ENVIRONMENTAL ANALYSIS OF CHEMICAL POLLUTANTS
CONTENTS I PART ANALYTICAL TECHNIQUES 1 INTRODUCTION 2 PRECISION AND ACCURACY OF ANALYSIS QUALITY ASSURANCE AND QUALITY CONTROL IN ENVIRONMENTAL ANALYSIS PRECISION AND ACCURACY CONTROL CHARTS 3 ANALYSIS OF ORGANIC POLLUTANTS BY GAS CHROMATOGRAPHY SELECTION OF COLUMN DETECTORS CALIBRATION CALCULATIONS EXTERNAL STANDARD CALIBRATION ALTERNATIVE CALCULATION INTERNAL STANDARD METHOD ROUTINE ANALYSIS 4 ANALYSIS OF ORGANIC POLLUTANTS BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY TERMS AND DEFI NITIONS APPLICATION OF MASS SPECTROMETRY INTERPRETATION OF MASS SPECTRA NUMBER OF CARBON ATOMS “NITROGEN RULE” INDEX OF HYDROGEN DEFI CIENCY DETERMINATION OF MOLECULAR FORMULA CHEMICAL IONIZATION LIMITATION OF GC/MS ANALYSIS US EPA METHODS VOLATILE ORGANICS BY PURGE AND TRAP METHOD SEMIVOLATILE ORGANICS TUNING COMPOUND IDENTIFI CATION REFERENCES 5 EXTRACTION OF ORGANIC POLLUTANTS AND SAMPLE CLEANUP SAMPLE EXTRACTION LIQUID–LIQUID EXTRACTION SOLID PHASE EXTRACTION SOXHLET EXTRACTION SUPERCRITICAL FLUID EXTRACTION CLEANUP ACID–BASE PARTITIONING ALUMINA COLUMN CLEANUP SILICA GEL CLEANUP FLORISIL COLUMN CLEANUP GEL-PERMEATION CLEANUP SULFUR CLEANUP PERMANGANATE–SULFURIC ACID CLEANUP 6 TITRIMETRIC ANALYSIS ACID–BASE TITRATION CALCULATION OXIDATION–REDUCTION TITRATIONS STANDARDIZATION OF OXIDANTS REDUCING AGENT OXIDATION–REDUCTION INDICATORS IODOMETRIC TITRATION ROLE OF POTASSIUM IODIDE STARCH INDICATOR ARGENTOMETRIC TITRATION COMPLEXOMETRIC TITRATIONS POTENTIOMETRIC TITRATION END POINT DETECTION 7 COLORIMETRIC ANALYSIS 8 ANALYSIS OF METALS BY ATOMIC ABSORPTION AND EMISSION SPECTROSCOPY ATOMIC SPECTROSCOPY: AN OVERVIEW SAMPLE DIGESTION FOR METALS ATOMIC ABSORPTION SPECTROMETRY CHELATION–EXTRACTION METHOD HYDRIDE GENERATION METHOD COLD VAPOR METHOD FOR MERCURY DETERMINATION ACCURACY IN QUANTITATION STANDARD ADDITION ATOMIC EMISSION PLASMA SPECTROSCOPY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY 9 ION-SELECTIVE ELECTRODES ANALYSIS ENVIRONMENTAL SAMPLE ANALYSIS STANDARD CALIBRATION METHOD STANDARD ADDITION METHOD SAMPLE ADDITION METHOD 10 APPLICATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY IN ENVIRONMENTAL ANALYSIS 11 ION CHROMATOGRAPHY 12 AIR ANALYSIS SAMPLING PLAN AIR SAMPLING DIRECT COLLECTION OF AIR USE OF ADSORBENT TUBES AIR SAMPLING FOR PARTICULATES AND INORGANIC SUBSTANCES FLOW RATE CHEMICAL ANALYSIS 13 APPLICATION OF IMMUNOASSAY TECHNIQUES IN ENVIRONMENTAL ANALYSIS EXTRACTION I PART I SPECIFI C CLASSES OF SUBSTANCES AND AGGREGATE PROPERTIES 14 ALDEHYDES AND KETONES DERIVATIZATION WITH 2,4-DINITROPHENYLHYDRAZINE CHROMATOGRAPHIC COLUMNS AND CONDITIONS SAMPLE COLLECTION AND HOLDING TIME AIR ANALYSIS 15 ALKALINITY 16 BROMIDE PHENOL RED COLORIMETRIC METHOD PROCEDURE REAGENTS TITRIMETRIC METHOD DETERMINATION OF BROMIDE PLUS IODIDE DETERMINATION OF IODIDE 17 CHLORIDE MERCURIC NITRATE TITRIMETRIC METHOD ARGENTOMETRIC TITRIMETRIC METHOD AUTOMATED FERRICYANIDE COLORIMETRIC METHOD GRAVIMETRIC DETERMINATION OF CHLORIDE 18 CYANATE 19 CYANIDE, TOTAL SILVER NITRATE TITRIMETRIC METHOD COLORIMETRIC METHOD PREPARATION OF CYANIDE STANDARDS AND CALIBRATION CURVE DETERMINATION OF CYANIDE IN SOIL, SEDIMENT, AND SOLID WASTE CYANIDES IN AEROSOL AND GAS 20 CYANIDE AMENABLE TO CHLORINATION ALTERNATIVE PROCEDURE 21 EMERGING POLLUTANTS: NONIONIC SURFACTANTS—ALKYLPHENOLS AND THEIR ETHOXYLATES STRUCTURES SAMPLE EXTRACTIONS AND ANALYSIS: GENERAL DISCUSSION SPE–LC/MS METHOD (LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY (LC-MS/MS)) SPE–GC/MS METHOD 22 EMERGING POLLUTANTS: ORGANOPHOSPHATE FLAME RETARDANTS, PLASTICIZERS, AND LUBRICANTS ANALYSIS OF INDOOR DUST 23 EMERGING POLLUTANTS: PHARMACEUTICALS AND PERSONAL CARE PRODUCTS US EPA METHOD SUMMARY OF THE METHOD SAMPLE PREPARATION SAMPLE CLEANUP LC-MS/MS ANALYSIS QUALITATIVE DETERMINATION AND QUANTIFI CATION QUALITY ASSURANCE/QUALITY CONTROL SAMPLE COLLECTION, PRESERVATION, AND HOLDING TIME 24 EMERGING POLLUTANTS: STEROIDS AND HORMONES OUTLINE OF THE PROCEDURE SAMPLE COLLECTION, PRESERVATION, AND STORAGE GC CONDITIONS MS CONDITIONS CALIBRATION AND QUANTITATION QUALITY CONTROL 25 FLUORIDES COLORIMETRIC SPADNS METHOD AUTOMATED COLORIMETRIC METHOD 26 HALOACETIC ACIDS ALTERNATIVE METHODS 27 HALOGENATED HYDROCARBONS SOLVENT EXTRACTION SAMPLE COLLECTION AND PRESERVATION INTERNAL STANDARDS/SURROGATES AND TUNING COMPOUNDS 28 HARDNESS HARDNESS DETERMINATIONS TITRATION 29 HERBICIDES: CHLOROPHENOXY ACID ANALYSIS HYDROLYSIS ESTERIFI CATION GAS CHROMATOGRAPHIC ANALYSIS 30 HERBICIDES: GLYPHOSATE WATER ANALYSIS HPLC METHOD SAMPLING AND STORAGE DETECTION LIMIT MISCELLANEOUS METHODS FOR ANALYSIS OF GLYPHOSATE RESIDUES IN WATER, SOIL, SLUDGE, FRUIT, AND VEGETABLE EXTRACTS 31 HYDROCARBONS TOTAL PETROLEUM HYDROCARBONS GASOLINE RANGE ORGANICS DIESEL RANGE ORGANICS 32 HYDROCARBONS, POLYNUCLEAR AROMATIC HPLC COLUMNS AND CONDITIONS GC COLUMNS AND CONDITIONS SAMPLE EXTRACTION AND CLEANUP REFERENCE 33 NITROGEN (AMMONIA) SAMPLE DISTILLATION COLORIMETRIC NESSLERIZATION METHOD REAGENTS AND STANDARDS COLORIMETRIC PHENATE METHOD ION-SELECTIVE ELECTRODE 34 NITROGEN (NITRATE) CADMIUM REDUCTION METHOD APPARATUS, REAGENTS, AND STANDARDS MISCELLANEOUS REDUCTION METHOD NITRATE ELECTRODE METHOD 35 NITROSAMINES 36 OIL AND GREASE PARTITION-GRAVIMETRY METHOD PARTITION-INFRARED METHOD SOLID PHASE PARTITION-GRAVIMETRIC METHOD HYDROCARBONS 37 OXYGEN DEMAND, BIOCHEMICAL GRAPHICAL CALCULATION METHOD MEASUREMENT OF DISSOLVED OXYGEN IODOMETRIC OR WINKLER METHOD ELECTRODE METHOD KINETICS OF BOD REACTION 38 OXYGEN DEMAND, CHEMICAL SAMPLE TREATMENT COLORIMETRIC ANALYSIS 39 OXYHALIDES ANALYSIS OF OXYHALIDES BY US EPA METHODS INTERFERENCE MISCELLANEOUS METHODS 40 PESTICIDES: CARBAMATE, UREA, AND TRIAZINE CARBAMATE PESTICIDES LC COLUMNS CHROMATOGRAPHIC CONDITIONS HYDROLYSIS CONDITIONS POSTCOLUMN DERIVATIZATION CONDITIONS FLUOROMETER CONDITIONS UREA PESTICIDES COLUMN LIQUID CHROMATOGRAPH MASS SPECTROMETER TRIAZINE PESTICIDES 41 PESTICIDES: ORGANOCHLORINE 42 PESTICIDES: ORGANOPHOSPHORUS ANALYSIS OF AQUEOUS AND SOLID SAMPLES 43 PH AND EH 44 PHENOLS DERIVATIZATION 45 PHOSPHORUS SAMPLE PRESENTATION CALIBRATION STANDARDS ION CHROMATOGRAPHY 46 PHTHALATE ESTERS 47 POLYCHLORINATED BIPHENYLS QUANTITATION ALTERNATE ANALYTICAL METHODS 48 POLYCHLORINATED DIOXINS AND DIBENZOFURANS ALUMINA CLEANUP CARBON COLUMN CLEANUP GC/MS ANALYSIS SAMPLE PRESERVATION AND HOLDING TIME 49 RADIOACTIVITY UNITS OF MEASUREMENT INSTRUMENTS FOR MEASURING RADIOACTIVITY GAS-FLOW PROPORTIONAL COUNTERS ALPHA SCINTILLATION COUNTERS LIQUID SCINTILLATION COUNTERS ALPHA SPECTROMETERS GAMMA SPECTROMETERS DETERMINATION OF GROSS ALPHA AND GROSS BETA RADIOACTIVITY EVAPORATION METHOD GROSS ACTIVITY OF THE SAMPLE ACTIVITY OF DISSOLVED AND SUSPENDED MATTER ACTIVITY OF SEMISOLID SAMPLES COPRECIPITATION METHOD FOR GROSS ALPHA ACTIVITY SPECIFI C RADIONUCLIDES RADIUM PRECIPITATION METHOD AND ALPHA COUNTING SEQUENTIAL PRECIPITATION METHOD MEASUREMENT OF RADIUM-224 BY GAMMA SPECTROSCOPY RADON URANIUM DETERMINATION OF TOTAL ALPHA ACTIVITY DETERMINATION OF ISOTOPIC CONTENT OF URANIUM ALPHA ACTIVITY RADIOACTIVE STRONTIUM TRITIUM RADIOACTIVE IODINE PRECIPITATION METHOD ION-EXCHANGE METHOD DISTILLATION METHOD RADIOACTIVE CESIUM REAGENT SOLUTION 50 SEMIVOLATILE ORGANIC COMPOUNDS 51 SILICA GRAVIMETRIC METHOD AMMONIUM MOLYBDATE COLORIMETRIC METHOD REAGENT 52 SULFATE TURBIDIMETRIC METHOD 53 SULFI DE ANALYSIS OF SULFI DE IN WATER SCREENING TEST FOR SULFI DE SAMPLE PRETREATMENT ANALYSIS OF DISSOLVED SULFI DE IN WATER IODOMETRIC METHOD METHYLENE BLUE COLORIMETRIC METHOD METHYLENE BLUE SOLUTION: PREPARATION AND STANDARDIZATION STANDARDIZATION 54 SULFI TE 55 SURFACTANT: ANIONIC SAMPLE ANALYSIS 56 THIOCYANATE REAGENTS AND CALIBRATION STANDARDS SPOT TEST FOR THIOCYANATE 57 VOLATILE ORGANIC COMPOUNDS APPARATUS GC AND MS CONDITIONS SOIL, SEDIMENTS, AND SOLID WASTES US EPA’S SW METHODS US EPA METHOD TO-14A US EPA’S SOLID WASTES 846 METHODS NIOSH METHOD GC COLUMN AND CONDITIONS II PART I SELECTED INDIVIDUAL COMPOUNDS 58 ACETALDEHYDE ANALYSIS OF AQUEOUS SAMPLE 59 ACETONE ANALYSIS OF AQUEOUS SAMPLES 60 ACETONITRILE ANALYSIS OF AQUEOUS AND NONAQUEOUS SAMPLES 61 ACROLEIN 62 ACRYLONITRILE 63 ANILINE DESCRIPTION 64 ARSINE 65 ASBESTOS 66 BENZENE 67 BENZIDINE 68 BENZYL CHLORIDE 69 1,3-BUTADIENE 70 CAPTAN 71 CARBON DISULFI DE 72 CARBON MONOXIDE 73 CARBON TETRACHLORIDE 74 CHLOROACETIC ACID 75 CHLOROBENZENE 76 CHLOROFORM 77 2-CHLOROPHENOL 78 CUMENE 79 CYANOGEN AIR ANALYSIS (SUGGESTED METHOD) 80 CYANURIC ACID 81 DIAZOMETHANE 82 DIBORANE 83 DICHLOROBENZENE 84 1,1-DICHLORETHYLENE 85 2,4-DICHLOROPHENOL 86 DIETHYL ETHER 87 2,4-DINITROTOLUENE 88 2,6-DINITROTOLUENE 89 EPICHLOROHYDRIN 90 ETHYLBENZENE 91 ETHYL CHLORIDE 92 ETHYLENE CHLOROHYDRIN 93 ETHYLENE DIBROMIDE 94 ETHYLENE GLYCOL ANALYSIS OF AQUEOUS AND NONAQUEOUS SAMPLES (SUGGESTED METHOD) 95 ETHYLENE OXIDE 96 FORMALDEHYDE 97 FREON 98 HYDROGEN CYANIDE 99 HYDROGEN SULFI DE 100 HYDROQUINONE 101 ISOPHORONE 102 METHANE ANALYSIS OF AQUEOUS SAMPLES AND SLUDGE DIGESTER GAS 103 METHYL BROMIDE 104 METHYL CHLORIDE 105 METHYLENE CHLORIDE 106 METHYL IODIDE 107 METHYL ISOBUTYL KETONE 108 METHYL ISOCYANATE 109 METHYL METHACRYLATE 110 NITROBENZENE 111 NITROGEN DIOXIDE 112 PENTACHLOROPHENOL 113 PHOSGENE 114 PYRIDINE 115 PYROCATECHOL 116 PYROGALLOL 117 RESORCINOL 118 STIBINE 119 STRYCHNINE 120 STYRENE 121 SULFUR DIOXIDE 122 TETRACHLOROETHYLENE 123 TETRAETHYLLEAD 124 TETRAETHYL PYROPHOSPHATE 125 TETRAHYDROFURAN 126 TOLUENE 127 TOLUENE-2,4-DIISOCYANATE 128 O-TOLUIDINE 129 1,1,1-TRICHLOROETHANE TRICHLOROETHYLENE 131 2,4,6-TRICHLOROPHENOL 132 VINYL CHLORIDE 133 XYLENE