9780824705039

Quantitative Chromatographic Analysis

by ;
  • ISBN13:

    9780824705039

  • ISBN10:

    0824705033

  • Edition: 1st
  • Format: Hardcover
  • Copyright: 2000-12-06
  • Publisher: CRC Press

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Summary

"Highlights critical factors involved in successful chromatographic analysis. Details analytical procedures; outlining sample preparation, collection, transportation, and storage. Provides step-by-step guidelines for producing analytical reports. "

Author Biography

Thomas E. Beesley is President, Advanced Separation Technologies, Inc. Benjamin Buglio is a retired Research Investigator, Hoffmann-La Roche, Inc., Nutley, New Jersey Raymond P. W. Scott is a sometime visiting professor in the Department of Chemistry at Georgetown University, Washington, D.C., and the Department of Chemistry at Birkbeck College, University of London, England

Table of Contents

Preface iii
PART 1 Introduction to Quantitative Chromatographic Analysis
The Critical Factors that Govern a Successful Quantitative Chromatographic Analysis
3(18)
Historical Introduction
3(6)
The Importance of Chromatography as an Analytical Technique
9(1)
Critical Factors Involved in a Successful Chromatographic Analysis
10(7)
Sample Transportation and Storage
12(1)
Sample Preparation
13(1)
Analytical Procedures
13(3)
Data Processing
16(1)
Analytical Reports
16(1)
Synopsis
17(1)
References
18(3)
Sample Collection, Transport and Storage
21(26)
Gas Samples
21(15)
Sampling for the Major Components of a Mixture of Permanent Gases
22(3)
Sampling for Minor Components of a Gas Mixture
25(4)
The Analysis of Flower Fragrances
29(2)
Head Space Analysis
31(2)
Solid Phase Micro-Extraction
33(3)
Liquid Sampling
36(2)
Solid Sampling
38(5)
Powder, Granules or Crystals
39(2)
Reduction of the Sample to Analytical Size
41(2)
Sample Size
43(1)
Synopsis
43(1)
Recommended Reading
44(3)
Sample Preparation
47(34)
Introduction to Sample Preparation
47(1)
Extraction Techniques
47(16)
Pre-Extraction Practices
48(3)
Solvent Extraction
51(4)
Solid Phase Extraction
55(4)
The Solvent Extraction of Solids
59(3)
Super-Critical Fluid Extraction
62(1)
Derivatization
63(11)
Esterification
64(4)
Acylation Reactions
68(4)
Post-Column Derivatization
72(2)
Concentration Techniques
74(3)
Synopsis
77(3)
References
80(1)
The Chromatography Detector
81(24)
Introduction
81(1)
The Dynamic Range of the Detector
82(1)
Detector Linearity
83(7)
The Determination of the Response Index of a Detector
85(5)
The Linear Dynamic Range of a Detector
90(1)
Detector Response
90(1)
Detector Noise
91(3)
Short Term Noise
91(1)
Long Term Noise
92(1)
Drift
92(1)
Measurement of Detector Noise
93(1)
Detector Sensitivity or the Minimum Detectable Concentration
94(2)
The Mass Sensitivity of a Chromatographic System
96(1)
The Concentration Sensitivity of a Chromatographic System
97(1)
The Maximum Capacity Factor of an Eluted Peak
98(3)
Practical Considerations
101(1)
Synopsis
101(2)
References
103(2)
Processing Chromatographic Data
105(50)
Introduction
105(1)
Chromatographic Resolution
105(2)
The Efficiency Required to Achieve a Specific Resolution
107(3)
Peak Deconvolution
110(3)
The Detector Response
113(3)
Chromatographic Data Processing
116(19)
Manual Data Processing
116(7)
Computer Data Processing
123(8)
Data Processing
131(4)
Some Simple Computing Techniques
135(4)
Chromatographic Control
139(1)
Quantitative Analytical Methods for GC and LC
139(10)
Quantitative Analysis Using Reference Standards
141(8)
Quantitative Analysis by TLC
149(1)
Comparative Spot Assessment by Visual Estimation
149(1)
Synopsis
150(2)
References
152(3)
PART 2 Quantitative Gas Chromatographic Analysis
Gas Chromatographic Apparatus for Quantitative Analysis
155(50)
Gas Supplies
156(14)
Gas Supplies from Tanks or Cylinders
159(1)
Pure Air Generators
159(1)
Pure Nitrogen Generators
159(1)
Hydrogen Generators
160(1)
Pressure Controllers
160(1)
Flow Controllers
161(1)
Flow Programmers
162(8)
Injection Devices
170(9)
Gas Sampling Systems
171(2)
Packed Column Injection Systems
173(1)
Open Tubular Column Injection Systems
174(5)
Automatic Injection Systems
179(1)
The Column Oven
179(7)
The Temperature Programmer
180(6)
Detector Ovens
186(1)
Column/Detector Connecting Conduits
187(1)
Gas Chromatography Detectors
187(7)
The Flame Ionization Detector
188(3)
The Nitrogen Phosphorus Detector (NPD)
191(3)
The Electron Capture Detector
194(7)
The Katharometer Detector
198(3)
Synopsis
201(2)
References
203(2)
Gas Chromatography Applications
205(40)
The Extraction and Analysis of Carbonyl Compounds from Some Natural Products
208(3)
Determination of Insecticides in Drinking Water Using Dual Electron Capture and Nitrogen Phosphorus Detection
211(2)
Analysis of Chlorobenzenes in Soil by Headspace Solid-Phase Extraction and Ion-Trap Mass Spectrometry
213(2)
Determination of Fentanyl in Whole Blood at the Subnanogram Level Using Nitrogen Sensitive and Mass Spectrometric Detection
215(4)
The Measurement of Within-Tree Variation in Lignin Components by Pyrolysis Gas Chromatography
219(3)
Use of Capillary Columns for Sample Microextraction
222(2)
Extraction Technique for the Analysis of Protective Clothing Breakthrough Indicator Pads
224(2)
Analysis of Pethidine and Methadone in Human Urine by Solid Phase Microextraction and Gas Chromatography
226(2)
The Determination of Methyl Mercury and Inorganic Mercury in Whole Blood by Head Space Cryofocusing Gas Chromatography with Atomic Adsorption Detection
228(2)
Determination of Inorganic Mercury in Whole Blood
229(1)
Determination of Organic Mercury in Whole Blood
229(1)
The Determination of ß-Alaninediacetic Acid in Waste Waters and Aquatic Environments
230(3)
Water Samples
231(1)
Sediments
231(2)
Method for Analyzing Organochlorine Pesticides in Water Using Solid Phase Microextraction and Pulsed Discharge Electron Capture Detection
233(2)
Use of Supercritical Fluid Extraction for the Determination of Steroids in Animal Tissue
235(4)
Synopsis
239(1)
References
240(5)
PART 3 Quantitative Liquid Chromatography Analysis
Liquid Chromatographic Apparatus for Quantitative Analysis
245(42)
The Basic Liquid Chromatograph
245(10)
The Solvent Supply System
246(2)
Liquid Chromatography Pumps
248(5)
Sample Valves
253(2)
Column Ovens
255(1)
General Comments on Detectors
255(1)
Data Acquisition and Processing
256(1)
The Modern Versatile Liquid Chromatograph
256(5)
Liquid Chromatography Detectors
261(1)
The UV Detectors
262(10)
The Fixed Wavelength UV Absorption Detector
262(4)
The Variable Wavelength Detector
266(2)
The Diode Array Detector
268(4)
The Fluorescence Detector
272(5)
The Electrical Conductivity Detector
277(4)
The Refractive Index Detector
281(3)
Synopsis
284(2)
References
286(1)
Liquid Chromatography Applications
287(34)
The Determination of Bixin and Norbixin in Human Blood Plasma
288(4)
Determination of the Enantiomers of Methamphetamine and Its Metabolites in Urine
292(2)
Trace Enrichment of Alkylthio-s-triazine Herbicides by Supported Liquid Membrane Techniques
294(3)
The Determination of Trace Amounts of the Transition Metals in Parenteral Solutions
297(3)
Determination of Theophylline and Caffeine in Blood Serum by Direct Injection
300(2)
The Determination of Spectinomycin Residues in Various Tissue Types from Husbandry Animals
302(4)
The Determination of Alternariol in Tomato Paste by Solid Phase Extraction and Liquid Chromatography Using Fluorescence Detection
306(3)
Automated Determination of Amphetamine Enantiomers Employing Two-Dimensional Column Switching
309(2)
Determination of N-Methyl Carbamate Pesticides in Foods Using Solvent Extraction at Elevated Temperatures with Minicolumn Cleanup
311(3)
Ascorbic Acid Determination in Foodstuffs by Microdialysis Sampling and Liquid Chromatography with Electrochemical Detection
314(2)
Synopsis
316(2)
References
318(3)
PART 4 Thin Layer Chromatography
Thin Layer Chromatography Apparatus
321(28)
Elution Development in Thin Layer Chromatography
322(2)
Thin Layer Chromatography Chambers
324(5)
Continuous Plate Development
329(1)
Forced-Flow Development
330(2)
Sample Application
332(5)
Detection Techniques and the Quantitative Evaluation of TLC Spots
337(3)
The Iodine Reagent
338(1)
The Sulfuric Acid Spray
339(1)
Chromic-Sulfuric Acid Spray
339(1)
Fluorescence
339(1)
Scanning Densitometry
340(5)
Synopsis
345(2)
References
347(2)
Thin Layer Chromatography Applications
349(24)
Measurement Methods
349(3)
The Assay of Sulfamethazine in Pork Carcasses
352(2)
The Determination of Aflatoxins in Palm Kernels
354(2)
Determination of the Platelet-Activating Factor and Other Phospholipids in Human Tears
356(2)
A Mass Spectometric Measurement of Peptide-Like Materials Using a Hybrid Thin Layer Plate as the Transport Interface to a Matrix Assisted Laser Desorption Ionization System
358(4)
Determination of Caffeine Using Both Densitometry Measurements and an Image Analyzing System
362(2)
The Use of Digital Auto-Radiography for the Analysis of Biological Samples and for Studying Drug Metabolism
364(2)
Purity Measurements of Phthaloyl-Amiodipine Using Over-Pressurized Thin Layer Chromatography
366(3)
Synopsis
369(2)
References
371(2)
Index 373

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