standart methods

METHODWASTE WATER

21st Edition

2005PREPARED AND PUBLISHED JOINTLY BYAmerican Public Health AssociationAmerican Water Works AssociationWater Environment Federation

JOINT EDITORIAL BOARD. AndrewD. Eaton, AWWA, Chair';....L?nore S. Clesceri, WEF.,-j Eugene W. Rice, APHA

- Arnold E. Greenherg (deceased), APHA

MANAGING EDITORMary Ann H. Franson

PUBLICATION OFFICEAmerican Public Health Association8001 Street, NWWashington, DC 20001-3 710

Centennial Edition

TABLE OF CONTENTS

PAGE

Part 1000 INTRODUCTION1010 INTRODUCTION 1-1

A. Scope and Application of Methods. . . . 1-1B. Statistics 1-1C. Glossary 1-3

1020 QUALITY ASSURANCE 1-4A. Introduction 1-4B. Quality Control 1-5C. Quality Assessment 1-12

1030 DATA QUALITY 1-13A. Introduction 1-13B. Measurement Uncertainty. 1-13C. Method Detection Level 1-17D. Data Quality Objectives 1-18E. Checking Correctness of Analyses . . . . 1-21

1040 METHOD DEVELOPMENT AND EVALUATION . . . 1-22

A. Introduction 1-22B. Method Validation , 1-22C. Collaborative Testing 1-24

1050 EXPRESSION OF-RESULTS 1-25

A. Units 1-25B. Significant Figures . . . : 1-26

1060 COLLECTION AND PRESERVATION

OF SAMPLES 1-27

A. Introduction 1-27B. Collection of Samples 1-29C. Sample Storage and Preservation 1-34

1080 REAGENT WATER 1-36

A. Introduction 1-36B. Methods for Preparation of Reagent

Water 1-36C. Reagent Water Quality 1-37

1090 LABORATORY OCCUPATIONAL HEALTH

AND SAFETY 1-38

A. Introduction 1-38B. Safe Laboratory Practices 1-39C. Laboratory Facility/Fixed Equipment . . 1-44D. Hazard Evaluation 1-45E. Personal Protective Equipment 1-46F. Worker Protection Medical Program. . . 1-49G. Provisions for Work with Particularly

Hazardous Substances 1-50H. Biological Safety 1-50I. Radiological Safety 1-51J. Chemical Hygiene Plan 1 -54

1100 WASTE MINIMIZATION AND DISPOSAL 1-55

A. Introduction 1-55B. Waste Minimization 1-55C. Waste Treatment and Disposal 1-55

Part 2000 PHYSICAL AND AGGREGATE PROPERTIES2010 INTRODUCTION 2-1

2020 QUALITY ASSURANCE/QUALITY CONTROL . . . 2-12110 APPEARANCE 2-1

2120 COLOR 2-1

A. Introduction 2-1B. Visual Comparison Method 2-2C. Spectrophotometric MethodSingle-

Wavelength Method (PROPOSED) . . 2-3D. Spectrophotometric MethodMulti-

Wavelength Method 2-4E. Tristimulus Spectrophotometric

Method 2-7F. ADMI Weighted-Ordinate

Spectrophotometric Method 2-72130 TURBIDITY 2-8

A. Introduction 2-8B. Nephelometric Method 2-9

2150 ODOR 2-11A. Introduction 2-11B. Threshold Odor Test 2-12

2160 TASTE 2-16

A. Introduction 2-16B. Flavor Threshold Test (FTT) 2-16C. Flavor Rating Assessment (FRA) . . . . 2-18

2170 FLAVOR PROFILE ANALYSIS 2-19

A. Introduction 2-19B. Flavor Profile Analysis 2-19

2310 ACIDITY 2-24

A. Introduction .__. . . 2-24B. Titration Method 2-24

2320 ALKALINITY 2-27A. Introduction 2-27B. Titration Method 2-27

2330 CALCIUM CARBONATE SATURATION 2-30

A. Introduction 2-30B. Indices Indicating Tendency of a Water

to Precipitate CaCO3 or DissolveCaCO3 2-31

C. Indices Predicting the Quantity ofCaCO3 That Can Be Precipitated orDissolved 2-34

D. Diagrams and Computer Codes forCaCO3 Indices 2-35

2340 HARDNESS 2-37A. Introduction 2-37B. Hardness by Calculation 2-37C. EDTA Titrimetric Method 2-37

2350 OXIDANT DEMAND/REQUIREMENT 2-40

TABLE OF CONTENTS

A. Introduction 2-40B. Chlorine Demand/Requirement 2-41C. Chlorine Dioxide

Demand/Requirement 2-42D. Ozone Demand/RequirementBatch

Method 2-43E. Ozone Demand/Requirement Semi-

Batch Method 2-432510 CONDUCTIVITY 2-44

A. Introduction 2-44B. Laboratory Method 2-47

2520 SALINITY 2-48A. Introduction 2-48B. Electrical Conductivity Method 2-49C. Density Method 2-50D. Algorithm of Practical Salinity 2-50

2530 FLOATABLES ' 2-51A. Introduction 2-51B. Paniculate Floatables 2-51C. Trichlorotrifiuoroethane-Soluble

Floatable Oil and Grease 2-532540 SOLIDS 2-55

A. Introduction 2-55B. Total Solids Dried at 103-105C 2-56C. Total Dissolved Solids Dried at 180C . 2-57D. Total Suspended Solids Dried

at 103-105C . . . , 2-58E. Fixed and Volatile Solids Ignited at

55OC 2-59F. Settleable Solids 2-59G. Total, Fixed, and Volatile Solids in

Solid and Semisolid Samples 2-602550 TEMPERATURE 2-61

A. Introduction 2-61B. Laboratory and Field Methods 2-61

2560 PARTICLE COUNTING AND SIZE DISTRIBUTION . 2-62A. Introduction 2-62B. Electrical Sensing Zone Method 2-66C. Light-Blockage Methods 2-68D. Light-Scattering Method 2-69

2570 ASBESTOS 2-70A. Introduction 2-70B. Transmission Electron Microscopy

Method 2-712580 OXIDATION-REDUCTION POTENTIAL (ORP). . . 2-75

A. Introduction 2-75B. Oxidation-Reduction Potential

Measurement in Clean Water 2-762710 TESTS ON SLUDGES 2-79

A. Introduction 2-79B. Oxygen-Consumption Rate 2-79C. Settled Sludge Volume 2-80D. Sludge Volume Index 2-81E. Zone Settling Rate 2-82F. Specific Gravity 2-83

G. Capillary Suction Time 2-83H. Time-to-Filter 2-85I. Modified Settled Sludge Volume 2-86

2720 ANAEROBIC SLUDGE DIGESTER GASANALYSIS 2-87

A. Introduction 2-87B. Volumetric Method 2-88C. Gas Chromatographic Method 2-89

2810 DISSOLVED GAS SUPERSATURATION 2-92A. Introduction 2-92B. Direct-Sensing Membrane-Diffusion

Method 2-92

Part 3000 METALS3010 INTRODUCTION 3-1

A. General Discussion 3-1B. Sampling and Sample Preservation. . . . 3-2C. General Precautions 3-3

3020 QUALITY ASSURANCE/QUALITY CONTROL . . . 3-4A. Introduction 3-4B. Quality Control Practices 3-4

3030 PRELIMINARY TREATMENT OF SAMPLES 3-5A. Introduction 3-5B. Filtration for Dissolved and Suspended

Metals 3-6C. Treatment for Acid-Extractable Metals . 3-6D. Digestion for Metals 3-7E. Nitric Acid Digestion 3-8F. Nitric Acid-Hydrochloric Acid

Digestion 3-9G. Nitric Acid-Sulfuric Acid Digestion . . . 3-10H. Nitric Acid-Perchloric Acid Digestion . . 3-10I. Nitric Acid-Perchloric Acid-

Hydrofluoric Acid Digestion 3-10J. Dry Ashing 3-11K. Microwave-Assisted Digestion .'~7 . . . . 3-11

3110 METALS BY ATOMIC ABSORPTIONSPECTROMETRY 3-13

3111 METALS BY FLAME ATOMIC ABSORPTIONSPECTROMETRY 3-13

A. Introduction 3-13B. Direct Air-Acetylene Flame Method. . . 3-17C. Extraction/Air-Acetylene Flame

Method 3-19D. Direct Nitrous Oxide-Acetylene Flame

Method 3-20E. Extraction/Nitrous Oxide-Acetylene

Flame Method 3-223112 METALS BY COLD-VAPOR ATOMIC ABSORPTION

SPECTROMETRY 3-23A. Introduction 3-23B. Cold-Vapor Atomic Absorption

Spectrometric Method 3-233113 METALS BY ELECTROTHERMAL ATOMIC

ABSORPTION SPECTROMETRY 3-25

TABLE OF CONTENTS

A. Introduction 3-25 3500-IrB. Electrothermal Atomic Absorption 3500-Fe

Spectrometric Method 3-273114 ARSENIC AND SELENIUM BY'HYDRIDE

GENERATION/ATOMIC ABSORPTION 35OO-PbSPECTROMETRY 3-32

A. Introduction 3-32B. Manual Hydride Generation/Atomic 3500-Li

Absorption Spectrometric Method. . . 3-33C. Continuous Hydride Generation/Atomic

Absorption Spectrometric Method. . . 3-37 3500-Mg3120 METALS BY PLASMA EMISSION

SPECTROSCOPY 3-38A. Introduction 3-38 3500-MnB. Inductively Coupled Plasma (ICP)

Method 3-393125 METALS BY INDUCTIVELY COUPLED PLASMA/ 3500-Hg

MASS SPECTROMETRY 3-45 3500-MoA. Introduction 3-45 3500-NiB. Inductively Coupled Plasma/Mass 3500-Os

Spectrometry (ICPMS) Method . . . . 3-45 3500-Pd3130 METALS BY ANODIC STRIPPING 3500-Pt

VOLTAMMETRY 3-53 3500-KA. Introduction ' 3-53B. Determination of Lead, Cadmium,

and Zinc 3-5435OO-A1 ALUMINUM '. ; 3-57

A. Introduction 3-57 3500-ReB. Eriochrome Cyanine R Method 3-58 3500-Rh

3500-Sb ANTIMONY 3-60 3500-Ru3500-As ARSENIC 3-61 35OO-Se

A. Introduction 3-61B. Silver Diethyldithiocarbamate Method. . 3-61

3500-Ba BARIUM 3-6335OO-Be BERYLLIUM 3-633500-Bi BISMUTH 3-643500-B BORON 3-6435OO-Cd CADMIUM 3-64 3500-Ag3500-Ca CALCIUM .- 3-65 35OO-Na

A. Introduction 3-65B. EDTA Titrimetric Method 3-65

3500-Cs CESIUM 3-663500-Cr CHROMIUM - 3-67 3500-Sr

A. Introduction 3-67B. Colorimetric Method . . .'" 3-67C. Ion Chromatographic Method 3-69 3500-Te

3500-Co COBALT 3-71 3500-T13500-Cu COPPER 3-71 3500-Th

A. Introduction 3-71 3500-SnB. Neocuproine Method 3-72 3500-TiC. Bathocuproine Method 3-73 3500-U

3500-Ga GALLIUM 3-74 . 3500-V3500-Ge GERMANIUM 3-753500-Au GOLD 3-753500-In INDIUM 3-75 3500-Zn

IRIDIUM 3-75IRON 3-76A. Introduction 3-76B. Phenanthroline Method 3-77LEAD 3-79A. Introduction 3-79B. Dithizone Method 3-80LITHIUM 3-82A. Introduction 3-82B. Flame Emission Photometric Method . . 3-82MAGNESIUM 3-83A. Introduction 3-83B. Calculation Method 3-84MANGANESE 3-84A. Introduction 3-84B. Persulfate Method 3-84MERCURY 3-86MOLYBDENUM 3-86NICKEL 3-87OSMIUM 3-87PALLADIUM 3-87PLATINUM 3-87POTASSIUM 3-88A. Introduction 3-88B. Flame Photometric Method 3-88C. Potassium-Selective Electrode

Method 3-89RHENIUM 3-90RHODIUM 3-90RUTHENIUM 3-90SELENIUM 3-91A. Introduction 3-91B. Sample Preparation 3-92C. Colorimetric Method 3-94D. Determination of Volatile Selenium . . . 3-96E. Determination of Nonvolatile Organic '

Selenium Compounds 3-96SILVER 3-98SODIUM 3-98A. Introduction 3-98B. Flame Emission Photometric

Method 3-99STRONTIUM 3-101A. Introduction 3-101B. Flame Emission Photometric Method . . 3-101TELLURIUM 3-103THALLIUM 3-103THORIUM 3-103TIN 3-103TITANIUM 3-104URANIUM 3-104VANADIUM 3-104A. Introduction 3-104B. Gallic Acid Method 3-105ZINC 3-106

TABLE OF CONTENTS

A. Introduction 3-106B. Zincon Method 3-106

Part 4000 INORGANIC NONMETALLICCONSTITUENTS

4010 INTRODUCTION 4-14020 QUALITY ASSURANCE/QUALITY CONTROL . . . 4-1

A. Introduction 4-1B. Quality Control Practices 4-1

4110 DETERMINATION OF ANIONS BY IONCHROMATOGRAPHY 4-3

A. Introduction 4-3B. Ion Chromatography with Chemical

Suppression of Eluent Conductivity . . 4-3C. Single-Column Ion Chromatography

with Direct Conductivity Detection . . 4-6D. Ion Chromatographic Determination of

Oxyhalides and Bromide 4-74120 SEGMENTED CONTINUOUS FLOW ANALYSIS . . . 4-11

A. Introduction 4-11B. Segmented Flow Analysis Method. . . . 4-11

4130 INORGANIC NONMETALS BY FLOW INJECTIONANALYSIS ' 4-13

A. Introduction 4-13B. Quality Control 4-13

4140 INORGANIC ANIONS BY CAPILLARY IONELECTROPHORESIS 4-14

A. Introduction 4-14B. Capillary Ion Electrophoresis with

Indirect UV Detection 4-144500-B BORON 4-23

A. Introduction 4-23B. Curcumin Method 4-23C. Carmine Method 4-25

4500-Br" BROMIDE 4-25A. Introduction 4-25B. Phenol Red Colorimetric Method . . . . 4-26C. (Reserved) - 4-27D. Flow Injection Analysis 4-27

4500-CO2 CARBON DIOXIDE 4-28A. Introduction 4-28B. Nomographic Determination of Free

Carbon Dioxide and the Three Formsof Alkalinity 4-28

C. Titrimetric Method for Free CarbonDioxide 4-33

D. Carbon Dioxide and Forms of Alkalinityby Calculation 4-34

4500-CN" CYANIDE 4-34A. Introduction 4-34B. Preliminary Treatment of Samples . . . . 4-37C. Total Cyanide after Distillation 4-39D. Titrimetric Method 4-41E. Colorimetric Method 4-41

F. Cyanide-Selective Electrode Method. . . 4-43G. Cyanides Amenable to Chlorination

after Distillation . . 4-44H. Cyanides Amenable to Chlorination

without Distillation(Short-Cut Method) 4-46

I. Weak Acid Dissociable Cyanide 4-47J. Cyanogen Chloride 4-48K. Spot Test for Sample Screening 4-49L. Cyanates 4-50M. Thiocyanate 4-51N. Total Cyanide after Distillation, by

Flow Injection Analysis 4-530 . Total Cyanide and Weak Acid

Dissociable Cyanide by FlowInjection Analysis 4-55

4500-C1 CHLORINE (RESIDUAL) 4-56A. Introduction 4-56B. Iodometric Method I 4-58C. Iodometric Method II 4-60D. Amperometric Titration Method 4-62E. Low-Level Amperometric Titration

Method 4-64F. DPD Ferrous Titrimetric Method 4-64G. DPD Colorimetric Method 4-67H. Syringaldazine (FACTS) Method . . . . 4-681. Iodometric Electrode Technique 4-69

4500-C1" CHLORIDE 4-70A. Introduction 4-70B. Argentometric Method . 4-70C. Mercuric Nitrate Method 4-71D. Potentiometric Method 4-73E. Automated Ferricyanide Method 4-74

. F. (Reserved) 4-75G. Mercuric Thiocyanate Flow Injection

Analysis "7 . . . . 4-754500-ClO2 CHLORINE DIOXIDE 4-77

A. Introduction 4-77B. Iodometric Method 4-77C. Amperometric Method I 4-78D. (Reserved) ' 4-79E. Amperometric Method II 4-79

4500-F~ FLUORIDE 4-82A. Introduction 4-82B. Preliminary Distillation Step 4-83C. Ion-Selective Electrode Method 4-84D. SPADNS Method 4-85E. Complexone Method 4-87F. (Reserved) 4-88G. Ion-Selective Electrode Flow Injection

Analysis 4-884500-H+ P H VALUE 4-90

A. Introduction 4-90B. Electrometric Method 4-90

4500-1 IODINE 4-95

TABLE OF CONTENTS XIX

A. Introduction 4-95 4500-OB. Leuco Crystal Violet Method 4-95C. Amperometric Titration Method 4-97

4500-r IODIDE 4-97A. Introduction 4-97B. Leuco Crystal Violet Method 4-98C. Catalytic Reduction Method 4-99D. Voltammetric Method 4-100

4500-KV IODATE 4-102A. Introduction . . . . : : 4-102 4500-O3

~B. Polarographic Method 4-1024500-N NITROGEN 4-103

A. Introduction 4-103 4500-PB. In-Line UV/Persulfate Digestion and

Oxidation with Flow InjectionAnalysis . 4-104

C. Persulfate Method 4-105D. Conductimetric Determination of

Inorganic Nitrogen .4-1074500-NH3 NITROGEN (AMMONIA) 4-108

A. Introduction 4-108B. Preliminary Distillation Step 4-109C. Titrimetric Method 4-110D. Ammonia-Selective Electrode Method. . 4-111E. Ammonia-Selective Electrode Method . .

Using Known Addition 4-112F. Phenate Method .' ; 4-114G. Automated Phenate Method 4-115H. Flow Injection Analysis 4-116

4500-NO2" NITROGEN (NITRITE) 4-118A. Introduction 4-118B. Colorimetric Method 4-118 4500-C. (Reserved) 4-120 KMnO4

4500-NO3~ NITROGEN (NITRATE) 4-120A. Introduction 4-120B. Ultraviolet Spectrophotometric 4500-SiO2

Screening Method 4-120C. Second-Derivative Ultraviolet

Spectrophotometric Method(PROPOSED) 4-121

D. Nitrate Electrode Method 4-122E. Cadmium Reduction Method. 4-123F. Automated Cadmium Reduction

Method 4-125G. (Reserved) 4-126 4500-S2"H. Automated Hydrazine Reduction

Method 4-126I. Cadmium Reduction Flow Injection

Method 4-1274500-Norg NITROGEN (ORGANIC) . . : 4-130

A. Introduction 4-130B. Macro-Kjeldahl Method 4-131C. Semi-Micro-Kjeldahl Method 4-132D. Block Digestion and Flow Injection

Analysis 4-133

OXYGEN (DISSOLVED) 4-136A. Introduction 4-136B. Iodometric Methods 4-136C. Azide Modification 4-138D. Permanganate Modification 4-140E. Alum Flocculation Modification 4-141F. Copper Sulfate-Sulfamic Acid

Flocculation Modification 4-141G. Membrane Electrode Method 4-141OZONE (RESIDUAL) 4-144A. Introduction 4-144B. Indigo Colorimetric Method 4-144PHOSPHORUS 4-146A. Introduction . . . 4-146B. Sample Preparation 4-149C. Vanadomolybdophosphoric Acid

Colorimetric Method 4-151D. Stannous Chloride Method 4-152E. Ascorbic Acid Method 4-153F. Automated Ascorbic Acid Reduction

Method 4-155G. Flow Injection Analysis for

Orthophosphate 4-156H. Manual Digestion and Flow Injection

Analysis for Total Phosphorus . . . . 4-158I. In-line UV/Persulfate Digestion

and Flow Injection Analysis forTotal Phosphorus 4-159

J. Persulfate Method for SimultaneousDetermination of Total Nitrogen andTotal Phosphorus 4-160

POTASSIUM PERMANGANATE 4-162A. Introduction 4-162B. Spectrophotometric Method 4-163SILICA - r . . 4-164A. Introduction 4-164B. (Reserved) 4-165C. Molybdosilicate Method . . . .' 4-165D. Heteropoly Blue Method 4-167E. Automated Method for Molybdate-

Reactive Silica 4-168F. Flow Injection Analysis for Molybdate-

Reactive Silicate 4-169SULFIDE 4-170A. Introduction 4-170B. Separation of Soluble and Insoluble

Sulfides 4-172C. Sample Pretreatment to Remove

Interfering Substances' or toConcentrate the Sulfide 4-173

D. Methylene Blue Method 4-174E. Gas Dialysis, Automated Methylene

Blue Method 4-175F. Iodometric Method 4-176

XX TABLE OF CONTENTS

G. Ion-Selective Electrode Method 4-177H. Calculation of Un-ionized Hydrogen

Sulfide.- 4-179. I. Distillation, Methylene Blue Flow

Injection Analysis Method 4-181J. Acid-Volatile Sulfide 4-182

4500-SO32" SULFITE 4-183A. Introduction 4-183B. Iodometric Method 4-183C. Phenanthroline Method 4-184

4500-SO42" SULFATE 4-186A. Introduction 4-186B. (Reserved) 4-186C. Gravimetric Method with Ignition of

Residue . 4-186D. Gravimetric Method with Drying of

Residue 4-187/ E. Turbidimetric Method 4-188

F. Automated Methylthymol BlueMethod 4-189

G. Methylthymol Blue Flow InjectionAnalysis 4-190

Part 5000 AGGREGATE ORGANIC CONSTITUENTS5010 INTRODUCTION 5-1

A. General Discussion ., 5-1B. Sample Collection and Preservation . . . 5-1

5020 QUALITY ASSURANCE/QUALITY CONTROL . . . 5-15210 BIOCHEMICAL OXYGEN DEMAND ( B O D ) . . . . 5-2

A. Introduction 5-2B. 5-Day BOD Test 5-2C. Ultimate BOD Test 5-7D. Respirometric Method 5-10

5220 CHEMICAL OXYGEN DEMAND (COD) 5-14A. Introduction 5-14B. Open Reflux Method 5-15C. Closed Reflux, Titrimetric Method. . . . 5-16D. Closed Reflux, Colorimetric Method. . . 5-18

5310 TOTAL ORGANIC CARBON (TOC) 5-19A. Introduction 5-19B. High-Temperature Combustion

Method 5-21C. Persulfate-Ultraviolet or Heated-

Persulfate Oxidation Method 5-23D. Wet-Oxidation Method 5-25

5320 DISSOLVED ORGANIC HALOGEN 5-26A. Introduction 5-26B. Adsorption-Pyrolysis-Titrimetric

Method 5-275510 AQUATIC HUMIC SUBSTANCES 5-32

A. Introduction 5-32B. Diethylaminoethyl (DEAE) Method . . . 5-33C. XAD Method 5-34

5520 OIL AND GREASE 5-35

A. Introduction 5-35B. Liquid-Liquid, Partition-Gravimetric

Method 5-37C. Partition-Infrared Method 5-39D. Soxhlet Extraction Method 5-40E. Extraction Method for Sludge Samples . . . 5-41F. Hydrocarbons 5-41G. Sold-Phase, Partition-Gravimetric Method. . 5-42

5530 PHENOLS 5-43A. Introduction 5-43B. Cleanup Procedure 5-44C. Chloroform Extraction Method 5-45D. Direct Photometric Method 5-47

5540 SURFACTANTS 5-47A. Introduction 5-47B. Surfactant Separation by Sublation. . . . 5-48C. Anionic Surfactants as MBAS 5-50D. Nonionic Surfactants as CTAS 5-53

5550 TANNIN AND LIGNIN 5-55A. Introduction 5-55B. Colorimetric Method 5-55

5560 ORGANIC AND VOLATILE ACIDS 5-56A. Introduction 5-56B. Chromatographic Separation Method for

Organic Acids 5-57C. Distillation Method 5-58D. Gas Chromatographic Method 5-59

5710 FORMATION OF TRIHALOMETHANES AND OTHERDISINFECTION BY-PRODUCTS 5-62

A. Introduction 5-62B. Trihalomethane Formation Potential

(THMFP) 5-64C. Simulated Distribution System

Trihalomethanes (SDS-THM) 5-68D. Formation of Other Disinfection By-

Products (DBPs) r 5-695910 UV-ABSORBING ORGANIC CONSTITUENTS . . . 5-71

A. Introduction 5-71B. Ultraviolet Absorption Method 5-72

Part 6000 INDIVIDUAL ORGANIC COMPOUNDS6010 INTRODUCTION 6-1

A. General Discussion 6-1B. Sample Collection and Preservation . . . 6-3C. Analytical Methods 6-4

6020 QUALITY ASSURANCE/QUALITY CONTROL . . . 6-6A. Introduction 6-6B. Quality Control Practices 6-6

6040 CONSTITUENT CONCENTRATION BY GASEXTRACTION 6-8

A. Introduction 6-8B. Closed-Loop Stripping, Gas

Chromatographic/Mass SpectrometricAnalysis 6-8

TABLE OF CONTENTS

C. Purge and Trap Technique 6-19D. Solid-Phase Microextraction (SPME) . . 6-19

6200 VOLATILE ORGANIC COMPOUNDS 6-23A. Introduction 6-23B. Purge and Trap Capillary-Column Gas

Chromatographic/Mass SpectrometricMethod 6-25

C. Purge and Trap Capillary-Column GasChromatographic Method 6-31

6211 METHANE 6-35A. Introduction 6-35B. Combustible-Gas Indicator Method . . . 6-35C. Volumetric Method 6-37

6231 1,2-DlBROMOETHANE (EDB) AND 1,2-DIBROMO-3-CHLOROPROPANE (DBCP) . . . 6-37

A. Introduction " 6-37B. Liquid-Liquid Extraction Gas

Chromatographic Method 6-37C. Purge and Trap Gas Chromatographic/

Mass Spectrometric Method 6-40D. Purge and Trap Gas- Chromatographic

Method 6-406232 TRIHALOMETHANES AND CHLORINATED

ORGANIC SOLVENTS ' 6-40A. Introduction 6-40B. Liquid-Liquid Extraction Gas

Chromatograpriic Method 6-41C. Purge and Trap Gas Chromatographic/

Mass Spectrometric Method 6-46D. Purge and Trap Gas Chromatographic

Method 6-466251 DISINFECTION BY-PRODUCTS: HALOACETIC

ACIDS AND TRICHLOROPHENOL . . 6-46A. Introduction 6-46B. Micro Liquid-Liquid Extraction Gas

Chromatographic Method 6-476252 DISINFECTION BY-PRODUCTS: ALDEHYDES

(PROPOSED) 6-57A. Introduction .- 6-57B. PFBHA Liquid-Liquid Extraction Gas

Chromatographic Method 6-586410 EXTRACTABLE BASE/NEUTRALS AND ACIDS . . 6-65

A. Introduction . . ._ 6-65B. Liquid-Liquid Extraction Gas


6420 PHENOLS 6-79A. Introduction 6-79B. Liquid-Liquid Extraction Gas

Chromatographic Method 6-79C. Liquid-Liquid Extraction Gas


6431 POLYCHLORINATED BlPHENYLS (PCBS) 6-85A. Introduction 6-85

B. Liquid-Liquid Extraction GasChromatographic Method 6-85

C. Liquid-Liquid Extraction GasChromatographic/Mass SpectrometricMethod 6-85

6 4 4 0 POLYNUCLEAR AROMATIC HYDROCARBONS . . . 6 - 8 6A. Introduction 6-86B. Liquid-Liquid Extraction

Chromatographic Method 6-86C. Liquid-Liquid Extraction Gas


6610 CARB AM ATE PESTICIDES 6-91A. Introduction 6-91B. High-Performance Liquid

Chromatographic Method 6-926630 ORGANOCHLORINE PESTICIDES 6-100

A. Introduction 6-100B. Liquid-Liquid Extraction Gas

Chromatographic Method 1 6-100AppendixStandardization of

Magnesia-Silica Gel Column byWeight Adjustment Based onAdsorption of Laurie Acid 6-107

C. Liquid-Liquid Extraction GasChromatographic Method II 6-108

D. Liquid-Liquid Extraction GasChromatographic/Mass SpectrometricMethod 6-115

6640 ACIDIC HERBICIDE COMPOUNDS 6-115A. Introduction 6-115B. Micro Liquid-Liquid Extraction Gas

Chromatographic Method 6-1166651 GLYPHOSATE HERBICIDE 6-126

A. Introduction 6-126B. Liquid Chromatographic Post-Column

Fluorescence Method 6-127

Part 7000 RADIOACTIVITY7010 INTRODUCTION 7-1

A. General Discussion 7-1B. Sample Collection and Preservation . . . 7-2

7020 QUALITY ASSURANCE/QUALITY CONTROL . . . 7-3A. Basic Quality Control Program 7-3B. Quality Control for Wastewater

Samples 7-6C. Statistics 7-6D. Calculation and Expression of Results. . 7-7

7030 COUNTING INSTRUMENTS 7-8A. Introduction 7-8B. Description and Operation

of Instruments 7-87040 FACILITIES 7-13

A. Counting Room 7-13

XXII TABLE OF CONTENTS

B. Radiochemistry Laboratory 7-14C. Laboratory Safety 7-14D. Pollution Prevention 7-14E. Waste Management 7-15

7110 GROSS ALPHA AND GROSS BETARADIOACTIVITY(TOTAL, SUSPENDED, AND DISSOLVED) . . . . 7-15

A. Introduction 7-15B. Evaporation Method for Gross Alpha-

Beta 7-15C. Coprecipitation Method for Gross Alpha

Radioactivity in Drinking Water. . . . 7-197120 GAMMA-EMITTING RADIONUCLIDES 7-20

A. Introduction 7-20B. Gamma Spectroscopic Method 7-20

7500-Cs RADIOACTIVE CESIUM 7-24A. Introduction 7-24

/ B. Precipitation Method 7-247500-1 RADIOACTIVE IODINE 7-25

A. Introduction 7-25B. Precipitation Method 7-26C. Ion-Exchange Method 7-27D. Distillation Method 7-28

7500-Ra RADIUM 7-29A. Introduction 7 7-29B. Precipitation Method 7-29C. Emanation Method 7-32D. Sequential Precipitation Method 7-38E. Gamma Spectroscopy Method 7-40

7500-Rn RADON 7-43A. Introduction 7-43B. Liquid Scintillation Method 7-43

7500-Sr TOTAL RADIOACTIVE STRONTIUMAND STRONTIUM-90 7-46

A. Introduction 7-46B. Precipitation Method 7-46

7500-3H TRITIUM 7-49A. Introduction 7-49B. Liquid Scintillation Spectrometric

Method 7-507500-U URANIUM 7-51

A. Introduction 7-51B. Radiochemical Method 7-51C. Isotopic Method 7-53

Part 8000 TOXICITY8010 INTRODUCTION 8-1

A. General Discussion 8-1B. Terminology 8-2C. Basic Requirements 8-3D. Conducting Toxicity Tests 8-4E. Preparing Organisms for Toxicity

Tests 8-7F. Toxicity Test Systems, Materials,

and Procedures 8-15

G. Calculating, Analyzing, and ReportingResults of Toxicity Tests 8-20

H. Interpreting and Applying Results ofToxicity Tests 8-24

I. Selected Toxicological Literature . . . . 8-258020 QUALITY ASSURANCE AND QUALITY CONTROL

IN LABORATORY TOXICITY TESTS 8-26A. General Discussion 8-26B. Elements of QA/QC 8-27

8030 MUTAGENESIS 8-30A. Introduction 8-30B. Salmonella Microsomal Mutagenicity

Test 8-318050 BACTERIAL BIOLUMINESCENCE 8-37

A. Introduction 8-37B. Bacterial Bioluminescence Test 8-37

8070 P450 REPORTER GENE RESPONSE TO DIOXIN-LIKE ORGANIC COMPOUNDS 8-40

A. Introduction 8-40B. The P450 RGS Test 8-40

8071 COMET/SINGLE-CELL GEL ELECTROPHORESISASSAY FOR DETECTION OF DNADAMAGE 8-42

A. Introduction 8-42B. Comet/Single-Cell Gel Electrophoresis

Assay 8-438080 SEDIMENT POREWATER TESTING 8-46

A. Introduction 8-46B. Sediment Collection and Storage 8-47C. Extraction of Sediment Pore Water . . . 8-47D. Toxicity Testing Procedures 8-49

8110 ALGAE 8-508111 BIOSTIMULATION (ALGAL PRODUCTIVITY) . . . 8-51

A. General Principles 8-51B. Planning and Evaluating Algal Assays . 8-51C. Apparatus V 8-52D. Sample Handling 8-53E. Synthetic Algal Culture Medium 8-53F. Inoculum 8-53G. Test Conditions and Procedures 8-54H. Effect of Additions 8-55I. Data Analysis and Interpretation 8-56

8112 PHYTOPLANKTON 8-57A. Introduction 8-57B. Inoculum 8-57C. Test Conditions and Procedures 8-57

8113 MARINE MACROALGAE 8-58A. Introduction 8-58B. Selecting and Preparing Macrocystis

pyrifera Sporophylls 8-59C. Toxicity Test Procedures 8-60D. Data Evaluation 8-62

8200 AQUATIC FLOWERING PLANTS 8-638211 DUCKWEED. . .' 8-63

A. Introduction 8-63

TABLE OF CONTENTS

B. Selecting and Preparing TestOrganisms 8-64

C. Toxicity Test Procedure 8-658220 AQUATIC EMERGENT PLANTS 8-66

A. Introduction 8-66B. Selecting and Preparing Test

Organisms 8-67C. Toxicity Test Procedure 8-69

8310 CILIATED PROTOZOA 8-70A. Introduction 8-70

- B. Growth Inhibition Test with FreshwaterCiliate Colpidium campylum 8-71

C. Chemotactic Test with FreshwaterCiliate Tetrahymena thermophila . . . 8-73

D. Growth Inhibition Test with the SoilCiliate Colpoda inflata 8-75

8420 ROTIFERS 8-76A. Introduction 8-76B. Selecting and Preparing Testing

Organisms 8-77C. Aquatic Toxicity Test,Procedures . . . . 8-78

8510 ANNELIDS. . . 8-80A. Introduction . 8-80B. Selecting and Preparing Test

Organisms 8-81C. Toxicity Test Procedures 8-86D. Sediment Test Procedures .Using the

Marine Polychaete Neanthesarenaceodentata 8-89

E. Sediment Test Procedures Using theFreshwater and Marine OligochaetesPristina leidyi, Tubifex tubifex, andLumbriculus variegatus . . . . . . . . 8-91

F. Data Evaluation 8-918610 MOLLUSKS 8-92


Organisms 8-93C. Short-Term Test Procedures Using

Marine Mollusk Larvae 8-94D. Sediment Test Procedures Using

Marine Bivalves 8-96E. Field Test Procedures Using Freshwater

and Marine Bivalves 8-978710 ARTHROPODS 8-1018711 DAPHNIA 8-101


Organisms 8-103C. Procedures 8-104

8712 CERIODAPHNIA 8-106A. Introduction 8-106B. Selecting and Preparing Test


8714 MYSIDS 8-111A. Introduction 8-111B. Selecting and Preparing Test

Organisms 8-112C. Toxicity Test Procedures 8-117

8740 DECAPODS 8-121A. Introduction 8-121B. Selecting and Preparing Test

Organisms 8-121C. Toxicity Test Procedures 8-128D. Data Evaluation 8-132

8750 AQUATIC INSECTS 8-133A. Introduction 8-133B. Selecting and Preparing Test

Organisms 8-133C. Toxicity Test Procedures 8-135D. Data Evaluation 8-137

8810 ECHINODERM FERTILIZATION ANDDEVELOPMENT 8-137


Organisms 8-138C. Echinoderm Fertilization Test 8-140D. Echinoderm Embryo Development

Test 8-1438910 FISH 8-146

A. Introduction 8-146B. Fish Selection and Culture Procedures. . 8-146C. Test Procedures 8-151

8921 FATHEAD MINNOW 8-157A. Introduction . 8-157B. Culture and Maintenance of Test


8930 AMPHIBIANS (PROPOSED) 8-166A. Introduction . . - - . . . 8-166B. Culture and Maintenance of Test


Part 9000 MICROBIOLOGICAL EXAMINATION9010 INTRODUCTION 9-19020 QUALITY ASSURANCE/QUALITY CONTROL . . . 9-2

A. Introduction 9-2B. Intralaboratory Quality Control

Guidelines 9-3C. Interlaboratory Quality Control 9-14

9030 LABORATORY APPARATUS 9-15A. Introduction 9-15B. Equipment Specifications 9-15

9040 WASHING AND STERILIZATION 9-179050 PREPARATION OF CULTURE MEDIA 9-18

A. General Procedures 9-18B. Water 9-19

TABLE OF CONTENTS

C. Media Specifications 9-199060 SAMPLES 9-20

A. Collection 9-20B. Preservation and Storage 9-22

9211 RAPID DETECTION METHODS 9-23A. Introduction 9-23B. Seven-Hour Fecal Coliform Test . . . . 9-23C. Special Techniques 9-23

9212 STRESSED ORGANISMS 9-25A. Introduction 9-25B. Recovery Enhancement 9-26

9213 RECREATIONAL WATERS 9-28A. Introduction ' 9-28B. Swimming Pools 9-29C. Whirlpools 9-31D. Natural Bathing Beaches 9-31E. Membrane Filter Technique for

Pseudomonas aeruginosa 9-33F. Multiple-Tube Technique for

Pseudomonas aeruginosa 9-339215 HETEROTROPHIC PLATE-COUNT . 9-34

A. Introduction 9-34B. Pour Plate Method 9-37C. Spread Plate Method . . . 9-38D. Membrane Filter Method 9-40

9216 DIRECT TOTAL MICROBIAL COUNT 9-41A. Introduction ; 9-41B. Epifluorescence Microscopic Method . . 9-41

9217 ASSIMILABLE ORGANIC CARBON 9-42A. Introduction 9-42B. Pseudomonas fluorescens Strain P-17,

Spirillum Strain NOX Method 9-449218 AEROBIC ENDOSPORES 9-47

A. Introduction 9-47B. Membrane Filter Method 9-48

9221 MULTIPLE-TUBE FERMENTATION TECHNIQUE FORMEMBERS OF THE COLIFORM GROUP 9-48

A. Introduction 9-48B. Standard Total Coliform Fermentation

Technique 9-49C. Estimation of Bacterial Density 9-53D. Presence-Absence (P-A) Coliform

Test 9-55E. Fecal Coliform Procedure 9-56F. Escherichia coli Procedure

(PROPOSED) 9-579222 MEMBRANE FILTER TECHNIQUE FOR MEMBERS

OF THE COLIFORM GROUP 9-59A. Introduction 9-59B. Standard Total Coliform Membrane

Filter Procedure 9-60C. Delayed-Incubation Total Coliform

Procedure 9-65D. Fecal Coliform Membrane Filter

Procedure 9-66

E. Delayed-Incubation Fecal ColiformProcedure 9-68

F. Klebsiella Membrane Filter Procedure. . 9-69G. MF Partition Procedures 9-70

9223 ENZYME SUBSTRATE COLIFORM TEST 9-72A. Introduction 9-72B. Enzyme Substrate Test 9-72

9224 DETECTION OF COLIPHAGES 9-74A. Introduction 9-74B. Somatic Coliphages Assay 9-75C. Male-Specific Coliphage Assay Using

Escherichia coli Famp 9-77D. Male-Specific Coliphage Assay Using

S a l m o n e l l a t y p h i m u r i u m W G 4 9 . . . . 9-78E. Single-Agar-Layer Method 9-80F. Membrane Filter Method 9-81

9225 DIFFERENTIATION OF THE COLIFORMBACTERIA 9-82

A. Introduction 9-82B. Culture Purification 9-83C. Identification 9-83D. Media, Reagents, and Procedures . . . . 9-84

9230 FECAL STREPTOCOCCUS AND ENTEROCOCCUSGROUPS 9-86

A. Introduction 9-86B. Multiple-Tube Technique 9-88C. Membrane Filter Techniques 9-88

9240 IRON AND SULFUR BACTERIA 9-91A. Introduction 9-91B. Iron Bacteria 9-91C. Sulfur Bacteria 9-95D. Bacteria Living in Acidic Environments. 9-97E. Enumeration, Enrichment, and Isolation

of Iron and Sulfur Bacteria 9-1019245 NITRIFYING BACTERIA 9-106

A. Introduction 9-106B. Multiple-Tube Method . . : 9-107

9250 DETECTION OF ACTINOMYCETES 9-109A. Introduction 9-109B. Actinomycete Plate Count 9-110

9260 DETECTION OF PATHOGENIC BACTERIA 9-111A. Introduction 9-111B. General Qualitative Isolation and

Identification Procedures forSalmonella 9-113

C. Immunofluorescence IdentificationProcedure for Salmonella 9-116

D. Quantitative Salmonella Procedures . . . 9-118E. Shigella 9-118F. Pathogenic Escherichia coli 9-120G. Campylobacter jejuni 9-121H. Vibrio cholerae 9-123I. Leptospira 9-125J. Legionella 9-127K. Yersinia enterocolitica 9-130

TABLE OF CONTENTS xxv

L. Aeromonas 9-131M.Mycobacterium 9-134

9510 DETECTION OF ENTERIC VIRUSES 9-136A. Introduction 9-136B. Virus Concentration from Small Sample

Volumes by Adsorption to andElution from Microporous Filters . . . 9-138

C. Virus Concentration from Large SampleVolumes by Adsorption to andElution from Microporous Filters . . . 9-141

'- D. Virus Concentration by AluminumHydroxide Adsorption-Precipitation . . 9-145

E. Hydroextraction-Dialysis withPolyethylene Glycol 9-147

F. Recovery of Viruses from SuspendedSolids in Water and Wastewater. . . . 9-148

G. Assay and Identification of Viruses inSample Concentrates 9-149

9610 DETECTION OF FUNGI 9-153A. Introduction 9-153B. Pour Plate Technique 9-156C. Spread Plate Technique. 9-157D. Membrane Filter Technique 9-158E. Technique for Yeasts 9-158F. Zoosporic Fungi 9-159G. Aquatic Hyphomycetes 9-160H. Fungi Pathogenic to Humans 9-160

9711 PATHOGENIC PROTOZOA 9-161A. Introduction 9-161B. Giardia and Cryptosporidium Methods . 9-162

C. Acanthamoeba 9-168

Part 10000 BIOLOGICAL EXAMINATION10010 INTRODUCTION 10-110200 PLANKTON 10-2

A. Introduction 10-2B. Sample Collection 10-3C. Concentration Techniques 10-10D. Preparing Slide Mounts 10-11E. Microscopes and Calibrations 10-12F. Phytoplankton Counting Techniques. . . 10-13G. Zooplankton Counting Techniques. . . . 10-17H. Chlorophyll 10-18I. Determination of Biomass

(Standing Crop) 10-26J. Metabolic Rate Measurements 10-28

10300 PERIPHYTON 10-32A. Introduction 10-32B. Sample Collection 10-32C. Sample Analysis 10-34D. Primary Productivity 10-37E. Interpreting and Reporting R e s u l t s . . . . 10-45

10400 MACROPHYTES 10-47A. Introduction 10-47B. Preliminary Survey 10-48C. Vegetation Mapping Methods 10-49D. Population Estimates 10-51E. Productivity 10-54

10500 BENTHIC MACROINVERTEBRATES 10-63A. Introduction 10-63B. Sample Collection 10-65C. Sample Processing and Analysis 10-74D. Data Evaluation, Presentation,

and Conclusions 10-7610600 FISHES 10-78

A. Introduction 10-78B. Data Acquisition 10-79C. Sample Preservation 10-88D. Analysis of Collections 10-89E. Investigation of Fish Kills 10-93

10700 BENTHIC MEIOFAUNA 10-9410750 NEMATOLOGICAL EXAMINATION 10-95

A. Introduction 10-95B. Collection and Processing Techniques

forNematodes 10-97C. Illustrated Key to Freshwater

Nematodes 10-9810900 IDENTIFICATION OF AQUATIC

ORGANISMS 10-113A. Procedure in Identification 10-114B. Key to Major Groups of Aquatic

Organisms (Plates 1-35) 10-114Acknowledgments 10-118

C. Key for Identification of FreshwaterAlgae Common in Water Suppliesand Polluted Waters(Plates 1A, IB, 28-35) -'. . 10-152

D. Index to Illustrations 10-157E. Selected Taxonomic References . . . . 10-160

SUPPLEMENT TO THE 21ST EDITION6610 CARBAMATE PESTICIDES S-l

A. Introduction S-lB. High-Performance Liquid

Chromatographic Method S-l6710 TRIBUTYLTIN S-10

A. Introduction S-10B. Gas Chromatographic/Mass

Spectrometric Method S-10C. Gas Chromatographic/Flame

Photometric Method S-15

INDEX 1-1

standart methods

Documents

introduction1010 introduction

titration method

method development

nephelometric method

method validation

quality assessment

edta titrimetric method

method detection level