Table of Contents

 

 

 

PART 1000

INTRODUCTION

 

1010

Introduction

1-1

A

Scope and Application of Methods

1-1

B

Statistics

1-1

C

Glossary

1-4

D

Dilution/Concentration Operations

1-5

1020

Quality Assurance

1-6

A

Introduction

1-6

B

Quality Control

1-7

C

Quality Assessment

1-15

1030

Data Quality

1-16

A

Introduction

1-16

B

Measurement Uncertainty

1-16

C

Method Detection Level

1-20

D

Data Quality Objectives

1-21

E

Checking Analyses’ Correctness

1-23

1040

Method Development and Evaluation

1-24

A

Introduction

1-24

B

Method Validation

1-25

C

Collaborative Testing

1-26

1050

Expression of Results

1-27

A

Units

1-27

B

Significant Figures

1-34

C

Other Considerations

1-36

1060

Collection and Preservation of Samples

1-37

A

Introduction

1-37

B

Collection of Samples

1-39

C

Sample Storage and Preservation

1-43

1080

Reagent Water

1-46

A

Introduction

1-46

B

Methods for Preparing Reagent-Grade Water

1-47

C

Reagent Water Quality

1-48

1090

Laboratory Occupational Health and Safety

1-49

A

Introduction

1-49

B

Safe Laboratory Practices

1-50

C

Laboratory Facility /Fixed Equipment

1-55

D

Hazard Evaluation

1-56

E

Persona! Protective Equipment

1 -57

F

Worker Protection Medical Program

1-60

G

Provisions for Work with Particularly Hazardous Substances

1-61

H

Biological Safety

1-61

I

Radiological Safety

1-62

J

Chemical Hygiene Plan

1-65

K

Mercury Use Avoidance in Laboratory

1-66

1100

Waste Minimization and Disposal

1-66

A

Introduction

1-66

B

Waste Minimization

1-66

C

Waste Treatment and Disposal

1-67

PART 2000

PHYSICAL AND AGGREGATE PROPERTIES

 

2010

Introduction

2-1

2020

Quality Assurance/Quality Control

2-1

A

Introduction

2-1

B

Quality Control Practices

2-1

2110

Appearance

2-5

2120

Color

2-5

A

Introduction

2-5

B

Visual Comparison Method

2-6

C

Spectrophotometric—S ingle-Wavelength Method (PROPOSED)

2-7

D

Spectrophotometric—Multi-Wavelength Method

2-8

E

Tristimulus Spectrophotometric Method

2-9

F

ADMI Weighted-Ordinate Spectrophotometric Method

2-11

2130

Turbidity

2-12

A

Introduction

2-12

B

Nephelometric Method

2-13

2150

Odor

2-15

A

Introduction

2-15

B

Threshold Odor Test

2-16

2160

Taste

2-19

A

Introduction

2-19

B

Flavor Threshold Test (FTT)

2-20

C

Flavor Rating Assessment (FRA)

2-22

2170

Flavor Profile Analysis

2-23

A

Introduction

2-23

B

Flavor Profile Analysis

2-24

2310

Acidity

2-31

A

Introduction

2-31

B

Titration Method

2-31

2320

Alkalinity

2-34

A

Introduction

2-34

B

Titration Method

2-34

2330

Calcium Carbonate Saturation

2-37

A

Introduction

2-37

B

Indices Indicating Tendency of a Water to Precipitate or Dissolve CaCO3

2-38

C

Indices Predicting the Quantity of CaCO3 That Can Be Precipitated or Dissolved

2-41

D

Graphical and Computer Methods for CaCO3 Indices

2-42

2340

Hardness

2-44

A

Introduction

2-44

B

Hardness by Calculation

2-44

C

EDTA Titrimetric Method

2-44

2350

Oxidant Demand/Requirement

2-47

A

Introduction

2-47

B

Chlorine Demand/Requirement

2-48

C

Chlorine Dioxide Demand/Requirement

2-49

D

Ozone Demand/Requirement—Batch Method

2-50

E

Ozone Demand/Requirement—Semi-Batch Method

2-50

2510

Conductivity

2-52

A

Introduction

2-52

B

Laboratory Method

2-54

2520

Salinity

2-55

A

Introduction

2-55

B

Electrical Conductivity Method

2-56

C

Density Method

2-57

D

Algorithm of Practical Salinity

2-58

2530

Floatables

2-58

A

Introduction

2-58

B

Particulate Floatables

2-59

C

Trichlorotrifluoroethane-Soluble Floatable Oil and Grease

2-61

2540

Solids

2-62

A

Introduction

2-62

B

Total Solids Dried at 103-105°C

2-64

C

Total Dissolved Solids Dried at 180°C

2-65

D

Total Suspended Solids Dried at 103-105°C

2-66

E

Fixed and Volatile Solids Ignited at55O°C

2-67

F

Settleable Solids

2-67

G

Total, Fixed, and Volatile Solids in Solid and Semisolid Samples

2-68

2550

Temperature

2-69

A

Introduction

2-69

B

Laboratory and Field Methods

2-69

2560

Particle Counting and Size Distribution

2-70

A

Introduction

2-70

B

Electrical Sensing Zone Method

2-75

C

Light-Blockage Methods

2-76

D

Light-Scattering Method

2-77

2570

Asbestos

2-78

A

Introduction

2-78

B

Transmission Electron Microscopy Method

2-79

2580

Oxidation-Reduction Potential (ORP)

2-84

A

Introduction

2-84

B

Oxidation-Reduction Potential Measurement in Clean Water

2-84

2710

Tests on Sludges

2-88

A

Introduction

2-88

B

Oxygen-Consumption Rate

2-88

C

Settled Sludge Volume

2-89

D

Sludge Volume Index

2-90

E

Zone Settling Rate

2-90

F

Specific Gravity

2-91

G

Capillary Suction Time

2-92

H

Time-to-Filter

2-93

I

Modified Settled Sludge Volume

2-94

2720

Anaerobic Sludge Digester Gas Analysis

2-95

A

Introduction

2-95

B

Volumetric Method

2-96

C

Gas Chromatographic Method

2-97

2810

Dissolved Gas Supersaturation

2-100

A

Introduction

2-100

B

Direct-Sensing Membrane-Diffusion Method

2-100

PART 3000

METALS

 

3010

Introduction

3-1

A

General Discussion

3-1

B

Sampling and Sample Preservation

3-1

C

General Precautions

3-3

3020

Quality Assurance/Quality Control

3-3

A

Introduction

3-3

B

Quality Control Practices

3-4

3030

Preliminary Treatment of Samples

3-6

A

Introduction

3-6

B

Filtration for Dissolved and Suspended Metals

3-6

C

Treatment for Acid-Extractable Metals

3-7

D

Digestion for Metals

3-7

E

Nitric Acid Digestion

3-9

F

Nitric Acid-Hydrochloric Acid Digestion

3-10

G

Nitric Acid-Sulfuric Acid Digestion

3-10

H

Nitric Acid-Perchloric Acid Digestion

3-10

I

Nitric Acid-Perchloric Acid- Hydrofluoric Acid Digestion

3-11

J

Dry Ashing

3-11

K

Microwave-Assisted Digestion

3-11

3110

Metals by Atomic Absorption Spectrometry

3-14

3111

Metals by Flame Atomic Absorption Spectrometry

3-14

A

Introduction

3-14

B

Direct Air-Acetylene Flame Method

3-18

C

Extraction/Air-Acetylene Flame Method

3-20

D

Direct Nitrous Oxide-Acetylene Flame Method

3-21

E

Extraction/Nitrous Oxide-Acetylene Flame Method

3-22

3112

Metals by Cold-Vapor Atomic Absorption Spectrometry

3-23

A

Introduction

3-23

B

Cold-Vapor Atomic Absorption Spectrometric Method

3-23

3113

Metals by Electrothermal Atomic Absorption Spectrombtry

3-25

A

Introduction

3-25

B

Electrothermal Atomic Absorption Spectrometric Method

3-28

3114

Arsenic and Selenium by Hydride Generation/Atomic Absorption Spectrometry

3-34

A

Introduction

3-34

B

Manual Hydride Generation/Atomic Absorption Spectrometric Method

3-34

C

Continuous Hydride Generation/Atomic Absorption Spectrometric Method

3-38

3120

Metals by Plasma Emission Spectroscopy

3-40

A

Introduction

3-40

B

Inductively Coupled Plasma (ICP) Method

3-40

3125

Metals by Inductively Coupled Plasma- Mass Spectrometry

3-46

A

Introduction

3-46

B

Inductively Coupled Plasma—Mass Spectrometry (ICP-MS) Method

3-47

3130

Metals by Anodic Stripping Voltammetry

3-57

A

Introduction

3-57

B

Determination of Lead, Cadmium, and Zinc

3-57

3500-A1

Aluminum

3-61

A

Introduction

3-61

B

Eriochrome Cyanine R Method

3-61

3500-As

Arsenic

3-64

A

Introduction

3-64

B

Silver Diethyldithiocarbamate Method

3-65

35OO-Ca

Calcium

3-67

A

Introduction

3-67

B

EDTA Titrimetric Method

3-67

3500-Cr

Chromium

3-68

A

Introduction

3-68

B

Colorimetric Method

3-69

C

Ion Chromatographic Method

3-71

3500-Cu

Copper

3-73

A

Introduction

3-73

B

Neocuproine Method

3-74

C

Bathocuproine Method

3-75

3500-Fe

Iron

3-76

A

Introduction

3-76

B

Phenanthroline Method

3-77

3500-Pb

Lead

3-80

A

Introduction

3-80

B

Dithizone Method

3-81

3500-Li

Lithium

3-82

A

Introduction

3-82

B

Flame Emission Photometric Method

3-83

3500-Mg

Magnesium

3-84

A

Introduction

3-84

B

Calculation Method

3-84

3500-Mn

Manganese

3-85

A

Introduction

3-85

B

Persulfate Method

3-85

3500-K

Potassium

3-87

A

Introduction

3-87

B

Flame Photometric Method

3-87

C

Potassium-Selective Electrode Method

3-88

3500-Se

Selenium

3-89

A

Introduction

3-89

B

Sample Preparation

3-91

C

Colorimetric Method

3-93

D

Determination of Volatile Selenium

3-94

E

Determination of Nonvolatile Organic Selenium Compounds

3-95

3500-Na

Sodium

3-96

A

Introduction

3-96

B

Flame Emission Photometric Method

3-97

3500-Sr

Strontium

3-98

A

Introduction

3-98

B

Flame Emission Photometric Method

3-99

3500-V

Vanadium

3-100

A

Introduction

3-100

B

Gallic Acid Method

3-101

3500-Zn

Zinc

3-102

A

Introduction

3-102

B

Zincon Method

3-102

3500

Other Metals

3-104

3500-Sb

Antimony

3-104

3500-Ba

Barium

3-104

3500-Be

Beryllium

3-104

3500-Bi

Bismuth

3-105

3500-B

Boron

3-105

3500-Cd

Cadmium

3-105

3500-Cs

Cesium

3-105

3500-Co

Cobalt

3-106

3500-Ga

Gallium

3-106

3500-Ge

Germanium

3-106

3500-Au

Gold

3-107

3500-In

Indium

3-107

3500-Ir

Iridium

3-107

3500-Hg

Mercury

3-107

3500-Mo

Molybdenum

3-108

3500-Ni

Nickel

3-108

3500-Os

Osmium

3-108

3500-Pd

Palladium

3-109

3500-Pt

Platinum

3-109

3500-Re

Rhenium

3-109

3500-Rh

Rhodium

3-109

3500-Ru

Ruthenium

3-110

3500-Ag

Silver

3-110

3500-Te

Tellurium

3-110

3500-Tl

Thallium

3-111

3500-Th

Thorium

3-111

35OO-Sn

Tin

3-111

35OO-Ti

Titanium

3-111

3500-U

Uranium

3-112

PART 4000

INORGANIC NONMETALLIC CONSTITUENTS

 

4010

Introduction

4-1

4020

Quality Assurance/Quality Control

4-1

A

Introduction

4-1

B

Quality Control Practices

4-1

4110

Determination of Anions by Ion Chromatography

4-5

A

Introduction

4-5

B

Ion Chromatography with Chemical Suppression of Eluent Conductivity

4-5

C

Single-Column Ion Chromatography with Direct Conductivity Detection

4-8

D

Ion Chromatographic Determination of Oxyhalides and Bromide

4-9

4120

Segmented Continuous Flow Analysis

4-13

A

Introduction

4-13

B

Segmented Flow Analysis Method

4-13

4130

Inorganic Nonmetals by Flow Injection Analysis

4-15

A

Introduction

4-15

B

Quality Control

4-15

4140

Inorganic Anions by Capillary Ion Electrophoresis

4-16

A

Introduction

4-16

B

Capillary Ion Electrophoresis with Indirect UV Detection

4-16

4500-B

Boron

4-25

A

Introduction

4-25

B

Curcumin Method

4-25

C

Carmine Method

4-27

4500-Br–

Bromide

4-28

A

Introduction

4-28

B

Phenol Red Colorimetric Method

4-28

C

(Reserved)

4-29

D

How Injection Analysis

4-29

4500-CO2

Carbon Dioxide

4-30

A

Introduction

4-30

B

Nomographic Determination of Free Carbon Dioxide and the Three Forms of Alkalinity

4-31

C

Titrimetric Method for Free Carbon Dioxide

4-31

D

Carbon Dioxide and Forms of Alkalinity by Calculation

4-36

4500-CN–

Cyanide

4-37

A

Introduction

4-37

B

Preliminary Treatment of Samples

4-39

C

Total Cyanide after Distillation

4-41

D

Titrimetric Method

4-43

E

Colorimetric Method

4-44

F

Cyanide-Selective Electrode Method

4-45

G

Cyanides Amenable to Chlorination after Distillation

4-46

H

Cyanides Amenable to Chlorination without Distillation (Short-Cut Method)

4-48

I

Weak Acid Dissociable Cyanide

4-49

J

Cyanogen Chloride

4-50

K

Spot Test for Sample Screening

4-51

L

Cyanates

4-52

M

Thiocyanate

4-53

N

Total Cyanide after Distillation, by Flow Injection Analysis

4-55

0

Total Cyanide and Weak Acid Dissociable Cyanide by Flow Injection Analysis

4-57

4500-CI

Chlorine (Residual)

4-58

A

Introduction

4-58

B

Iodometric Method I

4-60

C

Iodometric Method II

4-62

D

Amperometric Titration Method

4-64

E

Low-Level Amperometric Titration Method

4-66

F

DPD Ferrous Titrimetric Method

4-66

G

DPD Colorimetric Method

4-69

H

Syringaldazine (FACTS) Method

4-70

I

Iodometric Electrode Technique

4-71

4500-CI

Chloride

4-72

A

Introduction

4-72

B

Argentometric Method

4-72

C

Mercuric Nitrate Method

4-73

D

Potentiometric Method

4-75

E

Automated Ferricyanide Method

4-76

F

(Reserved)

4-77

G

Mercuric Thiocyanate Flow Injection Analysis

4-77

4500-ClO2

Chlorine Dioxide

4-79

A

Introduction

4-79

B

Iodometric Method

4-79

C

Amperometric Method I

4-80

D

(Reserved)

4-81

E

Amperometric Method 11

4-81

4500-F–

Fluoride

4-83

A

Introduction

4-83

B

Preliminary Distillation Step

4-84

C

Ion-Selective Electrode Method

4-85

D

SPADNS Method

4-87

E

Complexone Method

4-88

F

(Reserved)

4-89

G

Ion-Selective Electrode Flow Injection Analysis

4-89

4500-H+

pH Value

4-91

A

Introduction

4-91

B

Electrometric Method

4-92

4500-I

Iodine

4-96

A

Introduction

4-96

B

Leuco Crystal Violet Method

4-97

C

Amperometric Titration Method

4-98

4500-I–

Iodide

4-99

A

Introduction

4-99

B

Leuco Crystal Violet Method

4-99

C

Catalytic Reduction Method

4-100

D

Vokammetric Method

4-101

4500-IO3–

Iodate

4-103

A

Introduction

4-103

B

Polarographic Method

4-103

4500-N

Nttrogen

4-104

A

Introduction

4-104

B

In-Line UV/Persulfate Digestion and Oxidation with Flow Injection Analysis

4-105

C

Persulfate Method

4-107

D

Conductimetric Determination of Inorganic Nitrogen

4-108

4500-NH3

Nitrogen (Ammonia)

4-110

A

Introduction

4-110

B

Preliminary Distillation Step

4-110

C

Titrimetric Method

4-112

D

Ammonia-Selective Electrode Method

4-113

E

Ammonia-Selective Electrode Method Using Known Addition

4-114

F

Phenate Method

4-115

G

Automated Phenate Method

4-116

H

Flow Injection Analysis

4-118

4500-NO2–

Nitrogen (Nitrite)

4-120

A

Introduction

4-120

B

Colorimetric Method

4-120

4500-NO3–

Nitrogen (Nitrate)

4-122

A

Introduction

4-122

B

Ultraviolet Spectrophotometric Screening Method

4-122

C

Second-Derivative Ultraviolet Spectrophotometric Method (PROPOSED)

4-123

D

Nitrate Electrode Method

4-124

E

Cadmium Reduction Method

4-125

F

Automated Cadmium Reduction Method

4-127

G

(Reserved)

4-128

H

Automated Hydrazine Reduction Method

4-128

I

Cadmium Reduction Flow Injection Method

4-129

4500-Norg

Nitrogen (Organic)

4-131

A

Introduction

4-131

B

Macro-Kjeldahl Method

4-132

C

Semi-Micro-Kjeldahl Method

4-134

D

Block Digestion and Flow Injection Analysis

4-135

4500-O

Oxygen (Dissolved)

4-137

A

Introduction

4-137

B

Iodometric Methods

4-137

C

Azide Modification

4-139

D

Permanganate Modification

4-140

E

Alum Flocculation Modification

4-142

F

Copper Sulfate-Sulfamic Acid Flocculation Modification

4-142

G

Membrane Electrode Method

4-143

45OO-O3

Ozone (Residual)

4-145

A

Introduction

4-145

B

Indigo Colorimetric Method

4-145

4500-P

Phosphorus

4-148

A

Introduction

4-148

B

Sample Preparation

4-151

C

Vanadomolybdophosphoric Acid Colorimetric Method

4-153

D

Stannous Chloride Method

4-154

E

Ascorbic Acid Method

4-155

F

Automated Ascorbic Acid Reduction Method

4-156

G

Flow Injection Analysis for Orthophosphate

4-157

H

Manual Digestion and Flow Injection Analysis for Total Phosphorus

4-159

I

In-line UV/Persulfate Digestion and Flow Injection Analysis for Total Phosphorus

4-160

J

Persulfate Method for Simultaneous Determination of Total Nitrogen and Total Phosphorus

4-162

4500-KMnO4

Potassium Permanganate

4-164

A

Introduction

4-164

B

Spectrophotometric Method

4-164

4500-SiO2

Silica

4-165

A

Introduction

4-165

B

(Reserved)

4-167

C

Molybdosilicate Method

4-167

D

Heteropoly Blue Method

4-169

E

Automated Method for Molybdate-Reactive Silica

4-170

F

Flow Injection Analysis for Molybdate-Reactive Silicate

4-171

4500-S2–

Sulfide

4-172

A

Introduction

4-172

B

Separation of Soluble and Insoluble Sulfides

4-174

C

Sample Pretreatment to Remove Interfering Substances or to Concentrate the Sulfide

4-175

D

Methylene Blue Method

4-175

E

Gas Dialysis, Automated Methylene Blue Method

4-177

F

Iodometric Method

4-178

G

Ion-Selective Electrode Method

4-179

H

Calculation of Un-ionized Hydrogen Sulfide

4-181

I

Distillation, Methylene Blue Flow Injection Analysis Method

4-183

J

Acid-Volatile Sulfide

4-184

4500-SO32–

Sulfite

4-185

A

Introduction

4-185

B

Iodometric Method

4-186

C

Phenanthroline Method

4-187

4500-SO42–

Sulfate

4-188

A

Introduction

4-188

B

(Reserved)

4-189

C

Gravimetric Method with Ignition of Residue

4-189

D

Gravimetric Method with Drying of Residue

4-190

E

Turbidimetric Method

4-190

F

Automated Methylthymol Blue Method

4-191

G

Methylthymol Blue Flow Injection Analysis

4-193

PART 5000

AGGREGATE ORGANIC CONSTITUENTS

 

5010

Introduction

5-1

A

General Discussion

5-1

B

Sample Collection and Preservation

5-1

5020

Quality Assurance/Quality Control

5-1

A

Introduction

5-1

B

Quality Control Practices

5-2

5210

Biochemical Oxygen Demand (BOD)

5-4

A

Introduction

5-4

B

5-Day BOD Test

5-5

C

Ultimate BOD Test

5-10

D

Respirometric Method

5-13

5220

Chemical Oxygen Demand (COD)

5-16

A

Introduction

5-16

B

Open Reflux Method

5-17

C

Closed Reflux, Titrimetric Method

5-19

D

Closed Reflux, Colorimetric Method

5-20

5310

Total Organic Carbon (TOC)

5-21

A

Introduction

5-21

B

High-Temperature Combustion Method

5-23

C

Persulfate-Ultraviolet or Heated-Persulfate Oxidation Method

5-25

D

Wet-Oxidation Method

5-28

5320

Dissolved Organic Halogen

5-29

A

Introduction

5-29

B

Adsorption-Pyrolysis-Titrimetric Method

5-29

5510

Aquatic Humic Substances

5-35

A

Introduction

5-35

B

Diethylaminoethyl (DEAE) Method

5-36

C

XAD Method

5-37

5520

Oil and Grease

5-38

A

Introduction

5-38

B

Liquid-Liquid, Partition-Gravimetric Method

5-40

C

Partition-Infrared Method

5-41

D

Soxhlet Extraction Method

5-42

E

Extraction Method for Sludge Samples

5-43

F

Hydrocarbons

5-44

G

Solid-Phase, Partition-Gravimetric Method

5-45

5530

Phenols

5-46

A

Introduction

5-46

B

Cleanup Procedure

5-47

C

Chloroform Extraction Method

5-47

D

Direct Photometric Method

5-49

5540

Surfactants

5-50

A

Introduction

5-50

B

Surfactant Separation by Sublation

5-51

C

Anionic Surfactants as MB AS

5-53

D

Nonionic Surfactants as CTAS

5-55

5550

Tannin and Lignin

5-58

A

Introduction

5-58

B

Colorimetric Method

5-58

5560

Organic and Volatile Acids

5-59

A

Introduction

5-59

B

Chromatographic Separation Method for Organic Acids

5-59

C

Distillation Method

5-61

D

Gas Chromatographic Method

5-62

5710

Formation of Trihalomethanes and Other Disinfection By-Products

5-64

A

Introduction

5-64

B

Trihalomethane Formation Potential (THMFP)

5-67

C

Simulated Distribution System Trihalomethanes (SDS-THM)

5-71

D

Formation of Other Disinfection By-Products (DBPs)

5-72

5910

UV-Absorbing Organic Constituents

5-74

A

Introduction

5-74

B

Ultraviolet Absorption Method

5-75

PART 6000

INDIVIDUAL ORGANIC COMPOUNDS

 

6010

Introduction

6-1

A

General Discussion

6-1

B

Sample Collection and Preservation

6-3

C

Analytical Methods

6-4

6020

Quality Assurance/Quality Control

6-6

A

Introduction

6-6

B

Quality Control Practices

6-7

6040

Constituent Concentration by Gas Extraction

6-11

A

Introduction

6-11

B

Closed-Loop Stripping, Gas Chromatographic/Mass Spectrometric Analysis

6-11

C

Purge and Trap Technique

6-22

D

Solid-Phase Microextraction (SPME)

6-22

E

Solid-Phase Microextraction (SPME) with CI GC/MS/MS

6-25

6200

Volatile Organic Compounds

6-30

A

Introduction

6-30

B

Purge and Trap Capillary-Column Gas Chromatographic/Mass Spectrometric Method

6-33

C

Purge and Trap Capillary-Column Gas Chromatographic Method

6-38

6211

Methane

6-43

A

Introduction

6-43

B

Combustible-Gas Indicator Method

6-43

C

Volumetric Method

6-45

6231

1,2-DlBROMOETHANE (EDB) AND 1,2-Dibromo-3-Chloropropane (DBCP)

6-45

A

Introduction

6-45

B

Liquid-Liquid Extraction Gas Chromatographic Method

6-45

C

Purge and Trap Gas Chromatographic/Mass Spectrometric Method

6-48

D

Purge and Trap Gas Chromatographic Method

6-48

6232

Trihalomethanes and Chlorinated Organic Solvents

6-48

A

Introduction

6-48

B

Liquid-Liquid Extraction Gas Chromatographic Method

6-49

C

Purge and Trap Gas Chromatographic/Mass Spectrometric Method

6-54

D

Purge and Trap Gas Chromatographic Method

6-54

6251

Disinfection By-Products: Haloacetic Acids and Trichlorophenol

6-55

A

Introduction

6-55

B

Micro Liquid-Liquid Extraction Gas Chromatographic Method

6-55

6252

Disinfection By-Products: Aldehydes (PROPOSED)

6-65

A

Introduction

6-65

B

PFBHA Liquid-Liquid Extraction Gas Chromatographic Method

6-66

6410

Extractable Base/Neutrals and Acids

6-73

A

Introduction

6-73

B

Liquid-Liquid Extraction Gas Chromatographic/Mass Spectrometric Method

6-74

6420

Phenols

6-87

A

Introduction

6-87

B

Liquid-Liquid Extraction Gas Chromatographic Method

6-87

C

Liquid-Liquid Extraction Gas Chromatographic/Mass Spectrometric Method

6-93

6431

polychlorinated Blphenyls (PCBs)

6-93

A

Introduction

6-93

B

Liquid-Liquid Extraction Gas Chromatographic Method

6-93

C

Liquid-Liquid Extraction Gas Chromatographic/Mass Spectrometric Method

6-93

6440

Polynuclear Aromatic Hydrocarbons

6-93

A

Introduction

6-93

B

Liquid-Liquid Extraction Chromatographic Method

6-94

C

Liquid-Liquid Extraction Gas Chromatographic/Mass Spectrometric Method

6-99

6450

Nitrosamines

6-99

A

Introduction

6-99

B

Carbonaceous-Resin Solid-Phase Extraction GC/MS Method

6-100

C

Micro Liquid-Liquid Extraction GC/MS Method

6-109

6610

Carbamate Pesticides

6-112

A

Introduction

6-112

B

High-Performance Liquid Chromatographic Method

6-113

6630

Orcanochlorine Pesticides

6-121

A

Introduction

6-121

B

Liquid-Liquid Extraction Gas Chromatographic Method I

6-121

 

Appendix—Standardization of Magnesia-Silica Gel Column by Weight Adjustment Based on Adsorption of Laurie Acid

6-127

C

Liquid-Liquid Extraction Gas Chromatographic Method II

6-128

D

Liquid-Liquid Extraction Gas Chromatographic/Mass Spectrometric Method

6-135

6640

Acidic Herbicide Compounds

6-135

A

Introduction

6-135

B

Micro Liquid-Liquid Extraction Gas Chromatographic Method

6-136

6651

Glyphosate Herbicide

6-146

A

Introduction

6-146

B

Liquid Chromatographic Post-Column Fluorescence Method

6-147

6710

Tributyl Tin

6-149

A

Introduction

6-149

B

Gas Chromatographic/Mass Spectrometric Method

6-149

C

Gas Chromatographic/Flame Photometric Detector Method

6-154

PART 7000

RADIOACTIVITY

 

7010

Introduction

7-1

A

General Discussion

7-1

B

Sample Collection and Preservation

7-2

7020

Quality System

7-3

A

Quality Systems/Quality Assurance/Quality Control Program

7-3

B

Quality Control for Wastewater Samples

7-8

C

Statistics

7-8

D

Calculation and Expression of Results

7-11

7030

Counting Instruments

7-12

A

Introduction

7-12

B

Description and Operation of Instruments

7-12

7040

Facilities

7-18

A

Counting Room

7-18

B

Radiochemistry Laboratory

7-18

C

Laboratory Safety

7-19

D

Pollution Prevention

7-19

E

Waste Management

7-19

7110

Gross Alpha and Gross Beta Radioactivity (Total, Suspended, and Dissolved)

7-20

A

Introduction

7-20

B

Evaporation Method for Gross Alpha-Beta

7-20

C

Coprecipitation Method for Gross Alpha Radioactivity in Drinking Water

7-23

7120

Gamma-Emitting Radionuclides

7-25

A

Introduction

7-25

B

Gamma Spectroscopic Method

7-25

7500-Cs

Radioactive Cesium

7-29

A

Introduction

7-29

B

Precipitation Method

7-29

7500-I

Radioactive Iodine

7-30

A

Introduction

7-30

B

Precipitation Method

7-30

C

Ion-Exchange Method

7-31

D

Distillation Method

7-32

7500-Ra

Radium

7-34

A

Introduction

7-34

B

Precipitation Method

7-34

C

Emanation Method

7-37

D

Sequential Precipitation Method

7-42

E

Gamma Spectroscopy Method

7-44

7500-Rn

Radon

7-49

A

Introduction

7-49

B

Liquid Scintillation Method

7-50

7500-Sr

Total Radioactive Strontium and Strontium-90

7-52

A

Introduction

7-52

B

Precipitation Method

7-53

75O0-3H

Tritium

7-56

A

Introduction

7-56

B

Liquid Scintillation Spectrometric Method

7-56

7500-U

Uranium

7-58

A

Introduction

7-58

B

Radiochemical Method

7-58

C

Isotopic Method

7-60

PART 8000

TOXICITY

 

8010

Introduction

8-1

A

General Discussion

8-1

B

Terminology

8-2

C

Basic Requirements

8-3

D

Conducting Toxicity Tests

8-4

E

Preparing Organisms for Toxicity Tests

8-7

F

Toxicity Test Systems, Materials, and Procedures

8-15

G

Calculating, Analyzing, and Reporting Results of Toxicity Tests

8-20

H

Interpreting and Applying Results of Toxicity Tests

8-24

I

Selected Toxicological Literature

8-25

8020

Quality Assurance and Quality Control In Laboratory Toxicity Tests

8-26

A

General Discussion

8-26

B

Elements of QA/QC

8-27

8030

Mutaoenesis

8-30

A

Introduction

8-30

B

Salmonella Microsomal Mutagenicity Test

8-32

8050

Bacterial Bioluminescence

8-38

A

Introduction

8-38

B

Bacterial Bioluminescence Test

8-38

8070

P450 Reporter Gene Response to Dioxm-Like Organic Compounds

8-41

A

Introduction

8-41

B

The P450 RGS Test

8-41

8071

Comet/Single-Cell Gel Electrophoresis Assay For Detection of DNA Damage

8-43

A

Introduction

8-43

B

Comet/Single-Cell Gel Electrophoresis Assay

8-44

8080

Sediment Porewater Testing

8-47

A

Introduction

8-47

B

Sediment Collection and Storage

8-48

C

Extraction of Sediment Pore Water

8-48

D

Toxicity Testing Procedures

8-50

8110

Algae

8-52

8111

Biostimulation (Algal Productivity)

8-52

A

General Principles

8-52

B

Planning and Evaluating Algal Assays

8-53

C

Apparatus

8-54

D

Sample Handling

8-54

E

Synthetic Algal Culture Medium

8-55

F

Inoculum

8-55

G

Test Conditions and Procedures

8-56

H

Effect of Additions

8-57

I

Data Analysis and Interpretation

8-57

8112

Phytoplankton

8-58

A

Introduction

8-58

B

Inoculum

8-58

C

Test Conditions and Procedures

8-58

8113

Marine Macroalgae

8-59

A

Introduction

8-59

B

Selecting and Preparing Macrocystis pyrifera Sporophylls

8-60

C

Toxicity Test Procedures

8-62

D

Data Evaluation

8-64

8200

Aquatic Flowering Plants

8-64

8211

Duckweed

8-65

A

Introduction

8-65

B

Selecting and Preparing Test Organisms

8-66

C

Toxicity Test Procedure

8-67

8220

Aquatic Emergent Plants

8-69

A

Introduction

8-69

B

Selecting and Preparing Test Organisms

8-70

C

Toxicity Test Procedure

8-71

8310

Ciliated Protozoa

8-73

A

Introduction

8-73

B

Growth Inhibition Test with Freshwater Ciliate Colpidium campylum

8-73

C

Chemotactic Test with Freshwater Ciliate Tetrahymena thermophila

8-75

D

Growth Inhibition Test with the Soil Ciliate Colpoda inflata

8-77

8420

Rotifers

8-79

A

Introduction

8-79

B

Selecting and Preparing Test Organisms

8-80

C

Toxicity Test Procedures

8-81

8510

Annelids

8-83

A

Introduction

8-83

B

Selecting and Preparing Test Organisms

8-83

C

Toxicity Test Procedures

8-89

D

Sediment Test Procedures Using the Marine Polychaete Neanthes arenaceodentata

8-91

E

Sediment Test Procedures Using the Marine Polychaete Polydora cornuta

8-93

F

Sediment Test Procedures Using the Freshwater and Marine Oligochaetes Pristina leidyi, Tubifex tubifex, and Lumbriculus variegates

8-94

G

Data Evaluation

8-95

8610

Mollusks

8-96

A

Introduction

8-96

B

Selecting and Preparing Test Organisms

8-96

C

Short-Term Test Procedures Using Marine Mollusk Larvae

8-98

D

Sediment Test Procedures Using Marine Bivalves

8-100

E

Field Test Procedures Using Freshwater and Marine Bivalves

8-101

8710

Arthropods

8-105

8711

Daphnia

8-105

A

Introduction

8-105

B

Selecting and Preparing Test Organisms

8-107

C

Toxicity Test Procedures

8-108

8712

Ceriodaphnia

8-110

A

Introduction

8-110

B

Selecting and Preparing Test Organisms

8-111

C

Toxicity Test Procedures

8-113

8714

Mysids

8-115

A

Introduction

8-115

B

Selecting and Preparing Test Organisms

8-116

C

Toxicity Test Procedures

8-121

8740

Decapods

8-125

A

Introduction

8-125

B

Selecting and Preparing Test Organisms

8-125

C

Toxicity Test Procedures

8-132

D

Data Evaluation

8-136

8750

Aquatic Insects

8-136

A

Introduction

8-136

B

Selecting and Preparing Test Organisms

8-137

C

Toxicity Test Procedures

8-139

D

Data Evaluation

8-140

8810

Echinoderm Fertilization and Development

8-141

A

Introduction

8-141

B

Selecting and Preparing Test Organisms

8-142

C

Echinoderm Fertilization Test

8-143

D

Echinoderm Embryo Development Test

8-148

8910

Fish

8-150

A

Introduction

8-150

B

Fish Selection and Culture Procedures

8-151

C

Toxicity Test Procedures

8-155

8921

Fathead Minnow

8-161

A

Introduction

8-161

B

Culture and Maintenance of Test Organisms

8-162

C

Toxicity Test Procedures

8-163

8930

Amphibians (PROPOSED)

8-170

A

Introduction

8-170

B

Culture and Maintenance of Test Organisms

8-171

C

Toxicity Test Procedures

8-174

PART 9000

MICROBIOLOGICAL EXAMINATION

 

9010

Introduction

9-1

9020

Quality Assurance/Quality Control

9-2

A

Introduction

9-2

B

Intralaboratory Quality Control Guidelines

9-4

C

Interlaboratory Quality Control

9-25

9030

Laboratory Apparatus

9-26

A

Introduction

9-26

B

Equipment Specifications

9-26

9040

Washing and Sterilization

9-30

9050

Preparation of Culture Media

9-31

A

General Procedures

9-31

B

Water

9-32

C

Media Specifications

9-32

9060

Samples

9-33

A

Collection

9-33

B

Preservation and Storage

9-35

9211

Rapid Detection Methods

9-36

A

Introduction

9-36

B

Seven-Hour Fecal Coliform Test

9-36

C

Special Techniques

9-37

9212

Stressed Microorganisms

9-39

A

Introduction

9-39

B

Recovery Enhancement

9-40

9213

Recreational Waters

9-42

A

Introduction

9-42

B

Swimming Pools

9-43

C

Whirlpools

9-45

D

Natural Bathing Beaches

9-46

E

Membrane Filter Technique for Pseudomonas aeruginosa

9-48

F

Multiple-Tube Technique for Pseudomonas aeruginosa

9-49

9215

Heterotrophic Plate Count

9-49

A

Introduction

9-49

B

Pour Plate Method

9-52

C

Spread Plate Method

9-54

D

Membrane Filter Method

9-56

E

Enzyme Substrate Method

9-57

9216

Direct Total Microbial Count

9-57

A

Introduction

9-57

B

Epifluorescence Microscopic Method Using Acridine Orange

9-58

9217

Assimilable Organic Carbon

9-59

A

Introduction

9-59

B

Pseudomonas fluorescens Strain P-17, Spirillum Strain NOX Method

9-61

9218

Aerobic Endospores

9-64

A

Introduction

9-64

B

Membrane Filter Method

9-64

9221

Multiple-Tube Fermentation Technique for Members of the Coliform Group

9-65

A

Introduction

9-65

B

Standard Total Coliform Fermentation Technique

9-66

C

Estimation of Bacterial Density

9-69

D

Presence-Absence (P-A) Coliform Test

9-73

E

Fecal Coliform Procedure

9-74

F

Escherichia coli Procedure Using Fluorogenic Substrate

9-75

G

Other Escherichia coli Procedures (PROPOSED)

9-76

9222

Membrane Filter Technique for Members of the Coliform Group

9-77

A

Introduction

9-77

B

Standard Total Coliform Membrane Filter Procedure

9-78

C

Delayed-Incubation Total Coliform Procedure

9-84

D

Thermotolerant (Fecal) Coliform Membrane Filter Procedure

9-85

E

Delayed-Incubation Thermotolerant (Fecal) Coliform Procedure

9-87

F

Klebsiella Membrane Filter Procedure

9-88

G

MF Partition Procedures

9-89

H

Simultaneous Detection of Total Coliform and E. coli by Dual-Chromogen Membrane Filter Procedure (PROPOSED)

9-90

I

Simultaneous Detection of Total Coliform and E. coli by Fluorogen/Chromogen Membrane Filter Procedure (PROPOSED)

9-91

9223

Enzyme Substrate Coliform Test

9-93

A

Introduction

9-93

B

Enzyme Substrate Test

9-93

9224

Detection of Coliphages

9-95

A

Introduction

9-95

B

Somatic Coliphage Assay

9-96

C

Male-Specific Coliphage Assay Using Escherichia coli Famp

9-98

D

Male-Specific Coliphage Assay Using Salmonella typhimurium WG49

9-99

E

Single-Agar-Layer Method

9-101

F

Membrane Filter Method

9-102

9225

Differentiation of Coliform Bacteria

9-103

A

Introduction

9-103

B

Culture Purification

9-104

C

Identification

9-105

D

Media, Reagents, and Procedures

9-107

E

Reporting Results

9-110

9230

Fecal Enterococcus/Streptococcus Groups

9-110

A

Introduction

9-110

B

Multiple-Tube Technique

9-111

C

Membrane Filter Techniques

9-112

D

Fluorogenic Substrate Enterococcus Test

9-115

9240

Iron and Sulfur Bacteria

9-116

A

Introduction

9-116

B

Iron Bacteria

9-117

C

Sulfur Bacteria

9-122

D

Enumerating, Enriching, and Isolating Iron and Sulfur Bacteria

9-124

E

Bacteria Living in Acidic Environments

9-130

9245

Nitrifying Bacteria

9-135

A

Introduction

9-135

B

Multiple-Tube Method

9-137

9250

Detection of Actinomycetes

9-138

A

Introduction

9-138

B

Actinomycete Plate Count

9-140

9260

Detection of Pathogenic Bacteria

9-142

A

Introduction

9-142

B

Salmonella

9-145

C

(Reserved)

9-150

D

(Reserved)

9-150

E

Shigella

9-150

F

Diarrheagenic Escherichia coli

9-153

G

Campylobacter

9-158

H

Vibrio

9-160

I

Leptospira

9-166

J

Legionella

9-169

K

Yersinia enterocolitica

9-174

L

Aeromonas

9-177

M

Mycobacterium

9-180

9510

Detection of Enteric Viruses

9-184

A

Introduction

9-184

B

Virus Concentration from Small Sample Volumes by Adsorption to and Elution from Microporous Filters

9-186

C

Virus Concentration from Large Sample Volumes by Adsorption to and Elution from Microporous Filters

9-189

D

Virus Concentration by Aluminum Hydroxide Adsorption-Precipitation

9-193

E

Hydroextraction-Dialysis with Polyethylene Glycol

9-195

F

Recovery of Viruses from Suspended Solids in Water and Wastewater

9-196

G

Assay and Identification of Viruses in Sample Concentrates

9-197

9610

Detection of Fungi

9-201

A

Introduction

9-201

B

Pour Plate Technique

9-204

C

Spread Plate Technique

9-205

D

Membrane Filter Technique

9-206

E

Technique for Yeasts

9-207

F

Zoosporic Fungi

9-207

G

Aquatic Hyphomycetes

9-208

H

Fungi Pathogenic to Humans

9-209

9711

Pathogenic Protozoa

9-210

A

Introduction

9-210

B

Detection of Giardia and Cryptosporidiwn in Water

9-215

C

Detection of Giardia and Cryptpsporidium in Wastewater

9-221

D

Infectivity of Cryptosporidiwn. in Cell Culture

9-222

PART 10000

BIOLOGICAL EXAMINATION

 

10010

Introduction

10-1

10200

Plankton

10-2

A

Introduction

10-2

B

Sample Collection

10-3

C

Concentration Techniques

10-11

D

Preparing Slide Mounts

10-13

E

Microscopes and Calibrations

10-15

F

Phytoplankton Counting Techniques

10-17

G

Zooplankton Counting Techniques

10-21

H

Chlorophyll

10-22

I

Determination of Biomass (Standing Crop)

10-30

J

Metabolic Rate Measurements

10-32

10300

Periphyton

10-36

A

Introduction

10-36

B

Sample Collection

10-36

C

Sample Analysis

10-38

D

Primary Productivity

10-41

E

Interpreting and Reporting Results

10-50

10400

Macrophytes

10-52

A

Introduction

10-52

B

Preliminary Survey

10-53

C

Vegetation Mapping Methods

10-53

D

Population Estimates

10-55

E

Productivity

10-59

10500

Benthic Macroinvertebrates

10-67

A

Introduction

10-67

B

Sample Collection

10-70

C

Sample Processing and Analysis

10-79

D

Data Evaluation, Presentation, and Conclusions

10-81

10600

Fishes

10-84

A

Introduction

10-84

B

Data Acquisition

10-85

C

Sample Preservation

10-94

D

Analysis of Collections

10-95

E

Investigation of Fish Kills

10-100

10700

Benthic Meiofauna

10-101

10750

Nematological Examination

10-102

A

Introduction

10-102

B

Collection and Processing Techniques for Nematodes

10-104

C

Illustrated Key to Freshwater Nematodes

10-106

10900

Identification of Aquatic Organisms

10-122

A

Procedure in Identification

10-122

B

Key to Major Groups of Aquatic Organisms (Plates 1-35)

10-122

 

Acknowledgments

10-126

C

Key for Identification of Freshwater Algae Common in Water Supplies and Polluted Waters (Plates 1A, IB, 28-35)

10-160

D

Index to Illustrations

10-165

E

Selected Taxonomic References

10-168

 

Index

1-1