Chemical Separations Principles, Techniques and Experiments

by Meloan, Clifton E.

• ISBN13: 9780471351979
• ISBN10: 0471351970
• Edition: 1st
• Format: Hardcover
• Copyright: 1999-10-06
• Publisher: Wiley-Interscience

Summary

Performing effective chemical separations-a step-by-step guide to the most commonly used techniques. How do experienced analysts go about making a chemical separation work? Through precise, detailed coverage of the principles, equipment, and techniques involved, this combination laboratory manual and reference source gives readers a working knowledge of an impressive array of separation methods. In forty-two chapters, it explores all major categories of separation, including those involving phase changes, extraction, chromatography, ion-exchange resins, electric fields, flotation, membranes, and miscellaneous techniques. With an emphasis on everyday practice rather than theory, Chemical Separations explains the principles and parameters of these methods with a minimum of mathematics, while providing 59 specific experiments to demonstrate proper procedures. Drawn from well-known commercial and academic laboratories and approved by national standard-setting organizations, these experiments feature step-by-step protocols for each separation scheme, precise instructions on setting up the apparatus, and helpful checklists for essential chemicals and supplies. With Chemical Separations as their guide, laboratory analysts and newcomers to chemical analysis will learn how to obtain quality analysis using commercial products, natural samples, and proven real-world laboratory techniques.

Author Biography

<b>CLIFTON E. MELOAN, phd</b>, is Professor Emeritus of Analytical Chemistry at Kansas State University, Manhattan, Kansas. Extensively published in the field, Dr. Meloan has served as a science advisor to the FDA for nearly 30 years.

Table of Contents

Introduction	1	(4)
SEPARATIONS INVOLVING PHASE CHANGES
Volatilization	5	(8)
Zone Melting	13	(8)
Distillation: General Information	21	(22)
Azeotropic and Extractive Distillations	43	(6)
Steam and Immiscible Solvents Distillation	49	(8)
Vacuum Distillation	57	(14)
Molecular Distillation and Sublimation	71	(14)
Lyophilization (Freeze Drying)	85	(8)
SEPARATIONS INVOLVING EXTRACTION
Extraction: General Concepts	93	(14)
Continuous Extraction	107	(10)
Countercurrent (Extraction) Chromatography: The Ito Coil-Planet Centrifugal Extractor	117	(12)
Solid Phase Extraction	129	(8)
Supercritical Fluid Extraction	137	(12)
SEPARATIONS INVOLVING CHROMATOGRAPHY
Chromatography: General Theory	149	(6)
Displacement and Multiple Column Partition Chromatography	155	(10)
Affinity Chromatography	165	(6)
Size Exclusion Chromatography (Gel Filtration; Gel Permeation)	171	(8)
Flash Chromatography	179	(4)
High Performance Liquid Chromatography (HPLC)	183	(28)
Gas--Liquid Chromatography (GLC)	211	(38)
Paper Chromatography	249	(6)
Thin Layer Chromatography	255	(14)
SEPARATIONS INVOLVING ION EXCHANGE RESINS
Ion Exchange	269	(8)
Ion Chromatography	277	(12)
Ion Retardation, Ion Exclusion, and Ligand Exchange	289	(10)
SEPARATIONS INVOLVING ELECTRIC FIELDS
Electrodeposition	299	(16)
Electrophoresis---General	315	(24)
Immunoelectrophoresis	339	(6)
Polyacrylamide Gel Disc Electrophoresis	345	(6)
Ion Focusing, SDS, and Two-Dimensional Electrophoresis	351	(8)
Capillary Zone Electrophoresis	359	(12)
Field Flow Fractionation	371	(14)
SEPARATIONS INVOLVING FLOTATION
Purge and Trap and Dynamic Headspace Analysis	385	(10)
Foam Fractionation, Gas-, and Liquid-Assisted Flotation	395	(18)
SEPARATIONS INVOLVING MEMBRANES
Osmosis and Reverse Osmosis	413	(10)
Dialysis and Electrodialysis	423	(8)
Filtering and Sieving	431	(18)
SEPARATIONS INVOLVING MISCELLANEOUS TECHNIQUES
Density Gradients	449	(6)
Centrifugation	455	(14)
Masking and Sequestering Agents	469	(4)
Solubility	473	(16)
Gas Analysis by Portable Orsat	489	(10)
APPENDIX A	499	(248)
Experiment 1 Volatilization: The Determination of CO2 in Either Limestone or Baking Powder	500	(4)
Experiment 2 Volatilization: The Determination of Mercury in Hair by Flameless Atomic Absorption Spectroscopy	504	(3)
Experiment 3 Zone Refining: The Separation of Traces of Methyl Red from Naphthalene	507	(2)
Experiment 4 Azeotropic Distillation: The Production of Absolute Ethanol from 95% Ethanol--Water	509	(7)
Experiment 5 Extractive Distillation: Separation of Cyclohexane from Benzene Using Aniline	516	(3)
Experiment 6 Steam Distillation: The Separation of Oil of Clove from the Whole Cloves	519	(2)
Experiment 7 Immiscible Solvents Distillation: The Use of Toluene to Remove Water from Fruits, Vegetables, and Meats	521	(2)
Experiment 8 Vacuum Distillation: A Vacuum Distillation to Purify the Solvent Dimethylformamide	523	(4)
Experiment 9 Molecular Distillation: The Determination of Vitamin E (Tocopherol) in Margarine	527	(5)
Experiment 10 Sublimation: The Separation of Benzoic Acid from Saccharin	532	(3)
Experiment 11 Entrainer Sublimation: The Separation of Caffeine from Coffee by Entrainer Sublimation	535	(3)
Experiment 12 Lyophilization: Preparing Freeze-Dried Beverages	538	(2)
Experiment 13 Continuous Extraction---Solvent Heavier Than Water: The Determination of Caffeine in Cola Drinks Using a Continuous Extractor; Solvent Heavier Type	540	(4)
Experiment 14 Continuous Extraction---Solvent Lighter Than Water: Separating the Anti-amoebic Alkaloids from Ipecac Syrup	544	(4)
Experiment 15 Continuous Extraction---The Soxhlet Extractor: Extracting Oil from Nutmeats	548	(2)
Experiment 16 Countercurrent Extraction: Separation of the Phenolic Flavor Components, Carvacrol and Thymol, from Oregano Leaves	550	(4)
Experiment 17 Solid Phase Extraction: Atrazine, Simazine, and Propazine in Ponds, Lakes, and Rivers (Supelco Applications)	554	(2)
Experiment 18 Supercritical Fluid Extraction: The Separation of Oil from Pecans	556	(5)
Experiment 19 Displacement Column Chromatography: The Separation of cis-trans-Azobenzene	561	(3)
Experiment 20 Multiple Column Partition Chromatography: The Separation of Codeine, Chlorpheniramine, and Phenylephrine in a Cough Syrup	564	(3)
Experiment 21 Affinity Chromatography: Separation of a Lectin from Soybeans	567	(5)
Experiment 22 Size Exclusion Chromatography: Gel Filtration Chromatography---The Separation of Vitamin B12 from Dextrans by Means of Sephadex G-100	572	(3)
Experiment 23 Flash Chromatography: Separation of Vanillin from Vanilla Extract	575	(4)
Experiment 24 High Performance Liquid Chromatography: Detecting Explosive Residues	579	(5)
Experiment 25 High Performance Liquid Chromatography: Separation of Aspirin, Acetaminophen, and Caffeine in Excedrin	584	(2)
Experiment 26 Gas-Liquid Chromatography---Arson Investigation: Detection of Accelerants in Debris by Head Space Analysis	586	(5)
Experiment 27 Gas-Liquid Chromatography---Determination of Antioxidants: The Determination of BHA and BHT Antioxidants in Breakfast Cereals	591	(4)
Experiment 28 Paper Chromatography: The Determination of Sulfamethazine, Sulfametrazine, and Sulfadiazine in Trisulfa Tablets	595	(4)
Experiment 29 Thin Layer Chromatography: Ascending TLC Separations Requiring Color Development---Vasodilator Drugs; the Aliphatic Nitrates	599	(2)
Experiment 30 ``Instant'' Thin Layer Chromatography: The Determination of Antihistamines in Drug Preparations	601	(5)
Experiment 31 Two-Dimensional Chromatography: Separation of Sulfamethazine or Carbadox from Medicated Feeds	606	(2)
Experiment 32 Ion Exchange: Separations of Several Cations in Mineral Water, Pond Water, or Low Acid Foods	608	(6)
Experiment 33 Ion Chromatography: The Separation of Corrosion Inhibitors and Contaminants in Engine Coolants	614	(3)
Experiment 34 Ion Retardation: Separating Salt and Urea from Urine	617	(1)
Experiment 35 Ion Exclusion: Determination of Total Vitamin C in Applesauce	618	(3)
Experiment 36 Ligand Exchange: Determination of Hydrazine, Methylhydrazine, and Dimethylhydrazine in Liquid Rocket Fuels	621	(2)
Experiment 37 Electrodeposition: The Determination of Copper and Nickel in a U.S. 5-Cent Piece	623	(5)
Experiment 38 Agar Horizontal Strip Electrophoresis: The Separation of the Isoenzymes of Lactic Dehydrogenase (LDH) in Blood Serum	628	(6)
Experiment 39 Agarose Gel Horizontal Strip Electrophoresis: DNA Fingerprinting---A Paternity Case	634	(8)
Experiment 40 Immunoelectrophoresis: Immunoelectrophoresis of Human Proteins in Urine or Serum	642	(4)
Experiment 41 Disc Electrophoresis: Identification of Fish Species by Their Amino Acid Pattern	646	(6)
Experiment 42 Ion Focusing Electrophoresis: Ion Focusing of Ferric Leghemoglobins from Soybean Root Nodules	652	(5)
Experiment 43 Capillary Zone Electrophoresis: Micellular Capillary Electrophoresis Separation of Aspartame Breakdown Products in Soft Drinks	657	(5)
Experiment 44 Field Flow Fractionation: Determination of the Size/Mass of Latex Spheres Using Sedimentation FFF	662	(3)
Experiment 45 Purge and Trap: Separation of Aroma and Flavor Compounds in Fresh and Aged Beer	665	(2)
Experiment 46 Foam Fractionation: Separation of Detergents from Waste Water	667	(4)
Experiment 47 Gas-Assisted Flotation: Separating Suspended Solids from River Water	671	(2)
Experiment 48 Liquid-Assisted Flotation---Tomatoes: Separating Fly Eggs and Maggots from Canned Tomatoes	673	(3)
Experiment 49 Liquid-Assisted Flotation---Cornmeal and Flour: Separating Insect Fragments and Rodent Hairs from Cornmeal and Flour	676	(5)
Experiment 50 Liquid-Assisted Flotation---Leafy Vegetables: Separating Mites, Aphids, and Thrips from Leafy Vegetables	681	(4)
Experiment 51 Osmosis: Determining the Osmotic Pressure of a Potato	685	(2)
Experiment 52 Dialysis: The Determination of Phosphatase in Milk to Determine Proper Pasteurization	687	(4)
Experiment 53 Air Filtration: Separating Pollen and Molds from Air	691	(3)
Experiment 54 Density Gradients for Soils: Comparing Soils at a Hit-and-Run Accident	694	(2)
Experiment 55 Centrifugation: The Separation of Fat from Milk and Ice Cream	696	(4)
Experiment 56 Masking and Sequestering Agents: The Determination of Zn Accelerators in Rubber Products	700	(3)
Experiment 57 Solubility of Plastic Materials: Separation and Identification of Thermoplastic Polymers	703	(1)
Experiment 58 Solubility of Fibers: Identification of Textile Fibers by Solubility Measurements	704	(3)
Experiment 59 Gas Analysis: Separation of CO2, O2, CO, and N2 from Car Exhaust Gas Fumes	707	(4)
APPENDIX B
Answers to the Review Questions	711	(36)
Index	747