Analytical Chemistry of Complex Matrices

1: Historical Background.- 2: Unit Processes of Analytical Procedures.- 2.1 Unit Process No. 1. Definition of the Problem.- 2.2 Unit Process No. 2. Choice of Method.- 2.3 Unit Process No. 3. Obtaining a Representative Sample and its Measurement.- 2.3.1 Solid Materials.- 2.3.2 Liquid Materials.- 2.3.3 Gaseous Materials.- 2.4 Unit Process No. 4. Preliminary Treatment of Sample.- 2.5 Unit Process No. 5. Separation of Analyte(s) from Interferences and Each Other.- 2.5.1 Separation by Masking.- 2.5.2 Separation by Precipitation.- 2.5.3 Separation by Solvent Extraction.- 2.5.4 Separation by Solid-Phase Extraction.- 2.5.5 Separation by Chromatography.- 2.5.6 Separation by Electrophoresis.- 2.6 Unit Process No. 6. Measurement.- 2.7 Unit Process No. 7. Statistical Assessment of Measurements.- 2.8 Unit Process No. 8. Calculation of Analytical Result and Solution to Problem.- 2.8.1 Quantitative Analysis.- 2.8.1.1 Calibration Curves.- 2.8.1.2 Standard Addition Method.- 2.8.1.3 Internal Standard Method.- 2.8.1.4 Internal Normalization Method.- 2.8.2 Qualitative Analysis.- 2.9 Rule of Computers and Microprocessors in Modern Analytical Methods.- 2.9.1 Instrument Operation.- 2.9.2 Data Recording and Storage.- 2.9.3 Data Processing and Analysis.- 2.9.4 Validation Testing.- 2.9.5 Software for Method Development.- 2.10 Automation of Unit Processes.- 2.10.1 Automation of Repetitive Analysis.- 2.10.2 Continuous On-Line Monitoring.- 2.10.3 Laboratory Robotics.- 2.10.4 Application of Robotics to Dissolution Tests.- 2.10.5 Application of Robotics to Drug Determination in Biological Fluids.- 3: Selected Analytical Problems Involving Inorganic Analytes Which Contain Elements From Groups IA-VIIIA and the Lanthanides.- 3.1 Determination of Sodium and Potassium in Mineral Water by Flame EmissionSpectrometry.- 3.1.1 Summary.- 3.1.2 Introduction.- 3.1.3 Procedure.- 3.2 Determination of Water Hardness, i.e. Total Calcium and Magnesium, by EDTA Titration.- 3.2.1 Summary.- 3.2.2 Introduction.- 3.2.3 Procedure.- 3.2.4 Calculation.- 3.3 Gravimetric Determination of Cerium in Ore.- 3.3.1 Summary.- 3.3.2 Introduction.- 3.3.3 Procedure.- 3.4 Spectrophotometric Determination of Titanium in Rock.- 3.4.1 Summary.- 3.4.2 Introduction.- 3.4.3 Procedure.- 3.4.4 Calculation.- 3.5 Determination of Vanadium(V) in Sea Water by Adsorptive Stripping Voltammetry.- 3.5.1 Summary.- 3.5.2 Introduction.- 3.5.3 Procedure.- 3.6 Determination of Trace Concentrations of Molybdenum in Water Samples by Solvent Extraction of a Neutrally Charged Chelate Followed by Atomic Absorption Spectrometry.- 3.6.1 Summary.- 3.6.2 Introduction.- 3.6.3 Procedure.- 3.7 Differential Thermal Analysis (DTA) of a Complex Manganese Compound Mn(PH2O2)H2O.- 3.7.1 Summary.- 3.7.2 Introduction.- 3.7.3 Procedure.- 3.8 Determination of Iron in an Ore by Redox Titration with Potassium Permanganate.- 3.8.1 Summary.- 3.8.2 Introduction.- 3.8.3 Procedure.- 3.8.4 Calculation.- 3.9 Determination of Cobalt in Soil Samples by Visible Spectrophotometry.- 3.9.1 Summary.- 3.9.2 Introduction.- 3.9.3 Procedure and Calculation.- 3.10 Gravimetric Determination of Nickel in Steel.- 3.10.1 Summary.- 3.10.2 Introduction.- 3.10.3 Procedure.- 4: Selected Analytical Problems Involving Inorganic and Organometallic Analytes Which Contain Elements From Groups IB-VIIB.- 4.1 Determination of Trace Concentrations of Copper in the Aqueous Environment by Stripping Voltammetry.- 4.1.1 Summary.- 4.1.2 Introduction.- 4.1.3 Procedure.- 4.1.4 Calculation.- 4.2 Determination of Organomercury Compounds in Fish Samples by HPLC--Cold Vapour AtomicAbsorption Spectrometry.- 4.2.1 Summary.- 4.2.2 Introduction.- 4.2.3 Procedure.- 4.3 Determination of Zinc in a Pharmaceutical Formulation by Ion-Exchange Separation and Complexometric Titration.- 4.3.1 Summary.- 4.3.2 Introduction.- 4.3.3 Procedure.- 4.4 Visible Spectrophotometric Determination of Boron in Plants.- 4.4.1 Summary.- 4.4.2 Introduction.- 4.4.3 Procedure.- 4.4.4 Calculation.- 4.5 Determination of Organolead Compounds in Air Samples by Gas Chromatography--Atomic Absorption Spectrometry.- 4.5.1 Summary.- 4.5.2 Introduction.- 4.5.3 Procedure.- 4.6 Determination of Nitrogen Dioxide in Air Samples by Sorbent Tube Collection--Colorimetry.- 4.6.1 Summary.- 4.6.2 Introduction.- 4.6.3 Procedure.- 4.6.4 Calculation.- 4.7 Determination of Arsenic in Hair Samples by Neutron Activation Analysis and in Wallpaper by X-ray Fluorescence Spectrometry.- 4.7.1 Summary.- 4.7.2 Introduction.- 4.7.3 Procedure.- 4.8 Determination of Antimony in Liver Samples using Hydride Generation--Atomic Absorption Spectrometry.- 4.8.1 Summary.- 4.8.2 Introduction.- 4.8.3 Procedure.- 4.9 Determination of Selenium in Natural Waters by Spectrofluorimetry.- 4.9.1 Summary.- 4.9.2 Introduction.- 4.9.3 Procedure and Calculation.- 4.10 Determination of Fluoride in Potable Water by Ion-Selective Electrode Measurements.- 4.10.1 Summary.- 4.10.2 Introduction.- 4.10.3 Procedure.- 4.10.4 Calculation.- 4.11 Multielement Analysis of a Biological Fluid by Inductively Coupled Plasma Mass Spectrometry (ICP-MS).- 4.11.1 Summary.- 4.11.2 Introduction.- 4.11.3 Procedure.- 5: Selected Analytical Problems Involving Organic Analytes Which are the Major or Minor Constituents of a Sample.- 5.1 Comparison of Analytical Methods Based on Visible Spectrophotometry, Solvent Extraction--UV Spectrophotometry,Voltammetry, NMR and HPLC for the Determination of the Active Constituents of Analgesic Formulations.- 5.1.1 Summary.- 5.1.2 Visible Spectrophotometric Method.- 5.1.2.1 Introduction.- 5.1.2.2 Procedure.- 5.1.2.3 Calculation.- 5.1.3 Solvent Extraction--UV Spectrophotometric Method.- 5.1.3.1 Introduction and Procedure.- 5.1.4 Voltammetric Method.- 5.1.4.1 Introduction.- 5.1.4.2 Procedure.- 5.1.5 NMR Method.- 5.1.5.1 Introduction.- 5.1.5.2 Calculation.- 5.1.6 HPLC Method.- 5.1.6.1 Introduction.- 5.1.6.2 Procedure.- 5.2 Stability-Indicating High-Performance Liquid Chromatographic Assay for Oxazepam Tablets and Capsules.- 5.2.1 Summary.- 5.2.2 Introduction.- 5.2.3 Procedure.- 5.3 Separation of Water-Soluble Vitamins by Capillary Zone Electrophoresis and Micellar Electrophoretic Capillary Chromatography (MECC).- 5.3.1 Summary.- 5.3.2 Introduction.- 5.3.3 Procedure.- 5.4 Air-Segmented Continuous-Flow Visible Spectrophotometric Determination of Cephalosporins in Drug Formulations by Alkaline Degradation to Hydrogen Sulphide and Formation of Methylene Blue.- 5.4.1 Summary.- 5.4.2 Introduction.- 5.4.3 Procedure.- 5.5 Use of IR Spectrometry to Identify an Active Raw Material, Procaine Penicillin G, Used in the Pharmaceutical Industry.- 5.5.1 Summary.- 5.5.2 Introduction.- 5.5.3 Procedure.- 5.6 Qualitative and Quantitative Analysis of a Polymeric Material using Thermogravimetric Analysis (TGA).- 5.6.1 Summary.- 5.6.2 Introduction.- 5.6.3 Procedure.- 6: Organic Trace Analysis of Low Molecular Weight Analytes in Environmental Samples and Biological Materials.- 6.1 Determination of Aromatic and Aliphatic Isocyanates in Workplace Atmospheres by HPLC.- 6.1.1 Summary.- 6.1.2 Introduction.- 6.1.3 Procedure.- 6.1.4 Calculation.- 6.2 Determination of Triazine Pesticide Residues inEnvironmental Samples by Enzyme-Linked Immunosorbent Assay (ELISA).- 6.2.1 Summary.- 6.2.2 Introduction.- 6.2.3 Procedure.- 6.3 Analysis of Alcoholic Beverages.- 6.3.1 Summary.- 6.3.2 Introduction.- 6.3.3 Procedure.- 6.4 Determination of Contaminating Antibiotic Trace Concentrations in Dairy Feedstuffs by GC--MS.- 6.4.1 Summary.- 6.4.2 Introduction.- 6.4.3 Procedure.- 6.5 Extraction of Cocaine and its Metabolites from a Urine Sample by Solid-Phase Extraction.- 6.5.1 Summary.- 6.5.2 Introduction.- 6.5.3 Procedure.- 6.6 Determination of Nitroglycerin, 2,4-Dinitrotoluene and Diphenylamine in Gunshot Residue by High-Performance Liquid Chromatography with Electrochemical Detection (HPLC--ED).- 6.6.1 Summary.- 6.6.2 Introduction.- 6.6.3 Procedure.- 6.7 Determination of Prozac (Fluoxetine) and its Demethylated Metabolite in Serum by HPLC with Fluorescence Detection.- 6.7.1 Summary.- 6.7.2 Introduction.- 6.7.3 Procedure.- 6.8 Direct Determination of Thioamide Drugs in Biological Fluids by Cathodic Stripping Voltammetry.- 6.8.1 Summary.- 6.8.2 Introduction.- 6.8.3 Procedure.- 6.8.4 Calculation.- 7: Analysis of High Molecular Weight Analytes.- 7.1 Analysis of Abnormal or Variant Haemoglobins by HPLC-Electrospray MS.- 7.1.1 Summary.- 7.1.2 Introduction.- 7.1.3 Procedure.- 7.2 Determination of Insulin by Radioimmunoassay (RIA).- 7.2.1 Summary.- 7.2.2 Introduction.- 7.2.3 Procedure.- 7.2.4 Calculation.- 7.3 Fluorescence of Europium Chelates and its Application to Fluoroimmunoassay of Prostate-Specific Antigen (PSA) in Human Serum.- 7.3.1 Summary.- 7.3.2 Introduction.- 7.3.3 Procedure.- References.