injector (SSL/PTV) Detector (FID/FPD) Data system package installation. NOTE For further details about set-up, injector and detector parameters programming, refer to the relevant Chapters in the TRACE GC Ultra Operating Manual. 30 Instruction Manual

31 UFM Column Installation Chapter 2 UFM Device Set-Up UFM Column Installation The column is connected to the injector and detector base fittings located in the GC oven. The GC oven controller accurately controls the column temperature. 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 CONFIGURE OVEN menu as described in the operating sequence How to Configure Column Oven for UFM on page 32. To install the UFM column refer to the instructions reported in the following operating sequences in Chapter 5. How to Connect the UFM Column Module in S/SL - FID/FPD Configuration How to Connect the UFM Column Module in S/SL - MS Configuration How to Connect the UFM Column Module in PTV - FID/FPD Configuration System Power Up If you have not already done so, connect the power cord to the GC. Plug the power cord into the appropriate power outlet. The power switch is located on the back side of the GC. Flip the switch to the ON position. Instruction Manual 31

32 Chapter 2 UFM Device Set-Up Configure Column Oven for UFM Configure Column Oven for UFM Configure the column oven following the operating sequence reported below. OPERATING SEQUENCE How to Configure Column Oven for UFM Use this sequence to configure the column oven 1. Press CONFIG, then scroll to Oven and press ENTER. 2. Scroll to Auto prep run. Press ON to enable automatic prep run. Press OFF if you want the prep run to be activated by pressing the PREP RUN key. 3. Scroll to PR timeout and set the duration of the prep run timeout. 4. Scroll to Enable UFM and set YES. 5. Scroll to Ready delay and set the delay time before the GC enters the Ready to Inject condition. 6. Scroll to Equil time and set the UFM column temperature equilibration time. 7. Scroll to Max Temp (UFM) and set the maximum allowable UFM column temperature. 8. When required, scroll to UFM Calibration to perform the calibration of the UFM column heating element. For details refer to operating sequence How to Perform an UFM Calibration on page Instruction Manual

33 UFM Calibration Chapter 2 UFM Device Set-Up UFM Calibration This operation must be carried out every time a new column is installed and when required by the system. UFM calibration is automatically verified every time the GC is powered on. Perform UFM Calibration following the instructions reported in the How to Perform an UFM Calibration operating sequence. At the end of the routine if calibration status is correct, the GC goes to READY condition. If not, you need to perform manually a calibration verify selecting the relevant option in UFM calibration menu and following the instructions reported in How to Perform a Manual Calibration Verify operating sequence. OPERATING SEQUENCE How to Perform an UFM Calibration This operating sequence contains the instructions to perform an UFM calibration. Before operating, verify that the UFM device is correctly installed, the external power module is switched on, the GC oven door is properly closed and the carrier gas flow is turned on. To perform calibration operate as follows: 1. Press CONFIG, then scroll to Oven and press ENTER to open the OVEN CONFIGURE menu. 2. Scroll to UFM Calibration and press ENTER to open UFM Calibration menu:. UFM CALIBRATION Exit w/o calibrate Start calibration Verify calibration NOTE To exit UFM Calibration menu without performing calibration, scroll to Exit w/o calibrate and press ENTER. Instruction Manual 33

34 Chapter 2 UFM Device Set-Up UFM Calibration 3. Scroll to Start calibration and press ENTER. The calibration routine is automatically performed. The following message is displayed. UFM CALIBRATION This operation may take up to 10 min! 4. During the routine, you can only visualize the actual temperature values and the elapsed time of the routine. UFM CALIBRATION Oven temp (40) Column temp (40) Elapsed time 1.25 Use <Stop> to abort NOTE To abort calibration, press STOP. A relevant message will be displayed. 5. At the end of the routine the following message will be displayed if the operation was successful. UFM CALIBRATION COMPLETED SUCCESSFULLY In case of error, the following message and the relevant error code number will be displayed. UFM CALIBRATION Warning Calibration FAILED ERROR No X 34 Instruction Manual

35 UFM Calibration Chapter 2 UFM Device Set-Up For further details, refer to Calibration Routine Error Messages in Chapter 4. OPERATING SEQUENCE How to Perform a Manual Calibration Verify You need to manually verify the calibration when the GC does not go to Ready condition at the end of the verify calibration automatic routine performed at the GC power on. The GC cannot perform an automatic calibration verify at power on if one of the following conditions subsists: the oven door is open the carrier gas is off the UFM power supply is off To manually perform verify calibration routine operate as follows. 1. Press CONFIG, then scroll to Oven and press ENTER to open the OVEN CONFIGURE menu. 2. Scroll to UFM Calibration and press ENTER to open UFM Calibration menu:. UFM CALIBRATION Exit w/o calibrate Start calibration Verify calibration 3. Scroll to Verify calibration and press ENTER. The verify calibration routine is performed. 4. During the routine, you can only visualize the actual values of temperatures and the elapsed time of the routine. Instruction Manual 35

36 Chapter 2 UFM Device Set-Up UFM Calibration VERIFYING UFM Oven temp (40) Column temp (40) Elapsed time 1.25 Use <Stop> to abort NOTE To abort verify calibration, press STOP. A relevant message will be displayed. 5. At the end of the routine the following message will be displayed if the operation was successful. UFM CALIBRATION Calibration verified SUCCESSFULLY In case of failure, a relevant message will be displayed. UFM CALIBRATION Warning Verify FAILED Refer to Calibration Routine Error Messages WARNING! If Verify calibration failed, it is mandatory to perform a new calibration. 36 Instruction Manual

37 Column Evaluation and Leak Check Chapter 2 UFM Device Set-Up Column Evaluation and Leak Check The circular sequence Automatic Leak Check, Manual Check for Leaks - Column Evaluation - Automatic Leak Check is the key for minimizing troubles related to leaks. Automatic Leak Check When you perform an Automatic Leak Check, the GC measures the column flow with a true mass flow sensor and compares it to the calculated flow from the original column constant to see if the numbers match. The instrument assumes a gas leak exists if there is a difference between these numbers and notify you that the system is not leak tight. When the Automatic Leak Check highlights leaks you should perform a manual leak check, to determine the location of the leaks following the instructions reported in Chapter 8 of the TRACE GC Ultra Maintenance and Troubleshooting Manual. You should execute the Automatic Leak Check: once a day every time you have disconnected the gas lines for any reason (e.g. to clean or replace a component of the system or to install a new column). NOTE Only a previous Column Evaluation, performed in a condition of true tightness, can ensure the validity of the subsequent Automatic Leak Check responses. Perform the Automatic Leak Check following the instructions reported in How to Perform an Automatic (DPFC) Leak Check operating sequence on page 41. Column Evaluation For pressure controlled injectors (S/SL, OCI, PTV and PPKD in wide bore mode), the indirect column flow control by automatic pressure programming relies on the calculation and predetermination of a column constant. The column evaluation is an automatic measurement of the column resistance that determines the column constant. Instruction Manual 37

38 Chapter 2 UFM Device Set-Up Column Evaluation and Leak Check Once the leak has been removed and the tightness of the system is reasonably sure, you should perform the Column Evaluation automatic control and compare the response with the K Factor values reported in K-Factor Quick Reference card. If the value obtained does not agree with the one reported on the card, this means that the leaks have not been repaired. Performing the Column Evaluation is the necessary condition for the success of any subsequent Automatic Leak Check. Perform the Column Evaluation following the instructions reported in How to Perform a Column Evaluation operating sequence on page 39. CAUTION Before performing column evaluation and automatic leak check, the UFM calibration must be successfully carried out. 38 Instruction Manual

39 Column Evaluation and Leak Check Chapter 2 UFM Device Set-Up OPERATING SEQUENCE How to Perform a Column Evaluation To perform the column evaluation, the system uses the correlation between the pressure applied to the flow and the column temperatures. This operation must be carried out every time a new column is installed. Before performing the column evaluation, a manual leak test of the system must be carried out. CAUTION Before performing Column Evaluation, carry out the leak check following the instructions reported in the TRACE GC Ultra Maintenance and Troubleshooting Manual. The GC must not be performing a run and must be isothermally stable before you can perform a column evaluation. 1. Press COLUMN EVAL to open the following menu: EVALUATE COLUMN? Exit w/o evaluation Eval Right column 1 Eval Left column 1 1. This item appears if the relevant channel is present and configured. 2. Scroll to the Right or Left column to evaluate and press ENTER. The column evaluation is automatically performed. NOTE To exit Column Evaluation menu without performing column evaluation, scroll to Exit w/o evaluation and press ENTER. 3. During the routine, you can only visualize the actual values of oven temp, pressure and column flow. Instruction Manual 39

40 Chapter 2 UFM Device Set-Up Column Evaluation and Leak Check EVALUATING R/L COLUMN Oven temp (52) Pressure (21) Col. flow (08) Use <Stop> to abort NOTE To abort column evaluation, press STOP. A relevant message will be displayed. 4. After a few minutes, the following message will be displayed if the operation was successful. Compare the response with the K Factor values reported in the K Factor Quick Reference card according to the carrier gas used. R/L.COL.EVALUATION COMPLETED SUCCESSFULLY K If the value obtained does not agree with the one reported on the K Factor Quick Reference card, this means that leaks have not been repaired. CAUTION NOTE The K factor values reported on the K Factor Quick Reference card are expected K factors for columns of exact dimensions. The K factors produced by you may vary somewhat. Large variations from the chart however will indicate a plugged column (high K constant) or a leak in the system (low K constant). Performing the Column Evaluation is the necessary condition for the success of any subsequent Automatic Leak Check. 6. In case of error, the relevant error message will be displayed. 40 Instruction Manual

41 Column Evaluation and Leak Check Chapter 2 UFM Device Set-Up OPERATING SEQUENCE How to Perform an Automatic (DPFC) Leak Check After you install a column and perform a manual leak check (as described in the Maintenance and Troubleshooting Manual) and column evaluation, you can use the automatic leak check function any time in the future to check for leaks. 1. To start the leak check, press LEAK CHECK. The options you can select (Right column or Left column) depend on the configuration of your GC. LEAK CHECK COLUMN? Exit w/o Leak check Eval Right column 1 Eval Left column 1 1. This item appears if the relevant channel is present and configured. 2. Scroll to the desired channel and press ENTER to start. The channel selected is automatically pressurized with carrier gas and sealed to perform the leak check. NOTE To exit Leak Check menu without performing leak check, scroll to Exit w/o Leak check and press ENTER. 3. During the routine, you can only visualize the actual values of oven temp, pressure and column flow. R/L.COL. LEAK CHECK Oven temp (52) Pressure (21) Col. flow (08) Use <Stop> to abort NOTE To abort leak check, press STOP. A relevant message will be displayed. Instruction Manual 41

42 Chapter 2 UFM Device Set-Up Column Evaluation and Leak Check 4. After a few minutes, the following message will be displayed if the operation was successful. R/L.LEAK CHECK COMPLETED SUCCESSFULLY Leak check passed. If not, an error message is displayed and you must search for leaks, then repeat the leak check. 42 Instruction Manual

43 Parameters Programming Chapter 2 UFM Device Set-Up Parameters Programming Column Oven Parameters Programming Set-up a Single Ramp or Multiple Temperature Program following the operating sequences reported below. OPERATING SEQUENCE Setting Up a Single Ramp Temperature Program This program raises the initial UFM column temperature to a specified final temperature at a specified rate and maintains the final temperature for a specified time. 1. Press OVEN to open the OVEN (UFM) menu. 2. Scroll to Temp and enter the initial temperature. 3. Scroll to Initial time and enter the time you want the column to maintain the initial temperature. 4. Scroll to Ramp 1 and press ON. Enter the ramp rate in C/minute for the column to reach the ramp s Final temp. 5. Scroll to Final temp 1 and enter the final temperature for the ramp. 6. Scroll to Final time 1 and enter the time the column will maintain the Final temp. 7. Scroll to Block temp and enter the temperature of the heating block. 8. To end the single ramp program, Ramp 2 must be Off. Instruction Manual 43

44 Chapter 2 UFM Device Set-Up Parameters Programming OPERATING SEQUENCE Setting Up a Multiple Ramp Temperature Program This program raises the initial column temperature to a specified final temperature through up to three ramps, each having a specified ramp rate, time, and temperature. 1. Press OVEN to open the OVEN(UFM) menu. 2. Scroll to Temp and enter the initial temperature. 3. Scroll to Initial time and enter the time you want the column to maintain the initial temperature. 4. Scroll to Ramp 1 and press ON. Enter the ramp rate in C/minute for the column to reach the ramp s Final temp. 5. Scroll to Final temp 1 and enter the final temperature for the first ramp. 6. Scroll to Final time 1 and enter the time the column will maintain the Final temp. 7. Scroll to Ramp 2 and press ON. Enter the ramp rate for the second temperature ramp. 8. Scroll to Final temp 2 and enter the final temperature for the second ramp. 9. Scroll to Final time 2 and enter the time the column will maintain the Final temp. 10. To end the multiple ramp temperature program, leave Ramp 3 set to Off. To add additional oven ramps, repeat the steps 7 through Scroll to Block temp and enter the temperature of the heating block. 44 Instruction Manual

45 Parameters Programming Chapter 2 UFM Device Set-Up Split/Spliless Injector Parameters Programming Program the Split/Splitless (S/SL) parameters following the operating sequence reported below. For further information refer to Chapter 6 of the TRACE GC Ultra Operating Manual. OPERATING SEQUENCE Setting Up the Split/Splitless Injector To set up Split/Splitless injector the following sequential steps are required: Programming Carrier Gas Programming S/SL Inlet Before you begin programming verify that a column is correctly installed and the system is free of leaks then operate as follows: Programming Carrier Gas Before you begin this operation check that the carrier gas type is correct for the analysis. Refer to Chapter 5 of the TRACE GC Ultra Operating Manual. To program carrier gas, proceed as follows: 1. Press LEFT CARRIER or RIGHT CARRIER to open the LEFT CARRIER or RIGHT CARRIER menu. LEFT CARRIER Col. Flow < Pressure 40.6 Flow mode con flow 2. Scroll to Flow mode and press MODE/TYPE or ENTER. Instruction Manual 45

46 Chapter 2 UFM Device Set-Up Parameters Programming 3. Scroll to Constant flow and press ENTER. LEFT CARRIER FLOW MODE * Constant flow < Constant pressure Programmed flow Programmed pressure 4. In LEFT CARRIER menu scroll to Col. Flow and set the appropriate value. Programming S/SL Inlet 1. Press LEFT INLET or RIGHT INLET to open the relevant INLET menu. LEFT INLET (S/SL) Temp Pressure Mode: split< The Mode: menu item displays the current operating mode. 2. Press MODE/TYPE to open the INLET MODE submenu. XX INLET MODE * Split < Splitless Splitless w/surge 3. Scroll to the mode of interest and press ENTER. 4. Scroll to Temp and press ON or enter the appropriate injector temperature using the numeric keypad. 5. Scroll to Const sept purge? and press YES. 46 Instruction Manual

47 Parameters Programming Chapter 2 UFM Device Set-Up Programmable Temperature Vaporizing Injector Parameters Programming Program the Programmable Temperature Vaporizing (PTV) parameters following the operating sequence reported below. For further information refer to Chapter 12 of the TRACE GC Ultra Operating Manual. OPERATING SEQUENCE Setting Up the Programmable Temperature Vaporizing Injector To set up Programmable Temperature Vaporizing injector the following sequential steps are required: Programming Carrier Gas Programming PTV Inlet Before you begin programming verify that a column is correctly installed and the system is free of leaks then operate as follows: Programming Carrier Gas Before you begin this operation check that the carrier gas type is correct for the analysis. Refer to Chapter 5 of the TRACE GC Ultra Operating Manual. To program carrier gas, proceed as follows: 1. Press LEFT CARRIER or RIGHT CARRIER to open the LEFT CARRIER or RIGHT CARRIER menu. RIGHT CARRIER Col. Flow < Pressure 40.6 Flow mode con flow 2. Scroll to Flow mode and press MODE/TYPE or ENTER. Instruction Manual 47

48 Chapter 2 UFM Device Set-Up Parameters Programming 3. Scroll to Constant flow and press ENTER. RIGHT CARRIER FLOW MODE * Constant flow < Constant pressure Programmed flow Programmed pressure 4. In CARRIER menu scroll to Col. Flow and set the appropriate value. Programming PTV Inlet 1. Press LEFT INLET or RIGHT INLET to open the relevant INLET menu. RIGHT INLET (PTV) Temp Pressure Mode: xxxxx< The Mode: menu item displays the current operating mode. 2. Press MODE/TYPE to open the INLET MODE submenu. XX INLET MODE PTV split PTV splitless PTV solvent split * CT split < CT splitless CT splitless w/srg 3. Scroll up to the CT split mode is selected, then press ENTER. 4. Scroll to Temp and press ON or enter the appropriate injector temperature using the numeric keypad. 48 Instruction Manual

49 Parameters Programming Chapter 2 UFM Device Set-Up FID/FPD Detector Parameters Programming Program the FID/FPD parameters following the operating sequence reported below. For further details, refer to the Chapter 17 or 21 of the TRACE GC Ultra Operating Manual. OPERATING SEQUENCE Programming an FID/FPD WARNING! Before you begin this operating sequence, do the following: Verify that all detector gases are connected, a column is correctly installed, and the system is free of leaks. Check the oven temperature and injector temperature. Check the carrier gas flow depending on the capillary or packed column in use. Hydrogen is a potentially dangerous gas. Refer to Using Hydrogen on page 16 for safety information. 1. Press LEFT DETECT or RIGHT DETECT to open the DETECTOR menu. 2. Set the detector base body temperature. 3. Change the hydrogen flow rate, if desired, according to the analytical requirement. 4. Change the air flow rate, if desired, according to the analytical requirement. 5. Change the make-up gas flow rate, if desired. 6. In case of FPD scroll to high voltage mode? and set On if high voltage is required. 7. When the detector base body is at the set temperature, scroll to Flame and press ON. This turns on the air and hydrogen flows and initiates the ignition sequence. The signal increases after the ignition. A sudden baseline deflection Instruction Manual 49

50 Chapter 2 UFM Device Set-Up Parameters Programming indicates that the flame is lit inside the detector. After a few seconds, the baseline should stabilize to the standing current level of the system. TEMPUS TOF MS Parameters Programming Program the TEMPUS TOF MS Detector parameters following the instructions reported in the relevant Instruction Manual. 50 Instruction Manual

51 3 Analysis This chapter provides information to run analyses with your TRACE GC Ultra equipped with the UFM device. Chapter at a Glance Performing an Analysis...52 Operating Procedures How to Perform an Analysis...52 Instruction Manual 51

52 Chapter 3 Analysis Performing an Analysis Performing an Analysis Use the following sequence to inject a sample into a split/splitless (S/SL) or a programmable temperature vaporizing (PTV) injector. OPERATING SEQUENCE How to Perform an Analysis Before injection, do the following: Verify that an UFM column is correctly installed, the correct liner is in the injector, and the system is free of leaks. Verify that UFM Calibration has been performed successfully. Verify that you have the proper syringe for the technique you are using: 51 mm needle for split or PTV injection mm needle for splitless injection Parameters Setting 1. Use LEFT CARRIER or RIGHT CARRIER to display the appropriate Carrier Gas Control Table. Verify you operate in the required constant flow mode. If not, scroll to Flow mode, press MODE/TYPE to access the selection menu, then select the correct mode. LEFT CARRIER 1 Col.flow Pressure 200 Flow mode con flow < 1. These settings could also be for a right carrier. 52 Instruction Manual

53 Performing an Analysis Chapter 3 Analysis 2. Use OVEN to display the Column Oven (UFM) Control Table. Set the oven temperature and the Oven Program required. 3. Use LEFT INLET or RIGHT INLET to display the appropriate S/SL or PTV Injector Control Table, according to the UFM device configuration. Set the required temperature Temp setpoint. Verify you operate in the required inlet mode: Split for S/SL CT split for PTV OVEN (UFM) Temp Initial Time 0.10 Ramp Final temp 250 Final time < Ramp 2 Off Block temp If not, scroll to Mode, press MODE/TYPE to access the selection menu. Select the correct mode, then set the all others required setpoints. LEFT INLET (S/SL) 1 RIGHT INLET (PTV) Temp Temp Pressure 200 Pressure 200 Mode: Split Mode: CT Split Total flow (155.5) Total flow (155.5) Split flow < Split flow < Split ratio 300 Split ratio These settings could also be used for a left/right inlet. Instruction Manual 53

54 Chapter 3 Analysis Performing an Analysis 4. Use LEFT DETECTOR or RIGHT DETECTOR to display the appropriate Detector Control Table. Set the required temperature Base Temp and the detector gases H2, Air and Mkup required setpoints. LEFT DETECTOR (FID) 1 LEFT DETECTOR (FPD) 1 Flame Off Flame Off Base temp Base temp Signal pa (5.5) FPD temp Ign.thresh 2.0 Signal pa (1.4) Flameout retry Off High voltage mode? N H H Air Air Mkup N < Mkup N These settings could also be used for a right detector. 5. In case of FPD, scroll to High voltage mode? and press ON if high voltage is required. 6. Ignite the FID/FPD flame scrolling to Flame and pressing ON. 7. Use LEFT SIGNAL or RIGHT SIGNAL to display the appropriate Detector Signal Control Table. Observe the FID/FPD flame signal on the display. This is the flame-on background offset. Scroll to Range and set the electrometer amplifier input range required. LEFT SIGNAL 1 Output (1000) Offset 100 Auto zero? Y/N Range 10^(0..3) 0< Analog filter Off Baseline Comp Off 1. These settings could also be used for a right signal. 54 Instruction Manual

55 Performing an Analysis Chapter 3 Analysis Manual Injection 1. Press PREP RUN. Depending on the mode you have programmed, the TRACE GC Ultra will perform the following operations: When the gas saver function is programmed, PREP RUN ends the gas saver mode and resets the split flow to the flow used during injection. In splitless mode, PREP RUN closes the split valve and will close the septum purge valve as programmed. In surge splitless mode, PREP RUN initiates the surge pressure. 2. When the Ready to Inject LED is lit, insert the syringe into the injector, wait for approximately 2 seconds, inject the sample rapidly, and rapidly remove the syringe from the injector. (This is the Hot Empty Needle technique.) 3. Press START. The GC will complete the analysis as programmed. Injection Using an Autosampler Before you begin autosampler injection, ensure that you have programmed the autosampler method in the AUTOSAMPLER menu and the autosampler sequence in the SEQUENCE menu. 1. Press PREP RUN. Depending on the mode you have programmed, the TRACE GC Ultra will perform the following operations: When the gas saver function is programmed, PREP RUN ends the gas saver mode and resets the split flow to the analytical flow. In splitless mode, PREP RUN closes the split valve and will close the septum purge valve as programmed. In surge splitless mode, PREP RUN initiates the surge pressure. 2. Press SEQ CONTROL. 3. Scroll to Start Sequence and press ENTER or START. Instruction Manual 55

56 Chapter 3 Analysis Performing an Analysis The autosampler will inject the samples according to the programmed method and sequence. 56 Instruction Manual

57 4 Maintenance and Troubleshooting This chapter provides maintenance guidelines and troubleshooting suggestions for the UFM device. Chapter at a Glance Maintenance...58 Messages...59 Instruction Manual 57

58 Chapter 4 Maintenance and Troubleshooting Maintenance Maintenance This paragraph contains a suggested guidelines to periodically perform the maintenance of the TRACE GC Ultra equipped with the UFM device. Maintaining the UFM Device This device does not require ordinary maintenance. 58 Instruction Manual

59 Messages Chapter 4 Maintenance and Troubleshooting Messages This paragraph contains the list of messages that may be displayed before or during the calibration and verify calibration routines, and general error messages that may occur during the UFM runs. Calibration Routine Error Messages The possible error messages that may be displayed before or during the Calibration routine are reported in the following table. Table 4-1. Calibration Routine Error Messages Error Message Cause Remedy UFM CALIBRATION UFM Column must be pressurized for UFM calibration! UFM CALIBRATION UFM Power must be on for UFM calibration! UFM CALIBRATION Door must be closed for UFM calibration! UFM CALIBRATION Can t execute while GC is running! UFM CALIBRATION Warning, CALIBRATION aborted by USER! Carrier gas line is closed or carrier flow turned OFF The external Power Module is not properly connected or turned Off. The GC door is open. You are starting calibration while the GC is running. You have selected the option Use <Stop> to abort during the calibration routine. Open the carrier gas line on the cylinder. Turn the carrier flow ON. Verify the connection between the Power Module and the UFM control Card. Turn the module On by using the power switch located on the rear panel. Close the GC door. To perform calibration wait the end of the analytical cycle or stop the GC. To perform calibration again, select the option Start calibration in UFM Calibration menu. Instruction Manual 59

60 Chapter 4 Maintenance and Troubleshooting Messages Table 4-1. Calibration Routine Error Messages (Continued) Error Message Cause Remedy UFM CALIBRATION The calibration routine time has Make sure that: Warning, exceeded the limit of 10 - all the electrical connections CALIBRATION aborted minutes. have been properly carried out. for TIMEOUT! - the column is pressurized. - the external power module is turned on. Repeat the calibration. If the error persists, contact your Thermo Fisher Scientific customer support organization. UFM CALIBRATION Warning, CALIBRATION FAILED Error No X The calibration failed due to a failure expressed by Error No X where X is a number from 1 to 6. 1 = Resistance of the column temperature sensor is too low. 2 = Resistance of the column temperature sensor is too high. 3 = Resistance temperature coefficient is too low. 4 = Resistance temperature coefficient is too high. 5 = First calibration point out of range. 6 = Calibration points difference out of range. Contact your Thermo Fisher Scientific customer support organization. 60 Instruction Manual

61 Messages Chapter 4 Maintenance and Troubleshooting Calibration Verify Routine Error Messages The possible error messages that may be displayed before or during the Verify Calibration routine are reported in the following table. Table 4-2. Calibration Verify Routine Error Messages Error Message Cause Remedy UFM VERIFY UFM Column must be pressurized for UFM calibration! UFM VERIFY UFM Power must be on for UFM calibration! UFM VERIFY Door must be closed for verifying UFM! UFM VERIFY Can t execute while GC is running! UFM CALIBRATION Warning VERIFY aborted by USER! UFM CALIBRATION Warning VERIFY aborted for TIMEOUT! UFM CALIBRATION Warning CALIBRATION FAILED Carrier gas line is closed or carrier flow turned OFF The external Power Module is not properly connected or turned Off. The GC door is open. You are starting calibration while the GC is running. You have selected the option Use <Stop> to abort during the verify calibration routine. The verify calibration routine time has exceeded the limit of 2.5 minutes. Verify calibration failed. Open the carrier gas line on the cylinder. Turn the carrier flow ON. Verify the connection between the Power Module and the UFM control Card. Turn the module On by using the power switch located on the rear panel. Close the GC door. To perform calibration wait the end of the analytical cycle or stop the GC. To perform calibration again, select the option Verify calibration in UFM Calibration menu. Perform a new calibration. Perform a new calibration Instruction Manual 61

62 Chapter 4 Maintenance and Troubleshooting Messages General Messages The following table details messages that are displayed in case of Not Ready conditions. Table 4-3. General Messages Message Description Cause NOT RDY-Waiting for UFM Power The column is not powered. Turn the external power module On. UFM Column temp The column temperature is not at the setpoint. Wait that the temperature reaches the setpoint. UFM XLine1 temp The Xline1 temperature is not at the setpoint. UFM XLine2 temp The Xline2 temperature is not at the setpoint. UFM block temp The UFM block temperature is not at the setpoint. UFM uncalibrated The column is not calibrated. Perform the calibration. Alarm Messages The following table lists alarm messages that may be displayed in case of fault. WARNING! When one of the error listed occurs, contact your Thermo Fisher Scientific customer support organization. 62 Instruction Manual

63 Messages Chapter 4 Maintenance and Troubleshooting Table 4-4. Alarm Messages Message Description Cause NOT RDY-Waiting for Temperature Error UFM Column temp UFM XLine1 temp UFM XLine2 temp TEMPERATURE SHUTDOWN UFM is out of Control! TEMPERATURE SHUTDOWN UFM Column Temperature over limits TEMPERATURE SHUTDOWN UFM Transfer line 1 Temperature over limits TEMPERATURE SHUTDOWN UFM Transfer line 2 Temperature over limits Temperature error due to hardware faults. UFM system failure. UFM column temperature has exceeded the set temperature limit. UFM transfer line 1 temperature has exceeded the set temperature limit. UFM transfer line 1 temperature has exceeded the set temperature limit. Verify that external power module is turned on. Try to turn it off then on again. If the problem persists, contact your Thermo Fisher Scientific customer support organization. Contact your Thermo Fisher Scientific customer support organization. Instruction Manual 63

64 Chapter 4 Maintenance and Troubleshooting Messages 64 Instruction Manual

65 5 UFM Device Installation This chapter provides the instructions to properly install the UFM device on your TRACE GC Ultra. It also contains operating sequences to remove the device from your GC when normal gas chromatography conditions are required. Chapter at a Glance Introduction...66 Getting Started...66 S/SL - FID/FPD Configuration...68 S/SL - MS Configuration...94 PTV - FID/FPD Configuration UFM Device Removal Operating Sequences How to Install the UFM Device in S/SL - FID/FPD Configuration...68 How to Connect the UFM Column Module in S/SL - FID/FPD Configuration..89 How to Install the UFM Device in S/SL - MS Configuration...94 How to Connect the UFM Column Module in S/SL - MS Configuration How to Install the UFM Device in PTV - FID/FPD Configuration How to Connect the UFM Column Module in PTV - FID/FPD Configuration.147 Removing UFM Device Instruction Manual 65

66 Chapter 5 Introduction Introduction The most important components of the UFM device are the following: Heating Block UFM Control Card External Power Module UFM Standard Outfit Who Performs the Installation of the Device The UFM device is already installed and configured on your GC. If, for any reason (e.g. to operate in normal GC conditions) the device is not installed or it is necessary to remove it from your GC and reinstall it again when required, carefully adhere to the instructions reported in this chapter. WARNING! The PTV Backflush option, if present, must be removed, due to its interference with the installation of the UFM device in the configuration with the PTV injector. Getting Started This paragraph contains the instructions to install the UFM device on your GC. WARNING! The installation must be carried out only by Thermo Fisher Scientific authorized and trained technical personnel. Before starting, the following preliminary operations must be carried out: 1. Cool the oven and detector base body to room temperature. 2. Close the gas supplies. 3. Turn off the main power on the rear panel of the GC. 4. Disconnect the main power cable from the rear of the GC. 66 Instruction Manual

67 Getting Started Chapter 5 5. If installed, disconnect the conventional capillary column and remove the column support. Perform the sequential operations required to properly install UFM Device according to the detector in use (FID, FPD or TEMPUS TOF MS) following the instructions reported in the relevant operating sequences. How to Install the UFM Device in S/SL - FID/FPD Configuration How to Connect the UFM Column Module in S/SL - FID/FPD Configuration How to Install the UFM Device in S/SL - MS Configuration How to Connect the UFM Column Module in S/SL - MS Configuration How to Install the UFM Device in PTV - FID/FPD Configuration How to Connect the UFM Column Module in PTV - FID/FPD Configuration To remove the UFM device, refer to Removing UFM Device operating sequence. Instruction Manual 67

68 Chapter 5 S/SL - FID/FPD Configuration S/SL - FID/FPD Configuration OPERATING SEQUENCE How to Install the UFM Device in S/SL - FID/FPD Configuration To properly install the UFM device, the following sequential operations must be performed: Remove the top and right side panels of the GC. Prepare the injector and detector base fittings. Install the heating block inside the GC oven. Install the column block fixing bracket. Install the control card into the GC electronic compartment (control unit). Connect the external power module. Connection of the cables. Remount GC panels. Connect the column module. Power on the GC. Configure the UFM device. Material Needed 2-mm Allen wrench 3-mm Allen wrench 10-mm Wrench 11-mm Wrench 15-mm Wrench 17-mm Wrench 68 Instruction Manual

69 S/SL - FID/FPD Configuration Chapter 5 1. Injector and detector cassette 2. Column oven door 3. Upper cover 4. Right hand-side panel Figure 5-1. The TRACE GC Ultra Removing the GC Panels This operation allows to access the GC upper parts and the electronic compartment. Remove the GC Top Cover 1. Lift the detector cover off the GC top cover. 2. Open the oven door and unscrew the two top cover fastening screws. Instruction Manual 69

70 Chapter 5 S/SL - FID/FPD Configuration 3. Push the cover back about 1 cm and lift it up and off the GC. Remove the GC Right Side Panel Figure 5-2. TRACE GC Ultra Top Cover 1. Loosen and remove the screw that secures the right side panel to the right upper rear corner of the GC by using the 3-mm Allen wrench. Refer to Figure Slide the side panel towards the back of the GC and then tilt the top of the side panel outwards. Continue to slide the panel towards the rear of the GC. 70 Instruction Manual

71 S/SL - FID/FPD Configuration Chapter 5 3. Hold the side panel parallel to the GC, and pull the lower edge of the panel away from the GC Right Panel Securing Screw Figure 5-3. TRACE GC Ultra Rear Panel Preparing the Injector and Detector Base This operation allows to accomodate the injector and detector bases, located inside the GC oven, to accept the UFM device. Removing the Injector and Detector Base Fittings Referring to Figures 5-4 and 5-5, operate as follows. Detector Base Body Injector Base Retaining Nut for Terminal Fitting 2. Capillary Column Adapter Figure 5-4. Preparing the Injector and the Detector (1) Instruction Manual 71

72 Chapter 5 S/SL - FID/FPD Configuration 1. Use the 17-mm and 10-mm wrenches respectively to unscrew the retaining nut at the bottom of the injector and the capillary column adapter at the bottom of the detector. 2. From the injector side, remove the retaining nut, the terminal fitting for capillary column and the silver seal. 3. From the detector side, remove the capillary column adapter and the silver seal. 5 4 Detector Base Body Injector Base Retaining Nut for Terminal Fitting 2. Terminal Fitting for Capillary Column 3. Silver Seal 4. Capillary Column Adapter 5. Silver Seal Figure 5-5. Preparing the Injector and the Detector (2) Replacing the Injector and Detector Base Fittings Referring to Figures 5-6 and 5-7, operate as follows. 4. On the injector side, insert the same terminal fitting previously removed into the bottom of the injector base interposing a new silver seal, then fingertighten the special retaining nut until it starts to grip the injector base. 72 Instruction Manual

73 S/SL - FID/FPD Configuration Chapter 5 5. On the detector side, insert the special terminal fitting into the bottom of the detector base, then finger-tighten the special retaining nut until it starts to grip the detector base. Detector Base Body Injector Base Silver Seal for Injector Base 2. Terminal Fitting for Capillary Column 3. Retaining Nut for Injector/Detector Base 4. Silver Seal for Detector base 5. Terminal Fitting for Detector Base Figure 5-6. Preparing the Injector and the Detector (3) 6. Use the 15-mm wrench to tighten both special retaining nuts. Use no more pressure than necessary to obtain a good seal (1/4 or 1/2 turn). Detector Base Body Injector Base Figure 5-7. Preparing the Injector and the Detector (4) Instruction Manual 73

74 Chapter 5 S/SL - FID/FPD Configuration Installing the Heating Block This operation allows to properly install the heating block on the injector and detector bases, located inside the GC oven. Fixing the Heating Block Against the Oven Ceiling Referring to Figure 5-9, operate as follows: Detector Base Body Injector Base Heating Block 2. Mounting Plate 3. Mounting Plate Holes 4. Mounting Plate Fixing Screws 5. Heater Element and Temperature Sensor Cable Figure 5-8. Installing the Heating Block (1) 1. Place the heating block against the ceiling of the oven paying attention to insert the injector and detector base fittings into the corresponding two holes present on the top of the heating block. 2. Verify that the injector and detector base fittings easily protrude inside the two holes present on the mounting plate. If not, lightly loose the mounting plate fixing screws, then try again. 74 Instruction Manual

75 S/SL - FID/FPD Configuration Chapter 5 3. Firmly holding the heating block against the oven ceiling, fix the mounting plate to the injector and detector base retaining nuts tightening the two fixing screws by using the 3-mm Allen wrench as shown in Figure 5-9. NOTE Make sure there is no free space between the heating block and the oven ceiling, to avoid possible cold spots Detector Base Retaining Nut 2. Injector Base Retaining Nut Figure 5-9. Installing the Heating Block (2) 4. Finger-tighten the threaded locking rings until them start to grip the detector and the injector retaining nuts. Use the 11-mm wrench to slightly tighten the threaded locking rings Threaded Locking Rings Figure Installing the Heating Block (3) Instruction Manual 75

76 Chapter 5 S/SL - FID/FPD Configuration Guiding the Heating Block Cable out of the Oven On the internal part of the column oven several fixing points are present. Look for the appropriate hole that allows the insertion of the cable as shown in Figure The cable, coming from the heating block, must be guided across this hole. Injectors-Detectors Cassette 1 Before starting operate as follows: 1. Insertion Hole Oven Ceiling Figure Installing the Heating Block (4) 1. Remove the hole cap located behind the injectors/detectors cassette as shown in Figure After the hole cap remotion, the insertion hole is visible Cables Exit Hole 2. Hole Cap Figure Installing the Heating Block (5) 76 Instruction Manual

77 S/SL - FID/FPD Configuration Chapter 5 2. Inside the GC oven, guide the heating block cable through the insertion hole until the cable protrudes from the GC upper panel as shown in Figures 5-13 and Heating Block Cable 2. Cables Insertion Hole Figure Installing the Heating Block (6) Figure Installing the Heating Block (7) Installing the Column Fixing Bracket This operation allows to install the bracket that will be used to fix the column cage when it will be connected to the heating block. Instruction Manual 77

78 Chapter 5 S/SL - FID/FPD Configuration 1. Loosen the Allen screw 1 that secures the right tab of the oven heater baffle as shown in Figure Oven Heater Baffle Right Tab Securing Allen Screw Figure Oven Heater Baffle 2. Move the column block bracket until the bracket arm couples the Allen screw, previously loosened, that secures the right tab of the oven heater baffle as shown in Figure Bracket Arm 2. Right Tab Allen Screw Figure Installation of the Column Block Fixing Bracket 2 78 Instruction Manual

79 S/SL - FID/FPD Configuration Chapter 5 Installing the UFM Control Card The UFM control card must be installed into the proper expansion slot marked A, B or C located on the left part of the GC mother board in the electronic compartment. Refer to Figures 5-17 and NOTE In the case all the expansion slots are occupied, it is necessary to remove one of the three detector control cards currently installed and replace it with the UFM control card. C B A Slot cover plate 2. Cover plates fixing screw 3. Free slot A B C. Extension slot position Figure Extension Slots Top View 1. Loosen the fixing screw of the slot cover plate that corresponds to the selected A, B or C expansion slot on the mother board. Instruction Manual 79

80 Chapter 5 S/SL - FID/FPD Configuration Detector control card expansion Slots 2. Additional heat control jumpers 3. Mother board Figure Detector Control Card Expansion Slots 2. Verify that the jumper marked Jx, adjacent to the defined control card connector on the mother board, is positioned between the pins 1 and 2. Refer to the following table. Expansion slot A B C Corresponding Jumper J8 J7 J6 80 Instruction Manual

81 S/SL - FID/FPD Configuration Chapter 5 Jumper Positioning Pins 1-2 = additional heat control enabled Pins 2-3 = additional heat control not enabled WARNING! The jumper marked Jx must be positioned between the pins 1 and Plug the UFM control card into the selected expansion slot on the mother board. 4. Fix the control card by using the same screw previously removed at point Connect the 2-pin connector of the free cable placed on the GC basement to the connector marked P1 located on the UFM control card as shown in Figure This connection allows the UFM electronics to take control of the fan. Figure Fan Cable WARNING! If the fan control cable is not properly connected to the P1 connector of the UFM control module, the UFM device will not function correctly. Instruction Manual 81

82 Chapter 5 S/SL - FID/FPD Configuration The result of the operation is shown in the example of Figure 5-20, where the expansion slot C on the mother board has been selected to install the card. NOTE The UFM control card will be automatically recognized at the GC power on pin Port pin Port 3. 6-pin Connector Figure Installation of the UFM Control Card On the top of the UFM control card the following connecting ports are present. a 9-pin port for the connection between the UFM control card and the heating block installed inside the GC oven. a 15-pin port for the connections between the UFM control card and the column cage. a 6-pin connector for the connection between the UFM control card and the external power module. 82 Instruction Manual

83 S/SL - FID/FPD Configuration Chapter 5 Installing the External Power Module The external power module, shown in Figure 5-21, supplies power to the column and the transfer lines heater. The module should be placed near the GC V MAINS POWER SUPPLY 4 Front View Rear View 1. Power On LED 2. Power Supply Socket 3. Power Supply On/Off Switch 4. 6-pin Connector 5. Fuse Figure The External Power Module Electrical Specifications. Power Supply Input: Vac; 50/60 Hz; 250 W Output: 32 Vdc Fuses F6.3A IEC127/I (5 x 20 mm) Instruction Manual 83

84 Chapter 5 S/SL - FID/FPD Configuration Connecting the Cables This operation consists in the following steps: Guiding the Column Cable Inside the Oven Connecting the Column Cable to the UFM Control Card Connecting the Heating Block Cable to the UFM Control Card Connecting the Power Module Cables Guiding the Column Cable Inside the Oven The same hole shown in Figure 5-11 allows the insertion of the column cable into the GC oven to power the analytical column when installed. 1. Guide the column cable through the insertion hole until the cable protrudes inside the GC oven ceiling as shown in Figures 5-22 and Figure Insertion of the Column Cable (1) 84 Instruction Manual

85 S/SL - FID/FPD Configuration Chapter 5 Figure Insertion of the Column Cable (2) 2. Leave the column cable inside the oven. This cable will be connected to the column cage when installed as described in the Installing the UFM column operating sequence. Connecting the Column Cable to the UFM Control Card 3. Connect the 15-pin connector of the column cable to the column port located on the top of the UFM control card as shown in Figure Column Cable 2. Column Port Figure Connection of the Column Cable Instruction Manual 85

86 Chapter 5 S/SL - FID/FPD Configuration Connecting the Heating Block Cable to the UFM Control Card 4. Connect the cable coming from the heating block previously installed to the second piece of cable provided as shown in Figure Heating Block Cable (1 st segment) 2. Heating Block Cable (2 nd segment) Figure Heating Block Cables Connection 5. Connect the 9-pin connector of the second piece of the cable to the heating block port located on the top of the UFM control card as shown in Figure Heating Block Cable 2. Heating Block Port Figure Connection of the Heating Block Cable Assembly 86 Instruction Manual

87 S/SL - FID/FPD Configuration Chapter 5 Connecting the Power Module Cables 6. Using the connection cable provided, connect the 6-pin connector located on the top of the UFM control card, as shown in Figure 5-27, to the 6-pin connector located on the power module rear panel as shown in Figure Power Module Cable 2. Power Module Port Figure Connection of the Power Module Cable (1) Power Module Cable 2. Power Module Connector Figure Connection of the Power Module Cable (2) Instruction Manual 87

88 Chapter 5 S/SL - FID/FPD Configuration 7. Snap the cable into one of the cable slots on the GC as shown in Figure Figure Connection of the Power Module Cable (3) The result of the connecting cables operation is shown in Figure 5-30 Figure Result of the Cables Connections Reinstalling the GC panels This operation allows to reinstall the GC panels 1. Reinstall all the GC panels proceeding in the reverse order of their removal (refer to Removing the GC Panels on page 69). 88 Instruction Manual

89 S/SL - FID/FPD Configuration Chapter 5 OPERATING SEQUENCE How to Connect the UFM Column Module in S/SL - FID/FPD Configuration This sequence contains the instructions to properly connect the UFM capillary column in S/SL - FID/FPD configuration. Material Needed 6-mm wrench Referring to Figure 5-31 operate as follows Heater Block 2. Detector Base 3. Injector Base 4. Graphite Ferrules (just included) 5. Retaining Nuts 6. Column Cage Figure Column Installation (1) Instruction Manual 89

90 Chapter 5 S/SL - FID/FPD Configuration The column module is supplied with a graphite ferrule in each column terminal. The two column terminals protruding from the module are already pre-cut at the right length to fit correctly the S/SL inlet and the GC detector. The longer terminal must fit the GC detector and the shorter on the S/SL: Detector Injector 82 mm 40 mm Figure Column Ends 1. Insert the column ends into the detector and injector base simultaneously and slide the module up to the detector and injector base respectively. 2. Push the column as far as possible into the detector and injector base. 3. Finger-tighten the column retaining nuts until they starts to grip the column. Tighten the two nuts simultaneously (a little bit each one per time) in order to avoid to mount the cage awry. 4. Use the 6-mm wrench to tighten the retaining nuts as shown in Figure Use enough pressure to obtain a good seal, but don t overtighten (1/4 turn). 90 Instruction Manual

91 S/SL - FID/FPD Configuration Chapter 5 Figure Column Installation (2) 5. Mount the cover of the heating block inserting the fixing pin into the proper hole as shown in Figure Heater Block Cover 2. Fixing Pin 3. Fixing Hole Figure Column Installation (3) Instruction Manual 91

92 Chapter 5 S/SL - FID/FPD Configuration 6. Finger-tighten the fixing pin knob until the cover adheres to the heating block as shown in Figure Fixing Pin Knob Figure Column Installation (4) 7. Fix the column cage to the bracket arm previously mounted inserting the fixing pin provided through the column cage as shown in Figure For details refer to Installing the Column Fixing Bracket Fixing Pin 2. Bracket Arm Figure Column Installation (5) 8. Finger-tighten the fixing pin knob until the cage is properly secured. 92 Instruction Manual

93 S/SL - FID/FPD Configuration Chapter 5 9. Finally, plug the column cable connector into the column port located on the bottom of the column cage as shown in Figure Column Port 2. Column Cable Connector Powering on the GC 1. Open the gas supplies. Figure Column Installation (6) 2. Reconnect the mains power cord to the GC. 3. Turn on mains power. Configuring the UFM Device To configure the UFM device refer to How to Configure Column Oven for UFM in Chapter 1. Instruction Manual 93

94 Chapter 5 S/SL - MS Configuration S/SL - MS Configuration OPERATING SEQUENCE How to Install the UFM Device in S/SL - MS Configuration To properly install the UFM device, the following sequential operations must be performed: Remove the top and right side panels of the GC. Prepare the injector and detector transfer line. Install the heating block inside the GC oven. Install the control card into the GC electronic compartment (control unit). Connect the external power module. Connection of the cables. Remount GC panels. Connect the column module. Power on the GC. Configure the UFM device. Material Needed 2-mm Allen wrench 3-mm Allen wrench 7/16 wrench 15-mm wrench 17-mm wrench 94 Instruction Manual

95 S/SL - MS Configuration Chapter Injector and detector cassette 2. Column oven door 3. Upper cover 4. Right hand-side panel Figure The TRACE GC Ultra Removing the GC Panels This operation allows to access the GC upper parts and the electronic compartment. Remove the GC Top Cover 1. Lift the detector cover off the GC top cover. 2. Open the oven door and unscrew the two top cover fastening screws. 3. Push the cover back about 1 cm and lift it up and off the GC. Instruction Manual 95

96 Chapter 5 S/SL - MS Configuration Remove the GC Right Side Panel Figure TRACE GC Ultra Top Cover 1. Loosen and remove the screw that secures the right side panel to the right upper rear corner of the GC by using the 3-mm Allen wrench. Refer to Figure Slide the side panel towards the back of the GC and then tilt the top of the side panel outwards. Continue to slide the panel towards the rear of the GC. 3. Hold the side panel parallel to the GC, and pull the lower edge of the panel away from the GC. 96 Instruction Manual

97 S/SL - MS Configuration Chapter 5 1 Figure TRACE GC Ultra Rear Panel Preparing the Injector and Detector Transfer Line This operation allows to accomodate the inner tube and the injector base, located inside the GC oven, to accept the UFM device. Removing the Injector Base Fittings 1. Right Panel Securing Screw 1. Use the 17-mm wrench to unscrew the retaining nut at the bottom of the injector. 2. Remove the retaining nut, the terminal fitting for capillary column and the silver seal as shown in Figure Instruction Manual 97

98 Chapter 5 S/SL - MS Configuration Injector Base Injector Base Retaining nut for terminal fitting 2. Terminal Fitting for Capillary Column 3. Silver Seal Figure Preparing the Transfer Line and the Injector (1) Removing the Transfer Line Inner Tube 3. Use the 7/16 wrench to unscrew the completely the retaining nut that secures the inner tube to the GC interface. 4. Carefully withdraw the inner tube completely as shown in Figure Injector Base 1 MS Detector Transfer Line 1. Transfer Line Inner Tube Figure Preparing the Transfer Line and the Injector (2) 98 Instruction Manual

99 S/SL - MS Configuration Chapter 5 Replacing the Injector Base Fittings 5. Insert the elbow fitting provided into the bottom of the injector base interposing a new silver seal as shown in Figure Injector Base Elbow Fitting 2. Special Retaining Nut 3. Elbow Tube 4. Stainless Steel Washer 5. Silver Seal for Injector Base Figure Preparing the Transfer Line and the Injector (3) 6. Finger-tighten the special retaining nut until it starts to grip the injector base paying attention to keep the elbow tube parallel to the front wall of the GC oven as shown in Figure Figure Preparing the Transfer Line and the Injector (4) Instruction Manual 99

100 Chapter 5 S/SL - MS Configuration 7. Use the 15-mm wrench to tighten the special retaining nut. Use no more pressure than necessary to obtain a good seal (1/4 or 1/2 turn). Replacing the Transfer Line Inner Tube 8. Carefully insert the transfer line inner tube provided in the interface interposing the proper vespel ferrule and nut. 9. Push the inner tube back as far as it will go in the interface as shown in Figure Injector Base Inner Tube 2. Securing Nut 3. Inner Tube Terminal Fitting 4. Vespel Ferrule Figure Preparing the Transfer Line and the Injector (5) Finger-tighten the securing nut until it starts to grip the interface fitting verifying that the inner tube terminal fitting is at the same level of the elbow tube terminal fitting as shown in Figure If not, carefully push the MS back or back up against the GC, making sure the interface is not stressed by the GC oven wall. 100 Instruction Manual

101 S/SL - MS Configuration Chapter 5 Injector Base Figure Preparing the Transfer Line and the Injector (6) 10. Use the 15-mm wrench to tighten the special retaining nut. Use no more pressure than necessary to obtain a good seal (1/4 or 1/2 turn). Installing the Heating Block This operation allows to properly install the heating block on the injector and detector bases, located inside the GC oven. Before starting the following operations must be performed: Guiding the Heating Block Cable out of the Oven Guiding the Column Cable Inside the Oven Fixing the Heating Block Guiding the Heating Block Cable out of the Oven On the internal part of the column oven several fixing points are present. Look for the appropriate hole that allows the insertion of the cable as shown in Figure The cable, coming from the heating block, must be guided across this hole. Instruction Manual 101

102 Chapter 5 S/SL - MS Configuration Injectors-Detectors Cassette 1 1. Insertion Hole Oven Ceiling Figure Cable Insertion Hole 1. Remove the hole cap located behind the injectors/detectors cassette as shown in Figure After the hole cap remotion, the insertion hole is visible Cables Exit Hole 2. Hole Cap Figure Cable Insertion Hole (2) 2. Inside the GC oven, guide the heating block cable through the insertion hole until the cable protrudes from the GC upper panel as shown in Figures 5-49 and Instruction Manual

103 S/SL - MS Configuration Chapter 5 Injector Base MS Detector Transfer Line Heating Block Cable 2. Cables Insertion Hole 3. Heating Block Figure Heating Block Cable (1) Figure Heating Block Cable (2) Guiding the Column Cable Inside the Oven The same hole shown in Figure 5-51 allows the insertion of the column cable into the GC oven to supply the analytical column when installed. Instruction Manual 103

104 Chapter 5 S/SL - MS Configuration Column Cable 2. Cables Insertion Hole 3. Heating Block Cable Figure Insertion of the Column Cable 1. Guide the column cable through the insertion hole until the cable protrudes inside the GC oven ceiling as shown in Figures 5-51 and Injector Base 2 MS Detector Transfer Line 1 1. Column Cable 2. Cables Inserting Hole Figure Insertion of the Column Cable (2) 104 Instruction Manual

105 S/SL - MS Configuration Chapter 5 2. Leave the column cable inside the oven. This cable will be connected to the column cage when installed as described in the Installing the UFM column operating sequence. Fixing the Heating Block Referring to Figure 5-53, operate as follows: 1. Turn the heating block horizontally. 2. Insert the transfer line inner tube into the support chamber as shown in Figure Injector Base MS Detector Transfer Line Figure Installing the Heating Block (1) Instruction Manual 105

106 Chapter 5 S/SL - MS Configuration 3. Turn the heating block vertically against the elbow fitting, on the injector base, paying attention to correctly place the nut and the elbow tube inside the relevant slots as shown in Figure Figure Installing the Heating Block (2) 4. Holding the heating block in place, mount the cover block paying attention to properly insert the two guide pins into the relevant holes provided on the cover block. 5. Fix the cover block using the proper Allen screws as shown in Figure Instruction Manual

107 S/SL - MS Configuration Chapter Cover Block 2. Fixing Screws 3. Guide Pins Figure Installing the Heating Block (3) Instruction Manual 107

108 Chapter 5 S/SL - MS Configuration Installing the UFM Control Card The UFM control card must be installed into the proper expansion slot marked A, B or C located on the left part of the GC mother board in the electronic compartment. Refer to Figures 5-56 and NOTE In the case all the expansion slots are occupied, it is necessary to remove one of the three detector control cards currently installed and replace it with the UFM control card. C B A Slot cover plate 2. Cover plates fixing screw 3. Free slot A B C. Extension slot position Figure Extension Slots Top View 1. Loosen the fixing screw of the slot cover plate that corresponds to the selected A, B or C expansion slot on the mother board. 108 Instruction Manual

109 S/SL - MS Configuration Chapter Detector control card expansion Slots 2. Additional heat control jumpers 3. Mother board Figure Detector Control Card Expansion Slots 2. Verify that the jumper marked Jx, adjacent to the defined control card connector on the mother board, is positioned between the pins 1 and 2. Refer to the following table. Expansion slot A B C Corresponding Jumper J8 J7 J6 Instruction Manual 109

110 Chapter 5 S/SL - MS Configuration Jumper Positioning Pins 1-2 = additional heat control enabled Pins 2-3 = additional heat control not enabled WARNING! The jumper marked Jx must be positioned between the pins 1 and Plug the UFM control card into the selected expansion slot on the mother board. 4. Fix the control card by using the same screw previously removed at point Connect the 2-pin connector of the free cable placed on the GC basement to the connector marked P1 located on the UFM control card as shown in Figure This connection allows the UFM electronics to take control of the fan. Figure Fan Cable WARNING! If the fan control cable is not properly connected to the P1 connector of the UFM control module, the UFM device will not function correctly. 110 Instruction Manual

111 S/SL - MS Configuration Chapter 5 The result of the operation is shown in the example of Figure 5-59, where the expansion slot C on the mother board has been selected to install the card. NOTE The UFM control card will be automatically recognized at the GC power on pin Port pin Port 3. 6-pin Connector Figure Installation of the UFM Control Card On the top of the UFM control card are present the following connecting ports are present. a 9-pin port for the connection between the UFM control card and the heating block installed inside the GC oven. a 15-pin port for the connections between the UFM control card and the column cage. a 6-pin connector for the connection between the UFM control card and the external power module. Instruction Manual 111

112 Chapter 5 S/SL - MS Configuration Installing the External Power Module The external power module, shown in Figure 5-21, supplies power to the column and the transfer lines heaters. The module should be placed near the GC V MAINS POWER SUPPLY 4 Front View Rear View 1. Power On LED 2. Power Supply Socket 3. Power Supply On/Off Switch 4. 6-pin Connector 5. Fuse Figure The External Power Module Electrical Specifications. Power Supply Input: Vac; 50/60 Hz; 250 W Output: 32 Vdc Fuses F6.3A IEC127/I (5 x 20 mm) 112 Instruction Manual

113 S/SL - MS Configuration Chapter 5 Connecting the Cables This operation consists in the following steps: Connecting the Column Cable to the UFM Control Card Connecting the Heating Block Cable to the UFM Control Card Connecting the Power Module Cables Connecting the Column Cable to the UFM Control Card 6. Connect the 15-pin connector of the column cable to the column port located on the top of the UFM control card as shown in Figure Column Cable 2. Column Port Figure Connection of the Column Cable Instruction Manual 113

114 Chapter 5 S/SL - MS Configuration Connecting the Heating Block Cable to the UFM Control Card 7. Connect the cable coming from the heating block previously installed to the second piece of cable provided as shown in Figure Heating Block Cable (1 st segment) 2. Heating Block Cable (2 nd segment) Figure Heating Block Cables Connection 8. Connect the 9-pin connector of the second piece of the cable to the heating block port located on the top of the UFM control card as shown in Figure Heating Block Cable 2. Heating Block Port Figure Connection of the Heating Block Cable Assembly 114 Instruction Manual

115 S/SL - MS Configuration Chapter 5 Connecting the Power Module Cables 9. Using the connection cable provided, connect the 6-pin connector located on the top of the UFM control card, as shown in Figure 5-64, to the 6-pin connector located on the power module rear panel as shown in Figure Power Module Cable 2. Power Module Port Figure Connection of the Power Module Cable (1) Power Module Cable 2. Power Module Connector Figure Connection of the Power Module Cable (2) Instruction Manual 115

116 Chapter 5 S/SL - MS Configuration 10. Snap the cable into one of the cable slots on the GC as shown in Figure Figure Connection of the Power Module Cable (3) The result of the connecting cables operation is shown in Figure 5-67 Figure Result of the Cables Connections Reinstalling the GC panels This operation allows to reinstall the GC panels 1. Reinstall all the GC panels proceeding in the reverse order of their removal (refer to Removing the GC Panels on page 95). 116 Instruction Manual

117 S/SL - MS Configuration Chapter 5 OPERATING SEQUENCE How to Connect the UFM Column Module in S/SL - MS Configuration This sequence contains the instructions to properly connect the UFM capillary column in S/SL - TEMPUS TOF MS configuration. Material Needed Graphite Ferrule 6-mm wrench Referring to Figure 5-68 operate as follows Column Cage 2. Column Bracket 3. Column Ends 4. Transfer Line Inner Tube 5. Injector Elbow Fitting Figure Column Installation (1) Instruction Manual 117

118 Chapter 5 S/SL - MS Configuration The column module is provided with a graphite ferrule in each column terminal. The two column terminals protruding from the module are already pre-cut at the right length to fit correctly the S/SL inlet and the MS. The longer terminal must fit the MS and the shorter the S/SL. Detector Injector 212 mm 73 mm Figure Column Installation (2) 1. Guide the column cage to insert the longer column ends into the transfer line inner tube. When guiding the column cage pay attention to place it on the column bracket. 2. Guide the column cage to insert the shorter column end into the elbow fitting, on the injector base. WARNING! Insert the shorter end of the column into the elbow fitting very gently. While guiding the column end into the elbow fitting, pay attention not to break the column. Refer to the following Figure. 118 Instruction Manual

119 S/SL - MS Configuration Chapter 5 NO YES 3. Finger-tighten the column retaining nuts until they starts to grip the column. Tightening the two nuts simultaneously (a little bit each one per time) in order to avoid to mount the cage awry. 4. Push the column as far as possible into the inner tube and injector base. 5. Use the 6-mm wrench to tighten the retaining nuts as shown in Figure Use enough pressure to obtain a good seal, but don t overtighten (1/4 turn). Instruction Manual 119

120 Chapter 5 S/SL - MS Configuration Figure Column Installation (3) 6. Fix the column cage to the bracket arm inserting the fixing pin provided through the column cage as shown in Figure Instruction Manual

121 S/SL - MS Configuration Chapter Fixing Pin Figure Column Installation (4) 7. Mount the cover of the heating block inserting the fixing pin into the proper hole as shown in Figure Finger-tighten the fixing pin knob until the cover adheres to the heating block. Instruction Manual 121

122 Chapter 5 S/SL - MS Configuration Heating Block Cover 2. Fixing Pin Figure Column Installation (5) 9. Finally, plug the column cable connector into the column port located on the bottom of the column cage as shown in Figure Instruction Manual

123 S/SL - MS Configuration Chapter Column Port 2. Column Cable Connector Powering On the GC 1. Open the gas supplies. Figure Column Installation (6) 2. Reconnect the mains power cord to the GC. 3. Turn on mains power. Configuring the UFM Device To configure the UFM device refer to How to Configure Column Oven for UFM in Chapter 1. Instruction Manual 123

124 Chapter 5 PTV - FID/FPD Configuration PTV - FID/FPD Configuration OPERATING SEQUENCE How to Install the UFM Device in PTV - FID/FPD Configuration To properly install the UFM device, the following sequential operations must be performed: Remove the top and right side panels of the GC. Prepare the injector and detector base fittings. Install the heating block inside the GC oven. Install the column block fixing bracket. Install the control card into the GC electronic compartment (control unit). Connect the external power module. Connection of the cables. Remount GC panels. Connect the column module. Power on the GC. Configure the UFM device. Material Needed 2-mm Allen wrench 2.5-mm Allen wrench 3-mm Allen wrench 7-mm wrench 10-mm wrench 15-mm wrench 124 Instruction Manual

125 PTV - FID/FPD Configuration Chapter 5 1. Injector and detector cassette 2. Column oven door 3. Upper cover 4. Right hand-side panel Figure The TRACE GC Ultra Removing the GC Panels This operation allows to access the GC upper parts and the electronic compartment. Remove the GC Top Cover 1. Lift the detector cover off the GC top cover. 2. Open the oven door and unscrew the two top cover fastening screws. 3. Push the cover back about 1 cm and lift it up and off the GC. Instruction Manual 125

126 Chapter 5 PTV - FID/FPD Configuration Remove the GC Right Side Panel Figure TRACE GC Ultra Top Cover 1. Loosen and remove the screw that secures the right side panel to the right upper rear corner of the GC by using the 3-mm Allen wrench. Refer to Figure Slide the side panel towards the back of the GC and then tilt the top of the side panel outwards. Continue to slide the panel towards the rear of the GC. 3. Hold the side panel parallel to the GC, and pull the lower edge of the panel away from the GC. 126 Instruction Manual

127 PTV - FID/FPD Configuration Chapter Right Panel Securing Screw Figure TRACE GC Ultra Rear Panel Preparing the Injector and Detector Base This operation allows to accommodate the injector and detector bases, located inside the GC oven, to accept the UFM device. Removing the Injector and Detector Base Fittings Referring to Figures 5-77 and 5-78, operate as follows. Detector Base Body Injector Base Retaining Nut for Terminal Fitting 2. Capillary Column Adapter Figure Preparing the Injector and the Detector (1) Instruction Manual 127

128 Chapter 5 PTV - FID/FPD Configuration 1. Use the 7-mm and 10-mm wrenches respectively to unscrew the retaining nut at the bottom of the injector and the capillary column adapter at the bottom of the detector. 2. From the injector side, remove the retaining nut and the injector guide. 3. From the detector side, remove the capillary column adapter and the silver seal. 4 Detector Base Body Injector Base Retaining Nut for Terminal Fitting 2. Injector guide 3. Capillary Column Adapter 4. Silver Seal Figure Preparing the Injector and the Detector (2) Replacing the Injector and Detector Base Fittings Referring to Figures 5-79 and 5-80, operate as follows. 4. On the injector side, replace the current injector guide with the special injector guide provided. Do not rescrew the retaining nut for terminal fitting. 5. On the detector side, insert the special terminal fitting into the bottom of the detector base, then finger-tighten the special retaining nut until it starts to grip the detector base. 128 Instruction Manual

129 PTV - FID/FPD Configuration Chapter 5 Detector Base Body Injector Base Injector Guide 2. Silver Seal for Detector base 3. Terminal Fitting for Detector Base 4. Retaining Nut for Detector base Figure Preparing the Injector and the Detector (3) 6. Use the 15-mm wrench to tighten the retaining nut for detector base. Use no more pressure than necessary to obtain a good seal (1/4 or 1/2 turn). Detector Base Body Injector Base Figure Preparing the Injector and the Detector (4) Instruction Manual 129

130 Chapter 5 PTV - FID/FPD Configuration Installing the Heating Block This operation allows to properly install the heating block on the injector and detector bases, located inside the GC oven. Installing the Heating Block Supporting Disk Referring to Figure 5-81, operate as follows: Detector Base Body 1 Injector Base Free Hole 2. Supporting Disk 3. Expander Fixing Screw 4. Side Hole Figure Supporting Disk Installation (1) Insert the supporting disk provided into the free hole present on the oven ceiling near to the injector base as shown in the section A of Figure A 1. Supporting Disk 2. Oven Ceiling 3. Free Hole 4. Supporting Disk External Crown 5. Spring 6. Supporting Disk Expanding Screw B Figure Supporting Disk Installation (2) 130 Instruction Manual

131 PTV - FID/FPD Configuration Chapter 5 7. Pull-up the disk until its external crown touches the ceiling of the oven as shown in section B of Figure NOTE If the supporting disk does not entry into the hole, unscrew the expanding screw located on the bottom of the disk, then try again. 8. Turn the supporting disk until the side hole present on the disk is oriented towards the injector base and properly aligned as shown in Figure CAUTION The proper alignment of the side hole is fundamental for the correct prosecution of the UFM device installation. Detector Base Body Retaining Bracket Injector Base WRONG CORRECT Figure supporting Disk Installation (3) 9. Keeping the supporting disk in place, tighten the expanding screw by using the 2.5-mm Allen wrench as shown in Figure Detector Base Body Injector Base Figure Supporting Disk Installation (4) Instruction Manual 131

132 Chapter 5 PTV - FID/FPD Configuration Fixing the Heating Block Against the Oven Ceiling Referring to Figure 5-85, operate as follows: Detector Base Body 7 Injector Base Heating Block 2. Mounting Plate 3. Mounting Plate Holes 4. Mounting Plate Fixing Screw 5. Heater Element and Temperature Sensor Cable 6. Block Fixing Screw 7. Heater Block supporting disk Figure Installing the Heating Block (1) 1. Place the heating block against the ceiling of the oven paying attention to insert the injector and detector base fittings into the corresponding two holes present on the top of the heating block. 2. Verify that the injector and detector base fittings easily protrude inside the two holes present on the mounting plate. If not, lightly loose the mounting plate fixing screws, then try again. 3. Firmly holding the heating block against the oven ceiling, fix the mounting plate to the injector and detector base fittings tightening the two fixing screws by using the 3-mm Allen wrench as shown in Figure NOTE Make sure there is no free space between the heating block and the oven ceiling, to avoid possible cold spots. 132 Instruction Manual

133 PTV - FID/FPD Configuration Chapter Detector Base Fitting 2. Injector Base Fitting Figure Installing the Heating Block (2) Guiding the Heating Block Cable out of the Oven On the internal part of the column oven several fixing points are present. Look for the appropriate hole that allows the insertion of the cable as shown in Figure The cable, coming from the heating block, must be guided across this hole. Injectors-Detectors Cassette 1 1. Insertion Hole Oven Ceiling Before starting operate as follows: Figure Installing the Heating Block (3) Instruction Manual 133

134 Chapter 5 PTV - FID/FPD Configuration 1. Remove the hole cap located behind the injectors/detectors cassette as shown in Figure After the hole cap remotion, the insertion hole is visible Cables Exit Hole 2. Hole Cap Figure Installing the Heating Block (4) 2. Inside the GC oven, guide the heating block cable through the insertion hole until the cable protrudes from the GC upper panel as shown in Figures 5-88 and Heating Block Cable 2. Cables Insertion Hole Figure Installing the Heating Block (5) 134 Instruction Manual

135 PTV - FID/FPD Configuration Chapter 5 Figure Installing the Heating Block (6) Installing the Column Fixing Bracket This operation allows to install the bracket that will be used to fix the column cage when it will be connected to the heating block. 1. Loosen the Allen screw 1 that secures the right tab of the oven heater baffle as shown in Figure Oven Heater Baffle Right Tab Securing Allen Screw Figure Oven Heater Baffle Instruction Manual 135

136 Chapter 5 PTV - FID/FPD Configuration 2. Move the column block bracket until the bracket arm couples the Allen screw, previously loosened, that secures the right tab of the oven heater baffle as shown in Figure Bracket Arm 2. Right Tab Allen Screw Figure Installation of the Column Block Fixing Bracket Instruction Manual

137 PTV - FID/FPD Configuration Chapter 5 Installing the UFM Control Card The UFM control card must be installed into the proper expansion slot marked A, B or C located on the left part of the GC mother board in the electronic compartment. Refer to Figures 5-93 and NOTE In the case all the expansion slots are occupied, it is necessary to remove one of the three detector control cards currently installed and replace it with the UFM control card. C B A Slot cover plate 2. Cover plates fixing screw 3. Free slot A B C. Extension slot position Figure Extension Slots Top View 1. Loosen the fixing screw of the slot cover plate that corresponds to the selected A, B or C expansion slot on the mother board. Instruction Manual 137

138 Chapter 5 PTV - FID/FPD Configuration Detector control card expansion Slots 2. Additional heat control jumpers 3. Mother board Figure Detector Control Card Expansion Slots 2. Verify that the jumper marked Jx, adjacent to the defined control card connector on the mother board, is positioned between the pins 1 and 2. Refer to the following table. Expansion slot A B C Corresponding Jumper J8 J7 J6 138 Instruction Manual

139 PTV - FID/FPD Configuration Chapter 5 Jumper Positioning Pins 1-2 = additional heat control enabled Pins 2-3 = additional heat control not enabled WARNING! The jumper marked Jx must be positioned between the pins 1 and Plug the UFM control card into the selected expansion slot on the mother board. 4. Fix the control card by using the same screw previously removed at point Connect the 2-pin connector of the free cable placed on the GC basement to the connector marked P1 located on the UFM control card as shown in Figure This connection allows the UFM electronics to take control of the fan. Figure Fan Cable WARNING! If the fan control cable is not properly connected to the P1 connector of the UFM control module, the UFM device will not function correctly. Instruction Manual 139