Quantitative Chromatographic Analysis

by Beesley; Thomas

• ISBN13: 9780824705039
• ISBN10: 0824705033
• Edition: 1st
• Format: Hardcover
• Copyright: 2000-12-06
• Publisher: CRC Press

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