STANDARD METHODS For tl1e Exatnination of Water and Wastewater SIXTEENTH EDITION Prepared and published jointly by: AMERICAN PUBLIC HEALTH ASSOCIATION AMERICAN WATER WORKS ASSOCIATION W A TER POLLUTION CONTRO L FEDERA TION Joint Editoria! Board ARNOLD E. GREENBERG, APRA, Cbairman R. RHODES TRUSSELL, A WW A L ENORE S. CLESCERI, WPCF MARY ANN H. FRANSON Managing Editor Publication Office: American Public Health Association 1015 Fifteenth Street NW Washington, DC 20005
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STANDARD METHODS For tl1e Exatnination of Water and Wastewater
SIXTEENTH EDITION
Prepared and published jointly by:
AMERICAN PUBLIC HEALTH ASSOCIATION
AMERICAN WATER WORKS ASSOCIATION
W A TER POLLUTION CONTRO L FEDERA TION
Joint Editoria! Board
ARNOLD E. GREENBERG, APRA, Cbairman
R. RHODES TRUSSELL, A WW A
L ENORE S. CLESCERI, WPCF
MARY ANN H. FRANSON
Managing Editor
Publication Office: American Public Health Association 1015 Fifteenth Street NW Washington, DC 20005
P art
P art
TABLE OF CONTENTS
100 GENERAL INTRODUCIION PAGE
3 101 APPLICATIONS ... . .... .
102 LABORATORY APPARATUS, R.EAGENTS, ANO TECHNIQUES. 3
104 PRECISION, ACCURACY, ANO CORRECTNESS OF ANALYSES 20
105
106
107
108
109
200
201
202
203
204
A. Precision and Accuracy . . . . . . . . 20 B. Quality Contro) in Chemical Analysis . . . 25 C. Checking Correctness of Analyses . . . . . 32
CoLLECTION ANO PRESERVATION OF SAMPLES 37
ION-EXCHANGE RESINS . . . . . . 44
REAGENT W ATER (TENTA TIVE) 44
SAFETY. . . . . . . . . . . . 46
BIBLIOGRAPHY . . . . . . . . 58
PHYSICAL EXAMINATION
INTROOUCTION . . . . . . . .
APPEARANCE. . . . . . . . . . . . . . . . . . . .
CALCIUM CARBONATE SATURATION (fENTATIVE).
COLOR .. . ....... . . .
A . Visual Comparison Method . B. Spectrophotometric Method . C. Tristimulus Filter Method .. D. ADMI Tristimulus Filter Method (fENTATIVE) .
E. Bibliography
205 CoNDUCTIVITY . . . . . . . . . . . . . .
206 Fl.OA T ABLES . . . . . . . . . . . . . . .
63
63
63
67
67 69 73 74 76
76
80
80 A . Particulate Floatab1es (TENT ATIVE) . B. Trichlorotrifluo:roethane-Soluble Floatable Oil and
Grease (TENTA TIVE) .
C. Bibliography . .
207 000R . ... . . .
208 0XYGEN TRANSFER
209 Souos ...... .
A. Total So1ids Dried at 103-lOs·c B. Total Dissolved Solids Dried at 180"C . C. Total Suspended Solids Dried at 103-to5•c .
xxi
83 85 85 92
92 93 95 96
Xxii
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TABLE OF CONTENTS
PAGE
D. Fixed and Volatile Solids Ignited at sso•c . . . . . . 97 E. Settleable Solids . . . . . . . . . . . . . . . . 98 F. Total, Fixed, and Volatile Solids in Solid and Semisolid
Samples . 99 G. Reference. . 100 H. Bibliography 100
210 SALINITY . . . . 101
102
102
109 122 122
A. Electrica1 Condu.ctivity Method . B. Hydrometric Method . C. Argentometric Method D. Reference. . E. Bibliography . . . . .
211 TASTE . . . . . . . . . . 122
A. Taste Threshold Test . 124 B. Taste Rating Test. 124 C. References . 125 D. Bib1iography . . 126
212 TEMPERATURE . . . 126
213 TESTS ON SLUDGES . 127
A. Oxygen-Consumption Rate 127 B. Settled Sludge Volume 129 C. S1udge Volume Index. 130 D. Zone Settling Rate 130 E. Specific Gravity. 132 F. References . 133 G. Bibliography . . 133
Thallium, Tin, and Zinc by Direct Aspiration into an Air-Acetylene Flame . . . . . . . . . . . . . . . . 157
B. Determination of Low Concentrations of Cadmium, Chromium, Cobalt, Copper, Iron, Lead, Manganese, Nickel, Silver, and Zinc by Chelation with Ammonium Pyrrolidine Dithiocarbamate (APDC) and Extraction into Methyl Isobutyl Ketone (MIBK). 160
C. Determination of Aluminum, Barium, Beryllium, Molybdenum, Osmium, Rhenium, Silioon, Thorium, Titanium, and Vanadium, by Direct Aspiration into a Nitrous Oxide-Acetylene Flame . . . . . . . . . . 162
D. Determination of Low Concentrations of Aluminum and Beryllium by Chelation with 8-Hydroxyquinoline and Extraction into Methyl lsobutyl Ketone. . . . . 164
E. Determination of Arsenic and Selenium by Conversion to Their Hydrides by Sodium Borohydride Reagent and Aspiration into an Atomic Absorption Atomizer. 165
F. Determinationof Mercuryby theCold VaporTechnique. 171
304 D ETERMINATION OF MICRO QUANTITIES OF ALUMINUM,
A. Atomic Absorption Spectrometric Method . B. Gallic Acid Method . .. ........ .
P AGE
226
226 226 228 228 228
229 229 231
232 232 232
234
234 234 236 236
236 236 237 237
238
238 238 240 241
242
242 242 245
245
246 246
249
249 250 251
252
252 252
xxvi T ABLE OF CONTENTS
PAGE
328 ZINC . 254
A. Atomic Absorption Spectrometric Method . 254 B. Dithizone Method I. 255 c. Dithizone Method II 257 D. Zincon Method . 259 E. Bibliography . 260
P art 400 DETERMINATION OF INORGANIC NONMETALLIC
CONSTITUENTS
401 INORGANIC NONMETALS-INTRODUCTION 265
402 ACIDITY. 265
403 ALKALINITY . 269 404 BORON. 274
A. Curcumin Metbod 274 B. Carmine Method . 276 c. Bibliography . 277
405 BROMIDE. 278
406 CARBON DIOXIDE 279 A. Nomographic Determination of Free Carbon Dioxide
and the Three Forms of Alkalinity 280 B. Titrimetric Method for F ree Carbon Dioxide. 285 c. Carbon Dioxide and Fonns of Alkalinity by
Calculation . 285 D. Bibliography . 286
407 CHLORIDE . 286 A. Argentometric Method 287 B. Mercuric Nitrate Method . 288 c. Potentiometric Method . 290 D. Automated Ferricyanide Method 292 E. Bibliography . 294
408 CHLORINE (REsiDUAL) . 294
A. lodometric Method I . 298 B. lodometric Method Il. 300 c. Amperometric Titration Method. 303 D. DPD Ferrous Titrimetric Method . 306 E. DPD Colorimetric Method . 309 F. Leuco Crystal Violet Method . 310 G. Syringaldazine (F ACTS) Method (TENTA TIVE) 313 H. References . 314 I. Bibliography . 31 5
T ABLE OF CONTENTS xxvii
409 CHLORINE 0 EMAND . .
PAGE
316
316 318 319
A. Laboratory Method . B. Field Method . . C. Bibliography . . . .
410 CHLORINE 0IOXIOE ..
A. lodometric Method . B. Amperometric Method C. DPD Method (TENTATIVE) . D. Bibliography . . . . . . . . .
319
320 322 323 324
411 CHLORINE R EQUIREMENT . . . . 325
A. Method for Contro! of Disinfection 325 B. Methods for Pu.rposes Other Than Disinfection Contro!. 327
412 CYANIDE. . . . . . . . . . . . . . . 327
A. Preliminary Treatment of Samples . 331 B. Total Cyanide a.fter Distillation 334 C. Titrimetric Method . . . . . . . . 336 D. Colorimetric Method . . . . . . . 337 E. Cyanide-Selective Electrode Method . 338 F. Cyanides Amenable to Chlorination after Distillation. 340 G. Cyanides Amenable to Chlorination without
Distillation (Short-Cut Method). 341 H. Weak and Dissociable Cyanide . 344 l. Cyanogen Chloride . . . . . . . 345 J. Spot Test for Sample Screening . 345 K. Cyanates . . 34 7 L. Thiocyanate 348 M. References 351
413 FLUORIDE . . 352
A. Preliminary Distillation Step 355 B. Electrode Method. . . . 357 C. SPADNS Metbod. . . . 359 D. Alizarin Visual Method. 361 E. Complexone Method 362 F. Bibliography . . . . . . 364
414 IODIDE. . . . . . . . . . . 364
A. Leuco Crystal Violet Method . 365 B. Catalytic Reduction Method. 367 C. References . 368 D. Bibliography . . . . . . . . 368
-xxviii T ABLE OF CONTENTS
PAGE
415 lODINE . 369
A. Leuco Crystal Vio1et Method (TENTA TIVE) 369 B. Amperometric Titration Method. 371
c. Bib1iography . 372
416 NITROOEN . 373
417 NITROGEN (AMMONIA) . 374
A. Preliminary Distillation Step 377 B. Nesslerization Method (Direct and Following
Distillation) 379 c. Phenate Method 382 D. Titrimetric Method . 383 E. Ammonia-Se1ective Electrode Method . 384 F . Ammonia-Se1ective E1ectrode Method Using Known
Addition. 386 G. Automated Phenate Method. 388 H. Bibliography . 390
418 NITROOEN (NITRATE) 391
A. Ultraviolet Spectrophotometric Screening Method 392 B. Nitrate E1ectrode Screening Method . 393 c. Cadmium Reduction Method . 394 D. Chromotropic Acid Method . 397 E. Devarda's AJloy Reduction Method . 398 F. Automated Cadmium Reduction Method
(TENTA TIVE). 400 G. Bibliography . 403
419 NITROOEN (NITRITE). 404
420 NITROOEN (ORGANIC) 406
A. Macro-Kjeldahl Method. 408 B. Semi-Micro-Kje1dahl Method (TENTATIVE) 411
421 OXYGEN (DISSOLVED) 413
A. lodometric Methods 416 B. Azide Modification . 418 c. Permanganate Modification . 420 D. Alum Floccu1ation Modification. 421 E. Copper Sulfate-Sulfamic Acid Floccu1ation
Modification . 421 F . Membrane Electrode Method . 422 G. References . 425
508 OXYOEN DEMAND (CHEMICAL). 532 A. Open Reflux Method . 533 B. Closed Reflux, T itrimetric Method 535 c. Closed Reflux, Colorimetric Method. 537 D . References . 538 E. Bibliography . 538
509 PESTICIDES (0RGANIC) . 538 A. Organochlorine Pesticides . 538
Appendix-Standardization of Magnesia-Silica Gel Column by Weight Adjustment Based on Adsorption of Lauric Acid . 548
B. Chlorinated Phenoxy Acid Herbicides . 550 c. Bibliography . 555
510 PHENOLS . 556
A. Cleanup Procedure . 557 B. Chloroform Extraction Method 558 c. Direct Photometric Method . 560
T ABLE OF CONTENTS xxxi
PAOE
D. Gas-Liquid Chromatographic Method . 561 E. Bibliography 570
511 SLUDOE DIOESTER GAS 571 A. Volumetric Method. 572 B. Gas Chromatographic Method 574 c. References . 577 D. Bibliography . 577
512 SURFACTANTS 577 A. Surfactant Separation by Sublation. 578 B. Anionic Surfactants as MBAS . 581 c. Nonionic Surfactants as CT AS 585 D . References . 588 E. Bibliography . 589
513 T ANNIN ANO L IONIN. 590
514 H ALOOENATED M ETHANES AND ETHANES BY PUROE
AND TRAP. 591
515 0ROANIC CoMPOUNDS CAUSINO T ASTE AND ÙDOR . 602
516 OROANIC CoNTAMINM'TS, Gas Chromatographic/ M ass
Spectrometric M ethod 612
P art 600 AUTOMATE D LABORATORY ANALYSES (deleted,
see specific constituents)
P art 700 EXAMINATION OF WATER AND WASTE WATER
FOR RADIOACfiVITY
701 INTRODUCTION . 625
A. Collection of Samples . 626 B. Counting Room 627 c. Counting Instruments. 627 D . Laboratory Reagents and Apparatus. 633 E. Expression of R esults . 634 F. Statistics . 634 G . Quality Assur ance 636 H . References . 637 l. Bibliography 637
702 RADIOACTIVITY IN WASTEWATER 638
703 GROSS ALPHA AND GROSS BETA RADIOACTIVITY (fOTAL,
SUSPENDED, AND DISSOLVED) 640
704 T OTAL RADIOACTIVE STRONTIUM AND STRONTIUM 90 IN
W ATER 646
705 RADIUM IN WATER BY PRECJPITATION. 652
xxxii T ABLE OF CONTENTS
PAGE
706 RADIUM 226 BY R.ADON IN WATER (SOLUBLE, SUSPENOED, ANO TOTAL) 657
707 RADIUM 228 (SOLUBLE) (TENTA TIVE) 667
708 TRITIUM . 670
709 RADIOACTIVE CESIUM 673
710 RADIOACTIVE lODINE 674
A. Precipitation Method . 675
B. Ion-Exchange Method. 676
c. Distillation Method . 678
D. Bibliography . 679
711 URANIUM 679
A. Radiochemical M ethod (TENTA TIVE) 680
B. Fluorometric Method (TENTA TIVE) . 682
c. Bibliography . 684
P art 800 TOXICITY TEST METHODS FOR AQUATIC
ORGANISMS
801 INTRODUCTION . 689 A. Terminology . 689 B. Basic Requirements for Toxicity Tests . 691
c. Conducting Toxicity Tests. 691
D. Preparing Organisms for Toxicity Tests 695
E. Toxicity Test Systems, Materials, and Procedures 707 F. Calculating, Analyzing, and Reporting Results of
Toxicity Tests 715
G. Interpreting and App1ying Results of T oxicity Tests 719
H. References . 720 l. Bibliography . 725
802 BIOSTJMULATION (ALGAL PRODUCTIVITY) 726 A. Generai Principles 726 B. Planning and Evaluating Algal Assays. 727 c. Apparatus 727 D . Sample Handling . 728 E. Synthetic Alga! Culture Medium 729 F. Inoculum. 729 G. Test Conditions and Procedures . 731 H. Effect of Additions . 733 I. Data Analysis and Interpretation 734 ] . References . 735 K. Bibliography . 735
803 TOXJCJTY TESTING WITH PHYTOPLANKTON (TENTA TIVE). 735
804 TOXICITY TEST PROCEDURES USING ZOOPLANKTON. 737
TABLE OF CONTENTS xxxiii
PAG E
A. Toxicity Test Procedures for Ciliated Protozoa (TENTATIVE) . . . . . . . . . . . . . . . 737
B. Toxicity Test Procedures for Daphnia (TENTA TIVE) . 739 C. Toxicity Test Procedures for the Calanoid Copepod,
Acartia tonsa (Dana) (TENTA TIVE) . . . . . 742
805 TOXICITY T EST PROCEDURES USJNG SCLERACTINIAN
CORAL (TENTATIVE). . . . . . . . . . 748
A. Selecting and Preparing Test Organisms . 749 B. Toxicity Test Procedures . . . . . 751 C. Evaluating and Reporting Results . . . . 753 D. References . . . . . . . . . . . . . . . 754
806 TOXICITY TEST PROCEDURES FOR ANNELIDS
(TENTATIVE). . . . . . . . . . . . . . 756
A. Selecting and Preparing Test Organisms . 757 B. Toxicity Test Procedures 760 C. Data Evaluation . . . . . . . . . . . . 763 D. Bibliography . . . . . . . . . . . . . . 763
807 TOXICITY 'fEsnNG PROCEDURES FOR CRUSTACEANS
(TENTATIVE). . . . . . . . . . . . 764
A. Selecting and Preparing Test Species. 765 B. Conducting the Toxicity Tests. 774 C. Reporting Results. 782 D. References . . . . . . . . . . 782 E. Bibliography . . . . . . . . . 785
808 TOXICITY TEST PROCEDURES FOR AQUA TIC I NSECTS
(TENTATIVE). . . . . . . . . . . . . . 786
A. Selecting and Preparing Test Organisms . 786 B. Toxicity Test Procedures 789 C. Data Evaluation 791 D. References . . . . . . . 791 E. Bibliography . . . . . . 791
809 TOXlCITY TEST PROCEDURES USING M OLLUSKS
(TENTA TI VE). . . . . . . . . . . . . . 792
A. Selecting and Preparing Test Organisms . 793 B. Conducting the Toxicity Tests . . 795 C. Reporting and Analyzing Results 798 D. References . . . . . . . . . . . 798 E. Bibliography . . . . . . . . . . 799
A. Standard Total Coliform Membrane Filter Procedure. 887 B. Delayed-Incubation Total Coliform Procedure . 894 C. Fecal Coliform Membrane Filter Procedure . . 896 D. Delayed-lncubation Fecal Coliform Procedure . 898
T ABLE OF CONTENTS
PAGE
E. Klebsiella Membrane Filter Procedure (TENTATIVE) . 899 F. Bibliography . 901
910 TESTS FOR THE FECAL STREPTOCOCCUS GROUP. 902
A . Multiple-Tube Technique . 904 B. Membrane Filter Technique. 905
c. Fecal Streptococcal Plate Count (TENTA TIVE) . 908 D. Bibliography . 909
9 11 D fFFERENTIATION OF THE COLIFORM G ROUP . 910
A. Culture Purifica tion. 910
B. Differentiation 910 c. Significance of Coliform Types 913
D. Media, Reagent-s, and Procedures 914
E. References . 916 F. Bibliography . 917
912 DETECTION OF PATHOGENIC MICROORGANISMS. 917
A. Generai Qualitative lsolation and Identification Procedures for Salmone/la 919
B. Immunofluorescence Identification Procedure for Sa/monella . 923
c. Quantitative Sa/monella Procedures . 926
D . Shigella 927
E. Enteropathogenic Escherichia coli . 928
F. Campylobacter jejuni . 928 G . Vibrio cholerae and NAG Vibrios . 930
H . Pathogenic Leptospires 932
I. Legionellaceae 934
J. Yersinia enterocolitica . 936 K . Pathogenic Protozoa 937
L. References . 941
M . Bibliography . 944
913 DETECTION OF ENTERIC VIRUSES . 946
A. Virus Concentration by Adsorption to and Elution from Microporous Filters (TENT ATIVE) . 948
B. Virus Concentration by Aluminum Hydroxide Adsorption-Precipitation (TENTA TIVE) 959
c. Hydroextraction-Dia1ysis with Polyethylene Glyco1 (TENTA TIVE). 961
D . Recovery of Viruses from Suspended Solids in Water and Wastewater (TENTA TIVE) 963
E. Assay and Identification of Viruses in Samp1e Concentrates (TENT ATIVE) . 964
E. References . 969
xxxvi T ABLE OF CONTENTS
PAGE
914 BACTERIOLOGICAL EXAMINATION OF RECREATIONAL WATERS. 974
A. Swimming Poo1s 974
B. Natural Bathing Beaches 976
c. Membrane Filter Technique for Pseudomonas
aeruginosa (TENT ATIVE) . 978
D. Multiple. Tube Technique for Pseudomonas aeruginosa
(TENTATIVE). 979
E. Bibliography . 980
915 DETECTION OF FUNGI 981
A. Pour Plate Technique. 982
B. Spread Plate Technique . 984
c. Membrane Filter Technique . 985
D. Technique for Y easts . 986
E. Zoosporic Fungi 987
F. Aquatic Hyphomycetes . 988
G. Pathogenic Fungi . 989
H. References . 990
l. Bibliography . 991
916 DETECTION OF ACTINOMYCETES 992
917 NEMATOLOGICAL EXAMINATION 995
A. Technique for Nematodes . 997 B. Illustrated Key to Fresh Water Nematodes 999 c. References . 1018
D . Bibliography . 1018
918 IDENTIFICATION OF IRON AND SULFUR BACTERIA. 1019
A. Iron Bacteria . 1020
B. Sulfur Bacteria . 1022
c. Enumeration, Enrichment, and Isolation of Iron and Sulfur Bacteria (TENTA TIVE) . 1025
D. References . 1029
919 RAPID DETECTJON METHODS. 1031
A. Seven-Hour Fecal Coliform Test (TENTATIVE) . 1031
B. Special Techniques (TENTA TIVE) 1032
c. Coliphage Detection (TENTA TIVE). 1033
D . References . 1035
920 STRESSED 0RGANISMS 1036
T ABLE OF CONTENTS xxxvii
PAGE
P art 1000 BIOLOGICAL EXAMINATION OF WATER
1001 INTRODUCTION , 1041
1002 PLANKTON. 1043
A. Introduction 1043 B. Sample Collection. 1044 c. Concentration Techniques . 1054 D. Mounting and Preparation for Examination 1055 E. Microscopes and Calibrations . 1057 F. Counting Techniques . 1060 G. Chlorophyll. 1067 H . Determination of Biomass (Standing Crop). 1072 l. Metabolic Rate Measurements. 1075 J. References . 1079
1003 PERIPHYTON . 1083
A. Introduction . 1083 B. Sample Collection. 1084 c. Sample AnaJysis 1085 D . Productivity 1088 E. Interpreting and Reporting Results 1099 F. References . 1100 G. Bib1iography . 1101
1004 MACROPHYTON. 1103
A. Introduction 1103 B. Preliminary Survey . 1104 c. Vegetation Mapping Methods . 1104 D . Population Estimates . 1106 E. Productivity 1110 F. References . 1111 G. Bibliography . 1111
1005 BENTHIC MACROINVERTEBRATES. 1113
A. Introduction . 1113 B. Samp1e Collection. 1114 c. Sarnple Processing and Analysis . 1125 D. Data Evaluation and Presentation . 1126 E. References . 1127 F. Bibliography . 1129
1006 F'IsH . 1131
A. Introduction . 1131
xxxvìiì
103:1 104:1 104:11
104:III 104:1V 105:1
1007
TABLE OF CONTENTS
PAGE
B. Sample Collection and Preservation . 1131
c. Quantitative Analysis of Fish Populations 1138
D. Sample Ana!ysis 1140
E. Fish ldentification 1141
F. lnvestigation of Fish Kills. 1145
G . References . 1146
H. Bibliography . 11 47
IDENTIFICATION OF AQUATIC 0RGANISMS. 1148
A. Procedure in Identification 1148
B. Key to Major Groups of Aquatic Organisms (Plates 1-38) . 1149
l. Key to Microscopic Organisms . 1149
2. Key t o Macroscopic Organisms. 1150
3. Key to M acroinvertebrates . 1150
4. Key to Crustaceans 1151 5. Key to Insect Pupae . 1152
6. Key to Insect Larvae, Nymphs, and Some Adults 1152
c. List of Common Types of Aquatic Organisms (Piates 1-38), by Trophic Leve! . 1153
ACKNOWLEDGMENTS . 1154
D. Key for ldentification of Freshwater Algae Common in Water Supplies and Polluted Waters (Color Plates A-F). . . . . . . 1194
l. Blue-Green Algae 1194 2. Diatoms . . . . . l I 96 3. Flagellate Algae . 1197 4. Green Algae and Associated Forms. l 198
E. Recent Changes in Names of Algae . 1201 F. lndex to Illustrations . . . . . 1203 G . Selected Taxonomic References 1207
INDEX . . . . . . . . . . . . . . 1217
TABLES
Conversion Factors . . . . . . . . . . . . . . . . . . . Factors for Computing Contro! Chart Lines . . . . . . . Data and Computations for Construction of Example x-R
18 27
Chart .................. . .... . Moving Average and Range Table . ......... . Conductivity Factors of lons Commonly Found in Water Summary of Special Sampling or Handling Requirements