Atnaujinkite slapukų nuostatas

El. knyga: Gas Chromatography-Mass Spectrometry: How Do I Get the Best Results?

(Anthias Consulting Ltd, UK), (GlaxoSmithKline, UK), (Domino Printing Sciences, UK), (University of Cologne, Germany), (Anthias Consulting Ltd, UK), (Jomo Kenyatta University of Agriculture and Technology, Kenya)
  • Formatas: 319 pages
  • Išleidimo metai: 28-Nov-2019
  • Leidėjas: Royal Society of Chemistry
  • Kalba: eng
  • ISBN-13: 9781839160042
Kitos knygos pagal šią temą:
Gas Chromatography-Mass Spectrometry: How Do I Get the Best Results?Didesnis paveikslėlis
  • Formatas: 319 pages
  • Išleidimo metai: 28-Nov-2019
  • Leidėjas: Royal Society of Chemistry
  • Kalba: eng
  • ISBN-13: 9781839160042
Kitos knygos pagal šią temą:

DRM apribojimai

  • Kopijuoti:

    neleidžiama

  • Spausdinti:

    neleidžiama

  • El. knygos naudojimas:

    Skaitmeninių teisių valdymas (DRM)
    Leidykla pateikė šią knygą šifruota forma, o tai reiškia, kad norint ją atrakinti ir perskaityti reikia įdiegti nemokamą programinę įrangą. Norint skaityti šią el. knygą, turite susikurti Adobe ID . Daugiau informacijos  čia. El. knygą galima atsisiųsti į 6 įrenginius (vienas vartotojas su tuo pačiu Adobe ID).

    Reikalinga programinė įranga
    Norint skaityti šią el. knygą mobiliajame įrenginyje (telefone ar planšetiniame kompiuteryje), turite įdiegti šią nemokamą programėlę: PocketBook Reader (iOS / Android)

    Norint skaityti šią el. knygą asmeniniame arba „Mac“ kompiuteryje, Jums reikalinga  Adobe Digital Editions “ (tai nemokama programa, specialiai sukurta el. knygoms. Tai nėra tas pats, kas „Adobe Reader“, kurią tikriausiai jau turite savo kompiuteryje.)

    Negalite skaityti šios el. knygos naudodami „Amazon Kindle“.

Gas chromatographymass spectrometry (GC-MS) is a powerful way to analyse a range of substances. It is used in everything from food safety to medicine. It has even been used to protect endangered vultures through analysis of poisonous pesticide molecules in their environment!



I want to apply this technique, where do I begin? Is GC-MS is the right technique to use? How do I prepare my samples and calibrate the instruments? This textbook has the answers to all these questions and more.



Throughout the book, case studies illustrate the practical process, the techniques used and any common challenges. Newcomers can easily search for answers to their question and find clear advice with coloured images on how to get started and all subsequent steps involved in using GC-MS as part of a research process. Readers will find information on collecting and preparing samples, designing and validating methods, analysing results, and troubleshooting. Examples of pollutant, food, oil and fragrance analysis bring the theory to life.



The authors use their extensive experience teaching GC-MS theory and practice and draw on their combined backgrounds applying the technique in academic and industry settings to bring this practical reference together. The authors also design and teach the Royal Society of Chemistrys Pan Africa Chemistry Network GC-MS course, which is supported by GSK.
1 Sample Collection and Preparation: How Do I Get My Sample Ready for GC-MS Analysis?
1(40)
1.1 How Do I Collect and Sample a Gas for GC or GC-MS Analysis?
2(8)
1.1.1 What Is Spot Analysis?
3(1)
1.1.2 How Do I Sub-sample with a Canister or Sampling Bag?
3(2)
1.1.3 What Is Active Sampling?
5(5)
1.1.4 What Is Passive Sampling?
10(1)
1.1.5 What Is Online Sampling?
10(1)
1.2 How Do I Sample and Prepare a Liquid for GC or GC-MS Analysis?
10(17)
1.2.1 How Do I Store My Liquid Samples?
11(1)
1.2.2 Which Solvents Can I Use in Sample Preparation for Injection into a GC?
11(2)
1.2.3 Which Sample Preparation Techniques Can Be Used for Liquid Samples with GC-MS Analysis?
13(1)
1.2.4 How Can I Prepare Liquid Samples with a Liquid Phase?
14(3)
1.2.5 How Can I Prepare Liquid Samples with a Solid Phase?
17(8)
1.2.6 How Can I Prepare Liquid Samples Thermally?
25(2)
1.3 How Do I Sample and Prepare a Solid for GC or GC-MS Analysis?
27(10)
1.3.1 Can I Use Thermal Desorption?
28(1)
1.3.2 When Should I Use Analytical Pyrolysis for Solid Samples?
29(3)
1.3.3 What Liquid Extraction Techniques Can Be Used?
32(2)
1.3.4 What Is Microwave Extraction?
34(1)
1.3.5 What Is Pressurised Fluid Extraction?
35(2)
1.4 When Should I Use Derivatisation in GC-MS Analysis?
37(3)
1.5 How Do I Know How Well My Sample Preparation Has Worked?
40(1)
2 How Do I Introduce My Samples into the GC Column?
41(27)
2.1 How Do I Inject My Sample into the GC?
41(2)
2.2 How Do I Transfer My Introduced Sample into the Analytical Column?
43(2)
2.3 How Do I Select Which Inlet Is Suited for My Application?
45(11)
2.3.1 On-column Inlets
45(1)
2.3.2 Split and Splitless Inlets
46(4)
2.3.3 Programmable Temperature Vaporiser Inlets
50(6)
2.4 Comparison of Injection Techniques
56(10)
2.4.1 How Do I Select and Optimise My Inlet Method Parameters and Consumables?
57(1)
2.4.2 Injection Volume
57(3)
2.4.3 Temperatures
60(1)
2.4.4 Sample Transfer Time to the Column
61(1)
2.4.5 Split/Vent Flows
61(1)
2.4.6 Liner Size and Style
62(1)
2.4.7 Liner Packing Material
63(1)
2.4.8 Deactivation
64(1)
2.4.9 Septum
65(1)
2.5 How Do I Introduce a Gas into the Gas Chromatograph?
66(2)
References
67(1)
3 Chromatographic Separation
68(20)
3.1 How Do I Assess the Quality of My Chromatographic Separation?
68(3)
3.1.1 Chromatographic Systems
68(1)
3.1.2 Separation Techniques
69(2)
3.2 How Do I Select the Right Stationary Phase and Column Chemistry?
71(2)
3.3 Theoretical Background and Definition of Chromatographic Terms
73(8)
3.3.1 Retention on the Column
73(2)
3.3.2 Capacity Factor
75(1)
3.3.3 Resolution
75(1)
3.3.4 Selectivity Factor
76(1)
3.3.5 Band Broadening and Column Efficiency
76(2)
3.3.6 Rate Theory and Band Broadening
78(3)
3.4 How Do I Select the Best Mobile Phase to Give Me the Best Efficiency?
81(2)
3.5 How Do I Reduce Retention Time?
83(2)
3.6 How Do I Evaluate the Separation of Closely Eluting Bands in a Chromatogram?
85(1)
3.7 How Do I Optimise Column Performance?
86(2)
Further Reading Materials
87(1)
4 How Do I Detect My Analytes?
88(11)
4.1 What Types of GC Detectors Are There?
88(2)
4.2 What Is a FID?
90(2)
4.2.1 How Does a FID Work?
91(1)
4.2.2 What Parameters Do I Need to Optimise When Using a FID?
91(1)
4.3 What Is an ECD?
92(2)
4.3.1 How Do an ECD and μECD Work?
92(1)
4.3.2 What Parameters Do I Need to Optimise When Using an ECD?
93(1)
4.4 What Is a Thermal Conductivity Detector?
94(1)
4.4.1 How Does a TCD Work?
94(1)
4.4.2 What Parameters Do I Need to Optimise When Using a TCD?
94(1)
4.5 Why Would I Choose a GC-MS Over Other GC Detectors?
95(1)
4.6 How Do I Connect My Analytical Column to Two or More Detectors?
96(3)
5 Mass Analysis
99(44)
5.1 A Historical Perspective: Why Do I Need Ions for MS Analysis?
99(3)
5.1.1 Are Mass Spectrometers Sophisticated Balances That Are Able to Determine the Mass of a Molecule?
101(1)
5.2 Introduction to Mass Spectrometry
102(7)
5.2.1 What Are the Basic Fundamentals Needed for Understanding MS?
102(1)
5.2.2 Mass
102(1)
5.2.3 Atoms of Elements and Isotopes
102(2)
5.2.4 Atomic Mass and the Unified Atomic Mass Unit
104(1)
5.2.5 Nominal Mass
104(1)
5.2.6 What Is the Mass-to-charge Ratio?
105(1)
5.2.7 Isotopic Mass and Monoisotopic Mass of a Molecule or Ion
106(2)
5.2.8 Relative Atomic and Molecular Mass
108(1)
5.3 Basic Aspects of MS Instrumentation and GC-MS
109(6)
5.3.1 Are All Compounds Suited for GC-MS Analysis?
109(1)
5.3.2 How Do I Select the Ionisation to Fit to a GC Front End Separation?
110(1)
5.3.3 How Do I Ensure That the Mass Spectrometer Will Produce Good Spectra?
111(2)
5.3.4 How Do I Keep My Mass Spectrometer Running Optimally?
113(1)
5.3.5 Why Do I Need a GC for the Analysis of a Complex Mixture of Compounds?
114(1)
5.3.6 Are There Artefacts From the Analytical Technique - What Should I Be Aware of?
114(1)
5.4 How are Ions Generated in a MS Instrument?
115(11)
5.4.1 Electron (Impact) Ionisation
115(7)
5.4.2 Chemical Ionisation
122(4)
5.5 How is the Mass-to-charge (m/z) Ratio Determined in Mass Spectrometer?
126(7)
5.5.1 Ion Acceleration
126(1)
5.5.2 Time of Flight Analysers
127(1)
5.5.3 Quadrupole Mass Analyser
128(2)
5.5.4 Quadrupole Ion Trap
130(1)
5.5.5 What Is Unit Mass Resolution?
131(1)
5.5.6 How Are the Separated Ions Detected?
132(1)
5.6 What Parameters Do I Need to Optimise When Using an MS?
133(7)
5.6.1 How Do I Choose the Scan Range and Scan Speed for My Analysis?
133(3)
5.6.2 How Do I choose My Ions for SIM and Set-up My SIM Groups?
136(1)
5.6.3 What Temperatures Need to Be Optimised in an MS?
137(1)
5.6.4 What is the Solvent Delay or Cut Time and How Do I Optimise It?
138(1)
5.6.5 What Detector Parameters Require Optimisation?
139(1)
5.6.6 What GC Parameter Considerations Are There When Hyphenating with an MS?
139(1)
Further Reading
140(1)
References
141(2)
6 What Is Qualitative Analysis and How Do I Perform It?
143(20)
6.1 How Can I Use My GC-MS Chromatogram and Spectral Data?
144(1)
6.2 What Information Can I Extract from the Chromatogram About Data Quality?
145(3)
6.2.1 What Is the Baseline?
145(1)
6.2.2 Chromatographic Resolution
146(1)
6.2.3 Column Efficiency
146(1)
6.2.4 Signal-to-Noise Ratio
146(1)
6.2.5 Peak Symmetry
147(1)
6.3 How Do I Determine If My Analytes Are Present or Not?
148(5)
6.3.1 How Do I Integrate Peaks?
148(1)
6.3.2 What Affects the Peak Integration?
149(1)
6.3.3 How Do I Integrate Coeluting Peaks?
150(1)
6.3.4 Retention Time
150(2)
6.3.5 Kovats Retention Index
152(1)
6.4 How Do I Identify Peaks?
153(10)
6.4.1 How Do I Extract a High-quality Mass Spectrum?
153(5)
6.4.2 How Do I Perform a Library Search?
158(4)
6.4.3 My Mass Spectrum Is Not in the Library, How Do I Determine What It Is?
162(1)
7 Basic Aspects of Mass Spectra Interpretation
163(42)
7.1 What Information Does the Molecular Ion in EI-MS [ M]+ Give Me?
163(8)
7.1.1 What Is a Molecular Ion?
163(1)
7.1.2 What Is the Nitrogen Rule?
164(2)
7.1.3 Double Bond-equivalents
166(2)
7.1.4 What Information Does the Isotopic Patterns of the Molecular Ion [ M]+ in El-Mass Spectra Give Me?
168(3)
7.2 What Information Do the EI-MS Fragment Ions Give Me?
171(32)
7.2.1 What Are Localised Charges?
172(1)
7.2.2 How Do I Correctly Discuss MS Fragmentation Processes?
173(1)
7.2.3 Typical Fragmentation and Rearrangement Reactions in EI-MS
174(1)
7.2.4 Fragmentation of Unactivated C-C Sigma Bonds: OE+ ->EE+ + R
175(5)
7.2.5 Fragmentation of Activated Sigma Bonds: Allylic and Benzylic Cleavage
180(6)
7.2.6 Fragmentation of Activated Sigma Bonds: (Alpha) a-bond Cleavage Relative to Heteroatoms
186(4)
7.2.7 Isomerisation Reactions Prior to Fragmentation: Hydrogen Shift Rearrangement Reactions in Alicyclic Compounds
190(2)
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?
192(4)
7.2.9 What Is the McLafferty Rearrangement Reaction?
196(5)
7.2.10 Retro Diels Alder Reaction
201(2)
Further Reading
203(1)
References
203(2)
8 What Is Quantitative Analysis and How Do I Perform It?
205(33)
8.1 How Can I Make Sure the System Is Ready for Quantitative Analysis?
207(1)
8.2 How Do I Calibrate My System to Obtain Quantitative Data?
208(11)
8.2.1 When Should I Use Normalisation as a Calibration Method?
209(1)
8.2.2 When Should I Use External Standardisation as a Calibration Method?
210(3)
8.2.3 When Should I Use Internal Standardisation as a Calibration Method?
213(5)
8.2.4 When Should I Use Standard Addition as a Calibration Method?
218(1)
8.3 How Do I Validate my Method?
219(18)
8.3.1 Linearity and Calibration Curves
220(2)
8.3.2 How Do I Calculate the Limit of Detection?
222(1)
8.3.3 How Do I Calculate the Limit of Quantitation?
223(1)
8.3.4 What Is the Difference Between Precision and Accuracy?
224(1)
8.3.5 How Do I Determine Accuracy?
225(1)
8.3.6 How Do I Measure Precision?
226(6)
8.3.7 How Do I Validate Standard Stability?
232(1)
8.3.8 How Do I Validate Sample Stability?
233(1)
8.3.9 How Do I Assess the Robustness and Ruggedness of My GC-MS Methods?
234(1)
8.3.10 Why Methods Fail
235(1)
8.3.11 Design of Experiments to Study the Robustness and Ruggedness
236(1)
Further Reading
237(1)
References
237(1)
9 How Do I Maintain My GC-MS?
238(33)
9.1 Do I Need to Perform Maintenance?
238(1)
9.2 What Should I Do Before I Perform Maintenance?
239(2)
9.2.1 Benchmarking
239(1)
9.2.2 Temperatures
240(1)
9.2.3 Gases
240(1)
9.2.4 Electricity
240(1)
9.3 What Tools Do I Need to Perform Maintenance?
241(1)
9.4 Where Is Maintenance Required and How Do I Perform It?
242(25)
9.4.1 Sample Vials, Caps and Septa
242(1)
9.4.2 Maintenance of the Sampling Device or Autosampler
243(3)
9.4.3 Maintenance on the Gas Chromatograph
246(11)
9.4.4 Maintenance of the Mass Spectrometer
257(10)
9.4.5 PC and Software Maintenance
267(1)
9.5 How Do I Know That My Maintenance Is Successful?
267(3)
9.5.1 How Do I Ensure My Instrument Is Working Correctly After Performing Maintenance?
267(1)
9.5.2 Sensitivity and Performance Checks
268(1)
9.5.3 Maintenance Log
268(2)
9.6 Conclusions
270(1)
10 How Do I Troubleshoot a Problem on My GC-MS?
271(29)
10.1 Introduction
271(1)
10.2 What Is the Troubleshooting Process?
272(3)
10.2.1 Always Be Prepared to Deal with Problems
272(1)
10.2.2 Define the Problem
272(1)
10.2.3 Gather Information About the Problem
273(1)
10.2.4 Verify Your Method and Sample
273(1)
10.2.5 Check the Symptoms
273(1)
10.2.6 Isolate the Problem
273(1)
10.2.7 Fix the Problem
274(1)
10.2.8 Verify and Record
275(1)
10.2.9 Prevent
275(1)
10.3 Useful Tools for Troubleshooting
275(1)
10.4 A Breakdown of Problem Areas
275(13)
10.4.1 Problem Areas: Samples
276(1)
10.4.2 Problem Areas: Gases and Plumbing
277(1)
10.4.3 Problem Areas: Autosampler
278(1)
10.4.4 Problem Areas: Inlets
278(4)
10.4.5 Problem Areas: Columns and Column Oven
282(2)
10.4.6 Problem Areas: GC Detectors
284(1)
10.4.7 Problem Areas: Vacuums
285(2)
10.4.8 Problem Areas: Mass Spectrometer
287(1)
10.4.9 Problem Areas: Computers and Data System
288(1)
10.5 Common Problems
288(9)
10.5.1 Leaks
288(3)
10.5.2 Contamination
291(4)
10.5.3 Sensitivity
295(1)
10.5.4 Activity
296(1)
10.5.5 Retention Time Shifts
296(1)
10.6 Summary
297(1)
10.7 Problems
297(3)
11 Conclusions
300(3)
Subject Index 303
Daugiau apie elektronines knygas Daugiau apie elektronines knygas
Pastovi nuoroda: https://www.kriso.lt/db/97818391600426e.html
Raktažodžiai: