Note: Intro -- Half Title -- Title -- Copyright -- Preface -- Introduction -- Contents -- 1 Sample Collection and Preparation: How Do I Get My Sample Ready for GC-MS Analysis? -- 1.1 How Do I Collect and Sample a Gas for GC or GC-MS Analysis? -- 1.1.1 What Is Spot Analysis? -- 1.1.2 How Do I Sub-sample with a Canister or Sampling Bag? -- 1.1.3 What Is Active Sampling? -- 1.1.4 What Is Passive Sampling? -- 1.1.5 What Is Online Sampling? -- 1.2 How Do I Sample and Prepare a Liquid for GC or GC-MS Analysis? -- 1.2.1 How Do I Store My Liquid Samples? -- 1.2.2 Which Solvents Can I Use in Sample Preparation for Injection into a GC? -- 1.2.3 Which Sample Preparation Techniques Can Be Used for Liquid Samples with GC-MS Analysis? -- 1.2.4 How Can I Prepare Liquid Samples with a Liquid Phase? -- 1.2.5 How Can I Prepare Liquid Samples with a Solid Phase? -- 1.2.6 How Can I Prepare Liquid Samples Thermally? -- 1.3 How Do I Sample and Prepare a Solid for GC or GC-MS Analysis? -- 1.3.1 Can I Use Thermal Desorption? -- 1.3.2 When Should I Use Analytical Pyrolysis for Solid Samples? -- 1.3.3 What Liquid Extraction Techniques Can Be Used? -- 1.3.4 What Is Microwave Extraction? -- 1.3.5 What Is Pressurised Fluid Extraction? -- 1.4 When Should I Use Derivatisation in GC-MS Analysis? -- 1.5 How Do I Know How Well My Sample Preparation Has Worked? -- 2 How Do I Introduce My Samples into the GC Column? -- 2.1 How Do I Inject My Sample into the GC? -- 2.2 How Do I Transfer My Introduced Sample into the Analytical Column? -- 2.3 How Do I Select Which Inlet Is Suited for My Application? -- 2.3.1 On-column Inlets -- 2.3.2 Split and Splitless Inlets -- 2.3.3 Programmable Temperature Vaporiser Inlets -- 2.4 Comparison of Injection Techniques -- 2.4.1 How Do I Select and Optimise My Inlet Method Parameters and Consumables? -- 2.4.2 Injection Volume -- 2.4.3 Temperatures. , 2.4.4 Sample Transfer Time to the Column -- 2.4.5 Split/Vent Flows -- 2.4.6 Liner Size and Style -- 2.4.7 Liner Packing Material -- 2.4.8 Deactivation -- 2.4.9 Septum -- 2.5 How Do I Introduce a Gas into the Gas Chromatograph? -- References -- 3 Chromatographic Separation -- 3.1 How Do I Assess the Quality of My Chromatographic Separation? -- 3.1.1 Chromatographic Systems -- 3.1.2 Separation Techniques -- 3.2 How Do I Select the Right Stationary Phase and Column Chemistry? -- 3.3 Theoretical Background and Definition of Chromatographic Terms -- 3.3.1 Retention on the Column -- 3.3.2 Capacity Factor -- 3.3.3 Resolution -- 3.3.4 Selectivity Factor -- 3.3.5 Band Broadening and Column Efficiency -- 3.3.6 Rate Theory and Band Broadening -- 3.4 How Do I Select the Best Mobile Phase to Give Me the Best Efficiency? -- 3.5 How Do I Reduce Retention Time? -- 3.6 How Do I Evaluate the Separation of Closely Eluting Bands in a Chromatogram? -- 3.7 How Do I Optimise Column Performance? -- 4 How Do I Detect My Analytes? -- 4.1 What Types of GC Detectors Are There? -- 4.2 What Is a FID? -- 4.2.1 How Does a FID Work? -- 4.2.2 What Parameters Do I Need to Optimise When Using a FID? -- 4.3 What Is an ECD? -- 4.3.1 How Do an ECD and µECD Work? -- 4.3.2 What Parameters Do I Need to Optimise When Using an ECD? -- 4.4 What Is a Thermal Conductivity Detector? -- 4.4.1 How Does a TCD Work? -- 4.4.2 What Parameters Do I Need to Optimise When Using a TCD? -- 4.5 Why Would I Choose a GC-MS Over Other GC Detectors? -- 4.6 How Do I Connect My Analytical Column to Two or More Detectors? -- 5 Mass Analysis -- 5.1 A Historical Perspective: Why Do I Need Ions for MS Analysis? -- 5.1.1 Are Mass Spectrometers Sophisticated Balances That Are Able to Determine the Mass of a Molecule? -- 5.2 Introduction to Mass Spectrometry. , 5.2.1 What Are the Basic Fundamentals Needed for Understanding MS? -- 5.2.2 Mass -- 5.2.3 Atoms of Elements and Isotopes -- 5.2.4 Atomic Mass and the Unified Atomic Mass Unit -- 5.2.5 Nominal Mass -- 5.2.6 What Is the Mass-to-charge Ratio? -- 5.2.7 Isotopic Mass and Monoisotopic Mass of a Molecule or Ion -- 5.2.8 Relative Atomic and Molecular Mass -- 5.3 Basic Aspects of MS Instrumentation and GC-MS -- 5.3.1 Are All Compounds Suited for GC-MS Analysis? -- 5.3.2 How Do I Select the Ionisation to Fit to a GC Front End Separation? -- 5.3.3 How Do I Ensure That the Mass Spectrometer Will Produce Good Spectra? -- 5.3.4 How Do I Keep My Mass Spectrometer Running Optimally? -- 5.3.5 Why Do I Need a GC for the Analysis of a Complex Mixture of Compounds? -- 5.3.6 Are There Artefacts From the Analytical Technique - What Should I Be Aware of? -- 5.4 How Are Ions Generated in a MS Instrument? -- 5.4.1 Electron (Impact) Ionisation -- 5.4.2 Chemical Ionisation -- 5.5 How Is the Mass-to-charge (m/z) Ratio Determined in a Mass Spectrometer? -- 5.5.1 Ion Acceleration -- 5.5.2 Time of Flight Analysers -- 5.5.3 Quadrupole Mass Analyser -- 5.5.4 Quadrupole Ion Trap -- 5.5.5 What Is Unit Mass Resolution? -- 5.5.6 How Are the Separated Ions Detected? -- 5.6 What Parameters Do I Need to Optimise When Using an MS? -- 5.6.1 How Do I Choose the Scan Range and Scan Speed for My Analysis? -- 5.6.2 How Do I Choose My Ions for SIM and Set-up My SIM Groups? -- 5.6.3 What Temperatures Need to Be Optimised in an MS? -- 5.6.4 What Is the Solvent Delay or Cut Time and How Do I Optimise It? -- 5.6.5 What Detector Parameters Require Optimisation? -- 5.6.6 What GC Parameter Considerations Are There When Hyphenating with an MS? -- References -- 6 What Is Qualitative Analysis and How Do I Perform It? -- 6.1 How Can I Use My GC-MS Chromatogram and Spectral Data?. , 6.2 What Information Can I Extract from the Chromatogram About Data Quality? -- 6.2.1 What Is the Baseline? -- 6.2.2 Chromatographic Resolution -- 6.2.3 Column Efficiency -- 6.2.4 Signal-to-Noise Ratio -- 6.2.5 Peak Symmetry -- 6.3 How Do I Determine if My Analytes Are Present or Not? -- 6.3.1 How Do I Integrate Peaks? -- 6.3.2 What Affects the Peak Integration? -- 6.3.3 How Do I Integrate Coeluting Peaks? -- 6.3.4 Retention Time -- 6.3.5 Kovats Retention Index -- 6.4 How Do I Identify Peaks? -- 6.4.1 How Do I Extract a High-quality Mass Spectrum? -- 6.4.2 How Do I Perform a Library Search? -- 6.4.3 My Mass Spectrum Is not in the Library, How Do I Determine What It Is? -- 7 Basic Aspects of Mass Spectra Interpretation -- 7.1 What Information Does the Molecular Ion in EI-MS [M]+˙ Give Me? -- 7.1.1 What Is a Molecular Ion? -- 7.1.2 What Is the Nitrogen Rule? -- 7.1.3 Double Bond-equivalents -- 7.1.4 What Information Does the Isotopic Patterns of the Molecular Ion [M]+˙ in EI-Mass Spectra Give Me? -- 7.2 What Information Do the EI-MS Fragment Ions Give Me? -- 7.2.1 What Are Localised Charges? -- 7.2.2 How Do I Correctly Discuss MS Fragmentation Processes? -- 7.2.3 Typical Fragmentation and Rearrangement Reactions in EI-MS -- 7.2.4 Fragmentation of Unactivated C-C Sigma Bonds: OE+˙ → EE+ + R˙ -- 7.2.5 Fragmentation of Activated Sigma Bonds: Allylic and Benzylic Cleavage -- 7.2.6 Fragmentation of Activated Sigma Bonds: (Alpha) α-bond Cleavage Relative to Heteroatoms -- 7.2.7 Isomerisation Reactions Prior to Fragmentation: Hydrogen Shift Rearrangement Reactions in Alicyclic Compounds -- 7.2.8 How Do Rearrangement Reactions Leading to the Loss of Very Stable Neutral Molecules Such as H2O, NH3, HCN, C2H4, CO, CO2 and So Forth Occur? -- 7.2.9 What Is the McLafferty Rearrangement Reaction? -- 7.2.10 Retro Diels Alder Reaction -- References. , 8 What Is Quantitative Analysis and How Do I Perform It? -- 8.1 How Can I Make Sure the System Is Ready for Quantitative Analysis? -- 8.2 How Do I Calibrate My System to Obtain Quantitative Data? -- 8.2.1 When Should I Use Normalisation as a Calibration Method? -- 8.2.2 When Should I Use External Standardisation as a Calibration Method? -- 8.2.3 When Should I Use Internal Standardisation as a Calibration Method? -- 8.2.4 When Should I Use Standard Addition as a Calibration Method? -- 8.3 How Do I Validate my Method? -- 8.3.1 Linearity and Calibration Curves -- 8.3.2 How Do I Calculate the Limit of Detection? -- 8.3.3 How Do I Calculate the Limit of Quantitation? -- 8.3.4 What Is the Difference Between Precision and Accuracy? -- 8.3.5 How Do I Determine Accuracy? -- 8.3.6 How Do I Measure Precision? -- 8.3.7 How Do I Validate Standard Stability? -- 8.3.8 How Do I Validate Sample Stability? -- 8.3.9 How Do I Assess the Robustness and Ruggedness of My GC-MS Methods? -- 8.3.10 Why Methods Fail -- 8.3.11 Design of Experiments to Study the Robustness and Ruggedness -- References -- 9 How Do I Maintain My GC-MS? -- 9.1 Do I Need to Perform Maintenance? -- 9.2 What Should I Do Before I Perform Maintenance? -- 9.2.1 Benchmarking -- 9.2.2 Temperatures -- 9.2.3 Gases -- 9.2.4 Electricity -- 9.3 What Tools Do I Need to Perform Maintenance? -- 9.4 Where Is Maintenance Required and How Do I Perform It? -- 9.4.1 Sample Vials, Caps and Septa -- 9.4.2 Maintenance of the Sampling Device or Autosampler -- 9.4.3 Maintenance on the Gas Chromatograph -- 9.4.4 Maintenance of the Mass Spectrometer -- 9.4.5 PC and Software Maintenance -- 9.5 How Do I Know That My Maintenance Is Successful? -- 9.5.1 How Do I Ensure My Instrument Is Working Correctly After Performing Maintenance? -- 9.5.2 Sensitivity and Performance Checks -- 9.5.3 Maintenance Log -- 9.6 Conclusions. , 10 How Do I Troubleshoot a Problem on My GC-MS?.