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FOCUS GC Version For MSGas ChromatographInstruction ManualPN 317 094 27, Revision May 2007

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FOCUS™ GC Version for MS - Instruction ManualMay 2007 EditionPart Number 317 094 27© 2007 Thermo Fisher Scientific Inc All rights reserved.Printed in Italy

Published by Thermo Electron S.p.A., Strada Rivoltana, 20090 Rodano - Milan - ItalyTel: +39 02 95059355 Fax: +39 02 95059388

Printing History: First Edition, released September 2003Second Edition, released April 2004Third Edition, released June 2004Fourth Esdition, released January 2005Fifth Edition, released October 2005Sixth Edition, released May 2007

DisclaimerTechnical 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 FOCUS™ GC Version for MS 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.

TrademarksFOCUS™ GC 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.

Declaration
Manufacturer: Thermo Electron S.p.A.Thermo Electron S.p.A. is the manufacturer of the instrument described in this manual and, as such, is responsible for the instrument safety, reliability and performance only if:
• installation

• re-calibration

• changes and repairs

have been carried out by authorized personnel and if:

• the local installation complies with local law regulations

• the instrument is used according to the instructions provided and if its operation is only entrusted to qualified trained personnel

Thermo Electron S.p.A. is not liable for any damages derived from the non-compliance with the aforementioned recommendations.

Thermo Electron S.p.A.Strada Rivoltana20090 RODANO (MI)ITALY

FOCUS GC MS Version -Instruction Manual iii

iv FOCUS GC MS Version -Instruction Manual

Contents
About This Manual...............................................................................................................................xiii
Overview.................................................................................................................................xiiiConventions Used in This Manual........................................................................................... xvInstrument Markings and Symbols .......................................................................................xviiiUsing the FOCUS GC Version for MS Document Set ............................................................ xxClassification of the Instrument ..............................................................................................xxiTechnical Features ..................................................................................................................xxiSafety Information .................................................................................................................xxii

Use of Gases..............................................................................................................xxiiUsing Hydrogen ....................................................................................................................xxiii

Using the Hydrogen Sensor .....................................................................................xxivCleaning and Decontamination .............................................................................................xxiv

Chapter 1FOCUS GC Description .................................................................................................................... 25

Instrument Overview................................................................................................................ 26FOCUS GC Components ............................................................................................ 26

Pneumatic Compartment................................................................................ 26Analytical Unit............................................................................................... 26Electronic Compartment ................................................................................ 27Status Panel.................................................................................................... 27

Gas Control ................................................................................................................. 27Carrier Gas Control........................................................................................ 27

Column Oven .............................................................................................................. 28Injector ........................................................................................................................ 28Column........................................................................................................................ 28MS Detector ................................................................................................................ 29Instrument Automation ............................................................................................... 29

GC Parts Description................................................................................................................ 30Front Panel .................................................................................................................. 30

Column Oven ................................................................................................. 31Status Panel.................................................................................................... 31Electronic Compartment ................................................................................ 32

Rear Panel ................................................................................................................... 34Carrier Gas Inlet Port ..................................................................................... 35Electrical Connections ................................................................................... 35Oven Exhaust Vent ........................................................................................ 37

Top Panel .................................................................................................................... 37

FOCUS GC Version for MS - Instruction Manual v

Contents

GC Left Hand-side Panel............................................................................................ 38Virtual Keypad ........................................................................................................... 39

Chapter 2Gas Control ........................................................................................................................................41

Gas Supplies ............................................................................................................................ 42Carrier Gas Regulation ............................................................................................................ 44Carrier Gas Parameters ............................................................................................................ 45

Flow Mode Selection Group Box............................................................................... 46Constant Flow................................................................................................ 46Constant Pressure .......................................................................................... 46On/Off Check Box......................................................................................... 47Vacuum Compensation ................................................................................. 47

Gas Saver Selection Group Box ................................................................................. 48Enable Check Box ......................................................................................... 48Flow (ml/min)................................................................................................ 48Time (min)..................................................................................................... 48

Chapter 3Column Oven .....................................................................................................................................49

Column Oven Overview.......................................................................................................... 50Oven Safety ................................................................................................................ 51

Oven Parameters...................................................................................................................... 52Graph .......................................................................................................................... 53Ramps Group Box ...................................................................................................... 53

Arrow Keys ................................................................................................... 53Initial / Temp Text Box ................................................................................. 54Initial / Hold Time text box ........................................................................... 54Ramp / Rate Text Boxes................................................................................ 54Ramp / Temp Text Boxes.............................................................................. 54Ramp / Hold Time Text Boxes...................................................................... 54

Oven Group Box......................................................................................................... 54Max Temp Text Box ..................................................................................... 55PrepRun Timeout........................................................................................... 55Equilibration Time (min) text box................................................................. 55

vi FOCUS GC Version for MS - Instruction Manual

Contents

Chapter 4Split/Splitless Injector (S/SL) ........................................................................................................... 57

S/SL Overview......................................................................................................................... 58Septum ........................................................................................................................ 62Liners .......................................................................................................................... 62

Packed Columns............................................................................................. 64S/SL Injection Techniques ....................................................................................................... 67

Split Injection Technique ............................................................................................ 67Splitless Injection Technique ...................................................................................... 69

Refocusing the Sample .................................................................................. 71Flooding ......................................................................................................... 72

S/SL Inlet Parameters............................................................................................................... 73Mode List Box ............................................................................................................ 74

Split ................................................................................................................ 74Splitless .......................................................................................................... 74Splitless w/surge ............................................................................................ 74

Inlet Group Box .......................................................................................................... 74Temperature check box and text box ............................................................. 75Split Flow check box and text box................................................................. 75Split Ratio text box ........................................................................................ 75Splitless Time text box................................................................................... 75

Purge Group Box ........................................................................................................ 75Constant Septum Purge check box ................................................................ 76Stop Purge Time text box .............................................................................. 76

Surge Group Box ........................................................................................................ 76Surge Pressure................................................................................................ 76Surge Duration ............................................................................................... 76

Chapter 5Column .............................................................................................................................................. 77

Introduction .............................................................................................................................. 78Using Correct Fittings................................................................................................. 78

Column Ferrules............................................................................................. 78Retaining Nuts ............................................................................................... 78

Installation................................................................................................................................ 79Keeping Leaks Under Control ................................................................................................. 82

Column Evaluation ..................................................................................................... 82Identifying and Removing Leaks................................................................................ 82

FOCUS GC Version for MS - Instruction Manual vii

Contents

Expected K Factor ...................................................................................................... 85K Factor Tables .......................................................................................................... 85

Helium Carrier Gas Theoretical K Factor ..................................................... 86Nitrogen Carrier Gas Theoretical K Factor ................................................... 87Hydrogen Carrier Gas Theoretical K Factor ................................................. 88

Column Conditioning .............................................................................................................. 91

Chapter 6Getting Started ..................................................................................................................................93

Configuring the FOCUS GC ................................................................................................... 94Connections Group Box ................................................................................ 95Option Group Box ......................................................................................... 95

Use Roadmap-Home Page....................................................................................................... 96GC Status and Actual Values ..................................................................................... 96

Status Page..................................................................................................... 97Actual Values Page........................................................................................ 98

FOCUS GC Setup.................................................................................................................... 99Carrier Box .................................................................................................. 100Handshake Group Box ................................................................................ 100Valves Group Box ....................................................................................... 101Buttons......................................................................................................... 101

Focus GC Pull-up Menu ........................................................................................................ 102Method Editing ...................................................................................................................... 103Oven....................................................................................................................................... 104

Ramps Group Box .................................................................................................... 105Oven Group Box....................................................................................................... 106

Inlet SSL ................................................................................................................................ 108Mode List Box .......................................................................................................... 109Inlet Group Box........................................................................................................ 109Purge Group Box ...................................................................................................... 110Surge Group Box ...................................................................................................... 110

Carrier .................................................................................................................................... 114Flow Group Box ....................................................................................................... 115Gas Saver.................................................................................................................. 115

MS Transfer Line................................................................................................................... 117MS Transfer Line Group Box................................................................................... 117

Run Table............................................................................................................................... 118Time, Item, and Settings Group Box........................................................................ 119

viii FOCUS GC Version for MS - Instruction Manual

Contents

Initial Values Group Box .......................................................................................... 119Buttons ...................................................................................................................... 119Add/Edit Run-Time Event Screen ............................................................................ 120

Event Time Group Box................................................................................ 120Valve Event.................................................................................................. 120External Event Group Box........................................................................... 121

Virtual Keypad ....................................................................................................................... 122Description ................................................................................................................ 122

Display Panel ............................................................................................... 122GC Status LEDs........................................................................................... 122Action Keys ................................................................................................. 123Data Entry Keys........................................................................................... 123

Keypad Menu............................................................................................................ 123File Menu ..................................................................................................... 123Send Method to GC ..................................................................................... 123Close ............................................................................................................ 123

Valves Manual Activations .................................................................................................... 124Inlet SSL Valves Group Box .................................................................................... 124Valve Vents Group Box............................................................................................ 124

Instrument Start-up................................................................................................................. 125

Chapter 7Maintenance and Troubleshooting ................................................................................................. 127

Maintenance ........................................................................................................................... 128How To Perform Maintenance.................................................................................. 128Suggested Maintenance Schedule............................................................................. 128

Septa............................................................................................................. 128Ferrules and Seals ........................................................................................ 129Traps ............................................................................................................ 129Detector Unit................................................................................................ 129

Maintenance Schedule Table .................................................................................... 129Instrument Cleaning.................................................................................................. 130

Maintaining a SSL Injector .................................................................................................... 131When Replacing the Septum..................................................................................... 131When Cleaning or Replacing the Liner..................................................................... 131If the Glass Liner Breaks Inside the Injector ............................................................ 132

Troubleshooting ..................................................................................................................... 140Instrument Troubleshooting...................................................................................... 141

FOCUS GC Version for MS - Instruction Manual ix

Contents

Error Messages ...................................................................................................................... 142Guide to Solve Analytical Problems...................................................................................... 143

Chapter 8Use of the Virtual Keypad .................................................................................................................147

Overview................................................................................................................................ 148The Display............................................................................................................... 148The Display LEDs .................................................................................................... 149The FOCUS GC Virtual Keypad.............................................................................. 150

Parameters Entry ......................................................................................... 151Virtual Keypad Main Menu................................................................................................... 152

Oven.......................................................................................................................... 152Inlet........................................................................................................................... 153Carrier ....................................................................................................................... 153

How to Perform a Leak Check .................................................................... 154How to perform a Column Evaluation ........................................................ 155

Detector .................................................................................................................... 155Signal ........................................................................................................................ 155Autosampler.............................................................................................................. 155Others........................................................................................................................ 156

Time....................................................................................................................................... 157Valves .................................................................................................................................... 158Run Time Events ................................................................................................................... 159Run-Log................................................................................................................................. 160Configuration......................................................................................................................... 162

When to Configure ................................................................................................... 162Configuration Menu ................................................................................................. 162

Oven Configuration Menu........................................................................... 163Carrier Configuration Menu ........................................................................ 163Autosampler Configuration Menu............................................................... 164General Configuration Menu....................................................................... 164Keyboard & Display Configuration Menu .................................................. 164Handshake Configuration Menu.................................................................. 165Time Configuration Menu........................................................................... 166Valves Configuration Menu ........................................................................ 166

Info/Diagnostics..................................................................................................................... 167

x FOCUS GC Version for MS - Instruction Manual

Contents

Appendix ACustomer Communication................................................................................................................ 169

How To Contact Us................................................................................................................ 169Europe ....................................................................................................................... 169Africa, Asia and Oceania .......................................................................................... 171North, Central and South America............................................................................ 172Reader Survey ........................................................................................................... 173

Glossary ..............................................................................................................................................175

Index ....................................................................................................................................................181

FOCUS GC Version for MS - Instruction Manual xi

Contents

xii FOCUS GC Version for MS - Instruction Manual

About This Manual
Overview
This Instruction Manual contains descriptions of the features and components of the FOCUS GC Version for MS gas chromatograph. Inside, you will find all of the information necessary for routine operation of your GC, including operating sequences, sample injection techniques, and diagrams and descriptions of the major components.

Chapter 1, FOCUS GC Version for MS Description, provides a basic overview of the features and options of the FOCUS GC gas chromatograph in the version for MS. After each brief description of a FOCUS GC component, you will find references to chapters in this manual containing more detailed information.

Chapter 2, Gas Control, contains information on controlling and programming the carrier and detector gas flows to the FOCUS GC.

Chapter 3, Column Oven, describes the features of the FOCUS GC column oven.

Chapter 4, Split/Splitless Injector (S/SL), describes the Split/Splitless (S/SL) injector and contains operating sequences for the different split/splitless operating modes.

Chapter 5, Column, describes the analytical columns installed in the FOCUS GC oven. The column is the heart of the gas chromatograph where the separation takes place.

Chapter 6, Getting Started, This chapter contains instructions to configure, set operating parameters and control your FOCUS GC Version for MS through Xcalibur software. Instructions to start-up the instrument are also included.

Chapter 7, Maintenance and Troubleshooting, contains information and operating sequences to perform the necessary maintenance of the instrument and also information concerning troubleshooting in case of malfunctioning.

Chapter 8, Use of the Virtual Keypad, provides basic information about of the functions and menus of the FOCUS GC Version for MS virtual keypad.

FOCUS GC Version for MS - Instruction Manual xiii

About This Manual Overview

Appendix A, Customer Communication, contains contact information for Thermo Fisher Scientific offices worldwide. Use the Reader Survey in this section to give us feedback on this manual and help us improve the quality of our documentation.

The Glossary contains definitions of terms used in this manual. This 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.

xiv FOCUS GC Version for MS - Instruction Manual

Conventions Used in This Manual About This Manual

Conventions Used in This ManualThe following symbols and typographical conventions are used throughout this manual.

Bold Bold text indicates names of windows, dialog boxes, and fields.

Italic Italic indicates cross references, first references to important terms defined in the glossary, and special emphasis.

Monospace Monospace, or Courier, indicates filenames and filepaths or text the user should enter with the keyboard.

MonospaceBold

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 Bold, uppercase sans serif font indicates the name of a key on a keyboard or keypad, such as ENTER.

CAUTIONThis symbol alerts you to an action or sequence that, if performed improperly, could damage the instrument.

NOTEThis symbol alerts you to important information related to the text in the previous paragraph.

WARNING!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.

FOCUS GC Version for MS - Instruction Manual xv

About This Manual Conventions Used in This Manual

This symbol indicates danger from hazardous chemicals.

This symbol indicates danger from high temperature surfaces or substances.

This symbol indicates a fire hazard.

This symbol indicates an explosion hazard.

This symbol indicates a toxic hazard.

This symbol indicates the presence of flammable materials.

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.

xvi FOCUS GC Version for MS - Instruction Manual

Conventions Used in This Manual About This Manual

This symbol indicates the user must wear protective shoes when performing the sequence.

This symbol indicates the user must wear protective clothing when performing the sequence.

This symbol indicates the user must wear gloves when performing the sequence.

FOCUS GC Version for MS - Instruction Manual xvii

About This Manual Instrument Markings and Symbols

Instrument Markings and SymbolsThe following table explains the symbols used on Thermo Fisher Scientific instruments. Only a few of them are used on the FOCUS GC gas chromatograph.

Symbol DescriptionDirect Current

Alternating Current

Both direct and alternating current

Three-phase alternating current

Earth (ground) terminal

Protective conductor terminal

Frame or chassis terminal

Equipotentiality

On (Supply)

Off (Supply)

3

xviii FOCUS GC Version for MS - Instruction Manual

Instrument Markings and Symbols About This Manual

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 Equipments (WEEE) placed on the european market after August, 13, 2005.

Symbol Description

FOCUS GC Version for MS - Instruction Manual xix

About This Manual Using the FOCUS GC Version for MS Document Set

Using the FOCUS GC Version for MS Document Set

The FOCUS GC Version for MS Document Set (CD-Rom PN 317 095 35) includes all manuals in electronic format, and serves as your library for information about the FOCUS hardware and software. The FOCUS GC Version for MS Document Set (PN 317 094 30) 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 317 094 28)This manual and diskette describes how to set up a workspace for the FOCUS GC and how to connect the FOCUS GC to the gas supplies and peripheral devices.

Instruction Manual (PN 317 094 27)This manual provides descriptions of the FOCUS GC hardware and software and instructions for their use.

Spare Parts Catalog (PN 317 094 29)This catalog contains a list of spare parts for the FOCUS GC.

xx FOCUS GC Version for MS - Instruction Manual

Classification of the Instrument About This Manual

Classification of the InstrumentEnvironmental Conditions

• Internal use.

• Altitude up to 2000 meters.

• Temperature from 15 to 35 °C.

• Maximum relative humidity between 30% and 85%.

• Voltage variations not exceeding 10% of the nominal value.

• Transients according to installation categories II.

• Degree of pollution according to IEC 664 (3.7.3) 2.

Technical FeaturesThe following table summarizes the major technical features of the FOCUS GCFeatures Description

• External Interface

— RS232 Serial Line

• Power Supply

— 120 Vac; 50/60 Hz; 1600 VA

— 230 Vac; 50/60 Hz; 1600 VA

• Dimensions

— 680 x 640 x 440 mm (h x l x w)

• Mass

—About 30 kg

FOCUS GC Version for MS - Instruction Manual xxi

About This Manual Safety Information

Safety InformationWARNING! The instrument must be used according to the specifications of this guide. Improper

use can adversely affect the instrument protection. The analytical operation requiresthe use of chemical substances having different hazard specifications. Before usingchemicals, please read the hazard indications and information reported in the SafetySheet supplied by the manufacturer referring to the relevant CAS (ChemicalAbstract Service) number.

Use of Gases

WARNING! Before using gases, carefully read the hazard indications and information reportedin the Safety Sheet supplied by the manufacturer referring to the CAS (ChemicalAbstract Service) number. It is the user’s responsibility to see that all local safetyregulations for the use of gases are obeyed.

xxii FOCUS GC Version for MS - Instruction Manual

Using Hydrogen About This Manual

Using HydrogenThe 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 aconcentration 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.

• Perform a bubble test to ensure that the hydrogen lines are leak-tight before using the instrument. Perform this test after the pressure test described in the Testing for Leaks paragraph in FOCUS GC Site Preparation and Installa-tion Guide Manual. Repeat this test to eliminate all leaks.

• Ensure your GC column oven has a Thermo Fisher Scientific hydrogen sen-sor. A hydrogen sensor continuously monitors the hydrogen level in the GC column oven.

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 recommended Thermo Fisher Scientific sensor, 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 61010 regulations if local regulations do not exist.

FOCUS GC Version for MS - Instruction Manual xxiii

About This Manual Cleaning and Decontamination

Using the Hydrogen SensorThe lower limit of the hydrogen sensor is 0.5% in volume. You should adjust thedetection threshold to 1% in volume, which is 25% of the hydrogen lower limit ofexplosion (4% in volume). In cases where the connections begin to leak or the column breaks, the sensor alerts the operator. Then it 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:

• 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! Never use hydrogen in FOCUS GC unless your GC oven has a hydrogen sensorinstalled.

Thermo Fisher Scientific CSEs are not authorized to install or repair any instrumentusing hydrogen as a carrier gas unless the instrument is equipped with the appro-priate sensor.

Cleaning and DecontaminationNormal usage of the FOCUS GC can cause the exterior to get dirty. Clean the outer surfaces by wiping them with a cloth dampened with water.

In the event that a hazardous material is spilled on or in the instrument, clean the spill according to the procedures in the Material Safety Data Sheet for that substance.

xxiv FOCUS GC Version for MS - Instruction Manual

FOCUS GC Version for MS - Instruction Manual

1
FOCUS GC Version for MS Description
This chapter provides a basic overview of the features and options of the FOCUS GC Version for MS gas chromatograph. After each brief description of a FOCUS GC component, you will find references to chapters in this manual containing more detailed information.

Chapter at a Glance…Instrument Overview............................................................................................26GC Parts Description............................................................................................30

25

Chapter 1FOCUS GC Version for MS Description Instrument Overview

Instrument OverviewThe FOCUS GC Version for MS consists of four major components, as shown in Figure 1-1.

FOCUS GC Components

Figure 1-1. FOCUS GC Components

Pneumatic CompartmentThe pneumatic compartment contains the carrier gas control circuit. It is completely electronic (digital pneumatics).

Analytical UnitThe analytical unit consists of two subcompartments:

• the column oven

• the injector compartment

1. Pneumatic Compartment 3. Electronic Compartment2. Analytical Unit 4. Status Panel

1 1

3 3

2

4

26 FOCUS GC Version for MS - Instruction Manual

Chapter 1Instrument Overview FOCUS GC Version for MS Description

Electronic CompartmentThe electronic compartment consists of two subcompartments:

• the high-voltage compartment

• the low voltage compartment

Status PanelThe status panel make up the FOCUS GC Version for MS user interface.

Gas ControlThe GC is equipped with digital pneumatics for carrier gas control.

Carrier Gas ControlCarrier gas is controlled electronically through an electronic pneumatic control module Digital Pressure Flow Control (DPFC) mounted in the pneumatic compartment.

DPFC ModuleThe DPFC module features the following:

• constant pressure or constant flow operating modes

• inlet pressure control (in kPa, psi, or bar) and column flow rate control(in mL/min)

• split flow control (in mL/min)

• septum purge flow control (in mL/min)

The DPFC module also allows the following operations:

— Column EvaluationTo automatically calculate the column constant.

— Leak CheckTo keep the system under control.

FOCUS GC Version for MS - Instruction Manual 27

Chapter 1FOCUS GC Version for MS Description Instrument Overview

— Gas Saver FunctionTo reduce the split flow after an injection to avoid the waste of expensive gases.

Refer to...Chapter 2, Gas Control.

Column OvenThe FOCUS GC column oven has a high degree of thermal stability and fast heating and cooling. The air circulation in the oven ensures the column is kept in a thermally homogenous and stable zone. This provides more precise analytical performance and helps prevent chromatogram peak distortion.

Refer To…Chapter 3. Column Oven.

Injector FOCUS GC is designed to operate with the Split/Splitless (S/SL) injector.This injector minimizes heavy component discrimination with optimized sample transfer to the column. You can use capillary and wide-bore columns with the Split/Splitless injector. With the appropriate adapter kit, you can also use packed columns.

Refer to...Chapter 4, Split/Splitless Injector (S/SL)

ColumnThe column is where the chromatographic separation of the sample occurs. Several types of columns are available for different chromatographic applications.

Refer to…Chapter 5, Column


Chapter 1Instrument Overview FOCUS GC Version for MS Description

MS DetectorFOCUS GC is designed to be coupled with a DSQ Mass Detector.

Instrument AutomationFOCUS GC Version for MS is fully controlled by the computer through Xcalibur software that is also used for data handling and interpretation of the acquired results. Therefore the instrument is not provided with independent keyboard and display. On the instrument front there is a Status Panel where you can monitor the instrument status.


Chapter 1FOCUS GC Version for MS Description GC Parts Description

GC Parts DescriptionThis paragraph gives you a detailed description of the instrument components.

Front Panel

Figure 1-2. Front Panel

Front Panel comprises the following parts:

• Column Oven

• Status Panel

• Electronic Compartment

1. Column Oven Door 3. Status Panel2. Column Oven Door Push Button 4. Electronic Compartment

1 2

34


Chapter 1GC Parts Description FOCUS GC Version for MS Description

Column OvenThe column oven, shown in Figure 1-3, is accessible opening the column oven door by pushing the relevant button.

Figure 1-3. Column Oven Internal View

Refer To...Chapter 4, Column Oven

Status PanelStatus panel, shown in Figure 1-4, is the user interface of the GC. It consists of a series of four Status LEDs showing the instrument’s status.

Figure 1-4. Status Panel

Refer also to Virtual Keypad.

The LEDs (Light Emitting Diodes) on the left side of the display screen indicate the FOCUS GC’s operating status. The status LEDs indicate the current operating mode and special settings activated by the operator. Table 1-1 lists and explains each status LED.



Electronic CompartmentIt is located on the bottom part of the GC, and it is accessible only by authorized Thermo Fisher Scientific technical personnel.

WARNING! Before opening the electrical compartment, cut off power supply to the instrument and disconnect the power cord.The electronic compartment, shown in Figure 1-5, comprises:

• Low Voltage Section

• High Voltage Section

Table 1-1. Status LED DescriptionsLED Description

Not Ready/Error This LED lights when the GC is not ready to make a run, usually because the specified oven temperature has not been reached. It remains lit if any additional equilibration time has been configured. It blinks when the GC has one or more error conditions.

Standby/Prep Run This LED lights when the GC is in Standby, waiting to be advanced to the Ready status. It blinks links while the GC prepares for a run, for example, while opening or closing valves as required by the method.

Ready to Inject This LED lights when the prep run has finished, indicating you can inject a sample or start an autosampler.

Run This LED lights when a run is in progress.



Figure 1-5. Electronic Compartment

Low Voltage SectionIt contains the electronic circuits to operate and control the instrument.

WARNING! A Li 3 V; 220 mA/h unrechargeable battery is present on the Main Board. The battery replacement must be performed only by specialized technical personnel.

High Voltage SectionIt contains the power circuits. The configuration of the instrument 120 or 230 Vac power supply is determined by the position of the voltage selector, factory set, located on the Main Board. According to the instrument power supply configuration, the breaker ON/OFF main switch changes as follows:

The high voltage section is provided with a series of protection fuses as reported in the following table:

Power Supply Breaker120 Vac 15A230 Vac 7A



Rear PanelThe Rear Panel is shown in Figure 13.

Figure 1-6. Rear Panel

Fuse Type ProtectionF1 F2A; IEC 127/I; (5 x 20 mm) Injector heater elementF2 F1A; IEC 127/I; (5 x 20 mm) 230 Vac Main power (Breaker)

120 Vac Main power (Breaker)F3 F2A; IEC 127/I; (5 x 20 mm) Auxiliary heater elementF4 F0.63A; IEC 127/I; (5 x 20 mm) Oven fan motorF5 F0.63A; IEC 127/I; (5 x 20 mm) Oven fan motor

1. Gas Inlet Port 3. Oven Exhaust Vent Area2. Electrical connections

1

3

2



Rear Panel comprises the following parts:

• Carrier Gas inlet port

• Electrical Connections

• Oven Exhaust Vent

Carrier Gas Inlet PortIt is located on the middle upper part of the instrument rear panel. Gas inlet port is directly connected to the DPFC module.

WARNING! Gas pressure must be controlled on the gauges provided on the gas tank of the supply gas line. The maximum inlet pressure is 1000 kPa (120 psi) to allow DPFC module to adjust pressure up to 1000 kPa.Commonly used gases are helium, hydrogen and nitrogen.

The default pressure unit is the kilopascal (kPa). You specify the pressure units in the Configuration menu. Refer to Configuring the Carrier Gas in Chapter 2.

The following gives a brief conversion guide for the most commonly used pressure units in gas chromatography.

100 kPa = 1 bar = 14.51 psi

Electrical ConnectionsElectrical connections al located on the rear part of the electronic compartment. As shown in Figure 1-7.

To Convert To Multiply bykPa bar 0.01

psi 0.145bar kPa 100

psi 14.51psi kPa 6.89

bar 0.0689



Figure 1-7. Electrical Connections

1. Breaker marked POWER to switch the instrument On/Off

• Position I = instrument ON

• Position O = instrument OFF

2. 120 or 230 Vac 50/60 Hz Main socket marked

3. 9-pin connector marked AUTOSAMPLER Not Used. Autosampler must be connected directly to PC.

4. 9-pin connector marked COMPUTER to dialog with the computer via RS232 serial line.

5. 15-pin connector marked TIMED EVENTS to automatically drive up to external valves.

6. 6-pin connector marked SAMPLER SIGNALS for the autosampler Start/Stop signals. It can be used also for an optional remote Start button when an autosampler is not used.

7. 8-pin connection marked GENERIC HANDSHAKE to cooperate with the Mass Detector during analysis.

8. 4-pin connection marked SIGNAL 0–1V-10V-GND for the detector analog signal output

OO

II

SIGNAL

TIMED EVENTS

GENERICHANDSHAKE

SAMPLER SIGNAL

AUTOSAMPLER

COMPUTER

POWER

ON

OFF

1 2 6 7 8 4

5 3



Oven Exhaust VentHot air [350°C (660°F)] exits through this vent during GC operation.Any material exposed to the oven exhaust must be able to withstand repeated exposure to temperatures of up to 350°C (660 °F).

WARNING! Oven exhaust vent can cause severe burns. Avoid working behind the instrument when the oven vents during cooling-down cycles. Do not expose gas tanks or bottles, chemicals, regulators, electrical cords, or other temperature-sensitive items to oven exhaust.

Top PanelTop panel is shown in Figure 1-8.

Figure 1-8. Rear Panel

Top Panel comprises the following parts:

• Injector port

• Split and Purge vents

For details refer to Chapter Split/Splitless Injector (S/SL)

1. Injector Port Split and Purge Vents

1

2



GC Left Hand-side PanelIt is shown in Figure 1-9.

Figure 1-9. GC Left Hand-side Internal View

It is provided with:

• a hole to allow the insertion of the mass detector transfer line inside the GC column oven

• a connection for the transfer line heater

The insulating material covering the hole must be removed before inserting the detector transfer line.

1. Detector Transfer Line Insertion Hole 2. Transfer Line Heater Connection

1

2



Virtual KeypadFigure 1-10 illustrates the virtual keypad for FOCUS GC available only by Xcalibur software.

Virtual keypad has three components:

• a line-line display

• display LEDs showing the instrument’s status

• a keypad for data entry.

Figure 1-10. User Interface

For detailed information about the Virtual Keypad refer to Chapter 8



2
Gas Control
This chapter contains information on controlling and programming the carrier gas flow to the FOCUS GC.

Chapter at a Glance…Gas Supplies .........................................................................................................42Carrier Gas Regulation .........................................................................................44Carrier Gas Parameters.........................................................................................45

Operating SequencesConfiguring the Carrier Gas .................................................................................43Configuring the Pressure Unit ..............................................................................43

41

Chapter 2Gas Control Gas Supplies

Gas SuppliesCommonly used carrier gas is helium, however FOCUS GC can be configured to use also nitrogen or hydrogen. You can specify the type of gas and pressure units the FOCUS GC displays.

• The default carrier gas is Helium (He)

• The default pressure unit is the kilo pascal (kPa).

WARNING! Hydrogen is a dangerous gas that, when mixed with air, may create an explosive mixture. The use of hydrogen as a carrier gas requires the operator’s extreme caution. Special precautions must be taken because of the risk of explosion. The gas chromatograph must be equipped with a hydrogen sensor if you use hydrogen as a carrier gas. Refer to Using Hydrogen for more information. All Thermo Fisher Scientific gas chromatographs are designed to use an inert gas as the carrier gas. If you wish to use hydrogen as a carrier gas, you must install a hydrogen sensor. Contact a Thermo Fisher Scientific sales representative if you plan to use hydrogen as the carrier gas in FOCUS GC. If you don’t have the hydrogen sensor, you must use an inert carrier gas.You specify the pressure units and the type of carrier gas in Configuration menu operating as described in the following Operating Sequences


Chapter 2Gas Supplies Gas Control

OPERATING SEQUENCEConfiguring the Carrier Gas

Carrier gas is already configured to Helium. To change the configuration, proceed as follows:

In Xcalibur FOCUS GC Setup page set the gas type required as carrier gas.

OPERATING SEQUENCEConfiguring the Pressure Unit

The Pressure Unit is already configured to kPa (kilo pascal). To change the configuration, use the virtual keypad as described in chapter 8 Use of the Virtual Keypad.

Once the pressure unit is selected, you must change also the Xcalibur configuration as follows:

In Xcalibur FOCUS GC Configuration page set the pressure unit required.


Chapter 2Gas Control Carrier Gas Regulation

Carrier Gas RegulationThis paragraph describes the automatic Digital Pressure and Flow Control (DPFC) of the FOCUS GC. You control the gas flow by programming parameters in the Carrier gas page. See Carrier Gas Parameters.

The DPFC module, provides:

• Flow and pressure control for the S/SL injector

• Gas saver mode

The DPFC module pneumatic circuit is represented in Figure 2-1.

Figure 2-1. DPFC Module

1. Flow Sensor 1 2. Proportional Valve 13. Pressure Sensor 4. Fixed Flow Regulator 5 mL/min5. On/Off Valve 1 6. Flow Sensor 27. Proportional Valve 2 8 Trap9. On/Off Valve 2 A: Carrier Gas InletB. Septum Purge Line C: Split Line

3

5

2

96 7 8C

B

A1

4


Chapter 2Carrier Gas Parameters Gas Control

Carrier Gas ParametersThe carrier is the gas used as mobile phase in gas chromatography. The carrier gas carries the analyte mixture through the GC column, where it is separated into its individual components. The carrier gas flows through the GC column at a specific rate, measured either as a linear velocity (cm/sec) or as a flow rate (mL/min).

Carrier page is accessible from the Roadmap-Home Page by clicking the icon. The instrument Setup dialog windows displays all configuration tabs.

Figure 2-2. Carrier Gas Page


Chapter 2Gas Control Carrier Gas Parameters

This page contains two group boxes:

• Flow Mode Selection Group Box

• Gas Saver Selection Group Box

Flow Mode Selection Group BoxThe controls you see on this page are dependent on the flow mode selection. Please select one of the following modes and jump to that topic for detailed information.

Two flow modes are available.

Constant FlowIn constant flow mode, the column flow is kept constant throughout the analysis. The pressure at the column head will change with the column temperature to maintain a consistent flow.

Constant PressureIn constant pressure mode, the pressure at the column head is kept constant throughout the analysis.

According to the carrier gas mode selected, the Flow List Box may visualize: Flow or Pressure.


Chapter 2Carrier Gas Parameters Gas Control

• Flow (ml/min)Enter a column flow for the analytical column.

• Pressure (kPa)Enter the inlet pressure for the analytical run

On/Off Check BoxCheck this box to enable flow (or pressure) to the inlet.When unchecked, the flow (or pressure) is cut off to the inlet

Vacuum Compensation

Check this box to compensate for a vacuum at the end of the analytical column. This is usually the case when the detector is a mass spectrometer. If the box is not checked, calculations are made for a normal GC detector, which is usually at atmospheric or slightly higher pressure.


Chapter 2Gas Control Carrier Gas Parameters

Gas Saver Selection Group Box

This group box contains gas saver controls, which reduce carrier gas consumption, especially when a large split flow is used.

Enable Check BoxCheck this box to activate the gas saver (Flow, Time).

Flow (ml/min)It is the value which the split flow is reduced after the injection for gas saving. This value is also maintained while the GC is in stand-by condition.

Time (min)The time after the injection when gas saver flow will be activated.



3
Column Oven
This chapter describes the features of the FOCUS GC column oven.

Chapter at a Glance…Column Oven Overview.......................................................................................50Oven Parameters...................................................................................................52

49

Chapter 3Column Oven Column Oven Overview

Column Oven OverviewThe FOCUS GC column oven, shown in Figure 3-1, provides a stable heating environment for the analytical column. The oven heats and cools quickly. Efficient air circulation ensures a high degree of thermal stability.

Figure 3-1. The Column Oven

Opening the oven door activates a safety microswitch, which automatically switches off the oven heating and the motor for the air circulation fans. Resistor elements powered by a circuit located within the GC control unit heats the oven. The oven temperature is monitored by a PT 100 platinum wire sensor and controlled by the GC control unit.

The column oven has the following capabilities:

• maximum temperature of 350 °C

• maximum temperature increase rate of 120 °C/min

• seven linear temperature ramps and eight levels

• minimum operating temperature of a few degrees above ambient, which is obtained by two modulated cooling flaps controlled by the GC, schematically shown in Figure 3-2.


Chapter 3Column Oven Overview Column Oven

• temperature control through

— Heater control

— Fine control of hot air exhaust

— Ambient air intake

• Usable space

— Width about 230 mm

— Height about 230 mm

— Depth about 150 mm

Figure 3-2. Oven Air Circulation

Oven SafetyOpening the oven door cuts off the power to the oven heater and fan. The setpoints are kept in memory. To return to normal operation, close the oven door.

WARNING! The oven vents at the rear of the GC discharge hot air during cooling.

1. Oven 2. Fan3. Air 4. Cooling Flaps


Chapter 3Column Oven Oven Parameters

Hydrogen is a potentially dangerous gas. When hydrogen is used as a carrier gas, the column oven must have a hydrogen sensor. Refer to Using Hydrogen for hydrogen safety information.

Oven ParametersThis page is the method editor for setting up parameters in the GC run. Oven page provides you full control of the GC

Oven page is accessible from the Roadmap-Home Page by clicking the icon.The instrument Setup dialog windows displays all configuration tabs.Controls are for running complex temperature programs (with up to seven levels of ramps) and controlling post run events.

Figure 3-3. Oven Page


Chapter 3Oven Parameters Column Oven

This page contains three selection boxes

• Graph

• Ramps Group Box

• Oven Group Box

GraphThe graph display a graphical representations of the oven temperature program including any post run events. The axes are temperature in degrees centigrade and time in minutes. An isothermal run just gives a flat line

Ramps Group BoxRamps controls allows to add or delete temperature ramps for the oven temperature program

Arrow KeysUse the up-down control to add or subtract the number of ramps to use in the oven temperature program. This is the rate in degrees Centigrade per minute the GC oven is ramped up or down from the initial temperature or the previous level’s final ramp temperature. Clicking on the Down arrow automatically adds a ramp level after the last one listed. Clicking on the Up arrow deletes the highest level or the one being displayed on the bottom



Initial / Temp Text BoxThe initial temperature the oven is set at the beginning of the temperature program. For isothermal runs, this is the oven temperature for the entire run. After Preready or Prep Run this is the temperature the oven will be at.

Initial / Hold Time text boxThe amount of time to maintain the initial temperature.

Ramp / Rate Text BoxesThe rate of change of the temperature when increasing it from one value to the next. Described in degrees Celsius per minute (°C/min). The ramp begins at the previous step’s final temperature value and proceeds to the current step’s final temperature at the specified rate.

Ramp / Temp Text BoxesThe temperature the oven is set at for the next ramp of the temperature program. For isothermal runs, this is the oven temperature for the run. After Prep Run this is the temperature the oven will be at.

Ramp / Hold Time Text BoxesThe time to maintain the temperature specified in the Final Value control box.

Oven Group BoxThis group box allows you to control the following functions:


Chapter 3Oven Parameters Column Oven

Max Temp Text BoxSpecify the maximum temperature for this run. The GC has a maximum temperature of 350°. The maximum allowable temperature for the column being used in the method is automatically set.

PrepRun TimeoutSpecify how long the GC should remain in the Ready to Inject mode before returning to Stand By. If the START button is not pressed within the prep run timeout period, then the GC will return to Stand By mode. This feature is a protective measure to keep the GC from being in the Ready to Inject mode too long. For example, this will prevent accumulation of contaminants on the analytical column when doing splitless injections.

Equilibration Time (min) text boxSpecify how much time the GC should wait after the initial conditions are met before going to standby.



4
Split/Splitless Injector (S/SL)
This chapter describes the Split/Splitless (S/SL) injector and contains operating sequences for the different split/splitless operating modes.

Chapter at a Glance…S/SL Overview .....................................................................................................58S/SL Injection Techniques....................................................................................67S/SL Inlet Parameters ...........................................................................................73

Operating SequencesInstalling a Liner and a Septum............................................................................65

57

Chapter 4Split/Splitless Injector (S/SL) S/SL Overview

S/SL OverviewThe S/SL injector, shown in Figure 4-1, is optimized for either split or splitless applications to ensure effective sample transfer into the column, minimizing heavy component discrimination.

Figure 4-1. Split/Splitless Injector

1. Septum Cap 7. Graphite Column Ferrule2. Septum 8. Capillary Column3. Graphite Liner Seal A. Carrier Gas Inlet4. Glass Liner B. Split Line5. Fixing Nut C. Septum Purge Line6. M4 Retaining Nut


Chapter 4S/SL Overview Split/Splitless Injector (S/SL)

For both split and splitless applications, the sample is injected through a septum into a glass liner in the vaporization chamber.The technique used, either split or splitless, determines the choice of the glass liner. You can control the injector temperature from ambient to 375 °C, although the actual injector temperature you use depends on the solvent choice and thermal stability of the samples.

The Digital Pressure Flow Control (DPFC) controls the split flow, while the septum purge flow is kept constant by a calibrated flow regulator. The S/SL injector is also equipped with electronically actuated On/Off valves for split and septum purge lines. See Figure 4-2

Figure 4-2. Gas Control

The septum purge system continually purge the septum with a flow of gas. This prevents the volatile components given off by the septum from entering the column. Figure 4-3 shows the septum purge system.

1. Flow Sensor 1 2. Proportional Valve 13. Pressure Sensor 4. Fixed Flow Regulator 5 mL/min5. On/Off Valve 1 6. Flow Sensor 27. Proportional Valve 2 8 Trap9. On/Off Valve 2 10. Split Line FilterA. Carrier Gas Inlet B. Septum Purge Line OutletC. Split Line Outlet

3

5

2

9 678

1

4

PurgeSplit

A

10

B

C



Figure 4-3. Septum Purge System

Figure 4-4 shows the S/SL injector components.

1. Spring 6. Graphite Liner Seal2. Septum 7. Glass Liner3. Septum Holder A. Carrier Gas Inlet4. Septum Support B. Septum Purge Line5. Liner Cap C. Split Line



Figure 4-4. Split/Splitless Injector Components

1. Septum Cap 9. Injector Body2. Spring 10. Metal Ring3. Septum Holder 11. Fixing Nut4. Septum 12. Silver Seal5. Septum Support 13. Terminal Fitting6. Liner Cap 14. Fixing Nut7. Liner 15. Graphite Column Ferrule8. Graphite Liner Seal 16. M4 Retaining Nut

10

13

14

15

16

11

12

8

9

1

2

3

4

5

6

7



Septum

Standard SeptumAlways use good quality septa, such as the BTO septa supplied with the FOCUS GC. Such septa resist deformation, have longer life expectancy, and have a low bleed level, even at high temperatures.

Microseal™ ValveS/SL injector is compatible to use Merlin Microseal™ High Pressure Valve instead of the standard septa.

NOTE To replace the standard septum with the Microseal™ Valve, the relevant installation kit is required.

LinersYou may install different types of glass liners depending on the injection mode used. Table 4-1 shows the liner options.

Table 4-1. Liner Sizes and ApplicationsID mm OD mm Application

5 8 Glass liner used for split injection3 8 Glass liner used for split injection3 8 Glass liner used for splitless injection5 8 Glass liner used for splitless injection5 8 Glass liner used for direct injections into a wide-bore

column.5 8 Glass liner used for split injections at high flow rates or for

the most polar solvents.



The glass liner used for direct splitless injection into a wide-bore column is tapered at the bottom. It is used with 0.53 mm ID columns. Figure 4-5 shows the tapered glass liner.

Figure 4-5. S/SL Wide-Bore Injection with a Tapered Liner

A laminar cup liner is used for split injections at high split flow rates or for the more polar solvents. This glass liner has a mixing chamber with an extended flow path that allows complete sample vaporization before the sample reaches the split point.

1. Carrier Gas Inlet 3. Septum Purge Line2. Split Line



Packed ColumnsWith a special conversion kit, you can install packed columns in the S/SL injector, as shown in Figure 4-6.

Figure 4-6. S/SL with a Packed Column




OPERATING SEQUENCEInstalling a Liner and a Septum

Materials required:

• liner

• septum

• tweezers

• graphite seal

• liner cap wrench (included with the GC)

NOTE The injector fittings may be hot.This sequence must be performed with the injector at working temperature.

1. Choose the correct liner for your application (see Table 4-1). Slide a graphite seal onto the liner from the bottom (the bevelled end) and push it to approximately 8–10 mm from top (the flat end).

CAUTION Be careful not to break the graphite or to allow graphite to enter the liner.

2. Hold the top of the liner with tweezers. Lower it, bevelled end first, into the injector. The liner should rest on the terminal fitting at the bottom of the injector.

3. Insert the liner cap and secure it with the liner cap wrench. The liner cap must be screwed down tight enough to ensure a good seal between the liner and the injector body.

4. Place the septum support in the injector. The septum support must lie flush with the top of the injector. If not, the liner cap may not be tight enough.

5. Use tweezers to pick up the septum. Place the septum into the septum holder, then place the holder on top of the complete injector assembly.

CAUTION To avoid contamination, do not touch the septum with your hands.



6. Gently screw the septum cap onto the injector assembly until finger-tight to hold the septum in place.

WARNING! If the injector is hot, use the liner cap wrench to turn the septum cap.Do not overtighten the septum cap. The septum will deform and may be difficult to penetrate with the syringe needle.


Chapter 4S/SL Injection Techniques Split/Splitless Injector (S/SL)

S/SL Injection TechniquesThis paragraph describes the different sample injection techniques.

Split Injection TechniqueIn split injection, only a part of the sample transfers into the column. The rest discharges through the split line.

The ratio of the split flow to the column flow (the split ratio) determines the amount of sample that enters the chromatographic column. Figure 4-7 illustrates the gas flows for the split injection technique.

You inject the sample into a glass liner inside the heated vaporization chamber. In the chamber, the sample undergoes rapid vaporization. The relatively high gas flow through the injector carries the vaporized sample rapidly down toward the head of the column.

At the column head, the sample splits in the split ratio. A portion of the sample goes into the column, while the remainder is carried out the split line. You set the column flow in the CARRIER menu and the split flow in the INLET menu.

Narrow bore columns, which have inherently low column flows, can produce relatively high split ratios.

NOTE Hot Empty Needle Injection TechniqueUsing conventional syringes in hot injectors may cause discrimination of higher boiling point components. This is due to partial sample vaporization within the hot syringe needle. We recommend you use a hot empty needle injection technique. This technique consists of drawing the sample volume into the syringe barrel followed by a small air gap, which ensures the syringe needle is empty. You insert the empty needle into the injector, wait a few seconds, inject the sample rapidly, and immediately remove the syringe.

Split injection is suitable for high-concentration sample analysis, headspace analysis, and isothermal analysis.


Chapter 4Split/Splitless Injector (S/SL) S/SL Injection Techniques

Figure 4-7. Split Injection Technique

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




Splitless Injection TechniqueSplitless injection is suitable for the analysis of compounds present in very low concentrations.

The splitless technique allows the entire sample to enter the column without splitting. This offers better sensitivity than the split technique.

With splitless injection, the split line is closed during sample injection and transfer to the column. Once the transfer is over, the split line reopens to flush the vaporization chamber of any remaining sample vapors. Figure 4-8 shows the split/splitless injector used for splitless injection.

During splitless injection, when the split valves are closed, the flow of gas through the injector is relatively low. It is equal to the column flow—only a few mL/min.

The vapor cloud generated by the vaporization of the liquid sample expands upward from the point of vaporization and can fill the liner. The injector can accept and quantitatively transfer to the column sample volumes of up to 5 μL.With injection volumes higher than 4 μL, the recovery of the sample injected can be improved by closing the septum purge together with the split valve during the splitless period. You can program this in the INLET menu when you select the Splitless mode. Condensation and subsequent loss of higher molecular mass compounds in the top region of the injector liner is prevented by effective heating over the whole length of the injector.



Figure 4-8. Splitless Injection Technique

The transfer of the vaporized sample from the injector to the column takes place very slowly due to the relatively low column flows involved. With typical carrier gas flow rates of 1–4 mL/min, the transfer can take between 30 and 90 seconds, depending on a variety of circumstances.

This transfer time is the splitless time. You can set the splitless time in the INLET menu when you select Splitless mode. For narrower diameter columns (< 0.22 mm) with inherently lower flows (< 1.0 mL/min), the transfer might never be

1. Carrier Gas Inlet 3. Split Line2. Septum Purge Line



completely achieved due to back diffusion of sample vapors in the injector at a higher rate than transfer into the column. You can counter this by using the splitless surge pressure mode. In this mode, the pressure in the injector temporarily increases during the splitless period to increase the flow into the column. You set the surge pressure, which activates during the Prep Run stage.

At the end of the splitless period, the split valve reopens and the split flow flushes the injector of any remaining sample vapors. In splitless injection, the absolute split flow is not important. It needs only be sufficient to purge the injector. Normally 40–50 mL/min is adequate.

Refocusing the SampleThe sample vapors enter the column over an extended period of time and produce very broad starting bands. To maintain column efficiency, some form of refocusing must take place in the column inlet before chromatography begins. To achieve this, keep the oven temperature to a sufficiently low value during the transfer of the sample to trap it on the column head by condensation or solvent effect.

This technique’s efficiency is greatly enhanced by correctly choosing conditions for column character, carrier gas flow rates, splitless time, column temperature, and injector liner internal diameter. All of these conditions can affect the transfer efficiency and refocusing.

• Solvent EffectTo refocus the compounds that elute at low temperature, the so-called solvent effect is used. It consists of the volatile compounds trapping in the solvent recondensed in column. It is obtained cooling the column to 20–25 °C below the solvent boiling point, combined with injection volumes of at least 1 μL. Isothermal analysis or temperature programming can then continue.

• Temperature EffectYou can refocus later eluting compounds without solvent effects by cooling the oven sufficiently during the transfer. The trapping temperature effect traps and refocuses the sample compounds.



FloodingSplitless injections may occasionally exhibit an effect known as flooding, which can result in peak distortion due to the solvent condensation.

NOTE Hot Empty Needle Injection TechniqueUsing conventional syringes in hot injectors may cause discrimination of higher boiling point components. This is due to partial sample vaporization within the hot syringe needle.We recommend you use a hot empty needle injection technique. This technique consists of drawing the sample volume into the syringe barrel followed by a small air gap, which ensures the syringe needle is empty. You insert the empty needle into the injector, wait a few seconds, inject the sample rapidly, and immediately remove the syringe.


Chapter 4S/SL Inlet Parameters Split/Splitless Injector (S/SL)

S/SL Inlet ParametersThis page is the method editor for setting up the injector parameters.

S/SL Inlet page is accessible from the Roadmap-Home Page by clicking icon.

Figure 4-9. S/SL Inlet Page

This page contains four group boxes.

• Mode List Box

• Inlet Group Box

• Purge Group Box

• Surge Group Box


Chapter 4Split/Splitless Injector (S/SL) S/SL Inlet Parameters

Mode List BoxUse this list box to select one of the following inlet operating mode.

Split The carrier flow is split in the injection port with the bulk going out the split vent. Use this injection type when analyzing high concentration or neat samples, or in instances where sensitivity is less important. The split vent remains open all the time. This method yields the sharpest peaks, if the split gas is properly mixed. Additionally, this technique can improve peak shape and resolution.

Splitless The split vent is closed during the injection to drive most of the sample into the column. Solvent effect is required to refocus the analytes, especially most volatile components. You can achieve solvent effect by keeping the oven 20 °C below the solvent boiling point. Splitless times of ~ 1 minute are typical.

Splitless w/surge A surge is applied during the splitless time to reduce residence time of the analytes in the inlet. This will reduce band broadening and may sharpen peaks, especially for more volatile components, which are not improved by cold trapping effects on the column. Usually this technique involves an oven temperature 50° C below the BP of analyte.

Inlet Group BoxUse this group box to set the following inlet operating parameters.


Chapter 4S/SL Inlet Parameters Split/Splitless Injector (S/SL)

Temperature check box and text boxThe setpoint for the inlet's temperature. Depending on the mode of injection, it should be set at a temperature appropriate to vaporize the sample and solvent.

Split Flow check box and text boxSpecify the total split flow coming out of the inlet. This is the total flow out of the inlet when the split valve is open.

Split Ratio text boxThe ratio of split vent flow to the column flow. Calculate the split ratio as shown: Split Ratio = (column flow + split vent flow) / (column flow).

Splitless Time text boxThe amount of time after the injection at which the split vent opens.

Purge Group BoxThis group controls the septum purge for the inlet.


Chapter 4Split/Splitless Injector (S/SL) S/SL Inlet Parameters

Constant Septum Purge check boxThe septum purge may be turned off during a splitless injection. Checking this box will keep the septum purge valve open continuously. By leaving this box unchecked, the analyst may close this valve during the injection splitless time.

Stop Purge Time text boxEnter the time (in minutes) for the septum purge valve to close after beginning the injection. The Constant Septum Purge check box has to be unchecked for this option to be used. This is usually set to the same time as the splitless time.

Surge Group BoxThis box is available when in Mode box splitless with surge injection option has been selected.

Surge PressureThe pressure applied during the splitless time to produce a surge of flow in the inlet to speed transfer of the sample. It may be used, depending upon the analysis, to sharpen peaks closer to the solvent’s boiling point where cold trapping is ineffective and solvent effect is the main refocusing mechanism. Try adding 8 psi or 55.157 kPa to the inlet and observe early peaks after the solvent to see if peak tailing is reduced.

Surge DurationThe amount of time a pressure surge is administered after the injection. Typically, set to coincide with the splitless time.



5
Column
This chapter describes the analytical column installed in the column oven.

Chapter at a Glance…Introduction ..........................................................................................................78Installation ............................................................................................................79Keeping Leaks Under Control..............................................................................82Column Conditioning ...........................................................................................91

Operating SequencesHow to Connect a Capillary Column ...................................................................79Manual Checking for Leaks .................................................................................83Performing a Column Evaluation.........................................................................84Performing an Automatic Leak Check .................................................................89

77

Chapter 5Column Introduction

IntroductionThe capillary column should be positioned inside the oven on the column support.

Using Correct Fittings To connect a capillary column to the injector and MS transfer line, you must use the proper column ferrules and retaining nuts.

Column FerrulesEncapsulated graphite ferrules are used to connect the capillary column to the S/SL injector.

Vespel ferrules are used to connect the capillary column to the MS interface. Refer to the MS Manual.

CAUTION Overtightening compression ferrules does not necessarily produce a stronger, leak-free joint. In fact, very often the reverse is true. Too much pressure can cause a leak in the joint and make it very difficult to reseal that particular joint when changing columns.

Table 5-1 lists the graphite ferrules to use depending on the capillary column external diameter. Ferrules that are the wrong size may cause leaks and contamination.

1. Depending on column manufacturer

Retaining NutsM4 split retaining nuts are used to connect capillary columns to injector. The nuts are split to allow easy installation and removal.

Table 5-1. FerrulesCapillary Column Graphite Ferrules

0.1 mm ID 0.25 mm ID / 0.35 mm ID1

0.25 mm ID 0.35 mm ID0.32 mm ID 0.45 mm ID0.53 mm ID 0.8 mm ID


Chapter 5Installation Column

InstallationThe column is installed in the GC oven and connects the injector to the detector.

CAUTION Each column has a maximum recommended operating temperature. To protect the column from excessively high temperatures, remember to set the Max temp parameter for the column oven in the Oven Group Box as described in Chapter 3.

OPERATING SEQUENCEHow to Connect a Capillary Column

To install the capillary column, the following sequential steps should be performed:

• Installing the Column Support

• Preparing a Capillary Column

• Connecting to an S/SL Injector

• Connecting to a MS Transfer Line

Installing the Column SupportTo install the column support into the GC oven, insert the four pins into the corresponding button-holes on the ceiling of the GC oven.

Preparing a Capillary ColumnTo prepare metal or fused silica capillary column operate as follows:

CAUTION Wear safety glasses to protect your eyes from flying particles while handling, cutting, or installing columns. Be careful handling columns to avoid accidental hand injuries.

Fused Silica Capillary ColumnTo obtain a correct cut of fused silica capillary column, use ceramic scoring wafer or sapphire scribe.


Chapter 5Column Installation

Materials required:

• ceramic scoring wafer or sapphire scribe.

1. Hold the capillary column between your thumb and index finger with the column extending past the tip of your index finger.

2. Score the column very gently. Excessive force could crush the column end.

3. Snap off the end of the column.

4. Inspect the column end for an even, flat cut.

Metal Capillary ColumnTo obtain a correct cut of metal capillary column, use a triangular file.

Materials required:

• Triangular file

1. Hold the capillary column between your thumb and index finger with the column extending past the tip of your index finger.

2. Score all round the column very gently.

3. Snap off the end of the column.

4. Inspect the column end for an even, flat cut.

Connecting to an S/SL InjectorBefore connecting the column, make sure the injector has been properly assembled and programmed and the column support has been installed in the GC oven. For more information about split/splitless injectors, refer to Chapter 5.

Materials required:

• M4 column retaining nut

• graphite ferrule

• typewriter correction fluid or a felt-tipped pen


Chapter 5Installation Column

• 6 mm wrench

1. Slide the graphite ferrule onto the capillary column with the beveled end facing the injector. Be careful to avoid damaging the graphite ferrule when inserting the column.

2. Cut at least 1 cm from the column end.

3. Place the column on the column support.

4. Use typewriter correction fluid or a felt-tipped pen to mark the correct position of the ferrule from the end of the column depending on the injection technique. The correct positions are as follows:

— 40 mm for split injection

— 64 mm for splitless injection

5. Insert the column about 2 cm into the injector and slide the ferrule on the column up to the injector base, then slide the retaining nut onto the column through the side cut. The FOCUS GC retaining nuts have a slotted design that makes them easy to add and remove.

6. Finger-tighten the column retaining nut until it starts to grip the column.

7. Adjust the column position so that the mark is even with the column retaining nut.

8. Use the 6 mm wrench to tighten the retaining nut using no more pressure than is necessary to obtain a good seal (1/4 to 1/2 turn).

9. Conduct a leak check of the column installation, as described in the paragraph Keeping Leaks Under Control on page 82.

Connecting to a MS Transfer LineBefore connect the outlet end of the column to the MS detector transfer line, refer to the FOCUS DSQ manual.


Chapter 5Column Keeping Leaks Under Control

Keeping Leaks Under ControlFOCUS GC features a series of automatized operations that make easier the task of keeping under control the tightness of your system.The sequence Manual Check for Leaks - Column Evaluation - Automatic Leak Check is the key for minimizing troubles related to leaks.After you install a column you must perform a manual leak check and column evaluation then you can use the automatic leak function at any time in the future to check for leaks

Column EvaluationOnce 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 Tables. Refer to Performing a Column Evaluation operating sequence.If the value obtained does not agree with the one reported on the card, this means that the leaks have not been repaired.Performing the Column Evaluation is the necessary condition for the success of any subsequent Automatic Leak Check.

Identifying and Removing LeaksIf the Automatic Leak Check (or any significant symptom) has notified a possible leak in the system, you should:

• Check the whole system for leaks, from the carrier gas inlet to the MS transfer line.

• Check the accessible, critical connections (column to injector, column to MS transfer line, split and purge valves, septum caps).

A possible leaks source may be the gas bottles/gas chromatograph connections. Check these lines before the others, if specific symptoms indicate that the leak is outside the gas chromatograph.

Refer to Performing an Automatic Leak Check


Chapter 5Keeping Leaks Under Control Column

OPERATING SEQUENCEManual Checking for Leaks

Before you begin this sequence, you must install the column into the injector, but not into the MS trasfer line.

Materials needed:

• silicon rubber septum of any dimension

Proceed as follows:

1. Carefully push the detector end of the capillary column into the rubber septum to seal it.

2. Close off splitting and purge valves on the injector (by using the virual keypad as described in chapter 8 Use of the Virtual Keypad)

3. Increase the carrier gas pressure to 150–200 kPa and allow the column and injector pressure to stabilize. This can take up to 30 seconds.

4. Reduce the pressure to 50 kPa.

5. Observe the actual pressure. In a leak-tight system, the pressure should not drop more than 1 kPa/minute.

6. If your installed column is leak tight, remove the septum and prepare the end of the column for installation into MS Transfer line.

7. If it is not leak tight, check the tightness of the column ferrule and repeat the leak check sequence.



OPERATING SEQUENCEPerforming a Column Evaluation

The column flow control in the FOCUS GC is indirect. This means that the GC regulates pressure to control the flow of gas through the column. To do this, the GC relies on a column constant. The column constant is a measure of the columns pneumatic resistance. Use the FOCUS GC’s column evaluation feature to automatically calculate the column constant.

To perform the column evaluation, the system uses the correlation between the applied pressure 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 checking for leaks of the system must be carried out.

The GC must not be performing a run and must be isothermally stable before you can perform a column evaluation.

1. In the Instrument Setup window, select the FOCUS Pull-up menu then the option Column Evaluation. The following dialog windows appears:

2. To start Column Evaluation press . You can visualize the actual values of Oven temperature, Pressure and Column flow.

NOTE To exit column evaluation menu without performing column evaluation, press



3. The GC automatically performs column evaluation.

NOTE To abort column evaluation press

4. After e few minutes a response message appears. Compare the response with the K Factor values, reported in paragraph Expected K Factor, according to the carrier gas used.

5. If the value obtained does not agree with the one reported on the k Factor Tables, this means that the leaks have not repaired.

CAUTION Column Evaluation can be performed also by using the virtual keypad as described in paragraph How to perform a Column Evaluation in Chapter 8.

Expected K FactorThe following tables indicate the expected K factors for columns of ideal dimensions when using helium, hydrogen, or nitrogen as a carrier gas. Use this information when interpreting results from a Column Evaluation.Deviations from this chart will occur due to dimensional tolerances.

For example, a 30 m x 0.25 mm column will typically give K factors of 1.5–2.0. Large deviations from the expected values will indicate leaks in the septum or column ferrule or a plugging of the column at the inlet or exit points.

K Factor Tables• Helium Carrier Gas Theoretical K Factor

• Nitrogen Carrier Gas Theoretical K Factor

• Hydrogen Carrier Gas Theoretical K Factor



Helium Carrier Gas Theoretical K Factor

COLUMN ID (mm)0.10 0.15 0.18 0.20 0.22 0.25 0.32 0.53

2.5 5.55 1.095 0.53 0.347 0.237 0.142 0.053

COLU

MN L

ENGT

H (m

)

5 11.1 2.19 1.06 0.694 0.474 0.284 0.106 0.014

6 13.3 2.63 1.27 0.833 0.569 0.341 0.127 0.017

7 15.5 3.07 1.48 0.971 0.663 0.398 0.148 0.020

8 17.8 3.51 1.69 1.11 0.758 0.455 0.169 0.022

9 20.0 3.95 1.90 1.25 0.853 0.511 0.191 0.025

10 22.2 4.39 2.11 1.39 0.948 0.568 0.212 0.028

15 6.58 3.17 2.08 1.42 0.852 0.318 0.042

20 8.77 4.23 2.78 1.90 1.14 0.423 0.056

25 11.0 5.29 3.47 2.37 1.42 0.529 0.070

30 13.2 6.34 4.16 2.84 1.70 0.635 0.084

35 15.3 7.40 4.86 3.32 1.99 0.741 0.098

40 17.5 8.46 5.55 3.79 2.27 0.847 0.113

45 19.7 9.52 6.24 4.26 2.56 0.953 0.127

50 21.9 10.6 6.94 4.74 2.84 1.06 0.141

55 24.1 11.6 7.63 5.21 3.13 1.16 0.155

60 12.7 8.33 5.69 3.41 1.27 0.169

65 13.7 9.02 6.16 3.69 1.38 0.183

70 14.8 9.71 6.63 3.98 1.48 0.197

75 15.9 10.4 7.11 4.26 1.59 0.211

80 16.9 11.1 7.58 4.55 1.69 0.225

85 18.0 11.8 8.06 4.83 1.80 0.239

90 19.0 12.5 8.53 5.11 1.91 0.253

95 20.1 13.2 9.00 5.40 2.01 0.267

100 21.1 13.9 9.48 5.68 2.12 0.281105 22.2 14.6 9.95 5.97 2.22 0.295



Nitrogen Carrier Gas Theoretical K Factor

COLUMN ID (mm)0.10 0.15 0.18 0.20 0.22 0.25 0.32 0.53

2.5 4.95 0.98 0.471 0.309 0.2155 0.126 0.047

COLU

MN L

ENGT

H (m

)

5 9.90 1.96 0.943 0.619 0.423 0.253 0.094 0.012

6 11.9 2.35 1.13 0.743 0.507 0.304 0.113 0.015

7 13.9 2.74 1.32 0.866 0.592 0.355 0.132 0.017

8 15.8 3.13 1.51 0.990 0.676 0.406 0.151 0.020

9 17.8 3.52 1.70 1.11 0.761 0.456 0.170 0.022

10 19.8 3.91 1.89 1.24 0.845 0.507 0.189 0.025

15 29.7 5.87 2.83 1.86 1.27 0.760 0.283 0.037

20 7.82 3.77 2.48 1.69 1.01 0.378 0.050

25 9.78 4.72 3.09 2.11 1.27 0.472 0.063

30 11.7 5.66 3.71 2.54 1.52 0.566 0.075

35 13.7 6.60 4.33 2.96 1.77 0.661 0.088

40 15.6 7.54 4.95 3.38 2.03 0.755 0.100

45 17.6 8.49 5.57 3.80 2.28 0.850 0.113

50 19.6 9.43 6.19 4.23 2.53 0.944 0.125

55 21.5 10.4 6.81 4.65 2.79 1.04 0.138

60 11.3 7.43 5.07 3.04 1.13 0.151

65 12.3 8.04 5.49 3.29 1.23 0.163

70 13.2 8.66 5.92 3.55 1.32 0.176

75 14.1 9.28 6.34 3.80 1.42 0.188

80 15.1 9.90 6.76 4.06 1.51 0.201

85 16.0 10.5 7.18 4.31 1.61 0.213

90 17.0 11.1 7.61 4.56 1.70 0.226

95 17.9 11.8 8.03 4.82 1.79 0.238

100 18.9 12.4 8.45 5.07 1.89 0.251

105 19.8 13.0 8.87 5.32 1.98 0.263



Hydrogen Carrier Gas Theoretical K Factor

COLUMN ID (mm)0.10 0.15 0.18 0.20 0.22 0.25 0.32 0.53

2.5 2.49 0.492 0.237 0.155 0.106 0.063 0.023

COLU

MN L

ENGT

H (m

)

5 4.98 0.984 0.474 0.311 0.213 0.127 0.047

6 5.98 1.18 0.569 0.374 0.255 0.153 0.057

7 6.97 1.38 0.664 0.436 0.298 0.178 0.066

8 7.97 1.57 0.759 0.498 0.340 0.204 0.076

9 8.96 1.77 0.854 0.560 0.383 0.229 0.085

10 9.96 1.97 0.949 0.623 0.425 0.255 0.095 0.012

15 14.9 2.95 1.42 0.934 0.638 0.382 0.142 0.019

20 19.9 3.93 1.90 1.25 0.850 0.510 0.190 0.025

25 24.9 4.92 2.37 1.56 1.06 0.637 0.237 0.031

30 5.90 2.85 1.87 1.28 0.765 0.285 0.037

35 6.89 3.32 2.18 1.49 0.892 0.332 0.044

40 7.87 3.80 2.49 1.70 1.02 0.380 0.050

45 8.85 4.27 2.80 1.91 1.15 0.427 0.057

50 9.84 4.74 3.11 2.13 1.27 0.475 0.063

55 10.8 5.22 3.42 2.34 1.40 0.522 0.069

60 11.8 5.69 3.74 2.55 1.53 0.570 0.076

65 12.7 6.17 4.05 2.76 1.66 0.617 0.082

70 13.7 6.64 4.36 2.98 1.78 0.665 0.088

75 14.7 7.12 4.67 3.19 1.91 0.712 0.095

80 15.7 7.59 4.98 3.40 2.04 0.760 0.101

85 16.7 8.06 5.29 3.61 2.17 0.807 0.107

90 17.7 8.54 5.60 3.83 2.29 0.855 0.114

95 18.6 9.01 5.91 4.04 2.42 0.902 0.120

100 19.6 9.49 6.23 4.25 2.55 0.950 0.126

105 20.6 9.96 6.54 4.46 2.68 0.997 0.133



OPERATING SEQUENCEPerforming an Automatic Leak Check

When you perform an automatic leak check of the FOCUS GC system, the GC measures the column flow with a true mass flow sensor and compares it to a calculated flow value obtained from the original column constant to see if the numbers match. The instrument detects a gas leak if there is a significant difference between the two values.

To start the leak check operate as follows:

1. In the Instrument Setup window, select the FOCUS Pull-up menu then the option Leak Check. The following dialog windows appears.

2. To start leak check press . You can visualize the actual values of Oven temperature, Pressure and Column flow.

NOTE To exit leak check menu without performing leak check, press .

3. The system is automatically pressurized with carrier gas and sealed to perform leak check.

NOTE To abort leak check press



4. At the end of the leak check, if the system is free of leaks the Leak Check Passed message will be visualized.

5. If leaks are found, an error message will be displayed. In this case, eliminate leaks and repeat the leak check procedure.

Note that only a previous Column Evaluation, performed in a condition of true tightness, can ensure the validity of the subsequent Automatic Leak Check responses.

CAUTION An automatic leak check can be performed also by using the virtual keypad as described in paragraph How to Perform a Leak Check in Chapter 8.


Chapter 5Column Conditioning Column

Column ConditioningTo ensure optimum analytical performance, a new column must be conditioned to remove contaminants and unwanted volatile compounds.Column conditioning is required to remove volatile contaminants adsorbed from the air.Column conditioning consists of passing a carrier gas flow through the column and heating the column to a temperature 20–50 °C above the maximum temperature that will be used for running analyses, provided that temperature is within the operating range of the column.For detailed information on column conditioning of your specific column, refer to the column manufacturer’s instructions.

CAUTION With the column already installed, before starting column conditioning, disconnect the column outlet from the MS detector. With the column not already installed, connect only the column inlet to the injector.


Chapter 5Column Column Conditioning



6
Getting Started
This chapter contains instructions to configure, set operating parameters and control your FOCUS GC Version for MS through Xcalibur software.

Chapter at a Glance…Configuring the FOCUS GC ................................................................................94Use Roadmap-Home Page....................................................................................96FOCUS GC Setup.................................................................................................99FOCUS GC Pull-up Menu..................................................................................102Method Editing...................................................................................................103Oven ...................................................................................................................104Inlet SSL.............................................................................................................108Carrier................................................................................................................. 114MS Transfer Line................................................................................................ 117Run Table............................................................................................................ 118Virtual Keypad....................................................................................................122Valves Manual Activations.................................................................................124Instrument Start-up .............................................................................................125

Operating ProceduresSetting Up a Single Ramp Temperature Program ..............................................106Setting Up Multiple Ramp Temperature Program..............................................107Programming the Split Mode ............................................................................. 111Programming the Splitless Mode ....................................................................... 112Programming the Surge Splitless Mode ............................................................. 113Programming The Carrier Gas Parameters......................................................... 116How to Start-up the Instrument ..........................................................................125

93

Chapter 6Getting Started Configuring the FOCUS GC

Configuring the FOCUS GCThis paragraph contains the instruction to configure your FOCUS GC.

On the PC desktop, click twice on the Instrument Configuration icon to enter Instrument Configuration Dialog Window.

Figure 6-1. Instrument Configuration Dialog Window

1. Select the FOCUS GC from the Available Device box.

2. Pressing ADD, the FOCUS GC moves to the Configure Device box.

3. After the FOCUS GC or DSQ is in the Configure Device box, you can enter configuration information by pressing CONFIGURE.

4. The following Page appears


Chapter 6Configuring the FOCUS GC Getting Started

Figure 6-2. FOCUS GC Configuration Page

where:

Connections Group Box

Option Group Box

5. Press OK to return Instrument Configuration Dialog Window, then press DONE to exit Instrument Configuration Dialog Window.

Parameter DescriptionSerial Port Select the Com Port where you have the FOCUS GC

connected.

Parameter DescriptionPressure Unit Select the pressure units to display in the Instrument Setup

Pages (kPa, Bar, PSI). Selecting different pressure units does not affect the GC.


Chapter 6Getting Started Use Roadmap-Home Page

Use Roadmap-Home PageFrom the Roadmap–Home Page, shown in Figure 6-3, you may display dialog windows to set FOCUS GC parameters and to display the current GC status and actual values.

On the PC desktop, click twice on the Excalibur icon to enter Excalibur program.

Figure 6-3. Roadmap-Home Page

GC Status and Actual ValuesStatus pages for your FOCUS GC are located on your Xcalibur Roadmap-Home page. Just highlight FOCUS GC from the Roadmap Status tab scroll list and see the following pages (status, temperatures, flows, and pressures) display the current GC status.


Chapter 6Use Roadmap-Home Page Getting Started

Status PageIn the Status window the message indicating the current status of the GC, the elapsed time and the remaining time of the analytical run are displayed.

General Group Box

Run Group Box

Emergency Conditions Group BoxWhen an emergency condition occur, a mark appears in the relevant box or in more boxes depending of the nature of the error.

Parameter DescriptionStatus Indicates if instrument is communicating to Xcalibur.

Parameter DescriptionElapsed time The amount of time that has elapsed since the run started.Remaining time The amount of time that remains before the run finishes.


Chapter 6Getting Started Use Roadmap-Home Page

Actual Values PageThe Actual Status page displays the actual and the setpoint values of the FOCUS GC parameters set in the Instrument Setup dialog window.

Parameter DescriptionEmergency Shutdown

Your Xcalibur software automatically checks this box if an error condition like a leaking hydrogen sensor or something is malfunctioning internally in your FOCUS GC. The software automatically shuts the FOCUS GC off.

Over temperature

This box is checked only when Xcalibur software detects the temperature is over the recommended level.

Shorted RTD This detected problem requires certified technical support. Contact your local Thermo Tech Support office for service.

Shorted oven RTD

This detected problem requires certified technical support. Contact your local Thermo Tech Support office for service.


Chapter 6FOCUS GC Setup Getting Started

FOCUS GC SetupThis paragraph contains instruction to set the carrier gas type to use, the signal selection (Handshake) to allows the correct cooperation between FOCUS GC and MS detector, and to configure external valves or devices.

On the Roadmap-Home Page, click on icon. The FOCUS Instrument Setup dialog window will be displayed visualizing all configuration tabs such as Oven, Inlet SSL, Carrier, MS Transfer Line and Run Table, required to set the GC parameters. Refer to paragraph Method Editing.

To return Roadmap-Home Page from each configuration tab press the button.To setup FOCUS GC, select Focus menu then the option Instrument Setup.

NOTE For further details about Focus menu, refer to paragraph FOCUS GC Pull-up Menu.The following FOCUS GC Setup Page will be displayed:

Figure 6-4. FOCUS GC Setup Page


Chapter 6Getting Started FOCUS GC Setup

Carrier Box

Handshake Group BoxThe FOCUS GC cooperates with a MS detector during the analysis. To allow the device to run properly, you must indicate how the signal will change.

Parameter DescriptionGas Type Select the type of carrier gas to use for the analyses (He, N2, H2).

Verify that the carrier gas used has been properly connected to the GC.

WARNING! Hydrogen is a potentially dangerous gas.

Parameter Range DescriptionRemote Start IN

Pulse High to Low (default)Pulse Low to High

This parameter allows another device to start the FOCUS GC.

Inhibit Ready

When Low (default)When High

This parameters delays readiness until the GC receives a signal from another device.

End of Run OUT


This parameter signals another device that the run has ended.

Autostart On/Off Check this box to turn on auto start execution.

Start of RUN OUT


This parameter signals another device that the run has started.

GC Ready OUT

When Low (default)When High

This parameter signals another device that the GC is ready.

Prep-Run OUT


This parameter signals another device that the GC is preparing for a run.


Chapter 6FOCUS GC Setup Getting Started

Valves Group BoxIn this box you can configure two gas sampling valves, when present, and program two external events to be the default condition for an external device. See also Run Table.

Buttons

Parameter Range DescriptionValve #1 None - Sampling Select in this box Sampling only if a gas sampling

valve is present and connected to the GC. Otherwise, select none.

Valve #2

EV #1 default

See Valve #1On - Off

Select the external event default condition. The external device will return to the condition specified by the external event you have programmed to be the default whenever the GC’s in Standby mode.

EV #2 default

See EV #1

Button DescriptionDONE Click this button to exitGET Click this button to get the current configuration from the GC.SEND Click this button to send the current configuration to the GC.


Chapter 6Getting Started FOCUS GC Pull-up Menu

FOCUS GC Pull-up MenuThe FOCUS menu, shown in Figure 6-5, is located on the Instrument Setup-menu bar

Figure 6-5. FOCUS GC Pull-up Menu

Option DescriptionInstrument Setup

Allows to perform instrument setup. Refer to paragraph Method Editing in this Chapter.

Send Method to GC

Downloads the GC portion of the current method from the Instrument Setup window to the GC.

Get Method from GC

Uploads the current method from the GC to the Instrument Setup window.

Start GC / Prep Run

Allows starting the GC run.

Stop GC Allows stopping the GC run.Keypad Allows accessing the GC control panel. Refer to paragraph

Virtual Keypad in this chapter. Column Evaluation

Allows to perform a column evaluation. Refer to Performing a Column Evaluation in Chapter 5.

Leak Check Allows to perform an automatic leak check. Refer to Performing an Automatic Leak Check in Chapter 5.


Chapter 6Method Editing Getting Started

Method EditingFrom the Roadmap-Home Page, click on icon. The Instrument Setup dialog window will be displayed where all the configuration tabs required to set the GC parameters are available:

• Oven

• Inlet SSL

• Carrier

• MS Transfer Line

• Run Table

To return Roadmap-Home Page from each configuration tab click the button.

Valves Allows valves manual activation. Refer to paragraph Valves Manual Activations in this chapter

Flow Calculator Useful to determine column pressure settings and flow rates through a capillary column.

Vapor Calculator

To rapidly calculate the expansion volume using several factors.

Option Description


Chapter 6Getting Started Oven

OvenThis page is the method editor for setting up parameters in the GC run.

Figure 6-6. The Oven Page

See also:

• Setting Up a Single Ramp Temperature Program

• Setting Up Multiple Ramp Temperature Program

To return Roadmap-Home Page click the button.


Chapter 6Oven Getting Started

Ramps Group BoxParameter Range Description

InitialTemperature

From 30 °C to 350 °Cin step of 1°C

In this box set the temperature in °C at which the oven is set and conditioned before the GC enters the sampling phase.

Initial Hold Time From 0 to 99.99 minutes

In this box set the time in minutes, the oven will be kept at the initial temperature.

Ramp 1 Rate (°C/min)

From 0.1 to 120 °C/minIn step of 0.1 °C/min

Rate for the temperature ramp from Initial Temperature to Temperature 1. In this box set the rate increment to reach the temperature set in Temperature 1.

Temperature 1 From 30 to 350 °CIn step of 1 °C

Temperature for second temperature program level. In this box set the target temperature in °C the oven must reach at the end of the Ramp 1 phase.

Hold Time 1 From 0 to 99.99 minutes

Duration of the second temperature program level Temperature 1. In this box set the time in minutes the oven will be kept at the Temperature 1.

Ramp 2Rate (°C/min)


Rate for the temperature ramp from Temperature 1 to Temperature 2. In this box set the rate increment to reach the temperature set in Temperature 2.

Temperature 2 From 30 to 350 °CIn step of 1 °C

Temperature for third temperature program level. In this box set the target temperature in °C the oven must reach at the end of the Ramp 2 phase.


Duration of the third temperature program level Temperature 2. In this box set the time in minutes the oven will be kept at the Temperature 2.

Ramp 3Rate (°C/min)


Rate for the temperature ramp from Temperature 2 to Temperature 3. In this box set the rate increment to reach the temperature set in Temperature 3.

Temperature 3 Form 30 to 350 °CIn step of 1 °C

Temperature for forth temperature program level. In this box set the target temperature in °C the oven must reach at the end of the Ramp 3 phase


Duration of the forth temperature program level Temperature 3. In this box set the time in minutes the oven will be kept at the Temperature 3.


Chapter 6Getting Started Oven

Oven Group Box

OPERATING SEQUENCESetting Up a Single Ramp Temperature Program

This program raises the initial oven temperature to a specified final temperature at a specified rate and maintains the final temperature for a specified time.

1. Enter in Initial Temp°C box the initial temperature.

2. Enter in Initial Hold Time (min) box the time you want the oven to maintain the initial temperature.

3. Enter in Ramp 1 Rate (°C/min) box the ramp rate for the oven to reach the ramp’s Ramp 1 Temp °C.

4. Enter in Ramp 1 Temp °C box the final temperature for the ramp.

5. Enter in Ramp 1 Hold Time (min) box the time the oven will maintain the final Ramp 1 Temp °C.

Parameter Range DescriptionAuto Prep Run

On -Off Check this box for the GC to automatically go to the Ready state when the initial conditions are met. If this box is not checked, you will have to press the START key located on the FOCUS GC virtual keypad or to select the option StartGC/PrepRun in Focus menu.

Max Temp (°C)

From 50 °C to 350 °CIn step of 1 °C

Specify the maximum temperature for this run.The software automatically sets the maximum allowable temperature for the column being used in the method.

Prep Run Timeout

From 0 to 99.00 minutes

Enter the duration of the Prep Run. The injection must occur within this time or the timeout will return the GC to Standby condition.

Equilibrium Time (min)

From 0 to 99.00 minutes

In this box set the time in minutes the GC has to wait before entering the sample phase. This time is used for conditioning the oven at the temperature specified in Initial Temperature box.


Chapter 6Oven Getting Started

OPERATING SEQUENCESetting Up Multiple Ramp Temperature Program

This program raises the initial oven temperature to a specified final temperature through up to seven ramps, each having a specified ramp rate, time, and temperature.

1. Enter in Initial Temp°C box the initial temperature.

2. Enter in Initial Hold Time (min) box the time you want the oven to maintain the initial temperature.


4. Enter in Ramp 1 Temp °C box the final temperature for the ramp.

5. Enter in Ramp 1 Hold Time (min) box the time the oven will maintain the final Ramp 1 Temp °C.

6. Press the up button to add a new ramp level.


8. Enter in the Ramp 2 Temp °C box the final temperature for the ramp.

9. Enter in the Ramp 2 Hold Time (min) box the time the oven will maintain the final Ramp 2 Temp °C.

To add additional oven ramps, repeat the steps 6 through 9.


Chapter 6Getting Started Inlet SSL

Inlet SSLThis page is the method editor for the Split/Splitless inlet injector.

Figure 6-7. The Inlet SSL Page

See also:

• Programming the Split Mode

• Programming the Splitless Mode

• Programming the Splitless Mode

• Gas Saver

• Valves Manual Activations



Chapter 6Inlet SSL Getting Started

Mode List Box

Inlet Group Box

Mode Description Set:Split Use this injection mode when analyzing high concentration or neat

samples, or in instances where sensitivity is less important. The split vent remains open all the time. This method yields the sharpest peaks if the split gas is properly mixed.

Split FlowSplit Ratio

Splitless The split vent is closed during the injection to drive most of the sample into the column. The solvent effect is required to refocus the analytes, especially more volatile compounds. You can achieve the solvent effect by keeping the analytical column or guard column slightly below the solvent's boiling point. Splitless times of about 1 minute are typical.

Split FlowSplitless Time

Splitless w/Surge

Same as Splitless but can also program a surge during an injection. Surge starts at Prep Run and continues until the surge duration time is finished. Surge is further defined in the Surge group Box.

Split FlowSplitless TimeSurge Pressure Surge Duration

Parameter Range DescriptionTemperature (°C)

From 100 °C to 375 °CIn steps of 1 °C0 = Off

Specify in this box the injector temperature setpoint.

Split Flow (ml/min)

From 10 to 100 ml/minIn steps of 1 ml/min0 = No Split

Check in this box to turn On the split flow. Specify the split flow coming out of the injector. Set 0, to close the split valve and to turn Off the split flow.

Split Ratio From 1 to 1000In steps of 1

It is displays only when Split mode is Selected. Specify the ratio of split flow compared to the column flow.

Splitless Time (min)

From 0 to 9.99 minutesIn steps of 0.01 minutes

Specify the length of time the split valve remains closed after a splitless injection. The timer begins at the start of the run.



Purge Group Box

Surge Group Box

Parameter Range DescriptionConstantSeptum Purge

Yes - No Check this box to activate a constant septum purge to continuously flush the septum with a purge flow of 5 ml/min when using helium or nitrogen as carrier gas or 10 ml/min when using hydrogen as carrier gas. When the Constant Septum Purge checkbox is unchecked, the following parameter needs to be programmed.

Stop Purge Time: (min)

From 0 to 9,99 minutesIn steps of 0.01 minutes

This option may be used only when the Constant Septum Purge checkbox is unchecked. Specify the length of time the purge valve remains closed after a splitless injection. This is usually set to the same time as the splitless time.

Parameter Range DescriptionSurge Pressure(kPa)

From 10 to 1000 kPaIn steps of 1 kPa

Specify the surge pressure to accelerate the transfer process of the substances from the injector to the column. The pressure surge starts in the Prep Run phase and ends at the end of the Surge Duration you program.

Surge Duration(min)

From 0 to 9.99 minutesIn steps of 0.01 minutes

Specify the duration of the surge pressure after run start.



OPERATING SEQUENCEProgramming the Split Mode

In split injection, only a portion of the sample transfers to the column. Most of it discharges through the splitting line. The ratio between the split flow and the column flow defines the amount of sample that enters the chromatographic system. The split and column flows must be set to obtain the correct split ratio necessary for the analysis.

Before you begin programming, do the following:

• Verify that a column is correctly installed, the correct liner is in the injector, and the system is free of leaks.

• Program the carrier gas flow as described in paragraph Carrier.

Proceed as follows:

1. I.n the Mode box select Split.

2. Set the appropriate Inlet Temperature.

3. Specify the split flow or the split ratio. To set Split Flow enter the value in the relevant box. The split ratio will be calculated for you.To set Split Ratio, enter the value in the relevant box. The split flow will be calculated for you.



OPERATING SEQUENCEProgramming the Splitless Mode

In splitless analyses, the splitting line is closed during the sample transfer onto the column. The time during which the splitting valve remains closed is called the splitless time. When the sample transfer ends, the split line reopens to purge the residual sample components, essentially solvent, out of the vaporization chamber. You can activate a constant septum purge, if necessary, to continuously flush the septum with a purge flow. The septum purge prevents septum bleed components from entering the column.




Proceed as follows:

1. In the Mode box select Splitless


3. Set the Split Flow and enter the desired value.

4. Specify the Splitless Time.

5. If constant septum purge is required, check the Constant Septum Purge box to activate a constant septum purge.If constant septum purge is not required, uncheck the Constant Septum Purge. boxIn the Septum Purge Time box enter the time the purge flow should be interrupted.



OPERATING SEQUENCEProgramming the Surge Splitless Mode




Proceed as follows:

1. In the Mode box select Splitless w/surge


3. Set the Split Flow and enter the desired value.

4. Specify the Splitless Time.

5. In the Surge Pressure box enter the value of the pressure surge.

6. In the Surge Duration box enter the duration of the pressure surge.

7. If constant septum purge is required, check the Constant Septum Purge box to activate a constant septum purge.If constant septum purge is not required, uncheck the Constant Septum Purge.In the Septum Purge Time box enter the time the purge flow should be interrupted.


Chapter 6Getting Started Carrier

CarrierThis page is the method editor for setting the carrier gas for the FOCUS GC inlet.

Figure 6-8. The Carrier Page

See also:

• Programming The Carrier Gas Parameters



Chapter 6Carrier Getting Started

Flow Group Box

Gas SaverGas saver controls reduce carrier gas consumption, especially when a large split flow is used. The gas saver options are set to come on at some point well after the injection to conserve gas. Checking the box will activate the feature of gas saver.

Parameter Range DescriptionFlow Mode Constant Flow

Constant PressureSet the operating mode required.Selecting Constant Flow, the column flow is kept constant throughout the analysis. The pressure at the column head will change with the column temperature to maintain a consistent flow. See Flow.Selecting Constant Pressure, the pressure at the column head is kept constant throughout the analysis. During a temperature program, the column flow decrease due to the increase of the carrier gas viscosity. See Pressure.

Flow

(ml/min)From 0.1 to 50.0 ml/minIn steps of 0.1 ml/min0 = Flow Off

It is displayed when Constant Flow is selected in Flow Mode box. Enter a column flow for the analytical column. When using an oven temperature program, run the GC to automatically increase the pressure constant flow on the column: This compensates a gas’s increased viscosity due to an increase of temperature.

Pressure(kPa)

From 7 to 700 kPaIn step of 1 kPa0 = Pressure Off

It is displayed when Constant Pressure is selected in Flow Mode box. Enter inlet pressure for the analytical run.

Vacuum

CompensationYes - No Check this box to compensate for a vacuum at the end of the

analytical column. When the box is not checked calculation are made considering the detector, which at atmospheric pressure.

Yes –No Checking this box enables flow to the inlet. When this box is not checked gas flow is cut off to the inlet.


Chapter 6Getting Started Carrier

OPERATING SEQUENCEProgramming The Carrier Gas Parameters

Before you begin this procedure, do the following:

• Check that the carrier gas type is correct for the analysis.

NOTE When you install a new column, you must perform a Column Evaluation.

1. Select the Carrier Constant Flow or Constant Pressure mode.

2. Enter the initial Flow or Pressure.If you selected Constant Flow mode, enter in the Flow (ml/min) box the desired value. The GC calculates the pressure necessary and adjusts the pressure as necessary to maintain the constant flow.If you selected Constant Pressure mode, then in the Pressure (kPa) box enter the desired value.

3. Activate the Gas Saver if required checking the Enable check button.Check the Gas Saver box to activates the gas saver control.In Flow (ml/min) and Time (min) boxes type the desired values.

Parameter Range DescriptionEnable On – Off Check this box to activate gas saver function to the inlet. The

Gas Saver Flow and Gas Saver Time parameters must be programmed.When this box is nor checked, gas saver function is not activated.

Flow (ml/min) From 10 to 500 ml/minIn step of 1 ml/min

Enter the desired flow after the injection or in Standby.

Time (min) From 0 to 9.99 minutesIn steps of 0.01 min

Enter the time after the injection when gas saver flow will be activated.


Chapter 6MS Transfer Line Getting Started

MS Transfer LineThis page is the method editor for setting and control the temperature of the MS transfer line.

Figure 6-9. The MS Transfer Line Page


MS Transfer Line Group Box

Parameter DescriptionCheck this box to activate the temperature control when required.

Ms Transfer Line (°C)

Set the desired temperature value from 0 to 450 °C.


Chapter 6Getting Started Run Table

Run TableThis page allows you program events to happen prior to or during a run. For example, a valve could open two minutes into a run. Listed in the run table page are settings entered prior to the run in the Run Time Event dialog box. Time, item, and settings display in this run table. Control listed in the Initial Values group box is for switching external device On/Off.

Figure 6-10. Run Table Page

See Also:

• Add/Edit Run-Time Event Screen



Chapter 6Run Table Getting Started

Time, Item, and Settings Group BoxAll selections made in the Add/Edit Run-Time Event screen display in this table. The categories display items important during a run-time event.

Initial Values Group BoxControls listed in the Initial Values group box are for setting default values for external events. After External events are made in the Add/Edit Run-Time Event screen, they display in the Run Table. Use the External event parameter to activate or deactivate the event.

Buttons

Option DescriptionTime Displays the time at which the run time event will occur. Item Displays which event (Valve, or External) was configured in the Add/Edit Run Time Event

screen.Setting Displays if the Valve event or the External event settings are On or Off.

Option DescriptionExternal Event #1 On

External Event #2 OnLocated on the back of your FOCUS GC is a port with two contacts that can be programmed to turn external devices On or Off. Pre-run conditions for External events are set on the Run Table page under the Initial Values group. From the Run Table page during a specific run time, you can change the status of these external switches

Button DescriptionADD Select this button to add a run-time event and to display the Add/Edit Run-Time Event screen.

Run-time events selected from the Add/Edit Run-Time Event screen are displayed on the Run Table page (under the Time, Item, and Setting columns.)

EDIT Select this button to edit a current run-time event and to edit items selected in the Add/Edit Run Time Event screen. Before selecting this button, select a run-item listed in the Time, Item, and Setting table. Then click the Edit button to display the Add/Edit Run-Time Event screen.

REMOVE Select this button to delete a current run-time event: First, select an item listed in the Time, Item, and Setting table, then click the Remove button to remove the selected run item.


Chapter 6Getting Started Run Table

Add/Edit Run-Time Event ScreenSelect the ADD or EDIT from the Run Table page to display the Add/Edit Run-Time Event screen. Events displayed on the Run Table page are from selections made in this screen

Figure 6-11. ADD/Edit Run-Time Event Screen

Event Time Group BoxUse the parameters listed in this group box to determine when to activate the event.

Valve EventThis group of parameters contains configuring options for valve events.

Option DescriptionPrep Run This option makes the selected event (Valve, or External)

happen before the run begins.Run Time This option makes the selected event (Valve, or External)

happen at the time specified during the run.


Chapter 6Run Table Getting Started

External Event Group BoxThis group of parameters contains options for external events. Each event selected here is displayed on the Run Table page.

Option DescriptionValve number Select from one to two pneumatic valves for each external

event to turn on from the Run Table page. If you use all two then none is available for other events.

Valve Type Sampling is available only. Sampling is a valve used to inject a volume of sample into the carrier stream.

Inject for This parameter is only available after selecting Sampling for a valve type. Specify how many minutes to inject the sample.

Setting For Sampling the settings are Load or Inject.

Option DescriptionExternal Number Select which of the two-(2) external events to program. The

GC has two available open collector outputs, which can be configured to switch external valves, switches, and other options. Select the numbered event matching the GC connection number.

Setting Select On or Off to set the external event at the specified programmed run time.


Chapter 6Getting Started Virtual Keypad

Virtual KeypadTo display the keypad, from Instrument Setup dialog windows, select Focus then Control Panel option. See also FOCUS GC Pull-up Menu.

For detailed information about the FOCUS GC Virtual Keypad refer to Chapter 8 Use of the Virtual Keypad

Figure 6-12. Control Panel - Virtual Keypad

Move your cursor across any region located in this illustration. Your cursor becomes a hand when a region has related popup topic. Use these topics to learn how the FOCUS GC keypad is functionally organized.

Description

Display PanelThe display panel displays the settings currently in use. Listed top to bottom on the display panel is typically a menu title bar, parameters, scroll indicators, and a cursor indicating your current position. Use the data-entry keys to navigate up or down the menu and to enter values.

GC Status LEDsThis region contains light emitting diodes, which indicate the FOCUS GC operating status. Observe the GC status periodically to determine what stage the GC is in during the run.


Chapter 6Virtual Keypad Getting Started

Action KeysUse these keys to start or interrupt activities, to display the instrument status and to open menus. Listed left to right are Start, Stop, Status, Home, Dec/Inc and Enter.

Data Entry KeysUse these keys to enter information into a displayed menu: Listed left to right: On/Yes, Clear, Off/No, Enter, (press to move up or down in menu), and the numerical keypad.

Keypad Menu

File MenuThis menu permits to access the following functions:

Get Method from GCThis function allows to transfer method data from GC to data system.

Send Method to GCThis function allows to transfer method data from data system to GC.

CloseThis function allows to close FOCUS GC virtual keypad.


Chapter 6Getting Started Valves Manual Activations

Valves Manual ActivationsTo display the relevant page, from Instrument Setup dialog windows, select Focus then Valve option. See also FOCUS GC Pull-up Menu.

Figure 6-13. Valves Dialog Window

Inlet SSL Valves Group BoxCheck in the relevant box to open or close the inlet valve of interest before or during a run.

Valve Vents Group BoxSet the Load or Inject position of the sampling valve (when present):Set On/Off the Event Valve #1 checking the relevant check box.


Chapter 6Instrument Start-up Getting Started

Instrument Start-upThis start-up sequence contains the instructions which combines the analytical procedure with the use of the Excalibur program.

OPERATING SEQUENCEHow to Start-up the Instrument

The sequence of instructions begins with the assumption that all the instruments of the system are ON, set and ready to initiate the analyses.

Preliminary CheckBefore start the GC, verify that the following operations have been already carried out:

• The carrier gas supply line is correctly connected to the DPFC module and the inlet pressure is set at the required value as described in Chapter 1.

• The FOCUS GC is properly electrically connected and configured.

• The carrier gas type is correctly set.

• The analytical column is correctly installed and conditioned.

• The correct liner is the SSL injector.

• The system is free of leak.

• The column evaluation has been carried out.

Setting the GC Parameters

1. In the Instrument Setup dialog window program the required Oven, Inlet SSL, Carrier, MS Transfer line and Run Table parameters as described in this chapter.

2. In the sequence set-up, program a sample run. Refer to Xcalibur manual for more information.


Chapter 6Getting Started Instrument Start-up

Performing an Injection

3. The FOCUS GC will automatically perform the PressRun operations. Depending on the SSL operating mode you have programmed, the FOCUS GC 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 the 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.

4. 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).

5. To start the run, press START button in Control Panel or again selecting Start GC/Preprun option in the FOCUS menu or again by pressing the optional remote Start button.

The GC will complete the analysis as programmed.



7
Maintenance and Troubleshooting
This chapter contains information and operating sequences to perform the necessary maintenance of the instrument and also information concerning troubleshooting in case of malfunctioning.

Chapter at a Glance…Maintenance .......................................................................................................128Maintaining a SSL Injector ................................................................................131Troubleshooting..................................................................................................140Error Messages ...................................................................................................142Guide to Solve Analytical Problems ..................................................................143

Operating ProceduresReplace the Standard Septum.............................................................................133Replace or Clean the Liner when a Standard Septum is Installed......................135

127

Chapter 7Maintenance and Troubleshooting Maintenance

MaintenanceThis paragraph provides information on the maintenance of the instrument. It also contains the instructions for the instrument shutdown.

WARNING! Before performing any operation of maintenance that requires the closure of the carrier gas, it is necessary to shut down the MS detector. Refer to the FOCUS DSQ manual.

How To Perform MaintenanceThermo Fisher Scientific authorized technical personnel under the instrument warranty or, when this has expired, possibly under a Service Contract Program will normally perform full instrument servicing. To ensure that your FOCUS GC always performs to its full potential, the operator must carry out a certain amount of routine maintenance on a regular basis.

Suggested Maintenance SchedulePreventive maintenance keeps your instruments running at peak performance.The recommended maintenance schedule, shown in the Maintenance Schedule Table, is based on a GC running multiple samples in an 8-hour day.You may need to adapt the schedule to your situation depending on:

• The number of analyses per day

• How clean the samples are

• The condition of the syringe needle

• Environmental conditions such as dirt and ambient temperature

SeptaSepta degrade over time. Different types will degrade at varying rates. Factors affecting septa life include:

• Number of samples injected

• Injector temperature

• Condition of the syringe needle


Chapter 7Maintenance Maintenance and Troubleshooting

Ferrules and SealsFerrules and seals should be replaced when they are too flat to produce a good seal.

NOTE Unless required applications necessitate frequent dismantling and replacement of columns and accessories, seals and ferrules normally need to be disturbed only when dismantling is required. However, the FOCUS GC should be periodically leak-tested and the seal tightened or replaced as necessary.

TrapsInternal and external traps in the gas line must be periodically serviced. It is advisable to check the state of the traps every time gas cylinder is replaced..

Detector UnitTo ensure optimum performance of the detector, refer to the relevant manual.

Make sure you not only perform each scheduled item, but that you record it as well, along with any observation about instrument performance. Your records and notes can be invaluable when trying to trace a service problem.In addition to the routine and preventive maintenance that you perform, we recommend annual inspections by Thermo Fisher Scientific customer service engineers. These yearly checkups ensure that your instrument remains in peak condition.

Maintenance Schedule Table.

Table 7-1. Standard Maintenance ScheduleFrequency Task

Daily Run Automatic Leak Test.

Run performance check standard as required by method.

Run calibration curve as required by method.

Note gas pressure when the weekly pressure check shows it to be below 5000 kPa (50 bar or 750 psig).


Chapter 7Maintenance and Troubleshooting Maintenance

Instrument Cleaning

WARNING! Cleaning must be performed with the instrument off and the power cord discon-nected.Normal usage of the FOCUS GC can cause the exterior to get dirty.Externally clean the instrument with a cloth dampened with soap and water solution, or with a household non-abrasive product, carefully avoid seeping of the products used inside the instrument.If you just suspect that a substance used for cleaning or a product submitted to analysis has infiltrated inside the instrument, immediately shut down the instrument and call an authorized customer support engineer for proper actions. The service engineer must be fully informed on the nature of the concerned substance. In the event that a hazardous material is spilled on or in the instrument, clean the spill according to the procedures in the Material Data Sheet for that substance.

WARNING! It is your responsibility to avoid that dangerous liquids and/or materials seepinginside the GC during operation and maintenance.

Weekly Change injector liner.

Check pressure of gas cylinders. Replace the cylinder when its pressure drops below 3500 kPa (35 bar or 500 psi).

Monthly Check for leaks from the primary gas supply to the GC.Semiannually Regenerate the S/SL inlet vent line trap.

Recondition or replace internal and external traps if present.

Table 7-1. Standard Maintenance Schedule (Continued)


Chapter 7Maintaining a SSL Injector Maintenance and Troubleshooting

Maintaining a SSL InjectorThe S/SL (Split/Splitless) injector will normally be serviced by Thermo Fisher Scientific authorized technical personnel. In order to operate, the injector requires periodic maintenance from the user. This maintenance includes:

• The replacement of the septum

• The cleaning or replacement of the liner

• The maintenance of the Merlin Microseal Valve when used instead of the standard septum.

When Replacing the SeptumThe septum should be replaced at least after every 200 injections, or every time a problem related to septum damage or wear occurs.It is a good practice to change the septum with a new one every time the liner is replaced.

CAUTION Use original Thermo Fisher Scientific standard septum. Septa from other manufacturers may show different rates of degradation.

When Cleaning or Replacing the LinerThe liner must be replaced periodically, depending on the number of injections performed and the characteristics of the samples injected. Typical symptoms will indicate that the liner must be replaced. The most common is the appearance of tailing peaks in the chromatogram, particularly for polar compounds.

It is good practice to replace the septum every time the liner is replaced.

You can replace the liner with a new one or clean the liner and reinstall it.

The following table shows the available types of liners and the indications for the correct choice.


Chapter 7Maintenance and Troubleshooting Maintaining a SSL Injector

If the Glass Liner Breaks Inside the InjectorWhen replacing or removing a glass liner, it might break inside the injector. In this case the broken parts of the liner must be removed from the injector, including the glass splinters that might fall into the lower part of the vaporization chamber. Refer to Removing a Broken Liner for instructions.The following Operating sequences help you to maintain properly the SSL injector.

• Replace the Standard Septum

• Replace or Clean the Liner when a Standard Septum is Installed

NOTE To replace a standard septum with the Microseal Valve, refer to the relevant Installation Guide.

Liner PNSplit injections, 3 mm 453 200 31Split injections, 5 mm 453 200 30Splitless injections, 3 mm 453 200 32Splitless injections, 5 mm 453 200 33Liner for direct injections into wide bore column 453 003 10Laminar cup liner for split injections at high split flow rates or for the most polar solvents.

453 003 20



OPERATING SEQUENCEReplace the Standard Septum

Material needed

• Non metallic sharp tool

• Septum

• Tweezers

WARNING! This operation must be carrier out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.

Preliminary Operations

1. Vent the MS system referring to the DSQ Manual.

2. While in Standby condition, in OVEN page set the initial oven temperature to 30 °C.

3. In INLET SSL page set the inlet temperature to 0 (0 = Off).

4. When the inlet reaches the room temperature, enter in CARRIER page and uncheck the flow box to cut off the gas flow to the inlet.

Removing the Septum

5. Unscrew the septum cap.

6. Remove the septum holder with septum, then the septum support. See A of Figure 7-1.

7. Remove the septum from the septum holder (use non-metallic tools). See B of Figure 7-1.

8. Insert a new septum into the septum holder. See B of Figure 7-1.

CAUTION Use tweezers to avoid touching the septum with your fingers.



Figure 7-1. Replace the Septum

Replacing the Septum

9. Clean the septum support from possible fragments left by the septum and reinsert it into the injector.

10. Place the septum holder on the top of the septum support (see C of Figure 7-1).

11. Tighten the injector cap to finger tight.

CAUTION Do not overtighten the injector cap. You could damage the septum and affect performance.

Restart the GC Conditions

12. In CARRIER, OVEN and INLET pages set the normal working conditions.

13. Perform an automatic leak check.



OPERATING SEQUENCEReplace or Clean the Liner when a Standard Septum is Installed

Material needed

• Liner cap removal tool

• Glass liner

• Graphite seal

• Ultrasonic bath

• Methanol/acetone mixture (1:1)

• Non metallic sharp tool

• Standard Septum

• Tweezers

WARNING! This operation must be carrier out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.When handling organics solvents you must take precautions to avoid health hazards.

Preliminary Operations

1. Vent the MS system referring to the DSQ Manual.

2. While in Standby condition, in OVEN page set the initial oven temperature to 30 °C.

3. In INLET SSL page set the inlet temperature to 0 (0 = Off).

4. When the inlet reaches the room temperature, enter in CARRIER page and uncheck the flow box to cut off the gas flow to the inlet.

Removing the Septum

5. Unscrew the septum cap.



6. Remove the septum holder with septum, then the septum support. See A of Figure 7-2.

Figure 7-2. Replace and Clean the Liner (1)

7. Use the liner cap wrench provided with the GC to remove the injector liner cap. See B of Figure 7-2.

8. Use tweezers to remove the liner with the graphite seal. See C of Figure 7-2.

CAUTION Be careful not to break the glass liner inside the injector when removing it. Glass splinters might fall into the lower part of the vaporization chamber. If the liner breaks, refer to Replace a Broken Liner.• If you are going to use a new liner, go to the step Cleaning the liner then

continue from the step Replacing the Liner.

• If you are going to clean the liner go to step Cleaning the liner then continue from the step Replacing the Liner.

• If you are going to remove a broken liner go to step Removing a Broken Liner then continue from the step Replacing the Linerr.



Cleaning the liner

a. Put the dirty liner into an ultrasonic bath filled with a methanol/acetone mixture (1:1) and sonicate it for about half an hour.

b. Using tweezers, remove the liner from the bath and dry it with compressed clean air.

NOTE For trace analysis, you should pre-treat the liner with a suitable silylating reagent prior to re-inserting it into the injector.

Removing a Broken Liner

a. Unscrew the nut that retains the analytical column, there move the analytical column with its ferrule. See D of Figure 7-3.

b. Unscrew the retaining nut at the bottom of the injector, the remove the terminal fitting with its silver seal. See E of Figure 7-3.

CAUTION Glass splinters from the broken liner will fall from the injector.

Figure 7-3. Replace a Broken Liner

c. With the aid of a pipe cleaner, remove the possible glass fragments from the vaporization chamber.



d. Reinsert the silver seal and the terminal fitting, and then tighten the nut that retains the terminal fitting. See F of Figure 7-3.

e. Insert the analytical column with its ferrule into the bottom of the injector in its previous position, then tighten the M4 retaining nut to hold the column in place. See G of Figure 7-3.

Replacing the Liner

9. Holding the new (or cleaned) liner with tweezers, place a graphite seal over the liner, making sure to leave a distance of about 10 mm between the seal and the liner end.

10. Using tweezers, insert the liner into the injector and push it gently towards the bottom fitting. See D of Figure 7-4.


CAUTION Make sure you insert the beveled end of the liner towards the bottom of the injector. Be careful not to damage the graphite seal or allow graphite to entering the liner. Should this occur, clean the liner with an inert gas.

11. Tighten the liner cap using the liner cap wrench provided with the GC. See E of Figure 7-4.



12. Remove the septum from the septum holder (use non-metallic tools).

13. Insert a new septum into the septum holder. See F of Figure 7-5.

CAUTION Use tweezers to avoid touching the septum with your fingers.


14. Clean the septum support from possible fragments left by the septum and reinsert it into the injector.

15. Place the septum holder on the top of the septum support (see G of Figure 7-5).

16. Tighten the injector cap to finger tight.

CAUTION Do not overtighten the injector cap. You could damage the septum and affect performance.

Restart the GC Conditions

17. In CARRIER, OVEN and INLET pages set the normal working conditions.

18. Perform an automatic leak check.


Chapter 7Maintenance and Troubleshooting Troubleshooting

TroubleshootingThis paragraph contains instructions for the instrument troubleshooting and a brief guide for the analytical troubleshooting.Systematic approach is required to cause identification and problem solving. For this is purpose, a method as the following one is suggested.

Electrical Connections• Ensure that the electrical line is grounded and the voltage supply stable.

• Verify that all the electrical connections between GC and eventual subsidiary units are correct.

Gases• Verify that the carrier gas line is turned on.

• Verify that the detector gases are set to the correct flow rate.

• Check that leaks are not present in the system.

Injection• Use syringe for gas chromatography having appropriate volume.

• The sample must be prepared and diluted correctly.

• Always inject the same sample volume.

• The split ratio must remain constant.

• If present, verify the autosampler performance.

• When an autosampler is used, the sample vials must be correctly crimped.

Chromatographic column• The column must be compatible with the analysis to be carried out; correctly

installed and conditioned before use.

• Verify that the column-to-inlet ferrule is not leaking.

• Verify the presence of gas leaking.


Chapter 7Troubleshooting Maintenance and Troubleshooting

• Check the column efficiency periodically.

Detector• Ensure that the detector parameters are correctly set.

• Check for eventual detector contamination.

Data System• Check that the Data System in use is properly connected.

Instrument TroubleshootingThe control unit of the GC performs a number of test routines to monitor and report on the status of the major chromatographic and control functions.Instrument malfunctioning, due to a component failure or to abnormal operating condition is identified by the red lighting of the Not Ready/Error LED located on the GC Status Panel.

The control unit of the GC performs a number of test routines to monitor and report on the status of the major chromatographic and control functions.Instrument malfunctioning, due to a component failure or to abnormal operating condition is identified by the red lighting of the Not Ready/Error LED located on the GC Status Panel.

When lit, this LED indicates that the injector and oven power has been cut off for safety reasons and an error message indicating the possible cause of error appears on the display. See Error Messages.


Chapter 7Maintenance and Troubleshooting Error Messages

Error MessagesThe following table reports the error messages and the explanation of the relevant correlated problem

Table 7-2. Error MessagesMessage Description

TEMP SHUTDOWN Loss of carrier

This message appears in two cases the carrier supply is missing and the actual pressure value is 0, or the actual pressure cannot reaches the setpoint value.

HARDWARE SHUTDOWN Oven T over limits

The oven temperature exceeds the temperature limits (350 °C). Error may be due to a probe malfunctioning.

HARDWARE SHUTDOWN Inlet T over limits

The inlet temperature exceeds the temperature limits (375 °C). Error may be due to a probe malfunctioning.

HARDWARE SHUTDOWN Det T over limits

The MS transfer line temperature exceeds the temperature limits (375 °C). Error may be due to a probe malfunctioning.

HARDWARE SHUTDOWN X line T over limits

This message appears when a MS detector is connected to the GC instead of FID. The MS detector transfer line detector temperature exceeds the temperature limits. Refer to the relevant MS detector manual.

TEMP SHUTDOWN Oven not heating

The oven is not heating.

TEMP SHUTDOWN Inlet not heating

The inlet not heating.

TEMP SHUTDOWN Det not heating

The detector is not heating.

TEMP SHUTDOWN X-line not heating

The MD detector transfer line not heating. Refer to the relevant MS detector manual.

TEMP SHUTDOWN Hydrogen alarm

Hydrogen flows inside the column oven. Probably leaks in the column connections or column breakage.

HARDWARE SHUTDOWN Undervoltage alarm

Voltage supply to electric circuits is too low.


Chapter 7Guide to Solve Analytical Problems Maintenance and Troubleshooting

Guide to Solve Analytical ProblemsRectifying faults in a chromatographic system is relatively simple, provided a logical and systematic problem-finding procedure is adopted.

Most faults can be identified from the chromatogram especially for test mixtures and we strongly recommend that a test mix be injected periodically to test the efficiency of the chromatographic system as well as the detector performance.Additionally, a leak must be performed should any part of the system be disturbed.

Finally, routine cleaning of injector and detector units will help to avoid problems occurring in the chromatographic system.


Chapter 7Maintenance and Troubleshooting Guide to Solve Analytical Problems

Baseline

Behavior Characteristics Cause Remedy

Drifting

Accumulation of stationary phase

Replace the end section of the column.

Carrier gas cylinder pressure too low to allow control

Replace the carrier gas cylinder or increase the pressure.

Drifting carrier gas or combustion gas flows

Check the gas controllers.

Accumulation of impurities in column

Check impurity levels in the gas source. Use correct gas purity.

Falling

Carrier gas leak in the system

Perform a leak test and ensure the tightness of the connections on the carrier gas line.

Column is baking out Allow enough time for the column to stabilize.

RisingAccumulation of impurities in column

Check impurity levels in the gas source. Use correct gas purity.

Contaminated detector Refer to detector ManualRising under temperature program operation

Column contaminated Recondition the column.

High-standing current

Carrier gas flow rate too high

Reduce the carrier gas flow.

Contaminated column Recondition the column.Contaminated gases Replace gas cylinders or gas

filters.


Chapter 7Guide to Solve Analytical Problems Maintenance and Troubleshooting


High-standing current(continued)

Excessive column stationary phase bleeding

Check the oven temperature, ensuring it doesn't exceed the column upper limit.Recondition the column.Replace the column.

Loose connections Ensure all interconnections and screw connections are tight.

Irregular shape

Dip after solvent peak

Detector contaminated Bake out or clean the detector.

S-shaped

Excessive column bleed during column temperature programming

Reduce the upper column temperature. Bake out the column. Install a high temperature column.

Oxygen contamination is decomposing the stationary phase

Install oxygen filters in carrier gas line.Check pneumatic and inlet systems for leaks. Use correct gas purity with low oxygen content.

Square wavesLarge AC power fluctuations; heavy equipment on same line

Use a dedicated clean AC line of sufficient amperage

Noise High-frequency noise

Contaminated detector Isolate the detector from electronics. If noise disappears, clean the detector.

Contaminated column Condition the column.Contaminated detector gas supply

Check the gas purity and install appropriate filters

Detector temperature higher than column maximum temperature

Reduce the detector temperature to the column temperature upper limit.


Chapter 7Maintenance and Troubleshooting Guide to Solve Analytical Problems


Noise(Continued)

High-frequency noise

External electrical interference

Attach an AC line monitor and check purity of the AC supply

Loose column fittings Tighten fittings accordingly.Loose detector electrical connections

Make sure the leads are properly connected.

Spiking External electrical interference

Attach an AC line monitor and check the purity of the AC supply



8
Use of the Virtual Keypad
This chapter provides basic information about of the functions and menus of the FOCUS GC Version for MS virtual keypad.

Chapter at a Glance…Overview ............................................................................................................148Virtual Keypad Main Menu................................................................................152Time....................................................................................................................157Valves .................................................................................................................158Run Time Events ................................................................................................159Run-Log..............................................................................................................160Configuration......................................................................................................162Info/Diagnostics .................................................................................................167

147

Chapter 8Use of the Virtual Keypad Overview

OverviewThe virtual keypad of the FOCUS GC has three components:

• a line-line display

• display LEDs showing the instrument’s status

• a keypad for data entry.

Each component is discussed in order from the top down. Figure 8-1 illustrates the complete FOCUS GC virtual keypad.

Figure 8-1. The Virtual Keypad

The DisplayThe display shows the menus you use to control the GC parameters, settings, and configuration options. The data entry keys allow you to scroll through, set, and modify the menu information.

Figure 8-2 shows the components of a typical menu display.

Figure 8-2. Components of the Menu Display

Menu TitleParameter Line

Actual Value

Setpoint Value

Scroll Indicator


Chapter 8Overview Use of the Virtual Keypad

The following are the menu display components:

Menu Title—This is the first line of each menu. The menu title remains at the top of the display and does not move, even when you scroll up and down the menu items.

Cursor—The cursor indicates the currently selected menu item. Use the UP ARROW and DOWN ARROW keys to move the cursor.

Setpoint Value and Actual Value—Many parameters display two values. The first value is the actual value of the GC parameter. You enter the second value, which is the setpoint.

Scroll Indicator—This item is found in the upper right corner of the display. It indicates when not-currently visible menu items exist. It appears in three ways:

• ↓, indicating that you can scroll downward

• ↑ , indicating that you can scroll upward

• , indicating that you can scroll in either direction

Currently Visible Menu Parameters—The display shows four lines of a menu at a time. Because the menu title always takes up the first line, three lines show menu items.

Not Currently Visible Menu Parameters—The display shows three menu items at a time. If a menu contains more than three lines, you can use the arrow keys to scroll through the rest of the menu items.

The Display LEDsThe LEDs (Light Emitting Diodes) on the left side of the display screen indicate the FOCUS GC’s operating status.The status LEDs indicate the current operating mode and special settings activated by the operator. Table 8-1 lists and explains each status LED.

↔


Chapter 8Use of the Virtual Keypad Overview

The FOCUS GC Virtual KeypadThe following Table lists and describe the keys on the FOCUS GC virtual keypad.

Table 8-1. Status LED DescriptionsLED Description

Not Ready/Error This LED lights when the GC is not ready to make a run, usually because the specified oven temperature has not been reached. It remains lit if any additional equilibration time has been configured. It blinks when the GC has one or more error conditions.

Standby/Prep Run This LED lights when the GC is in Standby, waiting to be advanced to the Ready status. It blinks links while the GC prepares for a run, for example, while opening or closing valves as required by the method or waiting for an external device such as a mass spectrometer.

Ready to Inject This LED lights when the prep run has finished, indicating you can inject a sample or start an autosampler.

Run This LED lights when a run is in progress.

Table 8-2. Keypad DescriptionsKey Description

The blue START key is a double function key. When pressed a first time it starts the PREP RUN function. When pressed a second time, it starts a run with programmed parameters after you manually inject a sample into the inlet. When a remote start by another device, such as an autosampler, has been programmed, the system automatically starts after injection.The red octagonal STOP key has the following functions:- stops a run in progress- resets the FOCUS GC from READY to NOT READYSTATUS key displays the instrument status and any reasons the GC is in Not Ready mode.


Chapter 8Overview Use of the Virtual Keypad

Parameters EntryThe user points to any of the parameter navigating with the keys HOME, SCROLL UP and SCROLL DOWN.

Only the bottom line is dedicated to parameters editing, first line is only for menu title and doesn’t scroll. Once you have reached the line related to the parameter to change, type the number with the numeric kaypad or increase or decrease the value by the INC and DEC keys. During parameter editing the value is blinking..

When the set value is the desired one, by pressing the key ENTER, the value is accepted.

Any key different from ENTER, INC, DEC will escape parameter editing without variation.

HOME key opens Main Menu and returns precedent page menu. The data entry keys allow you to scroll through, set, and modify the menu information.

Use the SCROLL UP and SCROLL DOWN arrow keys to scroll through a list of menus or to move the cursor to an editable field.

INC key (increase) allows increasing the parameter value.

DEC key (decrease) allows decreasing the parameter value.

ENTER key confirms changes to a selected menu item

OVEN Title Line

Temp 100 100 Editing Line

Table 8-2. Keypad Descriptions (Continued)Key Description


Chapter 8Use of the Virtual Keypad Virtual Keypad Main Menu

Virtual Keypad Main Menu To open main menu, press HOME key. Main menu contains the following page menus available sequentially by pressing the SCROLL UP and SCROLL DOWN arrow keys.

To open a page menu move the cursor up to the menu of interest, then press ENTER key. To return precedent page menu press HOME key.

OvenUse the Oven page to set temperatures, times and ramp rates. You can program up to seven temperature ramps per run.

FOCUS GC

OVEN

INLET

CARRIER

DETECTOR

SIGNAL

AUTOSAMPLER

OTHERS

OVEN

Temp 100 100

Initial time 90.00

Ramp 1 120.0

Final temp 1 100

Final time 1 60.00

Ramp 2 Off


Chapter 8Virtual Keypad Main Menu Use of the Virtual Keypad

InletUse this page to set inlet parameters such as temperature and split flow.The Mode menu items displays the current operating mode. Use INC and DEC keys to modify the selection.

The items in the inlet menu vary depending on the operating mode you select in the INLET menu. The following table shows the split/splitless inlet menu for the operating modes.

CarrierUse this page to display in the carrier menus vary with the pressure and flow modes you select.

INLET

Mode Split

Split Mode Splitless Mode Surge Splitless Mode

INLET INLET INLET

Temp 200.. 200

Mode Split

Total flow (150.0)

Split flow 100 100

Split ratio 1000.0

Temp 200..200

Mode Splitless

Total flow (150.0)

Split flow 100 100

Splitless time 1.00

Const sept purge Off

Stop purge for 1.00

Temp 200..200

Mode Surge Splitless

Total flow (150.0)

Split flow 100 100

Splitless time 1.00

Surge pressure 100

Surge duration 1.00

Const sept purge Off

Stop purge for 1.00

CARRIER

Flow mode Const flow



You have a choice of two flow modes:

• Constant pressure mode, which sets pressure only

• Constant flow mode which maintains a specific flow rate through the column.

The items in the carrier menu vary depending on the operating mode you select in the CARRIER menu. The following table shows carrier menu for the operating modes.

How to Perform a Leak Check

1. Scroll to Leak check and press ENTER to open Leak Check menu.

2. To start the leak check, scroll to Run leak check and press ENTER

CARRIER (He) CARRIER (He)

Pressure (100)

Col.Flow 12.0 12.0

Flow mode Const flow

Gas saver flow 100

Saver time 1.00

Vacuum comp. Off

Leak check

Column evaluation

Pressure 100 100

Col.Flow (10.0)

Flow mode Const Pres

Gas saver flow 100

Saver time 1.00

Vacuum comp. Off

Leak check

Column Evaluation

Carrier Menu in Constant Flow Mode

Carrier Menu in Constant Pressure Mode

LEAK CHECK

Run leak check

Exit w/o leak check


Chapter 8Virtual Keypad Main Menu Use of the Virtual Keypad

How to perform a Column Evaluation

1. Scroll to Column evaluation and press ENTER to open COLUMN EVALUATION menu.

2. To start column evaluation, scroll to Run column eval and press ENTER

DetectorUse this page to display the MS detector menu.

SignalThis page is not available.

AutosamplerAutosampler is controlled only by Xcalibur System.When the autosampler is not present or when the GC is connected to the data system, the following messages are respectively displayed..

COLUMN EVALUATION

Run column eval.

K = 100.0000

Exit w/o column eval

DETECTOR

MS Line Temp 100 100

AUTOSAMPLER AUTOSAMPLER

Not present Locked by Data System



Others.

Use this page to entry the following submenu:

• Time

• Valves

• Run Time Events

• Run-Log

• Configuration

• Info/Diagnostics

For details refer to the relevant paragraphs in this chapter.

OTHERS

Configuration


Chapter 8Time Use of the Virtual Keypad

TimeThis option allows you to visualize the following parameter

• Time

• Date

• Last run time

• Next run time

• Elapsed time and time remaining during the current run

• The column flow calculator

In Main Menu move the cursor until the Others page is selected, then press ENTER. Scroll to Time then press ENTER

When the GC is not running a menu appears as the following:

When the GC is running a menu appears as the following:

OTHERS

Time

TIME

Next routine 15.00

Last routine 120.00

We 13 Mar 2002 12:03

V=100 F=100.0 01:00

Flowmeter volume 100


Chapter 8Use of the Virtual Keypad Valves

ValvesUse this feature to specify and control up to four valves, as well as to manually change the state of inlet valves. For instance you can manually:

• Open or close the S/SL inlet valves before or during a run

• Switch a gas sampling valve from load to inject position

• Activate or deactivate an external event

In Main Menu move the cursor until the Others page is selected, then press ENTER. Scroll to Valves then press ENTER

When a gas sampling valve is not present a menu appears as the following:

TIME

Elapsed time 5.00

Time left 110.00

We 13 Mar 2002 12:03

V=100 F=100.0 01:00

Measured volume 100

OTHERS

Valves

VALVES

Split valve Off

Sept purge valve On

EV#1 Off

EV#2 Off


Chapter 8Run Time Events Use of the Virtual Keypad

When a gas sampling valve is present and configured (refer to Valves Configuration Menu in paragraph Configuration) a menu appears as the following:

Run Time EventsThis options allows you to program events to happen prior to or during a run. For instance, a valve could open two minute into a run.You can program:

• An output signal adjustment, such as autozero.

• A valve to open or close.

• An external event from another device.

In Main Menu move the cursor until Others page is selected, then press ENTER. Scroll to Run time event then press ENTER.

The first time you program a time event (Run Time Events empty) the following menu appears:

VALVES

Split valve Off

Sept purge valve On

GSValve#1 Load

EV#2 Off

OTHERS

Run Time Events

RUN TIME EVENTS

<None>

Add run time event


Chapter 8Use of the Virtual Keypad Run-Log

In RUN TIME EVENTS menu scroll to Add run time events and press ENTER: The following menu appears:.

Run-LogThis function displays the run log, which records error or the method modifications that happens during run time. It display the time and description any deviation that occur.

The run log keeps track of any errors or deviations during the run. This information can be used to meet good laboratory practice (GLP) standards.For example, if you interrupt the run for any reason, the run log will record the time the run stopped and an interpretation of the event. The Run-log is cleared and reset at the beginning of the next run.

When the run log contains entries, it is shown in the STATUS menu.

To see the journal of events, in Main Menu move the cursor until the Others page is selected, then press ENTER. Scroll to Run-log then press ENTER

An example of Run-log is shown below.

EDIT EVENTS

Event EV#1

Run time Pre run

Setpoint 2

Next event

OTHERS

Run-log


Chapter 8Run-Log Use of the Virtual Keypad

RUN LOG (XofY) 1

Itime 200.00 ’ 220.00at run time 0.50

ITemp 120 ’ 100at run time 2.00

Ftime 1.00 ’ 10.00at run time 2.50

Ramp2 50.0 ’ 120.0at run time 3.10

Oven T is 105 (110)

at run time 3.40

(continue)

2

3


Chapter 8Use of the Virtual Keypad Configuration

ConfigurationThis paragraph describes how to configure your FOCUS GC.

When to ConfigureThe FOCUS GC has few special set up sequences. After you first install and configure the instrument, you will need to reconfigure only after you make changes to the components. You must configure the system when:

• using the FOCUS GC for the first time

• changing carrier gases

• changing column types (to set the appropriate maximum oven temperature)

For details refer to Configuration Menu.

Configuration MenuIn Main Menu move to cursor until the Others page appears, then press ENTER.

.

Scroll to Configuration and press ENTER. The following table describes the items in the Configuration menu. Each item has a submenu.

OTHERS

Configuration

Table 8-3. Configuration MenuMenu Description

CONFIGURATION This line is the title barOven Controls preparatory actions such as an automatic prep

run, timeout, equilibration time.Carrier This parameter controls the type of carrier gas.Autosampler Not active


Chapter 8Configuration Use of the Virtual Keypad

Oven Configuration MenuThe FOCUS GC oven provides great flexibility in controlling and programming temperatures. In the CONFIGURE OVEN menu you can set various preparatory parameters.

Carrier Configuration MenuCommonly used gases are Helium, Nitrogen and Hydrogen.

You specify the type of carrier gas in the CONFIGURE CARRIER menu by using the INC and DEC key.

General This parameter controls the RS 232 Baud rate for the communication with an external device and the Main supply frequency

Keyboard and Display

This parameters controls keypad and display preferences.

Handshake This parameter configures the polarity of signals from external device

Time This parameter sets the time and dataValves This parameter controls an eventual gas sampling valve

CONFIGURE OVEN

Max temperature 300

Equilib. Time 10.00

Auto prep run Off

Auto start Off

Prep-run timeout 10

Table 8-3. Configuration Menu (Continued)Menu Description



WARNING! You cannot choose hydrogen as a carrier gas unless your instrument has a hydrogen sensor. See Using Hydrogen.

Autosampler Configuration MenuThe autosampler is controlled by the data system. When the autosampler is not present or if the GC is connected to the data system the following messages are respectively displayed:

General Configuration MenuUse this item to set the mains supply frequency of the country where the GC is installed. Use the INC and DEC key the select the required value.

Keyboard & Display Configuration MenuThis menu allows you to customize your keyboard and display.Keyboard beep leads to a submenu where you can specify when you want the GC to alert you with a keyboard sound. To move to the submenu, select Keyboard beep and press ENTER.

CONFIGURE CARRIER

Gas Type Helium

CONFIG AUTOSAMPLER CONFIG AUTOSAMPLER

Not present Locked by Data System

GENERAL CONFIG

Baud rate 38400

AC mains freq. 50


Chapter 8Configuration Use of the Virtual Keypad

Keyb. Beep causes the GC to beep when you press the key specified in the submenu.

Beep Submenu

Handshake Configuration MenuThe FOCUS GC can cooperate with other instruments, such as an autosampler or mass spectrometer, during analysis. To allow other devices to run properly, you must indicate how the signal will change. For example, the menu specifies that another device will start the GC when the remote start signal changes from high to low.

CONFIG KEYB. & DISP.

Keyboard lock Off

Keyb. Beep Enter key

Delimeter type “.”

Pressure unit kPa

Brightness 3

KEYBOARD BEEP:

All keys

Enter key press

On invalid key

Never



Time Configuration MenuThe current date and time are displayed. You can set this time from the CONFIGURE menu. When you open the CONFIGURE TIME menu, the following items appear:

NOTE Time is set on a 24-hour clock.

Valves Configuration MenuYou can configure two gas sampling valves, when present, and program two external events to be the default condition for an external device. See also Run Time Events

CONFIG HANDSHAKE

Remote start in H L

Inhibit ready High

End of run out H L

Start of run out H L

GC ready out High

Prep run out High

CONFIGURE TIME

Time: 18:14:11

Date: Mon 11/Mar/2002

CONFIGURE VALVES

Valve#1 Gas sampling

Valve#2 none

EV#1 default Off

EV#2 default On


Chapter 8Info/Diagnostics Use of the Virtual Keypad

Info/DiagnosticsUse this feature to bring up hardware, software and diagnostic information

In Main Menu move the cursor until the Others page is selected, then press ENTER. Scroll to Info/Diagnostics then press ENTER

A menu appears as the following:

OTHERS

Info/Diagnostics

INFO/DIAGNOSTICS

Serial #: 12345678

FW ver: 2.00.31

DPFC ver: 0.27

BOOT ver: 1 B.0

Manufact.: 1/Jan/02

Total runs 1234567

Ambient press 103.0

OV 31.8 F= 27 S=off

IN 41.8 F= 30 S=off

DT 25.3 F= 25 S=off

OVPL 3 10°C 0.7%

Table 8-4. Info/DiagnosticsParameter Description

INFO/DIAGNOSTICS This line is the title barSerial # T The number (eight figures) indicates the product code.FM ver: Indicates the version of the firmwareDPFC ver: Indicates the version of the DPFC module


Chapter 8Use of the Virtual Keypad Info/Diagnostics

BOOT ver: Data for Thermo Electron authorized technical personnel only.

Manufact.: Indicates the manufacturing date of your GC.Total runs The number (seven figures) Indicates the performed

analyses.Ambient press Indicates the ambient pressure expressed in kPa.OV, IN, DT, OVPL Diagnostics data for Thermo Electron authorized

technical personnel only.

Table 8-4. Info/DiagnosticsParameter Description



A
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Glossary
This section contains an alphabetical list and descriptions of terms used in this guide and the help diskette. It also includes abbreviations, acronyms, metric prefixes, and symbols.
AA ampere

ac alternating current

ADC analog-to-digital converter

Bb bit

B byte (8 b)

baud rate data transmission speed in events per second

CºC Celsius

CIP Carriage and Insurance Paid To

cm centimeter

CPU central processing unit (of a computer)

CSE Customer Service Engineer

Dd depth

DAC digital-to-analog converter

dc direct current

DS data system


Glossary

EECD Electron Capture Detector

EMC electromagnetic compatibility

ESD electrostatic discharge

FºF Fahrenheit

FID Flame Ionization Detector

FOB Free on Board

FPD Flame Photometric Detector

ft foot

Gg gram

gain A measure of the ability of an electronic circuit or device toincrease the magnitude of an electronic input parameter.

GC gas chromatograph

GND electrical ground

Hh height

h hour

harmonicdistortion

A high-frequency disturbance that appears as distortion of thefundamental sine wave.

HOT OC High Oven Temperature Cold On-Column Injector

HV high voltage


Glossary

Hz hertz (cycles per second)

IID inside diameter

IEC International Electrotechnical Commission

impulse See transient

in inch

I/O input/output

Kk kilo (103 or 1024)

K Kelvin

kg kilogram

kPa kilopascal

Ll length

l liter

lb pound

LED light-emitting diode

LVOCI Large Volume On-Column Injector

Mm meter (or milli [10-3])

M mega (106)

µ micro (10-6)

MBq megabecquerel


Glossary

mCi millicurie

meniscus The curved upper surface of a column of liquid.

min minute

mL milliliter

mm millimeter

m/z mass-to-charge ratio

Nn nano (10-9)

negative polarity The inverse of a detector signal polarity.

nm nanometer

NPD Nitrogen Phosphorous Detector

OOCI On-Column Injector

OD outside diameter

Ω ohm

Pp pico (10-12)

Pa pascal

PCB printed circuit board

PDD Pulsed Discharge Detector

PID Photoionization Detector

PKD Packed Column Injector

PN part number


Glossary

PPKD Purged Packed Column Injector

psi pounds per square inch

PTV Programmable Temperature Vaporizing Injector

RRAM random access memory

RF radio frequency

ROM read-only memory

RS-232 industry standard for serial communications

Ss second

S/SL Split/Splitless Injector

sag See surge

slow average A gradual, long-term change in average RMS voltage level,with typical durations greater than 2 s.

source current The current needed to ignite a source, such as a detectorlamp.

surge A sudden change in average RMS voltage level, with typicalduration between 50 µs and 2 s.

TTCD Thermal Conductivity Detector

transient A brief voltage surge of up to several thousand volts, with aduration of less than 50 µs.

V


Glossary

NOTE The symbol for a compound unit that is a quotient (for example, degrees Celsius per minute or grams per liter) is written with a negative exponent with the denominator. For example:° C min-1 instead of ° C/min g L-1 instead of g/L

V volt

V ac volts, alternating current

V dc volts, direct current

VGA Video Graphics Array

Ww Width

W Watt


Index
AAbout This Manual xiii
Conventions Used xvOverview xiii

Analytical Problems 143Analytical Unit 26

CCapillary Column

How to connect 79Carrier Gas

Control 27Inlet Port 35

Carrier Page 114Cleaning xxiv, 130Cleaning the unit 27Column 77

Conditioning 91Installation 79Keeping Leaks Under Control 82

Column Evaluation 82Column Ferrules 78Column Oven 28, 31Column oven 26Columns 28

Fittings 78Ferrules 78Retaining Nuts 78

Configuring the FOCUS GC 94Control Panel 27, 31

GC User Interface 39Conventions Used xvColumn

Using Correct Fittings 78

DDecontaminating the unit 27Decontamination xxivDetector 29Detector compartment 26Display 27, 148Display LEDs 149DPFC Module 27


EElectrical Connections 35Electronic Compartment 27, 32Error Messages 142Event Time Group Box 120Expected K Factor 85Exterior

cleaning xxivExternal Devices

Autosamplers 30External Event Group Box 121

FFerrules 78FOCUS GC version for MS

Components 26Configuration 94Description 25Document Set xx

Front Panel 30Instrument

Overview 26Setup 99Pull-up Menu 102

GGas Control 27

Carrier 27GC Left Hand-side Panel 38GC Parts

Description 30Getting Started 93Glass Liner

Breakage 132Guide to Solve Analytical Problems 143

HHazardous material

decontamination xxivspills xxiv

High Voltage Section 33High-voltage compartment 27Hot Empty Needle Injection 67, 72How To Perform Maintenance 128Hydrogen

181

Index

SensorUse xxiv

Use xxiiiHydrogen Sensor xxiv

IInitial Values 119Injector 28Injector compartment 26Inlet Parameters 73Inlet SSL Page 108Instrument

Automation 29Classification xxiMarkings xviiiSymbols xviii

Instrument Automation 29Instrument Cleaning 130Instrument Overview 26Instrument Troubleshooting 141Item 119

KK Factor 85

Tables 85Keypad 150

LLeak

Identifying 82Manual Checking 83Removing 82

Leal CheckPerforming an Automatic 89

LEDsDisplay 149Not Ready/Error 32, 150Standby/Prep Run 32, 150

Liner 65Cleaning 131Replacing 131

Liners 62Low Voltage Section 33

182

MMaintanance

SSL Injector 131Maintenance 127, 128

FID 140Schedule Table 129Suggested Schedule 128

Markings xviiiMaterial Safety Data Sheets xxivMethod Editing 103Methods and Sequences 30Microseal™ Valve 62MS Detector 29MS Transfer Line Page 117

NNot Ready/Error LED 32, 150

OOCI. See On-Column InjectorOn-Column Injector 28Oven Exhaust Vent 37Oven Page 104

PPneumatic Compartment 26Pneumatic compartment 26Preliminary Check 125

RRear Panel 34Replace the Standard Septum 133Retaining Nuts 78Roadmap-Home Page 96Run Table 118

SS/SL

Constant Septum Purge 76Injection Technique 67Injection Techniques 67Inlet Parameters 73Packed Column 64Parameters

Inlet 74


Index

PrametersPurge 75

Split Flow 75Split Ratio 75Splitless Time 75Stop Purge Time 76Surge Duration 76Surge Pressure 76Temperature 75Wide-Bore Injection with a Tapered Liner 63

S/SL Overview 58S/SL Parameters

Mode 74Surge 76

S/SL. See Split/Splitless InjectorSafety Information xxii

Use of Gases xxiisafety symbols xv–xixSample

Refocusing 71Septum 65Settings 119Solve Analytical Problems 143Solvent Effec 71Split 74Split Injection Technique 67Split/Splitless

Injector Components 61Split/Splitless Injector 57, 58

Liners 62Menus 65Overview 58Packed Columns 64Septum 62Split Injection Technique 67Splitless Injection Technique 69

cold trapping 71flooding 72sample refocusing 71solvent effect 71

Split/Splitless Injector (S/SL) 57Splitless 74Splitless Injection Technique 69Splitless w/surge 74SSL


Gas Control 59Septum Purge System 60

Standard Septum 62Cleaning 135Replacement 133, 135Replacing 131

Standby/Prep Run LED 32, 150Symbols xviii

TTechnical Features xxiTemperature Effect 71Time 119Top Panel 37Troubleshooting 127, 140

Instrument 141

UUse of Gases xxiiuser interface 27Using Hydrogen xxiiiUsing the Hydrogen Sensor xxiv

VValve Event 120Valves Manual Activations 124Virtual Keypad 122

183

Index

184

Operating SequencesConfiguring the Carrier Gas ..............................................................................................................43Configuring the Pressure Unit ...........................................................................................................43Installing a Liner and a Septum .........................................................................................................65How to Connect a Capillary Column .................................................................................................79Manual Checking for Leaks ...............................................................................................................83Performing a Column Evaluation ......................................................................................................84Performing an Automatic Leak Check ..............................................................................................89Setting Up a Single Ramp Temperature Program .............................................................................106Setting Up Multiple Ramp Temperature Program .............................................................................107Programming the Split Mode .............................................................................................................111Programming the Splitless Mode .......................................................................................................112Programming the Surge Splitless Mode ............................................................................................113Programming The Carrier Gas Parameters ........................................................................................116How to Start-up the Instrument .........................................................................................................125Replace the Standard Septum ............................................................................................................133Replace or Clean the Liner when a Standard Septum is Installed .....................................................135

List of FiguresFigure 1-1. FOCUS GC Components .............................................................................................26Figure 1-2. Front Panel....................................................................................................................30Figure 1-3. Column Oven Internal View ........................................................................................31Figure 1-4. Status Panel ..................................................................................................................31Figure 1-5. Electronic Compartment...............................................................................................33Figure 1-6. Rear Panel.....................................................................................................................34Figure 1-7. Electrical Connections..................................................................................................36Figure 1-8. Rear Panel.....................................................................................................................37Figure 1-9. GC Left Hand-side Internal View ................................................................................38Figure 1-10. User Interface ...............................................................................................................39

Figure 2-1. DPFC Module...............................................................................................................44Figure 2-2. Carrier Gas Page...........................................................................................................45

Figure 3-1. The Column Oven ........................................................................................................50Figure 3-2. Oven Air Circulation ....................................................................................................51Figure 3-3. Oven Page.....................................................................................................................52

Figure 4-1. Split/Splitless Injector ..................................................................................................58Figure 4-2. Gas Control...................................................................................................................59Figure 4-3. Septum Purge System...................................................................................................60Figure 4-4. Split/Splitless Injector Components .............................................................................61Figure 4-5. S/SL Wide-Bore Injection with a Tapered Liner .........................................................63Figure 4-6. S/SL with a Packed Column.........................................................................................64Figure 4-7. Split Injection Technique .............................................................................................68Figure 4-8. Splitless Injection Technique .......................................................................................70Figure 4-9. S/SL Inlet Page .............................................................................................................73

Figure 6-1. Instrument Configuration Dialog Window...................................................................94Figure 6-2. FOCUS GC Configuration Page ..................................................................................95Figure 6-3. Roadmap-Home Page...................................................................................................96Figure 6-4. FOCUS GC Setup Page................................................................................................99Figure 6-5. FOCUS GC Pull-up Menu............................................................................................102Figure 6-6. The Oven Page .............................................................................................................104Figure 6-7. The Inlet SSL Page.......................................................................................................108Figure 6-8. The Carrier Page...........................................................................................................114Figure 6-9. The MS Transfer Line Page .........................................................................................117

Figure 6-10. Run Table Page.............................................................................................................118Figure 6-11. ADD/Edit Run-Time Event Screen ..............................................................................120Figure 6-12. Control Panel - Virtual Keypad....................................................................................122Figure 6-13. Valves Dialog Window ................................................................................................124

Figure 7-1. Replace the Septum ......................................................................................................134Figure 7-2. Replace and Clean the Liner (1) ...................................................................................136Figure 7-3. Replace a Broken Liner ................................................................................................137Figure 7-4. Replace and Clean the Liner (2) ...................................................................................138Figure 7-5. Replace and Clean the Liner (3) ...................................................................................139

Figure 8-1. The FOCUS GC Versione for MS Virtual Keypad......................................................148Figure 8-2. Components of the FOCUS GC Menu Display ...........................................................148

List of TablesTable 1-1. Status LED Descriptions ..............................................................................................32

Table 4-1. Liner Sizes and Applications........................................................................................62

Table 5-1. Ferrules .........................................................................................................................78

Table 7-1. Standard Maintenance Schedule...................................................................................129Table 7-2. Error Messages .............................................................................................................142

Table 8-1. Status LED Descriptions ..............................................................................................150Table 8-2. Keypad Descriptions ....................................................................................................150Table 8-3. Configuration Menu .....................................................................................................162Table 8-4. Info/Diagnostics ...........................................................................................................167

Thermp Scientific - Operating Manual Focus GC

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