Analysis. Environmental. Handbook of. Pradyot Patnaik. Air, Water, Soil, and Solid Wastes. Chemical Pollutants in UNIVERSITATSBIBLIOTHEK HANNOVER
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1 Handbook of Environmental Second Edition Chemical Pollutants in, Water, Soil, and Solid Wastes Pradyot Patnaik TECHNISCHE INFORMATION SBIBLIOTHEK UNIVERSITATSBIBLIOTHEK HANNOVER CRC Press Taylor & Francis Group Boca Raton London New York CRC Press is an imprint of the Taylor & Francis Croup, an Informa business
2 Contents List of Tables Preface xxiii xxvti Preface to the First Edition xxix Acknowledgments Author Glossary of Terms: Units, Conversions, and Abbreviations xxxv xxxi xxxiii PART I Analytical Techniques 1. Introduction 3 2. Precision and Accuracy of 7 Quality Assurance and Quality Control in Environmental 7 Precision and Accuracy 8 Control Charts of Organic Pollutants by Gas Chromatography 21 Selection of Column 22 Detectors 25 Calibration 26 Calculations 27 External Standard Calibration 27 Alternative Calculation 29 Internal Standard Method 29 Routine of Organic Pollutants by Gas Chromatography/Mass Spectrometry 31 Terms and Definitions 31 Application of Mass Spectrometry 32 Interpretation of Mass Spectra 33 Number of Carbon Atoms 35 v
3 vi Contents "Nitrogen Rule" 36 Index of Hydrogen Deficiency 36 Determination of Molecular Formula 36 Chemical Ionization 38 Limitation of CC/MS 39 U.S. EPA Methods 39 Volatile Organics by Purge and Trap Method 40 Semivolatile Organics 41 Tuning 42 Compound Identification 44 Calibration 45 References Extraction of Organic Pollutants and Sample Cleanup 49 Sample Extraction 49 Liquid-Liquid Extraction 49 Solid Phase Extraction 51 Soxhlet Extraction 51 Supercritical Fluid Extraction 52 Cleanup 52 Acid-Base Partitioning 53 Alumina Column Cleanup 54 Silica Gel Cleanup 54 Florisil Column Cleanup 55 Gel-Permeation Cleanup 55 Sulfur Cleanup 55 Permanganate-Sulfuric Acid Cleanup Titrimetric 57 Acid-Base Titration 58 Calculation 61 Oxidation-Reduction Titrations 64 Standardization of Oxidants 68 Reducing Agent 69 Oxidation-Reduction Indicators 70 lodometric Titration 71 Role of Potassium Iodide 74 Reducing Agent 74 Standardization of Na2S Starch Indicator 76 Argentometric Titration 77 Complexometric Titrations 80 Potentiometric Titration 82 End Point Detection Colorimetric 85
4 Contents vii 8. of Metals by Atomic Absorption and Emission Spectroscopy 89 Atomic Spectroscopy: An Overview 90 Sample Digestion for Metals 91 Atomic Absorption Spectrometry 92 Chelation-Extraction Method 94 Hydride Generation Method 95 Cold Vapor Method for Mercury Determination 95 Accuracy in Quantitation 96 Standard Addition 97 Atomic Emission Plasma Spectroscopy 98 Inductively Coupled Plasma Mass Spectrometry Ion-Selective Electrodes 103 Environmental Sample 104 Standard Calibration Method 105 Standard Addition Method 106 Sample Addition Method Application of High-Performance Liquid Chromatography in Environmental Ion Chromatography 115 References Sampling Plan 121 Sampling 122 Direct Collection of 122 Use of Adsorbent Tubes 123 Sampling for Particulates and Inorganic Substances 124 Flow Rate 125 Chemical 125 Calculation Application of Immunoassay Techniques in Environmental 131 Extraction 133 Calculation 133 PART II Specific Aggregate Properties Classes of Substances and 14. Aldehydes and Ketones 137 Derivatization with 2,4-Dinitrophenylhydrazine 139 Chromatographic Columns and Conditions 141 Sample Collection and Holding Time
5 viii Contents 15. Alkalinity 145 Calculation Bromide 147 Phenol Red Colorimetric Method 147 Procedure 148 Reagents 148 Titrimetric Method 148 Determination of Bromide Plus Iodide 149 Procedure 149 Determination of Iodide 150 Calculation Chloride 153 Mercuric Nitrate Titrimetric Method 153 Procedure 154 Reagents 154 Argentometric Titrimetric Method 155 Procedure 155 Reagents 156 Automated Ferricyanide Colorimetric Method 156 Procedure 156 Reagents 157 Gravimetric Determination of Chloride 157 Procedure 157 Calculation Cyanate 159 Calculation 159 Procedure Cyanide, Total 161 Silver Nitrate Titrimetric Method 161 Procedure 162 Reagents 162 Colorimetric Method 162 Procedure 163 Preparation of Cyanide Standards and Calibration Curve 165 Reagents 166 Determination of Cyanide in Soil, Sediment, and Solid Waste 166 Cyanides in Aerosol and Gas Cyanide Amenable to Chlorination 169 Procedure 169 Alternative Procedure 170 Reagents Emerging Pollutants: Nonionic Surfactants Alkylphenols and Their Ethoxylates 173 Structures 174
6 Contents ix Sample Extractions and : General Discussion 175 SPE-LC/MS Method (Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)) 178 SPE-CC/MS Method 179 References Emerging Pollutants: Organophosphate Flame Retardants, Plasticizers, and Lubricants 183 of Indoor Dust 188 References Emerging Pollutants: Pharmaceuticals and Personal Care Products 191 U.S. EPA Method Summary of the Method 191 Sample Preparation 195 Sample Cleanup 201 LC-MS/MS 201 Qualitative Determination and Quantification 202 Quality Assurance/Quality Control 203 Sample Collection, Preservation, and Holding Time 204 References 204 Pollutants: Steroids and Hormones Emerging Outline of the Procedure 207 Sample Collection, Preservation, and Storage 209 GC Conditions 210 MS Conditions 210 Calibration and Quantitation 211 Quality Control 215 References Fluorides 217 Colorimetric SPADNS Method 217 Procedure 218 Automated Colorimetric Method Haloacetic Acids 219 Alternative Methods 220 References Halogenated Hydrocarbons 223 Solvent Extraction 225 Sample Collection and Preservation 228 Internal Standards/Surrogates and Tuning Compounds
7 X Contents 28. Hardness 233 Hardness Determinations 234 Calculation 234 Titration Herbicides: Chlorophenoxy Acid Sample Extraction 235 Hydrolysis 236 Esterification 237 Gas Chromatographic Herbicides: Glyphosate 243 Water 243 HPLC Method 243 Sampling and Storage 244 Detection Limit 244 Miscellaneous Methods for of Glyphosate Residues in Water, Soil, Sludge, Fruit, and Vegetable Extracts 245 References Hydrocarbons Total Petroleum Hydrocarbons 248 Gasoline Range Organics 249 Diesel Range Organics Hydrocarbons, Polynuclear Aromatic 253 HPLC Columns and Conditions 255 GC Columns and Conditions 255 MS Conditions 255 Sample Extraction and Cleanup Reference Nitrogen (Ammonia) 259 Sample Distillation 259 Reagents 260 Titrimetric Method 260 Reagents 261 Colorimetric Nesslerization Method 262 Procedure 262 Calculation 262 Reagents and Standards 263 Colorimetric Phenate Method 264 Procedure 264 Calculation 264 Reagents and Standards 265
8 Contents xi Ion-Selective Electrode 266 Procedure 267 Reagents and Standards Nitrogen (Nitrate) 269 Cadmium Reduction Method 269 Procedure 270 Apparatus, Reagents, and Standards 271 Miscellaneous Reduction Method 271 Nitrate Electrode Method 272 Procedure 272 Reagents Nitrosamines 273 Extraction References Oil and Grease 279 Partition-Cravimetry Method 280 Partition-Infrared Method 281 Solid Phase Partition-Gravimetric Method 282 Hydrocarbons 283 Sample Collection and Preservation 284 References Oxygen Demand, Biochemical 285 Graphical Calculation 287 Method 287 Measurement of Dissolved Oxygen 288 lodometric or Winkler Method 288 Electrode Method 289 Kinetics of BOD Reaction 290 Reference Oxygen Demand, Chemical 293 Sample Treatment 296 Colorimetric Oxyhalides 299 of Oxyhalides by U.S. EPA Methods 299 U.S. EPA Method U.S. EPA Method Interference 301 Sample Collection, Preservation, and Storage 302 Quality Control 302 Miscellaneous Methods 303 References 303
9 xii Contents 40. Pesticides: Carbamate, Urea, and Triazine 305 Carbamate Pesticides 306 LC Columns 306 Chromatographic Conditions 307 Hydrolysis Conditions 307 Postcolumn Derivatization Conditions 308 Fluorometer Conditions 308 Extraction 308 Urea Pesticides 309 Column 310 Liquid Chromatograph 310 Mass Spectrometer 310 Precision and Accuracy 311 Triazine Pesticides 311 Sample Extraction Pesticides: Organochlorine 315 Sample Extraction References Pesticides: Organophosphorus 323 of Aqueous and Solid Samples 324 Sample Extraction ph and Eh 331 Eh Phenols 337 Extraction Derivatization Phosphorus Sample Presentation 343 Colorimetric 345 Interference 346 Calibration Standards 346 Ion Chromatography Phthalate Esters
10 Contents xiii 47. Polychlorinated Biphenyls 353 Quantitation 355 Sample Extraction and Cleanup 356 Alternate Analytical Methods Polychlorinated Dioxins and Dibenzofurans Sample Extraction and Cleanup 360 Acid-Base Partitioning 360 Alumina Cleanup 360 Silica Gel Cleanup 361 Carbon Column Cleanup 361 GC/MS 361 Sample Preservation and Holding Time 362 References Radioactivity 363 Units of Measurement 363 Instruments for Measuring Radioactivity 365 Gas-Flow Proportional Counters 365 Alpha Scintillation Counters 366 Liquid Scintillation Counters 366 Alpha Spectrometers 367 Gamma Spectrometers 368 Determination of Gross Alpha and Gross Beta Radioactivity 368 Evaporation Method 369 Gross Activity of the Sample 369 Activity of Dissolved and Suspended Matter 370 Activity of Semisolid Samples 371 Coprecipitation Method for Gross Alpha Activity 372 Procedure 373 Specific Radionuclides 373 Radium 374 Precipitation Method and Alpha Counting 374 Precipitation and Emanation Method to Measure Radium as Radon Sequential Precipitation Method 377 Measurement of Radium-224 by Gamma Spectroscopy 377 Radon 378 Uranium 379 Determination of Total Alpha Activity 379 Determination of Isotopic Content of Uranium Alpha Activity 380 Radioactive Strontium 381 Tritium 383 Radioactive Iodine 384 Precipitation Method 385
11 xiv Contents Ion-Exchange Method 386 Distillation Method 387 Radioactive Cesium 389 Preparation of Ammonium Phosphomolybdate, (NH^PMo^O^ Reagent Solution 390 References Semivolatile Organic Compounds 393 Sampling and Storage 410 References Silica 413 Gravimetric Method 413 Procedure 414 Ammonium Molybdate Colorimetric Method 414 Procedure 415 Reagent Sulfate 417 Gravimetric Method 417 Interference 418 Procedure 418 Calculation 418 Turbidimetric Method 419 Procedure 419 Calculation 419 Reagents Sulfide 421 of Sulfide in Water 422 Screening Test for Sulfide 422 Sample Pretreatment 423 of Dissolved Sulfide in Water 423 lodometric Method 424 Procedure 424 Calculation 424 Reagents 425 Methylene Blue Colorimetric Method 426 Procedure 427 Methylene Blue Solution: Preparation and Standardization 428 Standardization 428 Reagents Sulfite 431 lodometric Method 431 Interference 432 Procedure 432 Calculation 432 Reagents 433
12 Contents xv Colorimetric Method 433 Procedure 434 Calculation 435 Reagents Surfactant: Anionic 437 Reagents 439 Sample 439 Calculation 439 Interference Thiocyanate 441 Colorimetric Method 441 Interference 441 Procedure 442 Calculation 442 Reagents and Calibration Standards 442 Spot Test for Thiocyanate 443 Procedure 443 Reagents Volatile Organic Compounds 445 Water 445 Apparatus 446 CC and MS Conditions 447 Soil, Sediments, and Solid Wastes 448 U.S. EPA's SW Methods U.S. EPA Method TO-14A 454 U.S. EPA's Solid Wastes 846 Methods 458 NIOSH Method GC Column and Conditions 459 MS Conditions 459 References 462 PART III Selected Individual Compounds 58. Acetaldehyde 467 of Aqueous Sample Acetone 469 of Aqueous Samples Acetonitrile 471 of Aqueous and Nonaqueous Samples
13 xvi Contents 61. Acrolein 473 of Aqueous and Nonaqueous Samples Acrylonitrile 475 of Aqueous and Nonaqueous Samples Aniline 477 Description 477 of Aqueous and Nonaqueous Samples Arsine Asbestos of Aqueous Samples Benzene 485 of Aqueous and Nonaqueous Samples Benzidine 487 of Aqueous and Nonaqueous Samples Benzyl Chloride 489 Description 489 of Aqueous and Nonaqueous Samples ,3-Butadiene Captan 493 of Aqueous and Nonaqueous Samples Carbon Disulfide 495 Description 495 of Aqueous and Nonaqueous Samples Carbon Monoxide Carbon Tetrachloride 499 of Aqueous and Nonaqueous Samples
14 Contents xvii 74. Chloroacetic Acid 501 of Aqueous Samples Chlorobenzene 505 of Aqueous and Nonaqueous Samples Chloroform 507 of Aqueous and Nonaqueous Samples Chlorophenol 509 of Aqueous and Nonaqueous Samples Cumene 511 of Aqueous and Nonaqueous Samples Cyanogen 513 (Suggested Method) Cyanuric Acid 515 of Aqueous and Nonaqueous Samples Diazomethane Diborane Dichlorobenzene 521 of Aqueous and Nonaqueous Samples ,1-Dichlorethylene 523 of Aqueous and Nonaqueous Samples ,4-Dichlorophenol 525 of Aqueous and Nonaqueous Samples Diethyl Ether 527 of Aqueous Samples
15 xviii Contents 87. 2,4-Dinitrotoluene 529 of Aqueous and Nonaqueous Samples ,6-Dinitrotoluene 531 of Aqueous and Nonaqueous Samples Epichlorohydrin 533 of Aqueous and Nonaqueous Samples Ethylbenzene 535 of Aqueous and Nonaqueous Samples Ethyl Chloride 537 of Aqueous Samples Ethylene Chlorohydrin 539 of Aqueous Sample Ethylene Dibromide 541 of Aqueous and Nonaqueous Samples Ethylene Glycol 543 of Aqueous and Nonaqueous Samples (Suggested Method) Reference Ethylene Oxide Formaldehyde 547 Water Freon of Aqueous Samples Hydrogen Cyanide 551 of Aqueous Samples Reference Hydrogen Sulfide
16 Contents xix 100. Hydroquinone 555 of Aqueous and Nonaqueous Samples Isophorone 557 of Aqueous and Nonaqueous Samples Methane 559 of Aqueous Samples and Sludge Digester Gas Methyl Bromide 561 of Aqueous Samples Methyl Chloride 563 of Aqueous and Nonaqueous Samples Methylene Chloride 565 of Aqueous and Nonaqueous Samples Methyl Iodide 567 of Aqueous Samples Methyl Isobutyl Ketone 569 of Aqueous and Nonaqueous Samples Methyl Isocyanate Methyl Methacrylate 573 of Aqueous Samples Nitrobenzene 575 of Aqueous and Nonaqueous Samples Nitrogen Dioxide Pentachlorophenol 579 of Aqueous and Nonaqueous Samples Phosgene
17 xx Contents 114. Pyridine 583 of Aqueous and Nonaqueous Samples Pyrocatechol 585 of Aqueous and Nonaqueous Samples Pyrogallol 587 of Aqueous and Nonaqueous Samples Resorcinol 589 of Aqueous and Nonaqueous Samples Stibine Strychnine 593 of Aqueous and Nonaqueous Samples Styrene 595 of Aqueous and Nonaqueous Samples Sulfur Dioxide Tetrachloroethylene 599 of Aqueous and Nonaqueous Samples Tetraethyllead 601 of Aqueous and Nonaqueous Samples Tetraethyl Pyrophosphate 603 of Aqueous and Nonaqueous Samples Tetrahydrofuran 605 of Aqueous Samples Toluene 607 of Aqueous and Nonaqueous Samples Toluene-2,4-Diisocyanate 609 of Aqueous and Nonaqueous Samples Reference 610
18 Contents xxi 128. o-toluidine 611 of Aqueous and Nonaqueous Samples ,1,1-Trichloroethane 613 of Aqueous and Nonaqueous Samples Trichloroethylene 615 of Aqueous and Nonaqueous Samples ,4,6-Trichlorophenol 617 of Aqueous and Nonaqueous Samples Vinyl Chloride 619 of Aqueous Samples Xylene 621 of Aqueous and Nonaqueous Samples Bibliography 625 Appendix A: Some Common QC Formulas and Statistics 629 Measurement of Precision 629 Standard Deviation 629 Relative Standard Deviation (RSD) 629 Standard Error of Mean (M) 630 Relative Percent Difference (RPD) 630 Measurement of Linearity of Data Points 630 Correlation Coefficient (y) 630 Measurement of Accuracy 632 Percent Spike Recovery by U.S. EPA Formula 632 Percent Spike Recovery by Alternate Method 632 Method Detection Limits for Organic Pollutants in Aqueous Samples 633 Method Detection Limit (MDL) 633 Appendix B: Sample Containers, Preservations, and Holding Times 635 Appendix C: Preparation of Molar and Normal Solutions of Some Common Reagents 639 Appendix D: Total Dissolved Solids and Specific Conductance: Theoretical Calculations 641 Total Dissolved Solids 641 Conductivity 642
19 xxii Contents Appendix E: Characteristic Masses of Miscellaneous Organic Pollutants (Not Listed in Text) for CC/MS Identification 649 Appendix F: Volatility of Some Additional Organic Substances (Not Listed in Text) for the Purge and Trap 653 Appendix C: NIOSH Methods for 657 Appendix H: A Full List of NIOSH Analytical Methods for Indoor (Update 2006) 667 Appendix I: U.S. EPA Methods for 691 Appendix J: Inorganic Test Procedures for of Aqueous Samples: EPA, SM, and ASTM Reference Methods 697 Appendix K: U.S. EPA'S Analytical Methods for Organic Pollutants in Aqueous and Solid Matrices 705 Chemical Compound Index 731 CAS Index 755 Index 771
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