ANNOTATED BIBLIOGRAPHY OF ANALYTICAL METHODS FOR CERCLA
HAZARDOUS SUBSTANCES
by
H. B. Kerfoot, J. L. Engels, D. F. Arnold, and A. R. Bujold
Lockheed Engineering and Management Services Company
Las Vegas, Nevada 89114
Prepared for the
Office of Emergency and Remedial Response
Contract Number 68-03-3050
Project Officer
Werner F. Beckert
Quality Assurance Division
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89114
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89114
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NITROGEN DIOXIDE AND NITRIC OXIDE
Air Samples
Laboratory Method 2
Compound CAS Number
Nitric Oxide 10102-43-9
Nitrogen Dioxide 10102-44-0
METHOD SUMMARY:
Analysis of air samples for the above oxides of nitrogen can be performed
by chromic acid oxidation and reaction with an azo-dye-forming reagent,
followed by colorimetry. A known volume of air (up to 2.4 liters) is passed
through a chromic acid oxidizer, nitric oxide is converted to nitrogen dioxide
by chromic acid, and the resulting nitrogen dioxide and the nitrogen dioxide
originally present are absorbed in an aqueous solution of sulfanilic acid,
acetic acid, acetone, and N-(l-naphthyl)-ethylenediamine dihydrochloride. The
red-violet color produced is measured spectrophotometrically at 550 nanometers.
This method does not identify any particular compound, but measures the total
amount of nitrogen dioxide present after oxidation of the sample by chromic
acid.
INTERFERENCES:
Any significant interferences due to sulfur dioxide should be eliminated
by the oxidation step. The addition of acetone to the color reagent retards
the fading of color from the presence of sulfur dioxide. A five-fold ratio of
ozone to nitrogen dioxide causes a slight orange tint in the solution.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable to total nitric
oxide/nitrogen dioxide concentrations in the range 4 to 10,000 micrograms per
cubic meter. Precision information is furnished.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.03, D3608-77; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analyses by this method is approximately $30-40, plus
sampling costs.
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NITROGEN DIOXIDE AND NITRIC OXIDE
Air Samples
Laboratory Method 3
Compound CAS Number
Nitric Oxide 10102-43-9
Nitrogen Dioxide 10102-44-0
METHOD SUMMARY:
Nitric oxide and nitrogen dioxide levels in air samples can be determined
by chemiluminescence. For measurement of only nitric oxide, the gas being
sampled is blended with ozone in a flow reactor, and the intensity of emitted
light from the reaction of nitric oxide with ozone is measured. To measure
total nitric oxide and nitrogen dioxide, the gas is diverted through a
converter that reduces nitrogen dioxide to nitric oxide before being admitted
to the flow reactor- The concentration of nitrogen dioxide can be obtained by
subtraction.
INTERFERENCES:
Possible interferences from hydrocarbons are eliminated by use of a red
sharp-cut off filter. Any compounds converted to nitric oxide in the converter
are potential interferences; ammonia does not interfere when the converter
temperature is below 300°C. Other organic nitrogen compounds may decompose to
liberate nitric oxide in the converter.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable over the follow-
ing ranges: nitric oxide, 10 micrograms to 30 milligrams per cubic meter;
nitrogen dioxide, 20 micrograms to 50 milligrams per cubic meter. Precision
and accuracy information is furnished.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.03, D3824-79; ASTM: Philadelphia, 19837~
COST INFORMATION:
Cost information has not been obtained.
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PHOSPHORUS
Air Samples
Laboratory Method
Compound
Aluminum Phosphide
0-0-Diethyl S-Methyl
Dithiophosphate
Diethyl-£-nitrophenyl
Phosphate
Diisopropyl Fluorophosphate
Hexaethyl Tetraphosphate
Lead Phosphate
Octamethylpyrophosphoramide
Phosphoric Acid
Phosphorus
Phosphorus Oxychloride
Phosphorus Pentasulfide
Phosphorus Trichloride
Sodium Phosphate, Dibasic
CAS Number
20859-73-8
3288-58-2
311-45-5
Compound
Sodium Phosphate,
Tribasic
55-
757-
7446-
152-
7664-
7723-
10025-
1314-
7719-
7558-
10039-
10028-
10140-
•91-4
•58-4
•27-7
•16-9
•38-2
•14-0
•87-3
•80-3
•12-2
•79-4
•32-4
•24-7
65-5
Tetraethyldithiopyro-
phosphate
Tetraethyl Pyrophosphate
Tris(2,3-Dibromopropyl)
Phosphate
Zinc Phosphide
CAS Number
7601-54-9
7785-84-4
10101-89-0
10361-89-4
7758-29-4
10124-56-8
3689-24-5
107-49-3
126-72-7
1314-84-7
METHOD SUMMARY:
Analysis for the above phosphorus-containing compounds in air may be
performed by inductively coupled plasma atomic emission spectroscopic (ICP)
analysis for phosphorus. A known volume of air is drawn through a cellulose
ester membrane filter. The filter is ashed with a mixture of nitric and per-
chloric acids and the digest analyzed by ICP. This method does not identify
any specific phosphorus-containing compound, but measures the total phosphorus
content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
phosphorus per cubic meter for a 500-liter sample. Limited precision and
accuracy information is furnished.
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REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
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PHOSPHORUS
Soil/Sediment Samples
Laboratory Method
Compound
CAS Number
Aluminum Phosphide 20859-73-8
Chlorpyrifos 2921-88-2
Coumaphos 56-72-4
Diazinon 333-41-5
Dichlorvos 62-73-7
0-0-Diethyl S-Methyl 3288-58-2
Dithiophosphate
Diethyl-£-nitrophenyl 311-45-5
Phosphate
Diisopropyl Fluorophosphate 55-91-4
Dimethoate 60-51-5
Disulfoton 298-04-4
Ethion 563-12-2
Hexaethyl Tetraphosphate 757-58-4
Lead Phosphate 7446-27-7
Malathion 121-75-5
Methyl Parathion 298-00-0
Mevinphos 7786-34-7
Naled 300-76-5
Octamethylpyrophosphoramide 152-16-9
Parathion 56-38-2
Phorate 298-02-2
Compound
Phosphoric Acid
Phosphorus
Phosphorus Oxychloride
Phosphorus Pentasulfide
Phosphorus Trichloride
Sodium Phosphate, Dibasic
Sodium Phosphate,
Tribasic
Tetraethyldithiopyro-
phosphate
Tetraethyl Pyrophosphate
Tris(2,3-Dibromopropyl)
Phosphate
Zinc Phosphide
CAS Number
7664-
7723-
10025-
1314-
7719-
7558-
10039-
10028-
10140-
7601-
7785-
101 01 -
10361-
7758-
10124-
3689-
-38-2
-14-0
•87-3
•80-3
•12-2
•79-4
•32-4
•24-7
65-5
•54-9
84-4
89-0
89-4
29-4
56-8
24-5
107-49-3
126-72-7
1314-84-7
METHOD SUMMARY:
Total recoverable phosphorus and organic phosphorus, resulting from the
compounds listed above, in sediment samples can be measured colorimetrically.
The sediment is ignited at 550°C for 2 hours, after which the residue is acid-
digested. The orthophosphate concentration in the acid extract is a measure of
the total phosphorus content; the inorganic phosphorus is determined by diges-
tion without ignition; the organic phosphorus is estimated by taking the
difference. The color development is based on the reaction of ammonium
molybdate with orthophosphate, followed by reduction with ascorbic acid to form
a blue molybdenum complex. Either manual or automated procedures may be used.
Antimony tartrate may be added to facilitate color development when following
the automated procedure. These methods measure all forms of phosphorus except
polyphosphates and minerals containing tightly bound phosphorus. They do not
identify the specific phosphorus-containing compounds present, but measure the
total phosphorus content of the sample.
INTERFERENCES:
Vanadium, zirconium, germanium, sulfide, tannins, lignins, hexavalent
chromium, arsenic, and silica can interfere, but the effects are reduced by
sample dilution. To prevent microbiological transformations that can result in
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changes of concentration of available phosphate, samples should be drained of
excess water immediately after collection and stored at 5°C or lower in the
dark.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The analytical range is 100 to 2000
micrograms per gram of sample. The range may be extended upwards by diluting
the sample. Precision and accuracy information is furnished.
REFERENCES:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Method D515-82; ASTM: Philadelphia, 1983, pp. 575-587.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, Method D4183-82; ASTM: Philadelphia, 1983, pp. 712-717.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 424C, 424D; APHA: Washington, 1980.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70 (list).
B-348
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PHOSPHORUS
Water Samples
Laboratory Method
Compound
Aluminum Phosphide
0-0-Diethyl S-Methyl
Dithiophosphate
Diethyl-£-nitrophenyl
Phosphate
Diisopropyl Fluorophosphate
Hexaethyl Tetraphosphate
Lead Phosphate
Octamethylpyrophosphoramide
Phosphoric Acid
Phosphorus
Phosphorus Oxychloride
Phosphorus Pentasulfide
Phosphorus Trichloride
Sodium Phosphate, Dibasic
CAS Number
20859-73-8
3288-58-2
311-45-5
55
757
7446
152
7664
7723
10025
1314
7719
7558'
10039'
10028
10140'
-91-4
-58-4
-27-7
-16-9
-38-2
-14-0
-87-3
-80-3
-12-2
-79-4
-32-4
-24-7
-65-5
Compound
Sodium Phosphate,
Tribasic
Tetraethyldithiopyro-
phosphate
Tetraethyl Pyrophosphate
Tri s(2,3-Dibromopropyl)
Phosphate
Zinc Phosphide
CAS Number
7601-54-9
7785-84-4
10101-89-0
10361-89-4
7758-29-4
10124-56-8
3689-24-5
107-49-3
126-72-7
1314-84-7
METHOD SUMMARY:
Analysis of water samples for the above phosphorus-containing compounds
and phosphorus ions can be performed by automated colorimetric analysis for
phosphorus. A 25-milliliter sample is digested with sulfuric acid, mercuric
sulfate, and potassium sulfate, heated for several hours in a block digester,
molybdate/antimony solution is added, and the resulting solution is analyzed
colorimetrically. This method does not differentiate between various
phosphorus-containing compounds, but gives the total amount of phosphorus
present in the sample.
INTERFERENCES:
Sample containers should be made of plastic or of borosilicate glass.
Samples should be preserved by acidification and refrigeration at 4°C if the
analysis cannot be performed on the day of collection.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is EPA-approved for the National Pollutant Discharge
Elimination System (NPDES) of the Clean Water Act. Precision and accuracy
information is provided.
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REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 365.4; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 424C, 424D; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual ASTM Book of Standards,
Vol. 11.01, Method D515-82(D); ASTM: Philadelphia, 1983.
Alberta Environmental Centre, Methods Manual for Chemical Analysis of Water and
Wastes, "Phosphorus, Total;" Publication No. AECV81-M1, Alberta Environmental
Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $45-50
(list).
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POTASSIUM
Air Samples
Laboratory Method
Compound CAS Number
Antimony Potassium Tartrate 28300-74-5
Potassium Arsenate 7784-41-0
Potassium Arsenite 10124-50-2
Potassium Chromate 7789-00-6
Potassium Cyanide 151-50-8
Potassium Dichromate 7778-50-9
Potassium Hydroxide 1310-58-3
Potassium Permanganate 7722-64-7
Potassium Silver Cyanide 506-61-6
Zirconium Potassium Fluoride 16923-95-8
METHOD SUMMARY:
Analysis of air samples for the above potassium compounds can be performed
by atomic absorption spectrometric (AA) analysis for potassium. Samples are
collected on cellulose ester membrane filters. The filter and the particulates
are digested with nitric acid, the digest diluted and analyzed by AA. This
method does not differentiate between potassium-containing compounds, but
measures the total potassium content of the sample.
INTERFERENCES:
Cesium should be added to samples and standards to control ionization
interference. The method of standard additions and/or background monitoring
may be needed to correct for interferences.
QUALITY CONTROL:
A minimum of 1 filter blank for every 10 filter samples must be analyzed.
Standard solutions should match the sample matrix as closely as possible.
Standards should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health for use over the range of 4.2 to 84 micrograms
potassium per cubic meter in a 240-liter sample of air. Precision information
is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method 173; Publication No. 77-157-A, U.S. DHEW:
Cincinnati, 1977.
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U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
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POTASSIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Antimony Potassium Tartrate 28300-74-5
Potassium Arsenate 7784-41-0
Potassium Arsenite 10124-50-2
Potassium Chromate 7789-00-6
Potassium Cyanide 151-50-8
Potassium Bichromate 7778-50-9
Potassium Hydroxide 1310-58-3
Potassium Permanganate 7722-64-7
Potassium Silver Cyanide 506-61-6
Zirconium Potassium Fluoride 16923-95-8
METHOD SUMMARY:
Analysis of soil/sediment samples for the above potassium compounds can be
performed by atomic emission spectrometric analysis for potassium. A 100-mill-
igram sample is digested with nitric acid, perchloric acid, hydrogen fluoride,
and boric acid, and analyzed. Samples should be stored in polyurethane bags
and frozen immediately after collection. This method does not differentiate
between potassium-containing compounds, but measures the total potassium con-
tent of the sample.
INTERFERENCES:
Standard and sample compositions should be closely matched. Solvent
extraction techniques may be necessary. Cesium should be added to samples and
standards to overcome ionization interference.
QUALITY CONTROL:
Quality control procedures are not provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The detection limit of the method is
approximately 100 micrograms per gram. Precision and accuracy information is
furnished.
REFERENCE:
Environment Canada, Analytical Methods Manual, NAQUADAT No. 19050; Environment
Canada, Inland Waters Directorate, Water Quality Branch: Ottawa, Canada, 1975.
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $20-30
t).
(list)
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POTASSIUM
Water Samples
Laboratory Method 1
Compound CAS Number
Antimony Potassium Tartrate 28300-74-5
Potassium Arsenate 7784-41-0
Potassium Arsenite 10124-50-2
Potassium Chromate 7789-00-6
Potassium Cyanide 151-50-8
Potassium Bichromate 7778-50-9
Potassium Hydroxide 1310-58-3
Potassium Permanganate 7722-64-7
Potassium Silver Cyanide 506-61-6
Zirconium Potassium Fluoride 16923-95-8
METHOD SUMMARY:
Analysis of water samples for the above potassium compounds can be per-
formed by atomic absorption (AA) spectrometric analysis for potassium. When
analysis is not to be performed soon after sample collection, samples should be
preserved by acidification with nitric acid. This method does not different-
iate between various potassium compounds, but measures the total amount of
potassium present in a sample.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
Standards should be analyzed each time a sample or set of samples is analyzed.
EPA/TECHNICAL STATUS:
This method is approved for the National Pollutant Discharge Elimination
System (NPDES). Precision and accuracy information is furnished. The detection
limit of the method is 5 micrograms per liter, the sensitivity 40 micrograms
per liter, and the optimum concentration range is 0.1 to 2 milligrams per liter
(APHA). Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 258.1: EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
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America Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 322A; APHA: Washington, 1980.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals by
Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S. DOE:
New York, 1983.
American Society for Testing and Materials, 1983 ASTM Book of Standards, Vol.
11.01, Method D4192-82; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list).
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POTASSIUM
Water Samples
Laboratory Method 2
Compound CAS Number
Antimony Potassium Tartrate 28300-74-5
Potassium Arsenate 7784-41-0
Potassium Arsenite 10124-50-2
Potassium Chromate 7789-00-6
Potassium Cyanide 151-50-8
Potassium Bichromate 7778-50-9
Potassium Hydroxide 1310-58-3
Potassium Permanganate 7722-64-7
Potassium Silver Cyanide 506-61-6
Zirconium Potassium Fluoride 16923-95-8
METHOD SUMMARY:
Analysis of water samples for the above potassium compounds can be per-
formed by flame photometric, colorimetric, or atomic absorption (AA) analysis
for potassium. In the colorimetric analysis, a 10-milliliter sample is reacted
with sodium cobaltinitrite and potassium dichromate in an acidic solution. The
excess dichromate is proportional to the amount of potassium originally present
and is determined colorimetrically with a spectrophotometer. Lower-level
samples should be analyzed by flame photometry. These methods do not identify
any specific potassium compound, but measure the total potassium content of the
sample.
INTERFERENCES:
When using flame photometry, samples containing particulate matter should
be filtered before analysis. Calcium, magnesium, and sodium may interfere. When
using colorimetry, the final colored solution may require filtration if it is
turbid. Colorimetric analysis should not be performed when ammonium ions are
present in the sample.
QUALITY CONTROL:
Samples should be stored in plastic containers. When performing colori-
metric analysis, a series of solutions of known potassium concentration must be
carried through the procedure with each set of samples. Using any method,
standards should be analyzed each time a set of samples is analyzed.
EPA/TECHNICAL STATUS:
These methods are approved for the National Pollutant Discharge Elimina-
tion System (NPDES). Precision and accuracy information is furnished. Concen-
trations of potassium above 0.1 milligram per liter can be detected by flame
photometry (APHA), and the optimum concentration range for the flame photometic
method is 1 to 100 milligrams per liter (ASTM).
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REFERENCES:
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 14th ed., Method 322B; APHA: Washington, 1975.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 258.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Method D4192-82; ASTM: Philadelphia, 1983.
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Potassium, Dissolved;" Publication No. AECV81-M1, Alberta Environ-
mental Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by these methods is approximately $20-40
(list).
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SELENIUM
Air Samples
Laboratory Method 1
Compound
Selenious Acid
Selenium
Selenium Dioxide
Selenium Disulfide
Selenourea
Sodium Selenite
Thallium(I) Selenide
CAS Number
7783-00-8
7782-49-2
7746-08-4
7488-56-4
630-10-4
10102-18-8
7782-82-3
12039-52-0
METHOD SUMMARY:
Analysis for the above selenium compounds in air may be performed by
filtration of air and analysis of the particulates on the filter for selenium
by X-ray fluorescence spectrometry. The method is non-destructive, so that
further analyses may be performed on samples. The sample-collection time may
be up to 8 hours, but analysis time is approximately 1 minute. The method
measures total selenium present in the sample and does not differentiate
between chemical compounds or selenium valence states.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-
fiber filters are acceptable for use only if they are of the highest purity.
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is given. The
method is sensitive to amounts of selenium above 40 micrograms.
REFERENCES:
Rhodes, J. R.; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786: American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R. ; Pradzynski, A. H.; Hunter, C. B.: Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927.
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
$20 (bid), plus sampling costs.
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SELENIUM
Air Samples
Laboratory Method 2
Compound CAS Number
Selenious Acid 7783-00-8
Selenium 7782-49-2
Selenium Dioxide 7746-08-4
Selenium Bisulfide 7488-56-4
Selenourea 630-10-4
Sodium Selenite 10102-18-8
7782-82-3
Thallium(I) Selenide 12039-52-0
METHOD SUMMARY:
Air samples may be analyzed for selenium and the above selenium compounds
by atomic absorption spectrometric analysis (AA) for selenium. The analysis is
performed by filtration of a known volume of air through a cellulose ester
membrane filter, followed by acid digestion of the filter and the deposited
material and AA analysis of the resulting solution. This method measures the
total selenium content of the air sampled and does not identify any specific
selenium compounds.
INTERFERENCES:
Flame interferences may be minimized by use of background correction and
an argon-hydrogen/air flame.
QUALITY CONTROL:
Percent recovery of spiked samples must be determined and, if below 95
percent, results should be corrected accordingly. A method blank should be
processed with each set of 10 or fewer samples. Duplicate analyses should
agree within 5 percent.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and has been validated over the range of 0.1 to 0.5 milli-
grams per cubic meter in a 360-liter sample. Precision and accuracy information
is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set M, Method SI 90; PB-265 029 (NTIS), U.S. DREW: Cincinnati, December 1976.
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U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S190; Publication No. 77-157-C, U.S. DREW:
Cincinnati, 1977.
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method S190; Publication No. 82-100, U.S. DHHS: Cincinnati,
August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $18-50
(list), plus sampling costs.
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SELENIUM
Air Samples
Laboratory Method 3
Compound CAS Number
Selenious Acid 7783-00-8
Selenium 7782-49-2
Selenium Dioxide 7746-08-4
Selenium Disulfide 7488-56-4
Selenourea 630-10-4
Sodium Selenite 10102-18-8
7782-82-3
Thallium (I) Selenide 12039-52-0
METHOD SUMMARY:
Analysis for the above selenium-containing compounds in air may be
performed by inductively coupled plasma atomic emission spectroscopic (ICP)
analysis for selenium. A known volume of air is drawn through a cellulose
ester membrane filter- The filter is ashed with a mixture of nitric and per-
chloric acids followed by analysis by ICP. The method does not identify any
specific selenium-containing compound, but measures the total selenium content
of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
selenium per cubic meter for a 500-liter sample. Limited precision and
accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-363
-------
SELENIUM
Air Samples
Laboratory Method 4
Compound CAS Number
Selenious Acid 7783-00-8
Selenium 7782-49-2
Selenium Dioxide 7746-08-4
Selenium Bisulfide 7488-56-4
Selenourea 630-10-4
Sodium Selenite 10102-18-8
7782-82-3
Thallium(I) Selenide 12039-52-0
METHOD SUMMARY:
The above particulate selenium compounds in air samples can be measured by
reaction-kinetic analysis. The analyte is collected from a known volume of air
on a membrane filter- The filter and particulates are wet-ashed with a mixture
of nitric and sulfuric acid and the resulting solution is neutralized with
sodium hydroxide. The selenite in the sample solution is reduced to elemental
selenium by sulfite and sulfide. The elemental selenium catalyzes the sulfide
reduction of methylene blue to the colorless leuco form in alkaline solution.
The selenium concentration is proportional to the rate of decolorization of the
methylene blue, which is measured spectrophotometrically- This method does not
identify any specific selenium compounds present, but measures the total
selenium content of the sample.
INTERFERENCES:
Copper(II), silver, antimony, and bismuth ions may interfere, but addi-
tion of ethylenediamine tetracetic acid (EDTA) should mask these ions.
QUALITY CONTROL:
A filter blank should be processed with the samples. Filter standards
should also be processed to determine recovery. The value of the blank and the
recovery should be used in the calculation of the results.
EPA/TECHNICAL STATUS:
This method is classifed as proposed by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 0.6 to 10
micrograms per cubic meter of air, with a 90-liter sample. Limited precision
and accuracy information is furnished.
B-364
-------
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Vol. 1, Method P&CAM181; Publication No. 77-157-A, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost information has not been obtained.
B-365
-------
SELENIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Selenious Acid 7783-00-8
Selenium 7782-49-2
Selenium Dioxide 7746-08-4
Selenium Bisulfide 7488-56-4
Selenourea 630-10-4
Sodium Selenite 10102-18-8
7782-82-3
Thallium(I) Selenide 12039-52-0
METHOD SUMMARY:
Analysis of soil/sediment samples for the above selenium compounds can be
performed by atomic spectrometric analysis for selenium. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and analyzed by atomic spectrom-
etry. Low selenium concentrations are determined by furnace atomic absorption
spectrometry (AA). Inductively coupled plasma (ICP) spectrometry is used to
analyze higher-concentration samples. These methods do not identify any speci-
fic selenium-containing compounds, but measure the total selenium content of
the sample.
INTERFERENCES;
Chlorides and sulfates in the sample may interfere. Nickel is added to
control sulfate interference. For each matrix analyzed, it is necessary to
determine if matrix effects and/or interferences require standard addition or
serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for
analyses under the Clean Water Act. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
B-366
-------
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 270.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Methods 3010, 3020, 3040, 3050, 6010, 7740: SW-846,
U.S. EPA: Washington, 1982.
Federal Register, 44_(233), December 3, 1979, pp. 69559-69564.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Selenium," pp. IV-88 to IV-98; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
COST INFORMATION:
Cost per sample for analysis by furnace AA is approximately $28-60; by
ICP, it is approximately $20.
B-367
-------
SELENIUM
Water Samples
Laboratory Method
Compound CAS Number
Selenious Acid 7783-00-8
Selenium 7782-49-2
Selenium Dioxide 7746-08-4
Selenium Bisulfide 7488-56-4
Selenourea 630-10-4
Sodium Selenite 10102-18-8
7782-82-3
Thallium(I) Selenide 12039-52-0
METHOD SUMMARY:
Analysis of water samples for the above selenium compounds can be per-
formed by atomic spectrometric analysis for selenium. A 100-milliliter sample
is digested with nitric acid and hydrogen peroxide and analyzed by atomic spec-
trometry. Low selenium concentrations are determined by furnace or gaseous
hydride atomic absorption spectrometry (AA). Inductively coupled plasma (ICP)
spectrometry is used to analyze higher-concentration samples. These methods do
not identify any specific selenium-containing compounds, but measure the total
selenium content of the sample.
INTERFERENCES:
Chlorides and sulfates in the sample may interfere, and nickel can be
added to control sulfate interference. For each matrix analyzed, it is
necessary to determine if matrix effects and/or interferences require standard
addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for Clean
Water Act analyses. The hydride method is applicable to concentrations from
0.2 to 5 micrograms per liter (Alberta Environment). Precision and accuracy
information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
B-368
-------
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 270.2, 270.3; EPA-600/4-79-020, U.S. EPA: Cincinnati,
March 1979.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Cincinnati, December 1982.
Federal Register, 44^233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 3010, 3020, 3040, 3050, 6010, 7740;
SW-846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Selenium," pp. IV-88 to IV-98; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 303E; APHA: Washington, 1983.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Method D3859-79; ASTM: Philadelphia, 1983.
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Selenium, Total;" Publication No. AECV81-M1, Alberta Environmental
Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by furnace AA is approximately $18-50 (list);
by ICP, it is approximately $10 (list).
B-369
-------
SILVER
Air Samples
Laboratory Method 1
Compound CAS Number
Potassium Silver Cyanide 506-61-6
Silver 7440-22-4
Silver Cyanide 506-64-9
Silver Nitrate 7761-88-8
METHOD SUMMARY:
Analysis for silver and the above silver compounds in air can be performed
by high-volume filtration with a glass-fiber filter, followed by acid digestion
of the filter with particles and analysis of the resulting solution by atomic
absorption spectrometry (AA). This method is not specific for particulate
silver metal or any silver-containing compound, but measures all silver and
silver compounds retained by the filter.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
A check standard should be analyzed each time a sample or set of samples
is processed.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 21 to 170
micrograms per cubic meter in a 240-liter sample of air. Precision information
is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. III. Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $18-50
(list), plus sampling costs.
B-370
-------
SILVER
Air Samples
Laboratory Method 2
Compound CAS Number
Potassium Silver Cyanide 506-61-6
Silver 7440-22-4
Silver Cyanide 506-64-9
Silver Nitrate 7761-88-8
METHOD SUMMARY:
Analysis for silver and the above silver-containing compounds in air may
be performed by inductively coupled plasma atomic emission spectroscopic (ICP)
analysis for silver. A known volume of air is drawn through a cellulose ester
membrane filter. The filter is ashed with a mixture of nitric and perchloric
acids and the digest analyzed by ICP. The method does not identify any
specific silver-containing compound, but measures the total silver content of
the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
silver per cubic meter, using a 500-liter sample. Limited precision and
accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this methods is approximately $10 (list),
plus sampling costs.
Note: NIOSH Method S182 (filter collection, acid digestion, analyses by DC
plasma emission spectrometry [DCP]) is applicable. (Reference provided
by reviewer.)
B-371
-------
SILVER
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Potassium Silver Cyanide 506-61-6
Silver 7440-22-4
Silver Cyanide 506-64-9
Silver Nitrate 7761-88-8
METHOD SUMMARY:
Analysis for the above silver compounds in soil/sediment samples can be
performed by inductively coupled plasma (ICP) or atomic absorption (AA) spec-
trometric analysis for silver. A 2-gram sample is digested with nitric acid
and hydrogen peroxide and analyzed by atomic spectrometry. For low concentra-
tions, ICP is used. Flame AA is used for higher concentrations. Analysis for
silver in oily samples may be performed by using ICP after dilution of the
sample with methyl isobutyl ketone (MIBK) or xylene, using standards miscible
with these solvents.
INTERFERENCES:
If adsorption to container walls or the formation of silver chloride is
suspected, ammonium hydroxide and cyanogen iodide should be added. The
summarized methods measure the total silver content of the sample and do not
identify specific silver compounds.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly, and at least 10 percent of the
analyses should be duplicates and/or standards. Standards should be analyzed
at least daily.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use in
Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 272.1; EPA-600/4-79-020, U.S. EPA; Cincinnati, 1979.
B-372
-------
Federal Register, 44_(233), December 3, 1979, pp. 69559-69564.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry;" pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 3040, 3050, 6010, 7740;
SW-846, U.S. EPA: Washington, 1982.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $20-30 (list);
by ICP, it is approximately $20 (list).
B-373
-------
SILVER
Water Samples
Laboratory Method
Compound CAS Number
Potassium Silver Cyanide 506-61-6
Silver 7440-22-4
Silver Cyanide 506-64-9
Silver Nitrate 7761-88-8
METHOD SUMMARY:
Atomic spectrometric analysis for silver may be used to analyze water
samples for the above silver compounds. A 100-milliliter sample is digested
with nitric acid and hydrogen peroxide, and the digest analyzed by atomic
spectrometry. Low silver concentrations are determined by furnace atomic
absorption spectrometry (AA) or by chelation-extraction AA. The digested
sample is extracted with ammonium pyrrolidinedithiocarbamate in methyl isobutyl
ketone and the extract analyzed by flame AA. Inductively coupled plasma spec-
trometry (ICP) or flame AA is used to analyze higher-concentration samples.
These methods do not identify any specific silver-containing compounds, but
measure the total silver content of the sample.
INTERFERENCES:
Chlorides and sulfates in the sample may interfere. Nickel can be added
to control sulfate interference. For each matrix analyzed, it is necessary to
determine if matrix effects and/or interferences require standard addition or
serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are EPA-approved for
Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
The detection limit is 10 microgams per liter for direct flame AA, the sensiti-
vity is 60 micrograms per liter, and the optimum concentration range is 0.1 to
4 milligrams per liter (APHA). The chelation-extraction AA method is applicable
in the range from 1 to 10 micrograms silver per liter (ASTM). Precision and
accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
B-374
-------
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 272.1, 272.2; EPA-600/4-79-020, U.S. EPA: Washington, 1979.
Federal Register, 44_(233), December 3, 1979. pp. 69559-69564.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055. U.S.
EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 3040, 3050, 6010, 7740:
SW-846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 303A, 303B; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Methods D3866(A), D3866(B), D3866(C): ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by furnace AA is approximately $18-50 (list):
by ICP, it is approximately $10 (list).
B-375
-------
SODIUM
Air Samples
Laboratory Method 1
Compound
Sodium Arsenate
Sodium Arsenite
Sodium Azide
Sodium Bifluoride
Sodium Bisulfite
Sodium Chromate
Sodium Cyanide
Sodium Bichromate
Sodium Dodecylbenzene
Sulfonate
Sodium Fluoride
Sodium Hydrosulfide
Sodium Hydroxide
Sodium Hypochlorite
CAS Number
7631-89-2
7784-46-5
26628-22-8
1333-83-1
7631-90-5
7775-11-3
143-33-9
10588-01-9
25155-30-0
7681-49-4
16721-80-5
1310-73-2
7681-52-9
10022-70-5
Compound
Sodium Methylate
Sodium Nitrite
Sodium Phosphate, Dibasic
Sodium Phosphate, Tribasic
Sodium Selenite
CAS Number
124-
7632-
7558-
10039-
10028-
10140-
7601-
7785-
10101-
10361-
7758-
10124-
10102-
7782-
•41-4
•00-0
•79-4
•32-4
•24-7
65-5
54-9
84-4
89-0
89-4
29-4
56-8
18-8
82-3
METHOD SUMMARY:
Analysis of air samples for the above sodium compounds can be performed by
atomic absorption (AA) spectrometric analysis for sodium. Samples are
collected with cellulose ester membrane filters. The filter and the particu-
lates are digested with nitric acid, the digest is diluted and analyzed by AA.
This method does not differentiate between sodium-containing compounds, but
measures the total sodium content of the sample.
INTERFERENCES:
Cesium should be added to samples and standards to control ionization
interference. The method of standard addition and/or background monitoring
may be needed to correct for interferences.
QUALITY CONTROL:
A minimum of 1 filter blank for every 10 filter samples must be analyzed.
Standard solutions should match the sample matrix as closely as possible.
Standards should be analyzed in duplicate. Precision information is furnished.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 2.1 to 42
micrograms per cubic meter in a 240-liter sample of air. Precision information
is furnished.
B-376
-------
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1: Method 173,; Publication No. 77-157-A, U.S. DREW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-377
-------
SODIUM
Air Samples
Laboratory Method 2
Compound
Sodium Arsenate
Sodium Arsenite
Sodium Azide
Sodium Bifluoride
Sodium Bisulfite
Sodium Chromate
Sodium Cyanide
Sodium Bichromate
Sodium Dodecylbenzene
Sulfonate
Sodium Fluoride
Sodium Hydrosulfide
Sodium Hydroxide
Sodium Hypochlorite
METHOD SUMMARY:
CAS Number
7631-89-2
7784-46-5
26628-22-8
1333-83-1
7631-90-5
7775-11-3
143-33-9
10588-01-9
25155-30-0
7681-49-4
16721-80-5
1310-73-2
7681-52-9
10022-70-5
Compound
Sodium Methylate
Sodium Nitrite
Sodium Phosphate, Dibasic
Sodium Phosphate, Tribasic
CAS Number
Sodium Selenite
124-
7632-
7558-
10039-
10028-
10140-
7601-
7785-
10101-
10361-
7758-
10124-
10102-
7782-
-41-4
•00-0
•79-4
•32-4
•24-7
•65-5
•54-9
•84-4
•89-0
89-4
29-4
56-8
18-8
82-3
Analysis for sodium ions from the above compounds in air may be performed
by inductively coupled plasma atomic emission spectroscopic (ICP) analysis for
sodium. A known volume of air is drawn through a cellulose ester membrane
filter. The filter and the particulates are ashed with a mixture of nitric and
perchloric acids and the digest analyzed by ICP. The method does not identify
any sodium-containing compound, but measures the total sodium content of the
sample.
INTERFERENCES;
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
sodium per cubic meter for a 500-liter sample. Limited precision and accuracy
information is furnished.
B-378
-------
REFERENCE;
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods. Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-379
-------
SODIUM
Soil/Sediment Samples
Laboratory Method
Compound
Sodium
Sodium Arsenate
Sodium Arsenite
Sodium Azide
Sodium Bifluoride
Sodium Bisulfite
Sodium Chromate
Sodium Cyanide
Sodium Bichromate
Sodium Dodecylbenzene
Sulfonate
Sodium Fluoride
Sodium Hydrosulfide
Sodium Hydroxide
Sodium Hypochlorite
METHOD SUMMARY:
CAS Number
7440-
7631
7784'
26628
1333-
7631
7775
143
10588
25155
-23-5
-89-2
-46-5
-22-8
-83-1
-90-5
-11-3
-33-9
-01-9
-30-0
Compound
Sodium Methylate
Sodium Nitrite
Sodium Phosphate, Dibasic
Sodium Phosphate, Tribasic
CAS Number
7681-49-4
16721-80-5
1310-73-2
7681-52-9
10022-70-5
Sodium Selenite
124-
7632-
7558-
10039-
10028-
10140-
7601-
7785-
10101-
10361-
7758-
10124-
10102-
7782-
•41-4
-00-0
•79-4
•32-4
•24-7
•65-5
•54-9
•84-4
•89-0
•89-4
•29-4
56-8
18-8
82-3
Atomic emission spectrometric analysis for sodium ions may be used to
analyze soil/sediment samples for the above sodium compounds. A 100-milligram
sample is digested with nitric acid, perchloric acid, hydrofluoric acid, and
boric acid, and analyzed. Samples should be stored in polyurethane bags and
frozen immediately after collection. This method does not differentiate
between sodium-containing compounds, but measures the total sodium content of
the sample.
INTERFERENCES:
Standard and sample compositions should be closely matched. Solvent
extraction techniques may be necessary. Cesium should be added to samples and
standards to overcome ionization interference.
QUALITY CONTROL:
Quality control procedures are not provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The detection limit of the method is
approximately 100 milligrams of sodium per kilogram. Precision and accuracy
information is furnished.
B-380
-------
REFERENCES:
Environment Canada, Analytical Methods Manual, NAQUADAT No. 19050; Environment
Canada, Inland Waters Directorate, Water Quality Branch: Ottawa, Canada, 1975.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Sodium, Dissolved;" Publication No. AECV81-M1, Alberta Environ-
mental Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-30
(list).
B-381
-------
SODIUM
Water Samples
Laboratory Method
Compound
Sodium
Sodium Arsenate
Sodium Arsenite
Sodium Azide
Sodium Bifluoride
Sodium Bisulfite
Sodium Chromate
Sodium Cyanide
Sodium Bichromate
Sodium Dodecylbenzene
Sulfonate
Sodium Fluoride
Sodium Hydrosulfide
Sodium Hydroxide
Sodium Hypochlorite
CAS Number
7440'
7631-
7784
26628
1333
7631'
7775
143
10588
25155
-23-5
-89-2
-46-5
-22-8
-83-1
-90-5
-11-3
-33-9
-01-9
-30-0
7681-49-4
16721-80-5
1310-73-2
7681-52-9
10022-70-5
Compound
Sodium Methylate
Sodium Nitrite
Sodium Phosphate, Dibasic
Sodium Phosphate, Tribasic
Sodium Selenite
CAS Number
124-
7632-
7558-
10039-
10028-
10140-
7601-
7785-
10101-
10361-
7758-
10124-
10102-
7782-
•41-4
•00-0
•79-4
•32-4
•24-7
•65-5
•54-9
•84-4
•89-0
89-4
29-4
56-8
18-8
82-3
METHOD SUMMARY:
Analysis of water samples for sodium ions from the above compounds can be
performed by flame photometric or atomic absorption (AA) spectrometric analysis
for sodium. Samples should be stored in polyethylene bottles and preserved by
acidification with nitric acid. This method does not identify specific sodium
compounds, but measures the total amount of sodium present in a sample.
INTERFERENCES:
When using flame AA, it may be necessary to add potassium to both standards
and samples to suppress ionization. When using flame photometry, samples
containing particulate matter should be filtered before analysis. Relatively
large amounts of potassium, calcium, chloride, sulfate, and bicarbonate can
interfere. Standards and samples should contain the same amounts of interfering
substances.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
Standards should be analyzed each time a sample or set of samples is analyzed.
EPA/TECHNICAL STATUS:
These methods are approved for the National Pollutant Discharge Elimina-
tion System (NPDES). Precision and accuracy information is furnished. For
flame photometry, the minimum detectable concentration is 0.1 milligrams sodium
B-382
-------
per liter (APHA), and the optimum concentration range is 1 to 100 milligrams
per liter (ASTM). For AA analysis the procedure is applicable over the range
of 0.2 to 3 milligrams sodium per liter (ASTM).
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 273.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. III., Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 14th ed.; APHA: Washington, 1975.
American Society for Testing and Materials, 1983 Annual Book of ASTM
Standards, Vol. 11.01, Method D4191-82; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list).
B-383
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STRONTIUM
Air Samples
Laboratory Method
Compounds CAS Number
Strontium Chromate 7789-06-2
Strontium Sulfide 1314-96-1
METHOD SUMMARY:
Atomic absorption spectrometric (AA) analysis for strontium can be used
for the analysis of air for the above strontium compounds. Samples are
collected by passage of a known volume of air through a cellulose ester mem-
brane filter. The filter and the particulates are digested with nitric acid,
and the resulting solution is diluted and analyzed by AA. This method does not
identify any specific strontium-containing compound, but measures the total
strontium content of the sample.
INTERFERENCES:
Cesium should be added to samples and standards to control ionization
interference, and lanthanum should be added as a releasing agent. The method
of standard additions and/or background correction may be needed to correct for
interferences.
QUALITY CONTROL:
A minimum of 1 filter blank for every 10 filter samples must be analyzed.
Standard solutions should match the sample matrix as closely as possible.
Standards should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 21 to 210
micrograms strontium per cubic meter for a 240-liter air sample. Precision
information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300 Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
B-384
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Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. III., Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-385
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STRONTIUM
Soil/Sediment Samples
Laboratory Method
Compounds CAS Number
Strontium Chromate 7789-06-2
Strontium Sulfide 1314-96-1
METHOD SUMMARY:
Analysis of soil/sediment samples for the above strontium compounds can be
performed by atomic absorption (AA) spectrometric analysis for strontium. A
100-milligram sample is digested with nitric acid, perchloric acid, hydrogen
fluoride, and boric acid, and analyzed. Samples should be stored in poly-
urethane bags and frozen immediately after collection. This method does not
identify any specific strontium-containing compounds, but measures the total
strontium content of the sample.
INTERFERENCES:
Standard and sample compositions should be closely matched. Sodium should
be added to both to overcome ionization interference. Solvent extraction
techniques may be necessary to improve the detection limit.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved• Precision and accuracy information is
furnished. The detection limit of this method is approximately 20 milligrams
per kilogram.
REFERENCES:
Environment Canada, Analytical Methods Manual, NAQUADAT No. 38050;
Environment Canada, Inland Waters Directorate, Water Quality Branch: Ottawa,
Canada, 1975.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-30
(list).
B-386
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STRONTIUM
Water Samples
Laboratory Method
Compounds CAS Number
Strontium Chromate 7789-06-2
Strontium Sulfide 1314-96-1
METHOD SUMMARY:
Analysis of water samples for the above strontium compounds can be per-
formed by atomic absorption (AA) spectrometric analysis for strontium. The
sample is filtered through a 0.45-micron membrane filter, a lanthanum
chloride/potassium chloride solution is added, and the resulting solution is
analyzed for strontium by AA. This method measures the total dissolved
strontium content of the sample, and does not identify any specific strontium-
containing compounds.
QUALITY CONTROL:
No quality control procedures are given.
INTERFERENCES:
Chemical interferences by silicon, aluminum, and phosphate are controlled
by the addition of lanthanum chloride. lonization suppression can be con-
trolled by the addition of potassium chloride.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable over the range
of 0.1 to 5 milligrams strontium per liter. For brackish water, sea water, and
brines, the method is applicable to the range 5 to 2000 milligrams per liter.
Precision and accuracy information is furnished.
REFERENCES:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Method D3920-80; ASTM: Philadelphia, 1983.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02 D3352074; ASTM: Philadelphia, 1983.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
B-387
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list).
B-388
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SULFATES (PARTICULATE)
Air Samples
Laboratory Method
Compound CAS Number
Aluminum Sulfate 10043-01-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Ferric Sulfate 10028-22-5
Ferrous Ammonium Sulfate 10045-89-3
Ferrous Sulfate 7720-78-7
7782-63-0
Mercuric Sulfate 7783-35-9
Nickel Sulfate 7786-81-4
Thallium(I) Sulfate 7446-18-6
Vanadyl Sulfate 27774-13-6
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of air samples for the above sulfates can be performed by colori-
metric analysis for sulfate ion. A known volume of air is passed through a
glass-fiber filter, using a high-volume sampler. Sulfate is extracted with hot
water. The resulting solution is allowed to react with an acidic color reagent
containing methylthymol blue and barium chloride, producing barium sulfate. The
pH of the mixture is adjusted to 12 to 13, and the remaining barium is complexed
with the methylthymol blue. The uncomplexed methylthymol blue, which is
equimolar to the sulfate removed as barium sulfate, is determined by measuring
its absorbance at 460 nm. This method is intended to be used with an automated
system. This method does not identify the specific sulfate-containing com-
pounds present, but measures the total sulfate content of the sample.
INTERFERENCES:
Interfering cations are removed by passing the sample through an ion-
exchange column.
QUALITY CONTROL:
A baseline should be determined with all reagents, feeding distilled water
through the sample line.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Single-laboratory precision and accuracy
information is furnished.
B-389
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REFERENCE;
Alberta Environmental Centre, Methods Manual for Chemical Analysis of
Atmospheric Pollutants, Method No. 25556; Alberta Environmental Centre: Alberta,
Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $45-60
(list).
B-390
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SULFATES
Water Samples
Laboratory Method 1
Compound CAS Number
Aluminum Sulfate 10043-01-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Ferric Sulfate 10028-22-5
Ferrous Ammonium Sulfate 10045-89-3
Ferrous Sulfate 7720-78-7
7782-63-0
Mercuric Sulfate 7783-35-9
Nickel Sulfate 7786-81-4
Thallium(I) Sulfate 7446-18-6
Vanadyl Sulfate 27774-13-6
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of water samples for the above sulfates can be performed by
determination of the sulfate ion concentration by gravimetric, turbidimetric,
or volumetric procedures. The gravimetric procedure is performed by addition
of barium chloride to the sample and gravimetric measurement of the precipit-
ated barium sulfate. The turbidimetric procedure involves addition of barium
chloride and glycerin to form a barium sulfate suspension and turbidimetric
analysis of it. The volumetric procedure involves titration of sulfate ion in
an acidic alcoholic solution with barium chloride, using thorin as the indi-
cator. For brackish water, sea water, and brines, the turbidimetric method,
with adjustment of the ionic strength to 2 molal, is used.
INTERFERENCES:
Both cations and anions can cause errors in barium sulfate precipitation;
potassium, iron, aluminum, phosphate, fluoride, and nitrate are common
interferences. Most metal ions interfere seriously with the volumetric
determination because of metal-thorin complex formation. Cation interferences
may be removed by use of cation-exchange resin. The effects of sulfite inter-
ferences can be eliminated in calculations. Sulfides are precipitated as zinc
sulfide. Chromate and dichromate ions are removed by treatment with hydrogen
peroxide to form trivalent chromium, followed by removal with cation-exchange
resin.
QUALITY CONTROL:
No quality control procedures are provided.
B-391
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EPA/TECHNICAL STATUS:
These methods are not EPA-approved. The gravimetric method is applicable
to samples containing 20 to 100 milligrams sulfate ion per liter. The
turbidimetric and volumetric methods are useful in the range of 10 to 100 and 5
to 1000 milligrams sulfate ion per liter, respectively. Precision and accuracy
information is furnished.
REFERENCES:
American Society for Testing and Material, 1983 Annual Book of ASTM Standards,
Vol 11.01, Methods D516-82(A), D516-92(B), D516-82(C); ASTM: Philadelphia,
1983.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D4130-82; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by the volumetric method is approximately
$20-30 (list).
B-392
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SULFATES
Water Samples
Laboratory Method 2
Compound CAS Number
Aluminum Sulfate 10043-01-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Ferric Sulfate 10028-22-5
Ferrous Ammonium Sulfate 10045-89-3
Ferrous Sulfate 7720-78-7
7782-63-0
Mercuric Sulfate 7783-35-9
Nickel Sulfate 7786-81-4
Thallium(I) Sulfate 7446-18-6
Vanadyl Sulfate 27774-13-6
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of water samples for the above sulfates can be performed by
precipitation and colorimetry. A sample is treated with barium chloride to
precipitate barium sulfate, and methylthymol blue indicator is added to form a
blue complex with any unprecipitated barium. The intensity of the color of the
barium-methylthymol blue complex is measured and compared with that of stan-
dards. This method does not identify any specific sulfate salts, but measures
the total dissolved sulfate concentration of the sample.
INTERFERENCES:
Cations, such as calcium, aluminum, and iron, that complex methylthymol
blue, are removed by passage of the sample through an ion-exchange column.
QUALITY CONTROL:
Duplicate and fortified samples should be processed as part of a quality
assurance program.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is suitable for use over the
range 5 to 300 milligrams sulfate per liter. Precision and accuracy informa-
tion is furnished.
B-393
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REFERENCE:
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Sulphate, Dissolved;" Publication No. AECV81-M1, Alberta Environ-
mental Centre, Vegreville, Alberta, Canada, 1981.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $30-35
(list).
B-394
-------
SULFIDES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Ammonium Sulfide 12135-76-1
Arsenic Disulfide 1303-32-8
Arsenic Trisulfide 1303-33-9
Hydrogen Sulfide 7783-06-4
Lead Sulfide 1314-87-0
Phosphorus Pentasulfide 1314-80-3
Selenium Disulfide 7488-56-4
Sodium Hydrosulfide 16721-80-5
Strontium Sulfide 1314-96-1
METHOD SUMMARY:
The determination of the above sulfides in a 1-gram soil/sediment sample
can be performed by colorimetric analysis for sulfide ions. The hydrogen
sulfide is distilled from the acidified solution into a trap containing cadmium
nitrate. When zinc acetate, dimethyl-p_-diphenylenediamine, and ferric chloride
are added to the distillate, methylene blue is formed. The intensity of the
resulting color is measured spectrophotometrically at 670 nm. This method
measures the total sulfide concentration in the sample and does not identify
specific sulfide compounds.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
One distilled water blank, one spiked sample, and one duplicate should be
analyzed with each set of ten samples.
EPA/TECHNICAL STATUS:
This method is in use in the CERCLA program. No precision or accuracy
information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Method 9030; SW-846, U.S. EPA: Washington, 1982.
B-395
-------
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Methods, "Methods for the Determination of
Sulfide," pp. IV-136 to IV-155; EPA-600/S4-84-038, U.S. Environmental Protec-
tion Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $38-60
(list).
B-396
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SULFIDES
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Sulfide 12135-76-1
Arsenic Trisulfide 1303-33-9
Hydrogen Sulfide 7783-06-4
Phosphorus Pentasulfide 1314-80-3
Sodium Hydrosulfide 16721-80-5
Strontium Sulfide 1314-96-1
METHOD SUMMARY:
Analysis of water samples for sulfide ions from the above compounds can be
performed by titrimetric or colorimetric determination of sulfide ions. In the
titrimetric analysis, a 200-milliliter sample is analyzed by the addition of
excess iodine and back-titration with sodium thiosulfate or phenylarsine oxide,
using starch as an indicator. For colorimetric analysis, a 7,5-milliliter
sample is combined with dimethyl-£-phenylenediamine and ferric chloride and
analyzed colorimetrically. Both methods measure the total sulfide content of
the sample and do not identify specific sulfide-containing compounds.
INTERFERENCES:
Samples must be taken with a minimum of aeration, and all water used must
be free of dissolved oxygen. If the titrimetric analysis is not to be started
immediately, the samples must be preserved with zinc acetate. Samples contain-
ing volatile iodine-consuming substances and reduced sulfur compounds may
require background correction for titrimetric analysis; acid-insoluble sulfides
and sulfide concentrations below 1 milligram/liter cannot be determined by this
method. For coloriraetric analysis, all water used should contain no dissolved
oxygen; acid-insoluble sulfides cannot be determined by this method. Color and
turbidity in the samples may interfere with colorimetry.
QUALITY CONTROL:
A blank should be processed with each set of samples, and a check standard
should be analyzed with each 10 samples. Ten percent of the samples should be
processed in duplicate, and fortified samples or standard reference materials
should be processed periodically.
EPA/TECHNICAL STATUS:
Both methods are in use in the CERCLA program and are approved for use in
Clean Water Act analyses. The titrimetric method is EPA-approved for use under
the Resource Conservation and Recovery Act (RCRA). The colorimetric method is
suitable over the range 0.02 to 20 milligrams sulfide per liter (Alberta
Environment). Precision and accuracy information is furnished.
B-397
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REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes. Methods 376.1, 376.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Method 9030; SW-846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Sulfide," pp. IV-136 to IV-155; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Sulphide, Total;" Publication No. AECV81-M1, Alberta Environ-
mental Centre, Vegreville, Alberta, Canada, 1981.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 427C, 427D; APHA: Washington, 1980.
COST INFORMATION:
Cost per sample for analysis by these methods is approximately $20-30
(list).
B-398
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SULFITES
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Bisulfite 10192-30-0
Ammonium Sulfite 10196-04-0
Sodium Bisulfite 7361-90-5
Zinc Hydrosulfite 7779-86-4
METHOD SUMMARY:
Analysis of water samples for the above sulfite compounds may be performed
by titration of sulfite ions. A 50-milliliter sample is mixed with 3 to 4
drops of phenolphthalein indicator and approximately 1 gram of starch indicator
to discharge the red color produced by phenolphthalein. The resulting solution
is titrated with a potassium iodide-iodate reagent. This method determines the
amount of sulfite ion present, and does not differentiate between various
sulfite-containing compounds.
INTERFERENCES:
Contact of the sample with air must be minimized, and the temperature must
be kept below 50°C. Other oxidizable substances, nitrite, copper, and heavy
metals may interfere.
QUALITY CONTROL:
A reagent blank must be analyzed periodically.
EPA/TECHNICAL STATUS;
This method is approved for the National Pollutant Discharge Elimination
System (NPDES) of the Clean Water Act. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 377.1: EPA-600/4-79-020, U.S. EPA: Washington, 1979.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 428; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, D1339-78; ASTM: Philadelphia, 1983.
B-399
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list).
B-400
-------
SULFUR COMPOUNDS (PARTICULATE)
Air Samples
Laboratory Method
Compound CAS Number
Ammonium Sulfamate 7773-06-0
Ammonium Sulfide 12135-76-1
Ammonium Sulfite 10196-04-0
Ammonium Thiosulfate 7783-18-8
Arsenic Disulfide 1303-32-8
Arsenic Trisulfide 1303-33-9
Chromic Sulfate 10101-53-8
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Ferric Sulfate 10028-22-5
Ferrous Ammonium Sulfate 10045-89-3
Ferrous Sulfate 7720-78-7
7782-63-0
Phosphorus Pentasulfide 1314-80-3
Selenium Disulfide 7488-56-4
Sodium Hydrosulfide 16721-80-5
Strontium Sulfide 1314-96-1
Thallium Sulfate 7446-18-6
Vanadyl Sulfate 27774-13-6
Zinc Hydrosulfite 7779-86-4
Zinc Sulfate 7733-02-0
Zirconium Sulfate 14644-61-2
METHOD SUMMARY:
Analysis for the above particulate sulfur compounds in air can be per-
formed by filtration of air and analysis of the filter media for sulfur by
X-ray fluorescence spectrometry- The technique is non-destructive, so further
analyses can be carried out on the material retained by the filter if desired.
This method measures the total amount of sulfur in the sample and does not
identify any specific sulfur-containing compound.
INTERFERENCES:
Some sulfide or hydrosulfide compounds can react with water during sampling
under humid conditions to form hydrogen sulfide, which may be lost from the
filter medium. Sulfates, sulfamates, sulfites, and thiosulfates will not be
lost under these conditions.
QUALITY CONTROL:
No quality control procedures are given,
B-401
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EPA/TECHNICAL STATUS:
The method is not EPA-approved. Precision information is furnished. This
method can detect concentrations of sulfur greater than 0.01 to 50 micrograms
per cubic meter of air.
REFERENCES:
Rhodes, J. R.; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.: Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927-
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
$20 (bid), plus sampling costs.
B-402
-------
THALLIUM
Air Samples
Laboratory Method 1
Compound CAS Number
Thallic Oxide 1314-32-5
Thallium 7440-28-0
Thallium(I) Acetate 563-68-8
Thallium(I) Carbonate 6533-73-9
Thallium(I) Chloride 7791-12-0
Thallium(I) Nitrate 10102-45-1
Thallium(I) Selenide 12039-52-0
Thallium(I) Sulfate 7446-18-6
METHOD SUMMARY:
Analysis for the above soluble thallium compounds in air samples can be
performed by high-volume filtration of air followed by atomic absorption (AA)
analysis for thallium. A known volume of air is passed through a cellulose
ester membrane filter, the filter is wet-ashed, and the resulting solution is
analyzed by AA for thallium. This method measures the total thallium content
of the air sampled and does not identify the specific thallium compounds
present.
INTERFERENCES:
The presence of insoluble thallium compounds will interfere.
QUALITY CONTROL;
The analyte recovery should be determined in duplicate and, if less than
95 percent, results should be corrected appropriately. Duplicate determinations
should agree within 5 percent.
EPA/TECHNICAL STATUS:
Method S306 is approved by the National Institute of Occupational Safety
and Health (NIOSH), and has been validated over the range of 0.034 to 0.15
milligrams thallium per cubic meter for a 540-liter sample. Precision and
accuracy information is furnished. NIOSH method P&CAM 173, classified as
operational, is for use over the range of 0.2 to 0.84 milligrams thallium per
cubic meter in a 240-liter sample. Precision information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set U, Method S306; PB-262 405 (NTIS), U.S. DHEW: Cincinnati, December 1976.
B-403
-------
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-404
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THALLIUM
Air Samples
Laboratory Method 2
Compound
Thallic Oxide
Thallium
Thallium(I)
Thallium(I)
Thalliura(T)
Thallium(I)
Thallium(I)
Thallium(I)
Acetate
Carbonate
Chloride
Nitrate
Selenide
Sulfate
CAS Number
1314-32-5
7440-28-0
563-68-8
6533-73-9
7791-12-0
10102-45-1
12039-52-0
7446-18-6
METHOD SUMMARY:
Analysis for the above thallium-containing compounds in air may be per-
formed by inductively coupled plasma atomic emission spectroscopic (ICP)
analysis for thallium. A known volume of air is drawn through a cellulose
ester membrane filter. The filter is ashed with a mixture of nitric and per-
chloric acids followed by analysis of the digest by ICP- The method does not
identify any specific thallium-containing compound, but measures the total
thallium content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
thallium per cubic meter for a 500-liter sample. Limited precision and
accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cinncinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list) ,
plus sampling costs.
B-405
-------
THALLIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Thallic Oxide 1314-32-5
Thallium 7440-28-0
Thallium(I) Acetate 563-68-8
Thallium(I) Carbonate 6533-73-9
Thallium(I) Chloride 7791-12-0
Thallium(I) Nitrate 10102-45-1
Thallium(I) Selenide 12039-52-0
Thallium(I) Sulfate 7446-18-6
METHOD SUMMARY:
Analysis of soil/sediment samples for the above thallium compounds can be
performed by atomic spectrometric analysis for thallium. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and analyzed by atomic spec-
trometry. For low concentrations, furnace atomic absorption spectrometry (AA)
is used, while flame AA is used for higher-concentration samples. These
methods do not identify any specific thallium-containing compounds, but measure
the total thallium content of the sample.
INTERFERENCES;
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for
analyses for the Clean Water Act. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 279.1, 279.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
B-406
-------
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 7480, 7481; SW-846, U.S. EPA:
Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by furnace AA is approximately $28-60 (list):
by flame AA, it is approximately $20-30 (list).
B-407
-------
THALLIUM
Water Samples
Laboratory Method
Compound CAS Number
Thallic Oxide 1314-32-5
Thallium 7440-28-0
Thallium (1) Acetate 563-68-8
Thallium (I) Carbonate 6533-73-9
Thallium (I) Chloride 7791-12-0
Thallium (I) Nitrate 10102-45-1
Thallium (I) Selenide 12039-52-0
Thallium (I) Sulfate 7446-18-6
METHOD SUMMARY:
Atomic spectrometric analysis for thallium can be used to measure the
above thallium compounds in water samples. A 100-milliliter sample is digested
with nitric acid and hydrogen peroxide and analyzed by atomic spectrometry.
For low concentrations, furnace atomic absorption spectrometry (AA) is used,
while flame AA is used for higher-concentration samples. These methods do not
identify any specific thallium-containing compounds, but measure the total
thallium content of the sample.
INTERFERENCES:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use
under the Clean Water Act. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D: Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 279.1, 279.2; EPA-600/4-79-020, U.S. EPA: Cincinnati,
1979.
Federal Register, 44_(233), December 3, 1979, pp. 69559-69564.
B-408
-------
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Methods 7840, 7841; SW-846, U.S. EPA: Washington,
1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption; HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricatng Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., 48(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by furnace AA is approximately $18-50 (list);
by flame AA, it is approximately $10-20 (list).
B-409
-------
THIOCYANATES
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Thiocyanate 1762-95-4
Lead Thiocyanate 592-87-0
Mercuric Thiocyanate 592-85-8
METHOD SUMMARY:
Analysis of water samples for the above thiocyanate-containing compounds
can be performed by colorimetric analysis for thiocyanate ions. The sample is
reacted with ferric nitrate at an acidic pH, and the intensity of the color of
the resulting blood-red iron-thiocyanate complex is measured at 460 nanometers.
This method does not identify any particular thiocyanate-containing compound,
but measures the total thiocyanate content of the sample.
INTERFERENCES:
Various interfering organic compounds can be removed by adsorption on
macroreticular resin prior to analysis. Hexavalent chromium interference is
removed by adjustment of the pH to 2 and addition of ferrous sulfate. Raising
the pH to 9 and filtration removes iron(III) and chromium(III). Reducing
agents are destroyed by addition of hydrogen peroxide. If the sample will be
used for cyanide determination, cadmium or lead salt should be added to remove
sulfide before the pH is raised.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable over the range
0.1 to 2 milligrams thiocyanate ion per liter, and higher concentrations can be
measured by suitable sample dilution. Precision and accuracy information is
furnished.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D4193-82; ASTM: Philadelphia, 198T!
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list).
B-410
-------
URANIUM
Water Samples
Laboratory Method 1
Compound CAS Number
Uranyl Acetate 541-09-3
Uranyl Nitrate 10102-06-4
36478-76-9
METHOD SUMMARY:
Analysis of water samples for the above uranium compounds can be performed
by X-ray fluorescence spectrometry. The water sample is filtered, acidified,
and treated with ultraviolet radiation to decrease subsequent filtering time
and improve recovery of the analyte. The uranium is coprecipitated with an
iron dibenzyldithiocarbamate carrier complex, and the precipitate is collected
by vacuum filtration. The precipitate on the filter is analyzed by wavelength-
dispersive X-ray fluorescence spectrometry. This method does not identify the
specific uranium-containing compounds present, but measures the total uranium
content of the sample.
INTERFERENCES:
The following ions cause no significant interferences at levels below 0.1
grams per liter: chloride, magnesium, calcium, sodium, potassium, and sulfate.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Limited precision and accuracy informa-
tion is furnished. This method is suitable for concentrations of uranium over
0.4 micrograms per liter.
REFERENCE:
Caravajal, G.; Mahan, K.; Leyden, D. "The Determination of Uranium in Natural
Waters at PPB Levels by Thin-Film X-ray Fluorescence Spectrometry after
Coprecipitation with an Iron Dibenzyldithiocarbamate Carrier Complex" Anal.
Chim. Acta., 135, 1982, pp. 205-214.
COST INFORMATION:
No cost information has been obtained.
B-411
-------
URANIUM
Water Samples
Laboratory Method 2
Compound CAS Number
Uranyl Acetate 541-09-3
Uranyl Nitrate 10102-06-4
36478-76-9
METHOD SUMMARY:
Analysis of water samples for the above uranium compounds can be accom-
plished by fluorescence spectrometric analysis for uranium. A nitrogen laser
at 337 nm is used as an excitation source. A chelating agent, Fluran®, is used
to increase fluorescence yield and the solution is buffered to the proper pH.
The method is applicable to continuous monitoring.
INTERFERENCES:
Fluorescence from organic compounds is eliminated by use of time- or
wavelength-discrimination techniques. High levels of carbonate and phosphate
ions interfere, but chloride and sulfate do not.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved for any regulatory program. No precision
and accuracy information is furnished.
REFERENCE:
Campen, W.; Bachmann, K. "Laser-Induced Fluorescence for the Direct Determina-
tion of Small Concentrations of Uranium in Water" Mikrochimica Acta Wein, II,
1979, pp. 159-170. ~~
COST INFORMATION:
No cost information has been obtained.
B-412
-------
VANADIUM
Air Samples
Laboratory Method 1
Compound CAS Number
Ammonium Vanadate 7803-55-6
Vanadium Pentoxide 1314-62-1
Vanadyl Sulfate 27774-13-6
METHOD SUMMARY:
Analysis for the above particulate vanadium compounds in air samples may
be performed by flame atomic absorption (AA) spectrometric determination of
vanadium. A known volume of air is drawn through a membrane or glass-fiber
filter. The filter with the collected particulates is digested with nitric or
nitric and hydrofluoric acids, and an aliquot of the resulting solution is
analyzed by AA, applying either direct aspiration or cupferron/butyl acetate
extraction techniques. This method does not identify any specific vanadium
compounds, but measures the total vanadium present in the sample.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
A blank should be processed with every 10 samples. Standard solutions
should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 420 to 6300
micrograms per cubic meter, using a 240-liter air sample. Precision informa-
tion is furnished. APHA has determined the detection limit to be 0.2 micro-
grams per cubic meter of air, using a 2000-cubic-meter sample.
REFERENCES:
U.S. Department of Health, Education and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
B-413
-------
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals'
by Atomic Absorption; HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23545; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
American Public Health Service, Methods of Air Sampling and Analysis, 2nd ed.,
Method 321; APHA: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20 (list),
or $55-65 if the extraction technique is used, plus sampling costs.
B-414
-------
VANADIUM
Air Samples
Laboratory Method 2
Compound CAS Number
Ammonium Vanadate 7803-55-6
Vanadium Pentoxide 1314-62-1
Vanadyl Sulfate 27774-13-6
METHOD SUMMARY:
Analysis for the above vanadium-containing compounds in air may be per-
formed by inductively coupled plasma atomic emission spectrometric (ICP)
analysis for vanadium. A known volume of air is drawn through a cellulose
ester membrane filter. The filter is ashed with a mixture of nitric and per-
chloric acids and the digest analyzed by ICP. The method does not identify any
specific vanadium-containing compound, but measures the total vanadium content
of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
vanadium per cubic meter, using a 500-liter sample. Limited precision and
accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list).
plus sampling costs.
B-415
-------
VANADIUM
Soil/Sediment Samples
Laboratory Method
Compound
Ammonium Vanadate
Vanadium Pentoxide
Vanadyl Sulfate
CAS Number
7803-55-6
1314-62-1
27774-13-6
METHOD SUMMARY:
Analysis of soil/sediment samples for the above vanadium compounds can be
performed by atomic spectrometric analysis for vanadium. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and the digest analyzed by
inductively coupled plasma (ICP) or flame atomic absorption (AA) spectrometry.
Analysis for vanadium in oily samples may be performed using ICP after sample
dilution with methyl isobutyl ketone (MIBK) or xylene, using standards miscible
with these solvents. These methods measure total vanadium present in the sample
and do not differentiate between compounds of vanadium.
INTERFERENCES:
The addition of aluminum (1000 milligrams per liter) to both standards and
samples will control interferences caused by high concentrations of aluminum
and titanium in the sample. For each matrix analyzed, it is necessary to
determine if matrix effects and/or interferences require standard addition or
serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use
under the Clean Water Act. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 286.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Federal Register. 44(233), December 3, 1979, pp. 69559-69564.
B-416
-------
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy." pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Methods 7840, 7841; SW-846, U.S. EPA: Washington,
1982.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N. ; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem. , 48^(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $20-30 (list):
by ICP, it is approximately $20 (list).
B-417
-------
VANADIUM
Water Samples
Laboratory Method 1
Compound CAS Number
Ammonium Vanadate 7803-55-6
Vanadium Pentoxide 1314-62-1
Vanadyl Sulfate 27774-13-6
METHOD SUMMARY:
Analysis of water samples for the above vanadium compounds can be per-
formed by atomic spectrometric analysis for vanadium. A 100-milliliter sample
is digested with nitric acid and hydrogen peroxide and the digest analyzed by
inductively coupled plasma (ICP) atomic spectrometry or by flame or furnace
atomic absorption spectrometry (AA). These methods do not differentiate
between various vanadium-containing compounds, but measure the total vanadium
content of the sample.
INTERFERENCES:
The addition of aluminum (1000 milligrams per liter) to both standards and
samples will control interferences caused by high concentrations of aluminum
and titanium in the sample. For each matrix analyzed, it is necessary to
determine if matrix effects and/or interferences require standard addition or
serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are EPA-approved for
analyses under the Clean Water Act and the Resource Conservation and Recovery
Act (RCRA). No precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 286.1, 286.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Federal Register. 44(233), December 3, 1979, pp. 69559-69564.
B-418
-------
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Cincinnati, December 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Methods 7840, 7841; SW-846, U.S. EPA: Washington,
1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 303C; APHA: Washington, 1980.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list);
for ICP, it is approximately $10 (list).
B-419
-------
VANADIUM
Water Samples
Laboratory Method 2
Compound CAS Number
Ammonium Vanadate 7803-55-6
Vanadium Pentoxide 1314-62-1
Vanadyl Sulfate 27774-13-6
METHOD SUMMARY:
Analysis of water samples for the above vanadium-containing compounds can
be performed by reaction-kinetic analysis for vanadium. Measurement of the
rate of the oxidation of gallic acid by the persulfate ion in acid solution,
which is proportional to the vanadium concentration, is performed by monitoring
the absorbance of the solution at 415 nanometers on a spectrophotometer. The
concentration of vanadium is quantified by use of a calibration curve. This
method does not identify any specific vanadium-containing compound, but
measures the total vanadium content of the sample.
INTERFERENCES:
Copper, iron, and, to a lesser degree, chromium, cobalt, molybdenum,
nickel, silver, and uranium interfere. Chloride and traces of bromide and
iodide interfere seriously, and these anions can be complexed with mercuric
ion.
QUALITY CONTROL;
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable in the range
from 1 to 100 micrograms vanadium per liter. Precision and accuracy informa-
tion is furnished.
REFERENCES:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, D3373-80; ASTM: Philadelphia, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 327B; APHA: Washington, 1980.
COST INFORMATION:
No cost information has been obtained.
B-420
-------
ZINC
Air Samples
Laboratory Method 1
Compound CAS Number
Zinc 7440-66-6
Zinc Acetate 557-34-6
Zinc Ammonium Chloride 14639-97-5
14639-98-6
52628-25-8
Zinc Borate 1332-07-6
Zinc Bromide 7699-45-8
Zinc Carbonate 3486-35-9
Zinc Chloride 7646-85-7
Zinc Cyanide 557-21-1
Zinc Fluoride 7783-49-5
Zinc Formate 557-41-5
Zinc Hydrosulfite 7779-86-4
Zinc Nitrate 7779-88-6
Zinc Phenolsulfonate 127-82-2
Zinc Phosphide 1314-84-7
Zinc Silicofluoride 16871-71-9
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of air samples for the above zinc compounds can be performed by
filtration of air and analysis of the filter deposit by X-ray fluorescence
spectrometry. The method is non-destructive, so that further analyses may be
performed on samples. The sample-collection time may be up to 8 hours, but
analysis time is approximately 1 minute. The method measures total zinc
present in the sample and does not identify any specific zinc compounds.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-
fiber filters are acceptable for use only if they are of the highest purity.
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is given. The
method should be applicable to concentrations above 0.001 micrograms of zinc
per cubic meter, depending on sample size, when at least 40 micrograms of
zinc are collected.
B-421
-------
REFERENCES:
Rhodes, J. R.; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L,
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., £(10), 1972, pp. 922-927.
COST INFORMATION:
Cost per sample for analysis by this method is $30 (list), $20 (bid),
plus sampling costs.
B-422
-------
ZINC
Air Samples
Laboratory Method 2
Compound CAS Number
Zinc 7440-66-6
Zinc Acetate 557-34-6
Zinc Ammonium Chloride 14639-97-5
14639-98-6
52628-25-8
Zinc Borate 1332-07-6
Zinc Bromide 7699-45-8
Zinc Carbonate 3486-35-9
Zinc Chloride 7646-85-7
Zinc Cyanide 557-21-1
Zinc Fluoride 7783-49-5
Zinc Formate 557-41-5
Zinc Hydrosulfite 7779-86-4
Zinc Nitrate 7779-88-6
Zinc Phenolsulfonate 127-82-2
Zinc Phosphide 1314-84-7
Zinc Silicofluoride 16871-71-9
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis for the above zinc-containing compounds in air may be performed
by inductively coupled plasma (ICP) or atomic absorption (AA) spectroscopic
analysis for zinc. A known volume of air is drawn through a cellulose ester
membrane filter. The filter is ashed with a mixture of nitric and perchloric
acids and the digest analyzed by ICP or AA spectrometric methods. The method
does not identify any specific zinc-containing compound, but measures the total
zinc content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
The AA method is not EPA-approved. The ICP method has been proposed by
the National Institute for Occupational Safety and Health (NIOSH) for use over
the range of 5 to 2000 micrograms zinc per cubic meter for a 500-liter sample.
Limited precision and accuracy information is furnished.
B-423
-------
REFERENCES:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS: Cincinnati,
August 1981.
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Method 322; APHA: Washington, 1977-
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list),
plus sampling costs: by ICP, it is approximately $10 (list), plus sampling
costs .
B-424
-------
ZINC
Air Samples
Laboratory Method 3
Compound CAS Number
Zinc 7440-66-6
Zinc Acetate 557-34-6
Zinc Ammonium Chloride 14639-97-5
14639-98-6
52628-25-8
Zinc Borate 1332-07-6
Zinc Bromide 7699-45-8
Zinc Carbonate 3486-35-9
Zinc Chloride 7646-85-7
Zinc Cyanide 557-21-1
Zinc Fluoride 7783-49-5
Zinc Formate 557-41-5
Zinc Hydrosulfite 7779-86-4
Zinc Nitrate 7779-88-6
Zinc Phenolsulfonate 127-82-2
Zinc Phosphide 1314-84-7
Zinc Silicofluoride 16871-71-9
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis for the above particulate zinc compounds in air samples may be
performed by flame atomic absorption (AA) spectrometric determination of zinc.
A known volume of air is drawn through a membrane or glass-fiber filter. The
filter with the collected particulates is digested with nitric or nitric and
hydrofluoric acids, and an aliquot of the solution containing the analyte is
analyzed by AA, applying either direct aspiration or cupferron/butyl acetate
extraction techniques. This method does not identify any specific zinc com-
pounds, but measures the total zinc present in the sample.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
A blank should be processed with every 10 samples. Standard solutions
should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 4.2 to 42
micrograms per cubic meter in a 240-liter air sample. Precision information
B-425
-------
is furnished. Alberta Environment has determined the detection limit to be
0.01 micrograms per cubic meter of air.
REFERENCES;
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23545; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-426
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ZINC
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Zinc 7440-66-6
Zinc Acetate 557-34-6
Zinc Ammonium Chloride 14639-97-5
14639-98-6
52628-25-8
Zinc Borate 1332-07-6
Zinc Bromide 7699-45-8
Zinc Carbonate 3486-35-9
Zinc Chloride 7646-85-7
Zinc Cyanide 557-21-1
Zinc Fluoride 7783-49-5
Zinc Formate 557-41-5
Zinc Hydrosulfite 7779-86-4
Zinc Nitrate 7779-88-6
Zinc Phenolsulfonate 127-82-2
Zinc Phosphide 1314-84-7
Zinc Silicofluoride 16871-71-9
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of soil/sediment samples for the above zinc compounds can be
performed by atomic spectrometric analysis for zinc. A 2-gram solid sample is
digested with nitric acid and hydrogen peroxide and analyzed by inductively
coupled plasma (ICP) or flame atomic absorption spectrometry (AA). Analysis
for zinc in oily samples may be performed by ICP after sample dilution with
methyl isobutyl ketone (MIBK) or xylene, using standards miscible with these
solvents. These methods do not identify any specific zinc-containing com-
pounds, but measure the total zinc content of the sample.
INTERFERENCES:
High levels of silicon in the sample may cause interference when using AA.
The use of polypropylene sample container caps is recommended to avoid possible
contamination by sample container cap liners. For each matrix analyzed, it is
necessary to determine if matrix effects and/or interferences require standard
addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed routinely, and at least 10 percent
of the analyses should be duplicates and/or standards.
B-427
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EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are EPA-approved for
analyses under the Clean Water Act. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 286.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Federal Register, 44_(233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Methods 7950, 7951; SW-846, U.S. EPA: Washington,
1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., 48_(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $20-30 (list);
by ICP, it is approximately $20 (list).
B-428
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ZINC
Water Samples
Laboratory Method 1
Compound CAS Number
Zinc 7440-66-6
Zinc Acetate 557-34-6
Zinc Ammonium Chloride 14639-97-5
14639-98-6
52628-25-8
Zinc Borate 1332-07-6
Zinc Bromide 7699-45-8
Zinc Carbonate 3486-35-9
Zinc Chloride 7646-85-7
Zinc Cyanide 557-21-1
Zinc Fluoride 7783-49-5
Zinc Formate 557-41-5
Zinc Hydrosulfite 7779-86-4
Zinc Nitrate 7779-88-6
Zinc Phenolsulfonate 127-82-2
Zinc Phosphide 1314-84-7
Zinc Silicofluoride 16871-71-9
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of water samples for zinc ions in the above compounds can be
performed by atomic spectrometric analysis for zinc. A 100-milliliter sample
is digested with hydrochloric/nitric acid or with nitric acid and hydrogen
peroxide and the digest is analyzed by inductively coupled plasma (ICP) or
flame atomic absorption (AA) spectrometry- Alternatively, the digested sample
can be chelated with pyrrolidinedithiocarbamic acid, the resulting complex
extracted into chloroform or methyl isobutyl ketone, and the solvent evaporated.
The residue is then dissolved in nitric acid and the resulting solution
analyzed by AA. These methods do not identify any specific zinc-containing
compounds, but measure the total zinc content of the sample.
INTERFERENCES:
High levels of silicon in the sample may cause interference when using AA.
The use of polypropylene sample container caps is recommended to avoid possible
contamination by sample container cap liner material. For each matrix
analyzed, it is necessary to determine if matrix effects and/or interferences
require standard addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed weekly, and at least 10 percent of
the analyses should be duplicates and/or standards.
B-429
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EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use in
Clean Water Act analyses. Precision and accuracy information is furnished.
The detection limit of the direct AA method is 0.005 milligrams per liter, the
sensitivity 0.02 milligrams per liter and the optimum concentration range 0.05
to 2 milligrams per liter (APHA). The chelation-extraction/AA procedure is
applicable over the range from 1 to 200 microgams zinc per liter (ASTM).
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 289.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency. Technical Additions to Methods for
Chemical Analysis of Water and Wastes. Method 200.7, EPA-600/4-82-055, U.S.
EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, Methods 7950, 7951; SW-846, U.S. EPA: Washington,
1982.
Federal Register, 44(233), December 3, 1979, pp. 69559-69564.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 328A; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
D1691(C), D1691(D); ASTM: Philadelphia, 1983"!
B-430
-------
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list),
or approximately $65 (list) with the chelation step; by ICP, it is approxi-
mately $10 (list).
B-431
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ZINC
Water Samples
Laboratory Method 2
Compound CAS Number
Zinc 7440-66-6
Zinc Acetate 557-34-6
Zinc Ammonium Chloride 14639-97-5
14639-98-6
52628-25-8
Zinc Borate 1332-07-6
Zinc Bromide 7699-45-8
Zinc Carbonate 3486-35-9
Zinc Chloride 7646-85-7
Zinc Cyanide 557-21-1
Zinc Fluoride 7783-49-5
Zinc Formate 557-41-5
Zinc Hydrosulfite 7779-86-4
Zinc Nitrate 7779-88-6
Zinc Phenolsulfonate 127-82-2
Zinc Phosphide 1314-84-7
Zinc Silicofluoride 16871-71-9
Zinc Sulfate 7733-02-0
METHOD SUMMARY:
Analysis of water samples for zinc ions in the above compounds can be
performed by colorimetric analysis for zinc. A sample is digested and treated
with Zincon® at pH 9, and the absorbance at 620 nanometers is measured.
Alternatively, the sample can be treated with dithizone and the resulting
zinc-dithizone complex extracted into carbon tetrachloride. The absorbance of
the zinc-dithizone complex at 535 nanometers is measured. These methods do not
identify any specific zinc-containing compound, but measure the total zinc
content of the sample.
INTERFERENCES:
Cadmium(II), aluminum, and manganese(II) interfere with the Zincon® method
Interference from bismuth, cadmium, cobalt, copper, gold, lead, mercury, nickel
palladium, silver, and stannous tin at low levels are eliminated by complexing
with sodium thiosulfate in the dithizone procedure. Ferric iron, residual
chlorine, and other oxidizing agents convert dithizone to a yellow-brown color.
Contamination from glassware containing zinc oxide can be a major problem.
Dithizone and dithizone complexes are rapidly decomposed in strong light.
QUALITY CONTROL:
No quality control procedures are given.
B-432
-------
EPA/TECHNICAL STATUS:
These methods are not EPA-approved. The Zincon® procedure is applicable
to 0.002 to 5 milligrams zinc per liter, while the dithizone method is
applicable to levels above 0.1 milligrams zinc per liter. Precision and
accuracy information is furnished.
REFERENCES:
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater. 15th ed., Methods 328B, 328C, 328D: APHA: Washington,
1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, D1691A, D1691B; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list).
B-433
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ZIRCONIUM
Air Samples
Laboratory Method
Compound
Zirconium Nitrate
Zirconium Potassium Fluoride
Zirconium Sulfate
Zirconium Tetrachloride
CAS Number
13746-89-9
16923-95-8
14644-61-2
10026-11-6
METHOD SUMMARY;
Atomic absorption (AA) spectrometric analysis for zirconium can be used
for the measurement of the above zirconium compounds in air samples. The
analysis is performed by cellulose ester membrane filtration of a known volume
of air, followed by acid digestion of the filter with the collected particu-
lates, and AA analysis of the resulting solution. This method does not
identify any specific zirconium compounds, but measures the total particulate
zirconium content of the sample.
INTERFERENCES:
Some experimental data suggest that the method does not work for zirconium
sulfate and that the presence of sulfate interferes. Addition of ammonium
fluoride is recommended to increase sensitivity.
QUALITY CONTROL:
A method blank should be processed with each set of 10 samples. Recovery
should be determined and, if less than 95 percent, results should be adjusted
accordingly. Duplicate analyses should agree within 5 percent.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 2 to 9 milligrams zirconium
per cubic meter for a 720-liter air sample. Precision and accuracy information
is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set M, Method S185; PB-265 029 (NTIS), U.S. DHEW: Cincinnati, December 1976^.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical.
Methods, 2nd ed., Vol. 3, Method S185; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
B-434
-------
COST INFORMATION:
Cost information has not been obtained.
B-177
-------
ARSENIC
Air Samples
Laboratory Method 6
Compound CAS Number Compound CAS Number
Arsenic 7440-38-2 Calcium Arsenite 52740-16-6
Arsenic Acid 1327-52-2 Cupric Acetoarsenite 12002-03-8
7778-39-4 Lead Arsenate 7784-40-9
Arsenic Disulfide 1303-32-8 7645-25-2
Arsenic Pentoxide 1303-28-2 10102-48-4
Arsenic Trichloride 7784-34-1 Potassium Arsenate 7784-41-0
Arsenic Trioxide 1327-53-3 Potassium Arsenite 10124-50-2
Arsenic Trisulfide 1303-33-9 Sodium Arsenate 7631-89-2
Cacodylic Acid 75-60-5 Sodium Arsenite 7784-46-5
Calcium Arsenate 7778-44-1
METHOD SUMMARY:
The above inorganic arsenic compounds in air samples can be measured by
graphite-furnace atomic absorption spectrometry. A known volume of air is
drawn through a sodium bicarbonate-impregnated cellulose ester filter and
cellulose backup pad. The filter and pad pair are digested with a nitric
acid-peroxide solution and nickel nitrate is added to modify the matrix. The
solution is analyzed by graphite-furnace atomic absorption spectrometry (AA).
This method does not identify any particular arsenic-containing compounds, but
measures the total arsenic content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks and standards are analyzed with the samples.
EPA/TECHNICAL STATUS:
This is an operational method as classified by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 0.67 to 32.2
micrograms per cubic meter, using a 400-liter sample. Precision and accuracy
information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, P&CAM 346; Publication No. 82-100, U.S. DHHS: Cincinnati,
August 1981.
B-178
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $28-75, plus
sampling costs.
B-179
-------
ARSENIC
Soil/Sediment Samples
Laboratory Method
Compound
Arsenic
Arsenic Acid
Arsenic Bisulfide
Arsenic Pentoxide
Arsenic Trichloride
Arsenic Trioxide
Arsenic Trisulfide
Cacodylic Acid
Calcium Arsenate
CAS Number
7440-
1327'
7778-
1303
1303-
7784'
1327-
1303-
75-
7778'
-38-2
-52-2
-39-4
-32-8
-28-2
-34-1
•53-3
-33-9
•60-5
-44-1
Compound
Calcium Arsenite
Cupric Acetoarsenite
Dichlorophenylarsine
Diethylarsine
Lead Arsenate
Potassium Arsenate
Potassium Arsenite
Sodium Arsenate
Sodium Arsenite
CAS Number
52740-
12002-
696-
692-
7784-
7645-
10102-
7784-
10124-
7631-
7784-
•16-6
-03-8
•28-6
•42-2
•40-9
•25-2
•48-4
•41-0
50-2
•89-2
46-5
METHOD SUMMARY:
Analysis of soil/sediment samples for arsenic and the above arsenic com-
pounds can be performed by atomic spectrometric analysis for arsenic. A 2-gram
sample is digested with nitric acid and hydrogen peroxide and analyzed by
atomic spectrometry. For low concentrations, furnace atomic absorption spec-
trometry (AA) is used, while inductively coupled plasma (ICP) spectrometry is
used for higher-concentration samples. This method measures the total arsenic
content of the sample, but does not identify specific arsenic compounds.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for the
Resource Conservation and Recovery Act (RCRA) and the Clean Water Act. Precision
and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23,'1982.
B-180
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U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes. Method 206.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
U.S. Environmental Protection Agency. Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 3010, 3020, 6010, 7060, 7061; SW-846,
U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Arsenic," pp. IV-77 to IV-87; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
Federal Register, 44(233), December 3, 1979, pp. 69559-69564.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., 4J?(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $38 (list); by ICP, it
is approximately $20 (list).
B-181
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Compound
Arsenic
Arsenic Acid
Arsenic Disulfide
Arsenic Pentoxide
Arsenic Trichloride
Arsenic Trioxide
Arsenic Trisulfide
Cacodylic Acid
Calcium Arsenate
ARSENIC
Water Samples
Laboratory Method 1
CAS Number
7440-
1327-
7778-
1303-
1303-
7784-
1327-
1303-
75-
7778-
•38-2
52-2
•39-4
32-8
•28-2
34-1
•53-3
33-9
•60-5
44-1
Compound
Calcium Arsenite
Cupric Acetoarsenite
Dichlorophenylarsine
Diethylarsine
Lead Arsenate
Potassium Arsenate
Potassium Arsenite
Sodium Arsenate
Sodium Arsenite
CAS Number
52740-
12002-
696-
692-
7784-
7645-
10102-
7784-
10124-
7631-
7784-
•16-6
•03-8
•28-6
•42-2
•40-9
•25-2
•48-4
41-0
•50-2
•89-2
•46-5
METHOD SUMMARY:
Analysis for arsenic and the above arsenic compounds in water can be
performed by atomic spectrometric analysis for arsenic. A 100-milliliter
sample is digested with nitric acid and hydrogen peroxide and analyzed by
atomic spectrometry. For low concentrations, furnace atomic absorption spec-
trometry (AA) is used, while inductively coupled plasma (ICP) spectrometry is
used for higher-concentration samples. These methods measure total arsenic,
and do not identify specific arsenic compounds.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use in
analysis for the Resource Conservation and Recovery Act (RCRA) and the Clean
Water Act. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
B-182
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U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and
Wastes, Method 206.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Technical Additions to Methods for Chemical
Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-005, U.S. EPA:
Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 6010, 7060, 7061; SW-
846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively-Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Federal Register, _44_(233), December 3, 1979, pp. 69559-69564.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., ^8(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for this analysis by AA is approximately $18-50 (list),
and $10 by ICP.
B-183
-------
ARSENIC
Water Samples
Laboratory Method 2
Compound CAS Number Compound CAS Number
Arsenic 7440-38-2 Calcium Arsenite 52740-16-6
Arsenic Acid 1327-52-2 Cupric Acetoarsenite 12002-03-8
7778-39-4 Dichlorophenylarsine 696-28-6
Arsenic Bisulfide 1303-32-8 Diethylarsine 692-42-2
Arsenic Pentoxide 1303-28-2 Lead Arsenate 7784-40-9
Arsenic Trichloride 7784-34-1 7645-25-2
Arsenic Trioxide 1327-53-3 10102-48-4
Arsenic Trisulfide 1303-33-9 Potassium Arsenate 7784-41-0
Cacodylic Acid 75-60-5 Potassium Arsenite 10124-50-2
Calcium Arsenate 7778-44-1 Sodium Arsenate 7631-89-2
Sodium Arsenite 7784-46-5
METHOD SUMMARY:
Atomic absorption spectrometry (AA) may be used for the analysis of
arsenic and the above arsenic compounds in water. A 25-milliliter sample is
combined with potassium iodide and the arsenic in the sample is reduced by
stannous chloride and converted to arsine with zinc metal. The arsine gas is
then analyzed by AA. Samples should be acidifed at the time of collection.
This method does not differentiate among arsenic-containing compounds, but
measures the total arsenic content of the sample.
INTERFERENCES:
High concentrations of antimony- chromium, cobalt, copper, iron, mercury,
molybdenum, nickel, silver, and tin will interfere. Organic matter in the
sample must be oxidized before analysis. Organic arsenic compounds must be
converted to inorganic compounds. Samples containing industrial waste should
be spiked to establish adequate recovery.
QUALITY CONTROL:
At least one duplicate sample should be analyzed every 10 samples. A
reference standard should be analyzed periodically.
EPA/TECHNICAL STATUS:
This method is approved for the National Pollutant Discharge Elimination
System (NPDES) and the Safe Drinking Water Act (SDWA). The method will deter-
mine arsenic concentrations of 2 micrograms arsenic per liter or greater and
the optimum concentration range is 2 to 20 micrograms arsenic per liter.
Precision and accuracy information is furnished.
B-184
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REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 206.3; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, " Methods for the Determina-
tion of Arsenic," pp. 1V-77 to IV-87: EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed.; APHA: Washington, 1980, pp. 160-163, 173-177.
American Society for Testing and Materials, 1983 ASTM Book of Standards, Vol.
11.01, Method D 2972-78; ASTM: Philadelphia, 1983.
Alberta Environmental Centre, Methods Manual for Chemical Analysis of Water and
Wastes, "Arsenic, Total:" Publication No. AECV81-M1, Alberta Environmental
Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $18-50
(list).
B-185
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ARSENIC
Water Samples
Laboratory Method 3
Compound CAS Number Compound CAS Number
Arsenic 7440-38-2 Calcium Arsenite 52740-16-6
Arsenic Acid 1327-52-2 Cupric Acetoarsenite 12002-03-8
7778-39-4 Dichlorophenylarsine 696-28-6
Arsenic Bisulfide 1303-32-8 Diethylarsine 692-42-2
Arsenic Pentoxide 1303-28-2 Lead Arsenate 7784-40-9
Arsenic Trichloride 7784-34-1 7645-25-2
Arsenic Trioxide 1327-53-3 10102-48-4
Arsenic Trisulfide 1303-33-9 Potassium Arsenate 7784-41-0
Cacodylic Acid 75-60-5 Potassium Arsenite 10124-50-2
Calcium Arsenate 7778-44-1 Sodium Arsenate 7631-89-2
Sodium Arsenite 7784-46-5
METHOD SUMMARY:
Arsenic and the above arsenic compounds in water samples can be measured
spectrophotometrically. The arsenic is reduced to arsine in acid solution in a
hydrogen generator. The arsine is passed through a scrubber to remove sulfide,
and absorbed in a solution of silver diethyldithiocarbamate dissolved in
pyridine or chloroform. The resultant red complex is measured in a spectro-
photometer at 535 nm. This method does not identify any specific arsenic
compounds, but measures the total arsenic content of the sample.
INTERFERENCES:
High concentrations of chromium, cobalt, copper, mercury, molybdenum,
nickel, and silver can interfere in the generation of arsine. Antimony salts
in the sample can form stibine, which interferes by yielding a red color with
maximum absorbance at 510 nm.
QUALITY CONTROL:
The original calibration curve should be checked daily by analysis of a
reagent blank and a standard.
EPA/TECHNICAL STATUS:
This method is approved for the National Pollutant Discharge Elimination
System (NPDES) and the Safe Water Drinking Act (SWDA). Precision and accuracy
information is furnished. The method is suitable for concentrations of arsenic
at or above 10 micrograms per liter.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water;
and Waste, Method 206.4; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
B-186
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American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 307B; APHA: Washington, B.C., 1980.
American Society for Testing and Materials, 1983 ASTM Book of Standards, Vol.
11.01, Method D 2972-78; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost information has not been obtained.
B-187
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ARSINES
Air Samples
Laboratory Method
Compound
Dichlorophenylarsine
Diethylarsine
CAS Number
696-28-6
692-42-2
METHOD SUMMARY:
Atomic absorption spectrometry may be used to analyze air samples for
the above arsines. Analysis is performed by passage of a known volume of air
through a charcoal-tube sampling device, followed by desorption with dilute
nitric acid and graphite-furnace atomic absorption (AA) analysis of the result-
ing solution. Nickel can be added to the solution to enhance the sensitivity.
This method does not differentiate among various arsine-containing compounds.
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
Interference by particulate arsenic compounds may be prevented by prefiltration
of air during sampling.
QUALITY CONTROL;
Samples should be analyzed in duplicate, and 50 percent of the analyses
should be standards, analyzed in duplicate if nickel is not added to the sample.
If the nickel addition is made, a method blank and a standard should be run
with every 10 samples.
EPA/TECHNICAL STATUS:
The method without using nickel is approved by the National Institute for
Occupational Safety and Health (NIOSH), and has been validated over the range
of 0.09 to 0.4 milligrams per cubic meter using a 10-liter sample. The method
using nickel is proposed by NIOSH for use over the range of 1 to 10 micrograms
per cubic meter. Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set J, Method S229; PB-263 959 (NTIS), U.S. DHEW: Cincinnati, December 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical.
Methods, 2nd ed., Vol. 3, Method S229; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
B-188
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $28-60
(list), plus sampling costs.
B-189
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BERYLLIUM
Air Samples
Laboratory Method 1
Compound CAS Number
Beryllium 7440-41-7
Beryllium Chloride 7787-47-5
Beryllium Fluoride 7787-49-7
Beryllium Nitrate 13597-99-4
7787-55-5
METHOD SUMMARY:
Analysis for the above particulate beryllium compounds in air can be
performed by atomic spectrometry. A known volume of air is passed through a
cellulose membrane filter, the filter is digested, and the resulting solution
is analyzed by graphite-furnace background-corrected atomic absorption (AA)
spectrometry or by flame AA spectrometry. This method measures the total non-
volatile beryllium content of the sample and does not identify specific
beryllium compounds.
INTERFERENCES:
No specific interferences are reported for the furnace AA method, while
high concentration of aluminum, silicon, and magnesium will interfere with the
flame method unless controlled by the addition of oxine (8-hydroxyquinoline) to
the standards and samples.
QUALITY CONTROL:
A method blank should be processed with each set of 10 samples, and the
analytical method recovery must be determined over the concentration range of
interest. The method blank and percent recovery results should be used in
the calculation of beryllium concentrations.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 2.7 to 11.8 micrograms
beryllium per cubic meter for the furnace AA method and 0.015 to 4.0 micrograms
per cubic meter for the flame AA method. Precision and accuracy information
is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analyticaj.
Methods, Method P&CAM 121; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
B-190
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U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set N, Method S339; PB-258 433 (NTIS), U.S. DREW: Cincinnati, September 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S339; Publication No. 77-157-C, U.S. DREW:
Cincinnati, 1977.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $18-50
(list), plus sampling costs.
B-191
-------
BERYLLIUM
Air Samples
Laboratory Method 2
Compound
Beryllium
Beryllium Chloride
Beryllium Fluoride
Beryllium Nitrate
CAS Number
7440-41-7
7787-47-5
7787-49-7
13597-99-4
7787-55-5
METHOD SUMMARY:
Beryllium and the above beryllium compounds in air samples can be measured
with arc emission spectrography. The sample is collected by cellulose membrane
filtration, by an impinger containing 10-percent nitric acid solution, or by an
electrostatic precipitator. The filter or impinger sample is ashed in nitric
acid and the residue is converted to the chloride form by evaporation with 1:1
hydrochloric acid. The residue is dissolved in hydrochloric acid and water,
concentrated, added to an electrode, and an AC arc is used to excite the
beryllium in the sample. The spectrum is recorded photographically and percent
transmittance is measured at 234.86 nanometers. This method does not identify
any specific beryllium-containing compounds, but measures the total beryllium
content of the sample.
INTERFERENCES:
High concentrations of iron in the sample will interfere.
QUALITY CONTROL:
A method blank and standards should be processed along with the samples.
EPA/TECHNICAL STATUS:
This is an operational method according to the National Institute for
Occupational Safety and Health (NIOSH), for use over the range of 0.001 to 0.05
micrograms beryllium on the electrode. No precision or accuracy information
is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 123; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 123; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
B-192
-------
COST INFORMATION:
Cost information has not been obtained.
B-193
-------
BERYLLIUM
Air Samples
Laboratory Method 3
Compound CAS Number
Beryllium 7440-41-7
Beryllium Chloride 7787-47-5
Beryllium Fluoride 7787-49-7
Beryllium Nitrate 13597-99-4
7787-55-5
METHOD SUMMARY:
Analysis for beryllium and the above beryllium-containing compounds in air
may be performed by inductively coupled plasma atomic emission spectroscopic
(ICP) analysis for beryllium. A known volume of air is drawn through a mixed
cellulose filter. The filter is ashed with a mixture of nitric and perchloric
acids followed by analysis of the resulting solution by ICP. This method does
not identify any specific beryllium-containing compounds, but measures the
total beryllium content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
beryllium per cubic meter, using a 500-liter sample. Limited precision and
accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-194
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BERYLLIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Beryllium 7440-41-7
Beryllium Chloride 7787-47-5
Beryllium Fluoride 7787-49-7
Beryllium Nitrate 13597-99-4
7787-55-5
METHOD SUMMARY:
Analysis of soil/sediment samples for the above beryllium compounds can be
performed by atomic spectrometric analysis for beryllium. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and analyzed by atomic spectrom-
etry. For low concentrations, furnace atomic absorption spectrometry (AA) is
used, while inductively coupled plasma spectrometry (ICP) or flame AA is used
for higher-concentration samples. This method does not differentiate between
the various beryllium compounds.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for analyses
for the Clean Water Act. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 210.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 6010, 7090, 7091; SW-
846, U.S. EPA: Washington, 1982.
B-195
-------
Federal Register, ^4_(233), December 3, 1979, pp. 69559-69564.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysts by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem. , ^8_(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $38 (list); by ICP,
it is approximately $20 (list).
B-196
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BERYLLIUM
Water Samples
Laboratory Method
Compound CAS Number
Beryllium 7440-41-7
Beryllium Chloride 7787-47-5
Beryllium Fluoride 7787-49-7
Beryllium Nitrate 13597-99-4
7787-55-5
METHOD SUMMARY:
Water samples can be analyzed for the above beryllium compounds by atomic
spectrometric analysis for beryllium. A 100-milliliter sample is digested with
nitric acid and hydrogen peroxide and analyzed by atomic spectrometry. For low
concentrations, furnace atomic absorption spectrometry (AA) is used, while
inductively coupled plasma spectrometry (ICP) or flame spectrometry can be used
for higher-concentration samples. These methods do not identify any particular
beryllium compound, but measure the total beryllium content of the sample.
INTERFERENCES:
Aluminum concentrations above 500 micrograms per liter can interfere.
Sodium and silicon concentrations above 1 milligram per liter depress the
beryllium absorbance. lonization suppression by addition of sufficient calcium
chloride to standards and samples to yield a final calcium concentration of 900
milligrams per liter may be used.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
A reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and approved for use in
analyses for the Clean Water Act. Precision and accuracy information is
furnished. The limits of detection are 25 raicrograms beryllium per liter for
flame AA, 0.3 micrograms per liter for ICP, and 0.2 micrograms per liter for
furnace AA.
REFERENCES:
U. S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
B-197
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U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 210.1, 210.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 079.
Federal Register, 44(233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Wastej_
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 6010, 7090, 7091; SW-
846, U.S. EPA: Washington, 1982.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7, EPA-600/4-82-055, U.S.
EPA: Cincinnati, December 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., ^8/3), 1976, pp. 516-519.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 303C; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, D 3645-78; ASTM: Philadelphia, 1983^
COST INFORMATION:
Cost per sample for analysis by AA is approximately $18-50 (list); by ICP,
it is approximately $10 (list).
B-198
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CADMIUM
Air Samples
Laboratory Method 1
Compound CAS Number
Cadmium 7440-43-9
Cadmium Acetate 543-90-8
Cadmium Bromide 7789-42-6
Cadmium Chloride 10108-64-2
METHOD SUMMARY:
Atomic spectrometry may be used for the analysis of the above cadmium
compounds in air samples. The analysis is performed by membrane-filtration of
a known volume of air, followed by acid digestion of the sampling medium,
solubilization with hydrochloric acid, and atomic absorption (AA) spectrometric
analysis of the resulting solution at 228.8 nm, either by direct aspiration or
by an ammonium pyrrolidine dithiocarbamate/methyl isobutyl ketone (APDC/MIBK)
solvent extraction procedure. This method measures the total cadmium content
of the sample and does not identify specific cadmium compounds.
INTERFERENCES:
Silicon has been reported to interfere with the analysis.
QUALITY CONTROL:
A method blank should be analyzed with each set of 10 or fewer samples.
The percent recovery should be determined and, if it is less than 95, results
corrected accordingly. Duplicate determinations should agree within 5 percent.
EPA/TECHNICAL STATUS:
Method S312 is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.12 to 0.98 milligrams
per cubic meter using a 25-liter sample. Method P&CAM 151 is an operational
method for use over the range of 0.01 to 0.2 milligrams per cubic meter.
Method P&CAM 173 is an operational method for use over the range of 4.2 to 84
micrograms per cubic meter using a 240-liter air sample. The APHA method is
applicable in an optimum range of 0.05 to 20.0 micrograms of cadmium per milli-
liter of solution. An atmospheric concentration of 0.005 micrograms particu-
late cadmium per cubic meter can be detected using a 2000-cubic meter air
sample. Environment Canada uses the solvent extraction procedure to obtain a
detection limit of 0.001 micrograms per cubic meter of air. Precision and
accuraccy information is furnished.
B-199
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REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical.
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S312; Publication No 77-157-C, U.S. DHEW:
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 151; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set W, Method S312; PB-262 406 (NTIS), U.S. DHEW: Cincinnati, December 1976.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method D-10, "Trace Metal
Analysis"; HASL-300, Environmental Measurements Laboratory, U.S. DOE: New York,
1983.
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Method 311; APHA: Washington, 1977^
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23536; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-200
-------
CADMIUM
Air Samples
Laboratory Method 2
Compound CAS Number
Cadmium 7440-43-9
Cadmium Acetate 543-90-8
Cadmium Bromide 7789-42-6
Cadmium Chloride 10108-64-2
METHOD SUMMARY:
Analysis for the above cadmium compounds in air may be performed by
filtration of air and analysis of the filter medium by X-ray fluorescence
spectrometry. The method is non-destructive, so that further analyses may be
performed on samples after this analysis. The method is sensitive to amounts
of cadmium above 40 micrograms, with a precision of 50 percent at that level.
The sample-collection time may be up to 8 hours, but analysis time is only
approximately 1 minute. The method measures total cadmium present in the
sample, and does not differentiate between cadmium compounds or valence states.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-
fiber filters are acceptable for use only if they are of the highest purity-
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method should be applicable to 0.01
to 1.0 microgram of cadmium per cubic meter, depending on sample size. Preci-
sion information is furnished.
REFERENCES:
Rhodes, J. R. ; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R. ; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927.
B-201
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list)
$20 (bid), plus sampling costs.
B-202
-------
CADMIUM
Air Samples
Laboratory Method 3
Compound CAS Number
Cadmium 7440-43-9
Cadmium Acetate 543-90-8
Cadmium Bromide 7789-42-6
Cadmium Chloride 10108-64-2
METHOD SUMMARY:
Analysis for cadmium and the above cadmium-containing compounds in air may
be performed by inductively coupled plasma spectroscopy (ICP) analysis for
cadmium. A known volume of air is drawn through a cellulose ester membrane
filter. The filter is ashed with a mixture of nitric and perchloric acids,
followed by ICP analysis. This method does not identify any specific cadmium-
containing compounds, but measures the total cadmium content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms cadmium
per cubic meter for a 500-liter sample. Limited precision and accuracy infor-
mation is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS: Cincinnati,
August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-203
-------
CADMIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Cadmium 7440-43-9
Cadmium Acetate 543-90-8
Cadmium Bromide 7789-42-6
Cadmium Chloride 10108-64-2
METHOD SUMMARY:
Analysis of soil/sediment samples for cadmium and the above cadmium com-
pounds can be performed by atomic spectrometric analysis for cadmium. A 2-gram
sample is digested with nitric acid and hydrogen peroxide and analyzed by
atomic spectrometry. For low concentrations, furnace atomic absorption spec-
trometry (AA) i.s used, while inductively coupled plasma spectrometry (ICP) or
flame AA is used for higher-concentration samples. These methods will not
differentiate between various cadmium compounds.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use in
Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 213.1, 213.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Federal Register, 4^_(233), December 3, 1979, pp. 69559-69564.
B-204
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U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3020, 6010, 7130, 7131; SW-846,
U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry," pp. IV-2 to IV-48, "Methods for the Determination of
Trace Metals Using Inductively-Coupled Plasma Atomic Emission Spectrometry,"
pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection Agency:
Las Vegas, 1984.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., ^(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $25-50 (list); by
ICP, it is approximately $20 (list).
B-205
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CADMIUM
Water Samples
Laboratory Method
Compound CAS Number
Cadmium 7440-43-9
Cadmium Acetate 543-90-8
Cadmium Bromide 7789-42-6
Cadmium Chloride 10108-64-2
METHOD SUMMARY
Analysis of water samples for the above cadmium compounds can be performed
by atomic spectrometric analysis for cadmium. A 100-milliliter sample is
digested with nitric acid and hydrogen peroxide and analyzed by atomic spec-
trometry. For low concentrations, furnace atomic absorption spectrometry (AA)
is used, while inductively coupled plasma spectrometry (ICP) or flame AA is
used for higher-concentration samples. This method measures cadmium, and does
not identify specific cadmium compounds.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for
Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
Precision and accuracy information is furnished. Limits of detection are 5
micrograms cadmium per liter for flame AA, 0.1 micrograms per liter for furnace
AA, and 4 micrograms per liter for ICP. APHA reports a detection limit of 2
micrograms per liter, a sensitivity of 25 micrograms per liter, and an optimum
concentration range of 50 to 200 micrograms per liter for flame AA.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 213.1, 213.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
B-206
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Federal Register, 44(233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U. S.
EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 6010, 7130, 7131;
SW-846, U.S. EPA: Washington, 1982.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method D-10, "Trace Metal
Analysis," pp. D-10-1 to D-10-2; HASL-300, Environmental Measurements Labora-
tory, U.S. DOE, New York, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 303A; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, D 3557-78; ASTM: Philadelphia, 1983.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectroraetry," Anal. Chem., 4^(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $18-50 (list); by ICP,
it is approximately $10 (list).
B-207
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CALCIUM
Air Samples
Laboratory Method 1
Compound CAS Number
Calcium Arsenate- 7778-44-1
Calcium Arsenite 52740-16-6
Calcium Carbide 75-20-7
Calcium Chromate 13765-19-0
Calcium Cyanide 592-01-8
Calcium Dodecyl- 26264-06-2
benzene Sulfonate
Calcium Hypochlorite 7778-54-3
METHOD SUMMARY:
Analysis for the above calcium compounds in air may be performed by
filtration of air and analysis of the filter medium for calcium by X-ray fluore-
scence spectrometry. The method measures total calcium present in the sample,
and does not differentiate between chemical compounds or calcium valence states.
The method is non-destructive, so that further analyses may be performed on
samples after this analysis. The sample-collection time may be up to 8 hours,
but analysis time is only approximately 1 minute.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling and glass-
fiber filters are acceptable for use only if they are of the highest purity.
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
method is sensitive to amounts above 40 micrograms of calcium. The method
should be applicable to 0.01 to 1.0 microgram of calcium per cubic meter,
depending on sample size.
REFERENCES:
Rhodes, J. R.; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for I_n Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
B-208
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Rhodes, J. R. ; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S. ; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
$20 (bid), plus sampling costs.
B-209
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CALCIUM
Air Samples
Laboratory Method 2
Compound CAS Number
Calcium Arsenate 7778-44-1
Calcium Arsenite 52740-16-6
Calcium Carbide 75-20-7
Calcium Chromate 13765-19-0
Calcium Cyanide 592-01-8
Calcium Dodecyl- 26264-06-2
benzene Sulfonate
Calcium Hypochlorite 7778-54-3
METHOD SUMMARY:
Analysis for the above calcium-containing compounds in air may be per-
formed by inductively coupled plasma atomic emission spectroscopic (ICP)
analysis for calcium. A known volume of air is drawn through a cellulose ester
membrane filter. The filter is ashed with a mixture of nitric and perchloric
acids followed by analysis by ICP. The method does not identify any specific
calcium-containing compounds, but measures the total calcium content of the
sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms calcium
per cubic meter, using a 500-liter sample. Limited precision and accuracy infor-
mation is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manaul of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-210
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CALCIUM
Air Samples
Laboratory Method 3
Compound CAS Number
Calcium Arsenate 7778-44-1
Calcium Arsenite 52740-16-6
Calcium Carbide 75-20-7
Calcium Chromate 13765-19-0
Calcium Cyanide 592-01-8
Calcium Dodecyl- 26264-06-2
benzene Sulfonate
Calcium Hypochlorite 7778-54-3
METHOD SUMMARY:
Analysis for the above particulate calcium compounds in air samples may be
performed by flame atomic absorption (AA) spectrometric determination of cal-
cium. A known volume of air is drawn through a membrane filter. The filter
with the collected particulates is digested with nitric acid, and the resulting
solution is analyzed by AA. This method does not identify any specific calcium-
containing compounds, but measures the total calcium content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL;
A blank should be processed with every 10 samples. Standard solutions
should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 4.2 to 210
micrograms per cubic meter, using a 240-liter air sample. Precision informa-
tion is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
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U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals"
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE, New York, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-212
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CALCIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Calcium Arsenate 7778-44-1
Calcium Arsenite 52740-16-6
Calcium Carbide 75-20-7
Calcium Chromate 13765-19-0
Calcium Cyanide 592-01-8
Calcium Dodecyl- 26264-06-2
benzene Sulfonate
Calcium Hypochlorite 7778-54-3
METHOD SUMMARY:
Analysis of soil/sediment samples for the above calcium compounds can be
performed by atomic spectrometric analysis for calcium. Samples of 100 milli-
grams are digested with nitric acid, perchloric acid, hydrogen fluoride, and
boric acid, mixed with a lanthanum chloride solution, and analyzed by atomic
absorption spectrometry. Samples should be stored in polyurethane bags and
frozen immediately after collection. This method does not differentiate among
calcium-containing samples, but measures the total calcium content of the
sample.
INTERFERENCES:
Standard and sample compositions should be closely matched, and solvent
extraction techniques may be necessary. An excess of sodium should be added to
the sample to reduce ionization interferences.
QUALITY CONTROL:
Quality control procedures are not provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The detection limit is 10 milligrams of calcium per kilogram of
sample (Environment Canada).
REFERENCES:
Environment Canada, Analytical Methods Manual, NAQUADAT No. 20050; Environment
Canada, Inland Waters Directorate, Water Quality Branch: Ottawa, Canada, 1975.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
B-213
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-60
(list).
B-214
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CALCIUM
Water Samples
Laboratory Method
Compound CAS Number
Calcium Arsenate 7778-44-1
Calcium Arsenite 52740-16-6
Calcium Carbide 75-20-7
Calcium Chromate 13765-19-0
Calcium Cyanide 592-01-8
Calcium Dodecyl- 26264-06-2
benzene Sulfonate
Calcium Hypochlorite 7778-54-3
METHOD SUMMARY:
Analysis of water samples for the above calcium compounds can be performed
by atomic spectrometric or titrimetric analysis for calcium. In titrimetric
analysis, a 50-milliliter sample is made basic with sodium hydroxide, mixed
with indicator, and titrated with a disodium ethylenediamine tetraacetate
(EDTA) solution. Alternatively, calcium in the sample can be precipitated
quantitatively at pH 5 with oxalate, the precipitated calcium oxalate dissolved
in acid, and the resulting solution titrated with potassium permanganate. In
AA analysis, samples with a high level of organic substances must be digested
before analysis. When analysis is not to be performed soon after sample
collection, samples should be preserved by acidification with nitric acid.
These methods do not differentiate among calcium compounds, but measure the
total amount of calcium present in a sample.
INTERFERENCES:
When using flame AA, lanthanum should be added to the samples and standards
to prevent possible interferences from phosphate, sulfate, and aluminum. High
concentrations of magnesium will cause the calcium determination to be low. A
large amount of alkali should be added to the sample and standards to control
ionization interference. In the precipitation/titration analysis, use of
an excess of oxalate overcomes interference by magnesium. Strontium oxalate
may precipitate with calcium and require a correction of results. Silica
interference may be removed by dehydration. Aluminum, iron, and manganese can
be precipitated by ammonium hydroxide after treatment with persulfate. Phos-
phate should be removed by precipitation as the ferric salt, and suspended
matter should be removed by centrifugation or filtration. When using EDTA
titrimetry, strontium and barium may interfere, and alkalinity in excess of 30
milligrams per liter may cause an indistinct endpoint. Raising the pH to 12 to
13 will reduce or eliminate magnesium interferences in the EDTA titration.
QUALITY CONTROL:
When using AA, standards should be analyzed each time a sample or set of
samples is analyzed. For each matrix analyzed, it is necessary to determine if
B-215
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matrix effects and/or interferences require standard addition or serial dilution
methods. Quality control information is not given for the titrimetric method.
EPA/TECHNICAL STATUS:
These methods are approved for the National Pollutant Discharge Elimination
Service (NPDES). Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 215.1, 215.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;1' HASL-300, Environmental Measurements Laboratory, U.S.
DOE, New York, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastes, 15th ed. Method 303A, 311A, 31 IB, 311C; APHA: Washington,
1980.
American Society for Testing and Materials, 1983 ASTM Book of Standards, Vol.
11.01, Methods D 511-82B and D 511-82C; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $10-20 (list); by
titration, it is approximately $20 (list).
B-216
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CHLORIDES
Air Samples
Laboratory Method 1
Compound CAS Number
Ammonium Chloride 12125-02-9
Antimony Trichloride 10025-81-9
Antimony Pentachloride 7647-18-9
Beryllium Chloride 7787-47-5
Cadmium Chloride 10108-64-2
Chromous Chloride 10049-05-5
Cupric Chloride 7447-39-4
Cyanogen Chloride 506-77-4
Ferric Chloride 7705-08-0
Ferrous Chloride 7758-94-3
Hydrochloric Acid 7647-01-0
Lead Chloride 7758-95-4
Nickel Chloride 7718-54-9
37211-05-5
Phosphorus Trichloride 7719-12-2
Thallium(I) Chloride 7791-12-0
Zinc Chloride 7646-85-7
METHOD SUMMARY:
The above chlorides in air samples may be measured with an ion selective
electrode. A known volume of air is passed through a midget impinger contain-
ing acetate buffer. The chloride collected is determined potentiometrically,
using a chloride ion electrode. This method does not identify the specific
chloride-containing compounds present, but measures the total chloride content
of the sample.
INTERFERENCES:
Sulfide ion can interfere, as well as bromide, thiosulfate, and ammonium
ions.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH) over the range of 0.1 to 1750 milligrams
of chloride ion per cubic meter, using a 200-liter sample. Limited precision
and accuracy information is provided.
B-217
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REFERENCE:
U.S. Deparment of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 115; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-19
(list), plus sampling costs.
B-218
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CHLORIDES
Air Samples
Laboratory Method 2
Compound CAS Number
Ammonium Chloride 12125-02-9
Antimony Trichloride 10025-91-9
Antimony Pentachloride 7647-18-9
Beryllium Chloride 7787-47-5
Cadmium Chloride 10108-64-2
Chromous Chloride 10049-05-5
Cupric Chloride 7447-39-4
Cyanogen Chloride 506-77-4
Ferric Chloride 7705-08-0
Ferrous Chloride 7758-94-3
Hydrochloric Acid 7647-01-0
Lead Chloride 7758-95-4
Nickel Chloride 7718-54-9
37211-05-5
Phosphorus Trichloride 7719-12-2
Thallium(I) Chloride 7791-12-0
Zinc Chloride 7646-85-7
METHOD SUMMARY:
Air samples can be analyzed for the above chloride compounds by passage of
a known volume of air through fritted glass absorbers, impingers, filters, or
an electrostatic precipitator. The sample is then dissolved and titrated with
mercuric nitrate in the presence of a mixed diphenylcarbazone-bromphenol blue
indicator. Mercuric ions react with chloride to form HgCl2> an^ tnen tne
excess mercuric ions react with the diphenylcarbazone to form a blue complex.
Fritted glass absorbers and impingers are used to sample gaseous chlorides,
while filters, impingers, or electrostatic precipitators are used for particu-
late chlorides. This method does not identify any particular chloride salt,
but measures the total inorganic chloride content of the sample.
INTERFERENCES:
Heavy metals can change the color of the solution at the endpoint and can
be removed by a cation exchanger. The sample must contain less than 2.5 milli-
grams of ferric ion plus chromate ion. The presence of sulfides or sulfites
requires treatment with hydrogen peroxide. Iodide, bromide, cyanate, and
thiocyanate are titrated and reported as chloride.
QUALITY CONTROL:
A reagent blank should be processed with each sample.
B-219
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EPA/TECHNICAL STATUS:
This method is not EPA-approved. This method is applicable over the range
of 0.07 to 1.5 milligrams of chloride per cubic meter, using a 30-liter air
sample. Precision and accuracy information is furnished.
REFERENCE:
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Method 202; APHA: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20 (list),
plus sampling costs.
B-220
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CHLORIDES
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Chloride 12125-02-9
Antimony Trichloride 10025-91-9
Antimony Pentachloride 7647-18-9
Beryllium Chloride 7787-47-5
Cadmium Chloride 10108-64-2
Chromous Chloride 10049-05-5
Cupric Chloride 7447-39-4
Cyanogen Chloride 506-77-4
Ferric Chloride 7705-08-0
Ferrous Chloride 7758-94-3
Hydrochloric Acid 7647-01-0
Lead Chloride 7758-95-4
Nickel Chloride 7718-54-9
37211-05-5
Phosphorus Trichloride 7719-12-2
Thallium(I) Chloride 7791-12-0
Zinc Chloride 7646-85-7
METHOD SUMMARY:
Analysis for the above chloride salts in water can be performed by
analysis for chloride. The analysis can be performed titrimetrically or
colorimetrically. Titrimetry can be done using a silver nitrate titrant and
potassium chromate indicator, a mercuric nitrate titrant and diphenylcarbazone
indicator, or a silver nitrate titrant and a silver/silver chloride electrode
and millivolt meter as an indicator. The colorimetric method involves addition
of ferric nitrate/mercuric thiocyanate to the sample, and the intensity of the
color of the blood-red ferric thiocyanate, formed by reaction with the thio-
cyanate displaced by chloride, is measured. This method does not identify any
particular chloride salt, but measures the total chloride content of the sample.
INTERFERENCES:
Bromide and iodide register as equivalent chloride concentrations in all
three titrimetric methods. Cyanide does the same in the silver nitrate/potas-
sium chromate titrimetric method, and sulfide, thiosulfate and sulfite ions
interfere, but can be removed by treatment with hydrogen peroxide. In the
mercuric nitrate titrimetric method, chromate, ferric, and sulfite ions above
10 milligrams per liter interfere. In the silver nitrate/potentiometric method
ferricyanide causes high results, chromate and dichromate interfere and should
be reduced to chromic ions, and ferric ions interfere if present in an amount
substantially above the chloride concentration. In the colorimetric method,
turbid samples should be filtered before analysis.
B-221
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QUALITY CONTROL:
Duplicate and fortified samples should be processed in accordance with a
quality assurance program.
EPA/TECHNICAL STATUS:
The mercuric nitrate titrimetric method and the colorimetric method are
EPA-approved for use under the Clean Water Act. The methods are suitable for
analysis of relatively clean samples in the range from 0.15 to 10 milligrams
chloride in a 50-milliliter sample (APHA). Precision and accuracy information
is furnished.
REFERENCES:
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 407; APHA: Washington, 1980.
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Chloride, Dissolved;" Publication No. AECV81-M1, Alberta Environ-
mental Centre, Vegreville, Alberta, Canada, 1981.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 325.1, 325.2, 325.3; EPA-600/4-79-020, U.S. EPA: Cincinnati,
1979.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20 (list).
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CHROMIC ACID AND CHROMATES
Air Samples
Laboratory Method
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Dichromate 7789-09-5
Calcium Chroraate 13765-19-0
Chromic Acid 11115-74-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Dichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Dichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOD SUMMARY:
Air samples may be analyzed for the above hexavalent chromium compounds by
colorimetry or by atomic spectrometry. The colorimetric analysis is performed
by passing a known volume of air through a polyvinyl chloride filter, leaching
the analyte from the filter with dilute sulfuric acid, and analyzing the
resulting solution for Cr(VI) with a spectrophotometer. After using the same
filtration procedure for sample collection, atomic spectrometric analysis is
performed by extraction of Cr(VI) from the filter with hexane/methyl isobutyl
ketone and ammonium pyrrolidinedithiocarbamate. The hexane solution is then
analyzed for chromium by atomic absorption spectrometry. These methods do not
identify any particular Cr(VI)-containing compound, but measure the total
Cr(VI) content of the sample.
INTERFERENCES:
Many heavy metals, such as iron, copper, nickel, and vanadium, can inter-
fere.
QUALITY CONTROL:
For the colorimetric method, a method blank must be processed with each
set of 10 samples and the collection efficiency of the filtration system must
be determined and used in calculations.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH) and validated over the range of 0.052 to 0.204 milligrams
chromium(VI) per cubic meter for a 22.5-liter air sample. Precision and
accuracy information is furnished.
B-223
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REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set 0, Method S317; PB-262 402 (NTIS), U.S. DREW: Cincinnati, 1976."
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S317; Publication No. 77-157-C, U.S. DHEWl
Cincinnati, 1977.
American Public Health Association, Methods of Air Sampling and Analysis,
2nd ed., Method 807; APHA: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by the colorimetric method is approximately
$20-30, plus sampling costs; for analysis by AA, it is approximately $20-50
(list), plus sampling costs.
B-224
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CHROMIUM
Air Samples
Laboratory Method 1
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acetate 1066-30-4
Chromic Acid 11115-74-5
Chromic Sulfate 10101-53-8
Chromium 7440-47-3
Chromous Chloride 10049-05-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Dichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Dichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOD SUMMARY:
Analysis for the above chromium compounds in air may be performed by fil-
tration of air and analysis of the filter and its contents for chromium by
X-ray fluorescence spectrometry. The method is non-destructive, so that
further analyses may be performed on samples after this analysis. The sample-
collection time may be up to 8 hours, but analysis time is approximately 1
minute.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-
fiber filters are acceptable for use only if they are of the highest purity.
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable. The method measures total chromium present in
the sample, and does not differentiate between chemical compounds or chromium
valence states.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished.
The method is sensitive to amounts of chromium above 7 micrograms and is
applicable to 0.01 to 1.0 microgram of chromium per cubic meter, depending on
sample size.
B-225
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REFERENCES:
Rhodes, J. R. ; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B. ; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6^(10), 1972, pp. 922-927.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
or $20 (bid) plus sampling costs.
B-226
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CHROMIUM
Air Samples
Laboratory Method 2
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acetate 1066-30-4
Chromic Acid 11115-74-5
Chromic Sulfate 10101-53-8
Chromium 7440-47-3
Chromous Chloride 10049-05-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Bichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Bichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOB SUMMARY:
Analysis for chromium and the above soluble chromium compounds in air
samples can be performed by filtration of a known volume of air through a
cellulose membrane filter, followed by acid digestion of the filter and its
contents and analysis of the resulting solution for chromium by atomic absorp-
tion (AA) spectrometry. This method measures the total nitric acid-soluble
chromium content of the sample and does not identify specific chromium com-
pounds or valence states.
INTERFERENCES:
Iron and nickel may interfere. Some chromium compounds may not be totally
dissolved by this procedure.
QUALITY CONTROL:
A method blank must be processed with each set of 10 samples and results
calculated using the method blank results.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH) and validated over the range of 0.493 to 1.830 milligrams
chromium per cubic meter, using a 90-liter sample. Measurement of lower
concentrations can be made by use of smaller solution volumes, longer sampling
times, or scale expansion. A method classified as operational by NIOSH is for
use over the range of 21 to 210 micrograms of chromium per cubic meter of air,
using a 240-liter sample. The detection limit stated by Alberta Environment is
B-227
-------
0.03 micrograms of chromium per cubic meter. The APHA states that a concentra-
tion of 0.005 micrograms chromium per cubic meter can be detected, using a
2000-cubic meter sample. Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set 0, Methods S323, S352; PB-262 402 (NTIS), U.S. DREW: Cincinnati, November
1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Methods S323, S352; Publication No. 77-157-C, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. Method P&CAM 152; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol 1., Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Alberta Environment, Methods Manual for Chemical Analyses of Atmospheric
Pollutants, Methods 23535, 23537; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Method 312; APHA: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-228
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CHROMIUM
Air Samples
Laboratory Method 3
Compound
Ammonium Chromate
Ammonium Dichromate
Calcium Chromate
Chromic Acetate
Chromic Acid
Chromic Sulfate
Chromium
Chromous Chloride
Lithium Chromate
Potassium Chromate
Potassium Dichromate
Sodium Chromate
Sodium Dichromate
Strontium Chromate
CAS Number
7788-
7789-
13765-
1066-
11115-
10101-
7440-
10049-
14307-
7789-
7778-
7775-
10588-
7789-
•98-9
•09-5
•19-0
30-4
74-5
53-8
•47-3
05-5
35-8
00-6
50-9
•11-3
•01-9
06-2
METHOD SUMMARY:
Analysis for the above chromium-containing compounds in air may be per-
formed by inductively coupled plasma atomic emission spectroscopic (ICP)
analysis for chromium. A known volume of air is drawn through a cellulose
ester membrane filter. The filter is ashed with a mixture of nitric and per-
chloric acid followed by analysis by ICP- This method does not identify any
specific chromium-containing compounds, but measures the total chromium content
of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms chromium
per cubic meter for a 500-liter sample. Limited precision and accuracy
information is furnished.
B-229
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REFERENCES:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Deter-
mination of Trace Metals Using Inductively Coupled Plasma Atomic Emission
Spectroscopy" pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Pro-
tection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-230
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CHROMIUM
Air Samples
Laboratory Method 4
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acid 11115-74-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Bichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Bichromate 10588-01-9
METHOB SUMMARY:
Particulate chromium compounds in air samples can be measured by reaction
kinetic analysis. The analyte is collected from a known volume of air on a
polyvinyl chloride filter. Chromium(VI) is extracted from the filter into
deionized distilled water by ultrasonic agitation and separated from interfer-
ing ions with a cation exchange resin. The chromium(VI) is determined by the
kinetics of a catalytic reaction. The chromium(VI) catalyzes the oxidation by
hydrogen peroxide of o-dianisidine to its semiquinone in an aqueous-ethanolic
solution near pH 4. The rate of production of the seraiquinone is proportional
to the concentration of chromium(VI) and is measured spectrophotometrically as
a function of time. This method does not identify any specific chromium-
containing compounds present, but measures the total chromium(VI) content of
the sample.
INTERFERENCES:
The ion exchange treatment step eliminates interfering ions.
QUALITY CONTROL:
A filter blank should be processed with the samples. Filters exposed to
standard air samples should also be processed to determine recovery. The value
of the blank and the recovery should be used in calculation of results.
EPA/TECHNICAL STATUS:
This method is classifed as proposed by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 0.01 to 0.25
milligrams chromium per cubic meter of air, using a 100-liter sample. Limited
precision and accuracy information is furnished.
B-231
-------
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 182; Publication No. 77-157-A, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost information has not been obtained.
B-232
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CHROMIUM
Air Samples
Laboratory Method 5
Compound
Ammonium Chrornate
Ammonium Dichromate
Calcium Chromate
Chromic Acetate
Chromic Acid
Chromic Sulfate
Chromium
Chromous Chloride
Lithium Chromate
Potassium Chromate
Potassium Dichromate
Sodium Chromate
Sodium Dichromate
Strontium Chromate
CAS Number
7788-
7789-
13765-
1066-
11115-
10101-
7740-
10049-
14307-
7789-
7778-
7775-
10588-
7789-
•98-9
09-5
•19-0
30-4
•74-5
53-8
•47-3
05-5
•35-8
00-6
•50-9
11-3
•01-9
06-2
METHOD SUMMARY:
Analysis of air for chromium and the above chromium-containing compounds
can be performed by colorimetry. A known volume of air is passed through
silver metal membrane filters for soluble particulate chromium and compounds,
while insoluble chromium particulates are collected on cellulose ester-type
membrane filters. The collected samples are oxidized to transform all chromium
present to the hexavalent state, which is then reacted with _s-diphenylcarbazide.
The intensity of the color of the resulting complex is measured with a spectro-
photometer. This method does not identify any specific chromium-containing
compound, but measures the total hexavalent and/or trivalent chromium content
or the total bivalent and metallic chromium content of the sample. The method
requires a special fusion step for determination of insoluble chromium in
particulates.
INTERFERENCES:
Iron and vanadium react with _s-diphenylcarbazide to produce yellow-brown
colors, and mercury produces a violet precipitate very slowly, which can be
avoided by the addition of sodium chloride. Extraction at pH 4 with 8-quinolinol
can be used to remove large amounts of iron, molybdenum, copper, and vanadium.
Nitrates are detrimental to color stability, and interferences from iron can be
reduced by addition of phosphate buffer before the color reagent.
QUALITY CONTROL:
No quality control procedures are provided.
B-233
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EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable to chromium
concentrations of 0.02 milligrams and greater per cubic meter, using a 150-liter
sample. Limited precision and accuracy information is furnished.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards
Vol. 11.03, Method D 3586-77; ASTM: Philadelphia, 1983.'
COST INFORMATION:
Cost information has not been obtained.
B-234
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CHROMIUM
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Dichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acetate 1066-30-4
Chromic Acid 11115-74-5
Chromic Sulfate 10101-53-8
Chromium 7740-47-3
Chromous Chloride 10049-05-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Dichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Dichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOD SUMMARY:
Analysis of soil/sediment samples for the above chromium compounds can be
performed by atomic spectrometric analysis for chromium. A 2-gram solid sample
is digested with nitric acid and hydrogen peroxide, and analyzed by inductively
coupled plasma (ICP) or flame atomic absorption spectrometry (AA). Analysis
for chromium in oily samples may be performed by ICP, after diluting the sample
with methyl isobutyl ketone (MIBK) or xylene, using standards miscible with
these solvents. These methods measure only the total chromium content of
samples and do not differentiate between various compounds and/or oxidation
states.
INTERFERENCES:
Iron, nickel, and other metals in the sample may cause interferences when
using flame atomic absorption spectrometry.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
Standards should be analyzed at least daily and a reference standard should be
analyzed weekly. At least 10 percent of the analyses should be duplicates
and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for
Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
Limited precision and accuracy information is furnished.
B-235
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REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072); U.S. EPA: Cincinnati, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 218.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Cincinnati, December 1982.
Federal Register, ^4_(233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 3040, 3050, 6010, 7190,
7191; SW-846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., 48(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $20-30 (list); by ICP,
it is approximately $20 (list).
B-236
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CHROMIUM
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acetate 1066-30-4
Chromic Acid 11115-74-5
Chromic Sulfate 10101-53-8
Chromium 7740-47-3
Chromous Chloride 10049-05-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Bichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Bichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOB SUMMARY:
Analysis for the above chromium compounds in water samples may be per-
formed by atomic spectrometric analysis for chromium. A 100-milliliter sample
is digested with nitric acid and hydrogen peroxide and analyzed by atomic
spectrometry. For low concentrations, either furnace atomic absorption
spectrometry (AA) or extraction of the sample at pH 3 to 9 with ammonium
pyrrolidinedithiocarbamate and methyl isobutyl ketone and AA analysis of the
extract is used, while inductively coupled plasma (ICP) spectrometry or flame
AA can be used for higher-concentration samples. This method measures total
chromium concentration and does not identify specific chromium-containing
compounds or chromium oxidation states.
INTERFERENCES:
Iron, nickel, and cobalt at 100 micrograms per liter and magnesium at 30
milligrams per liter cause a negative interference in flame AA, which can be
eliminated by additon of 8-hydroxyquinoline to samples.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly, and at least 10 percent of the
analysis should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for
Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
B-237
-------
Precision and accuracy information is furnished. The detection limit is 0.05
milligrams chromium per liter for flame AA analysis, 21 micrograms chromium per
liter for furnace AA, and 7 micrograms chromium per liter for ICP (instrumental
detection limit).
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 218.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Federal Register, 44(233). December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste^
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 6010, 7190, 7191;
SW-846, U.S. EPA: Washington, 1982.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 303A, 303B; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Method D1687; ASTM: Philadelphia, 1983.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by furnace AA is approximately $18-50 (list):
by ICP, approximately $10 (list); by extraction/AA, approximately $30-80
(list); and by flame AA, approximately $10-20 (list).
B-238
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CHROMIUM, HEXAVALENT
Air Samples
Laboratory Method
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acid 11115-74-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Dichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Dichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOD SUMMARY:
The above hexavalent chromium compounds in air samples may be measured by
colorimetry. A known volume of air is drawn through a polyvinyl chloride
filter. The filter is extracted with hot 3-percent sodium carbonate/2-percent
sodium hydroxide solution to dissolve all Cr(VI) and to protect it from
reduction to Cr(III). The extract is acidified with sulfuric acid, sym-
diphenylcarbazide is added, and the absorbance of the resulting solution at 540
nanometers is measured. This method does not identify any specific chromium
compound, but measures the total hexavalent chromium content of the sample.
INTERFERENCES:
High concentrations of iron, vanadium, mercury, or nitrate in the sample
can interfere.
QUALITY CONTROL:
One method blank is processed along with every 10 samples, and its value
is used as a correction in the final calculation.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 0.5 to 10 micrograms per
cubic meter, using a 600-liter sample. Precision and accuracy information is
furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 6, Method P&CAM 319; Publication No. 80-125, U.S. DHHS:
Cincinnati, August 1980.
B-239
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-50
(list), plus sampling costs.
B-240
-------
CHROMIUM, HEXAVALENT
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chromate 13765-19-0
Chromic Acid 11115-74-5
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Dichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Dichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOD SUMMARY:
Soil/sediment samples may be analyzed for the above hexavalent chromium
compounds by coprecipitation and atomic absorption spectrometry (AA), by color-
imetry, or by chelation-extraction and atomic spectrometry. The sample must be
digested before analysis. For analysis by coprecipitation/AA, the hexavalent
chromium in a sample is coprecipitated as lead chromate, and the lead chromate
is separated from the supernatant. It is reduced, redissolved, and measured as
trivalent chromium using either flame or furnace AA. For analysis by colori-
metry, the dissolved hexavalent chromium is reacted with diphenylcarbazide and
the concentration of the product is measured spectrophotometrically. For
analysis by the chelation-extraction method, the hexavalent chromium in the
sample is chelated and extracted with methyl isobutyl ketone (MIBK), and the
extract is analyzed by flame AA.
INTERFERENCES:
Samples containing high concentrations of sulfate and chloride should be
diluted before coprecipitation/AA analysis. High concentrations of molybdenum,
vanadium, iron, and mercury in the sample may interfere with colorimetric
analysis. High concentrations of other metals in the sample may interfere with
chelation-extraction/AA procedures. In all cases, the samples should be
stored at 4°C and the analysis should be carried out as soon as possible.
QUALITY CONTROL:
For every sample matrix analyzed, it must be determined if a reducing
condition or chemical interference is present by analysis of a fortified
sample. Recovery must be 85 to 115 percent for colorimetry. The method of
standard additions may be necessary. Spikes, blanks, duplicates, and check
standards must be analyzed approximately every 10 to 15 samples.
B-241
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EPA/TECHNICAL STATUS:
These methods are approved for the Resource Conservation and Recovery Act
(RCRA, 40 CFR, Part 261, Identification and Listing of Hazardous Wastes).
Precision or accuracy information is not furnished.
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 7195, 7196, 7197; SW-846, U.S.
EPA: Washington, 1982.
COST INFORMATION:
Cost per sample for analysis by chelation-extraction/AA is approximately
$30-65 (list); by colorimetry, approximately $20-25 (list); and by coprecipita-
tion/AA, approximately $20-70 (list).
B-242
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CHROMIUM, HEXAVALENT
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Chromate 7788-98-9
Ammonium Bichromate 7789-09-5
Calcium Chroraate 13765-19-0
Chromic Acetate 1066-30-4
Chromic Acid 11115-74-5
Chromic Sulfate 10101-53-8
Lithium Chromate 14307-35-8
Potassium Chromate 7789-00-6
Potassium Bichromate 7778-50-9
Sodium Chromate 7775-11-3
Sodium Bichromate 10588-01-9
Strontium Chromate 7789-06-2
METHOB SUMMARY:
Water samples may be analyzed for the above hexavalent chromium compounds
by coprecipitation and atomic absorption spectrometry (AA), by colorimetry, or
by chelation-extraction and AA. The sample must be digested before analysis.
For analysis by coprecipitation/AA, the hexavalent chromium in a sample is
coprecipitated as lead chromate and the lead chromate is separated from the
supernatant. It is reduced, redissolved, and measured as trivalent chromium
using either flame or furnace AA. For analysis by colorimetry, the dissolved
hexavalent chromium sample is reacted with diphenylcarbazide and the product
concentration is measured spectrophotometrically. For analysis by the chela-
tion-extraction method, the hexavalent chromium in a 100-milliliter sample is
chelated and extracted with methyl isobutyl ketone (MIBK), and the extract is
analyzed by flame AA.
INTERFERENCES:
Samples containing high concentrations of sulfate and chloride should be
diluted before coprecipitation/AA analysis. High concentrations of molybdenum,
vanadium, iron, and mercury in the sample may interfere with colorimetric
analysis. High concentrations of other metals in the sample may interfere with
chelation-extraction/AA procedures. In all cases, the samples should be
stored at 4°C and the analysis should be carried out as soon as possible.
QUALITY CONTROL:
For every sample matrix analyzed, it must be determined if a reducing
condition or chemical interference is present by analysis of a fortified sample,
Recovery must be 85 to 115 percent for colorimetry. The method of standard
additions may be necessary. Spikes, blanks, duplicates, and check standards
must be analyzed approximately every 10 to 15 samples.
B-243
-------
EPA/TECHNICAL STATUS:
These methods are approved for the Resource Conservation and Recovery Act
(RCRA, 40 CFR, Part 261, Identification and Listing of Hazardous Wastes).
Precision and accuracy information is furnished. The colorimetric method is
applicable over the range from 0.01 to 0.4 milligrams chromium per liter.
Limited precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste;
Physical/Chemical Methods, 2nd ed., Methods 7195, 7196, 7197; SW-846, U.S.
EPA: Washington, 1982.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 218.5; EPA-600/4-82-055, U.S.
EPA: Cincinnati, December 1982.
Alberta Environmental Centre, Methods Manual for Chemical Analysis of Water and
Wastes, "Chromium, Hexavalent, Dissolved;" Publication No. AECV81-M1, Alberta
Environmental Centre: Vegreville, Alberta, Canada, 1981.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 3128; APHA: Washington, 1980.
COST INFORMATION;
Cost per sample for analysis by chelation extraction/AA is approximately
$30-65 (list); by colorimetry, approximately $20-25 (list) and by coprecipita-
tion/AA, approximately $20-70 (list).
B-244
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CHROMIUM, TRIVALENT
Water Samples
Laboratory Method
Compound CAS Number
Chromic Acetate 1066-30-4
Chromic Sulfate 10101-53-8
METHOD SUMMARY:
A colorimetric method may be used to analyze water samples for the above
trivalent chromium compounds, which are decomposition products of hexavalent
chromium compounds after reaction with organic molecules or other easily
oxidized substances. A 150-milliliter sample is mixed with hydrochloric acid
and ion exchange resin to remove any hexavalent chromium present. The remain-
ing chromium is oxidized, concentrated, acidified, then treated with sym-
diphenylcarbazide color reagent. The intensity of the developed color is
measured by spectrophotometer or filter photometer and is proportional to the
original amount of trivalent chromium in the sample. This method does not
differentiate between trivalent chromium-containing compounds, but measures the
total trivalent chromium content of the sample.
INTERFERENCES:
This method should not be used if organic matter in the sample cannot be
easily oxidized or is present in greater concentrations than 100 milligrams per
liter. Precipitable hydroxides and large concentrations of iron may interfere.
Large amounts of phosphate or alkali earth metals may cause the loss of chromium.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The method will determine trivalent chromium concentrations of 0.5
to 5.0 milligrams per liter.
REFERENCE:
American Society for Testing and Materials, Annual Book of ASTM Methods,
Volume 11.01, Method D 1687; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $50-55
(list).
B-245
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COBALT
Air Samples
Laboratory Method 1
Compound CAS Number
Cobaltous Bromide 7789-43-7
Cobaltous Formate 544-18-3
Cobaltous Sulfamate 14017-41-5
METHOD SUMMARY:
Analysis for the above particulate cobalt compounds in air samples may be
performed by flame atomic absorption (AA) spectrometric determination of cobalt.
A known volume of air is drawn through a membrane or glass-fiber filter. The
filter with the collected particulates is digested with nitric or nitric and
hydrofluoric acids, and an aliquot of the solution containing the analyte is
aspirated into the AA, either by direct aspiration, or after filter digestion,
the resulting solution is extracted, and the resulting extract is then analyzed
by AA. This method does not identify any specific cobalt-containing compound,
but measures the total cobalt content of the sample.
INTERFERENCES:
Some cobalt compounds may not be dissolved completely by this procedure.
QUALITY CONTROL:
A blank should be processed with every 10 samples. Standard solutions
should be analyzed in duplicate.
EPA/TECHNICAL STATUS;
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 2.1 to 210
micrograms of cobalt per cubic meter, using a 240-liter air sample. Precision
information is furnished. The detection limit stated by Alberta Environment is
0.001 micrograms of cobalt per cubic meter-
REFERENCES:
U.S. Department of Health, Education and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW, 1977.
Alberta Environment Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23538, Alberta Environmental Centre: Vegreville,
Alberta, Ontario, 1981.
B-246
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Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-247
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COBALT
Air Samples
Laboratory Method 2
Compound CAS Number
Cobaltous Bromide 7789-43-7
Cobaltous Formate 544-18-3
Cobaltous Sulfamate 14017-41-5
METHOD SUMMARY:
Analysis for the above cobalt-containing compounds in air may be performed
by inductively coupled plasma atomic emission spectroscopic (TCP) analysis for
cobalt. A known volume of air is drawn through a cellulose ester membrane
filter. The filter is ashed with a mixture of nitric and perchloric acids
followed by analysis by ICP- This method does not identify any specific
cobalt-containing compound, but measures the total cobalt content of the
sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms
cobalt per cubic meter, using a 500-liter sample. Limited precision and
accuracy information is furnished.
REFERENCES:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals by Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-125: EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
B-248
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs).
B-249
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COBALT
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Cobaltous Bromide 7789-43-7
Cobaltous Formate 544-18-3
Cobaltous Sulfamate 14017-41-5
METHOD SUMMARY:
Analysis of soil/sediment samples for the above cobalt compounds can be
performed by atomic absorption spectrometry (AA). Samples of 100 milligrams
are digested with perchloric acid, nitric acid, hydrofluoric acid, and boric
acid, and analyzed for cobalt by AA. Samples should be stored in polyurethane
bags and frozen immediately after collection. This method does not identify
any specific cobalt compound, but measures the total cobalt content of the
sample.
INTERFERENCES:
Chemical interferences in the sample may require solvent extraction
techniques; standard and sample compositions should be closely matched.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCES:
Environment Canada, Analytical Methods Manual; NAQUADAT No. 27050, Environment
Canada, Inland Waters Directorate, Water Quality Branch: Ottawa, Canada, 1975.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-30
(list).
B-250
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COBALT
Water Samples
Laboratory Method
Compound CAS Number
Cobaltous Bromide 7789-43-7
Cobaltous Formate 544-18-3
Cobaltous Sulfamate 14017-41-5
METHOD SUMMARY:
Analysis of water samples for the above cobalt compounds can be performed
by atomic spectrometric analysis for cobalt. A 100-milliliter sample is
digested with nitric acid and hydrogen peroxide and analyzed by atomic
spectrometry. For low concentrations, either furnace atomic absorption
spectrometry (AA) or extraction of the sample at pH 2 to 10 with ammonium
pyrrolidine dithiocarbamate and methyl isobutyl ketone followed by AA analysis
of the extract is used, while inductively coupled plasma spectrometry (ICP) can
be used for higher-concentration samples. This method measures the total
cobalt content of the sample and does not differentiate among various cobalt-
containing compounds.
INTERFERENCE:
No specific interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly, and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for Clean
Water Act analyses. Precision and accuracy information is furnished. The
detection limit for flame AA is 30 micrograms cobalt per liter, the sensitivity
is 0.2 milligrams per liter, and the optimum concentration range is 0.5 to 10
milligrams per liter (APHA). The chelation-extraction method is applicable in
the range 10 to 1000 micrograms of cobalt per liter (ASTM).
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 219.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
B-251
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Federal Register, 44(233), December 3, 1979, pp. 69559-69564.
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol.
Ill, Available Laboratory Analytical Methods, " Methods for the Determination of
Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectroscopy,"
pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection Agency:
Las Vegas, 1984.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 303A, 303B, APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Method D 3558-82; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by AA is approximately $18-60 (list); by ICP,
it is approximately $10 (list).
B-252
-------
COPPER
Air Samples
Laboratory Method 1
Compound CAS Number
Copper 7440-50-8
Copper Cyanides 544-92-3
Cupric Acetate 142-71-2
Cupric Acetoarsenite 12002-03-8
Cupric Chloride 7447-39-4
Cupric Nitrate 3251-23-8
Cupric Oxalate 5893-66-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Cupric Tartrate 815-82-7
METHOD SUMMARY:
Atomic absorption spectrometry may be used to analyze air samples for
dusts and mists containing the above copper compounds. A known volume of
air is drawn through a cellulose ester membrane, followed by acid digestion of
the sampling media and atomic absorption (AA) spectrometric analysis of the
resulting solution. This method measures the total copper content of the
sample and does not identify specific copper compounds.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
The percent recovery of the analysis must be determined for each sample or
set of samples processed.
EPA/TECHNICAL STATUS:
This method is approved for National Institute for Occupational Safety and
Health (NIOSH) compliance analyses and has been validated over the range of 0.5
to 2 milligrams of copper per cubic meter. Precision and accuracy information
is furnished. A method classified by NIOSH as operational is for use over the
range of 21 to 210 micrograms of copper per cubic meter of air, using a 240-
liter sample. The limit of detection is 0.01 micrograms per cubic meter of air
(Alberta Environment). An atmospheric concentration of 0.005 micrograms per
cubic meter can be detected for a minimum sample volume of 2000 cubic meters
(APHA).
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set M, Method S186; PB-265 029 (NTIS), U.S DHEW: Cincinnati, 1976.
B-253
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U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S186; Publication No. 77-157-C, U.S. DHEW^
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.jT.
DREW: Cincinnati, 1977.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals";
DOE: New York, 1983.
Alberta Environment, Methods Manual for Chemical Analyses of Atmospheric
Pollutants, Method 23535, 23539; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Method 313; APHA: Washington, 1977-
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-254
-------
COPPER
Air Samples
Laboratory Method 2
Compound CAS Number
Copper 7440-50-8
Copper Cyanides 544-92-3
Cupric Acetate 142-71-2
Cupric Acetoarsenite 12002-03-8
Cupric Chloride 7447-39-4
Cupric Nitrate 3251-23-8
Cupric Oxalate 5893-66-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Cupric Tartrate 815-82-7
METHOD SUMMARY:
Analysis for the above copper compounds in air may be performed by filtra-
tion of air and analysis of the filter medium for copper by X-ray fluorescence
spectrometry. The method is non-destructive, so that further analyses may be
performed on samples. The sample-collection time may be up to 8 hours, but
analysis time is approximately 1 minute. The method measures total copper
present in the sample, and does not differentiate between chemical compounds or
copper valence states .
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-
fiber filters are acceptable for use only if they are of the highest purity.
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is sensitive to amounts of
copper above 35 micrograms and is applicable to 0.01 to 1.0 microgram of copper
per cubic meter, depending on sample size. Precision information is furnished.
REFERENCES:
Rhodes, J. R.; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
B-255
-------
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas "
Environ. Sci. Technol., 6_(10), 1972, pp. 922-927.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list)
$20 (bid), plus sampling costs.
B-256
-------
COPPER
Air Samples
Laboratory Method 3
Compound
CAS Number
Copper
Copper Cyanide
Cupric Acetate
Cupric Acetoarsenite
Cupric Chloride
Cupric Nitrate
Cupric Oxalate
Cupric Sulfate
Cupric Sulfate, Ammoniated
Cupric Tartrate
7440-50-8
544-92-3
142-71-2
12002-03-8
7447-39-4
3251-23-8
5893-66-3
7758-98-7
10380-29-7
815-82-7
METHOD SUMMARY:
Analysis for the above copper-containing compounds in air may be performed
by inductively coupled plasma atomic emission spectroscopic (ICP) analysis for
copper. A known volume of air is drawn through a filter, the filter is ashed
with a mixture of nitric and perchloric acids, and the resulting solution is
analyzed by ICP. This method does not identify any specific copper-containing
compound, but measures the total copper content of the sample.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms copper
per cubic meter, using a 500-liter sample. Limited precision and accuracy
information is furnished.
REFERENCES:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
B-257
-------
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-258
-------
COPPER
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Copper 7440-50-8
Copper Cyanides 544-92-3
Cupric Acetate 142-71-2
Cupric Acetoarsenite 12002-03-8
Cupric Chloride 7447-39-4
Cupric Nitrate 3251-23-8
Cupric Oxalate 5893-66-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Cupric Tartrate 815-82-7
METHOD SUMMARY:
Analysis of soil/sediment samples for the above copper compounds can be
performed by atomic spectrometric analysis for copper. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and analyzed by inductively
coupled plasma (1CP) or flame atomic absorption (AA) spectrometry. Flame AA
spectrometry is not recommended for low levels of copper. These methods do not
identify specific copper-containing compounds, but measure the total copper
content of the sample.
INTERFERENCES:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analyzed weekly, and at least 10 percent
of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for Clean
Water Act analyses. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 219.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
B-259
-------
Federal Register, 4^(233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 3010, 3020, 3050, 6010, 7210, 72fT;
SW-846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry-." pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem. , ^8_(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $24 (list); by
ICP, it is approximately $20 (list).
B-260
-------
COPPER
Water Samples
Laboratory Method
Compound CAS Number
Copper 7440-50-8
Copper Cyanides 544-92-3
Cupric Acetate 142-71-2
Cupric Acetoarsenite 12002-03-8
Cupric Chloride 7447-39-4
Cupric Nitrate 3251-23-8
Cupric Oxalate 5893-66-3
Cupric Sulfate 7758-98-7
Cupric Sulfate, Ammoniated 10380-29-7
Cupric Tartrate 815-82-7
METHOD SUMMARY:
Analysis of water samples for the above copper compounds can be performed
by atomic spectrometric analysis for copper. A 100-milliliter sample is
digested with nitric acid and hydrogen peroxide and analyzed by flame-atomiza-
tion atomic absorption spectrometry (AA) or inductively coupled plasma spec-
trometry (ICP). Furnace atomization, rather than flame, AA is recommended for
low levels of copper. For low levels, chelation/extraction with ammonium
pyrrolidine dithiocarbamate in chloroform followed by digestion and AA analysis
can also be used. These methods do not identify specific copper-containing
compounds, but measure the total copper content of the sample.
INTERFERENCES:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
QUALITY CONTROL:
A reference standard should be analzyed weekly- Standards should be
analyzed at least daily, and at least 10 percent of the analyses should be
duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for Clean
Water Act and Resource Conservation and Recovery Act analyses. Precision and
accuracy information is furnished. The detection limit is 0.02 milligrams per
liter, the sensitivity is 0.12 milligrams per liter, and the optimum concentra-
tion range is 0.3 to 10 milligrams per liter for flame AA (APHA). For the
chelation/extraction AA method, the optimum concentration range is 2 to 500
micrograms per liter (ASTM).
B-261
-------
REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 220.1, 200.2; EPA-600/4-79-020, U.S. EPA: Cincinnati,
1979.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Cincinnati, 1982.
Federal Register, ^4(233), December 3, 1979, pp. 69559-69564.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 3050, 6010, 7210, 7211;
SW-846, U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by Atomic
Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, J. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption"; HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 303A; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, D1688-82; ASTM: Philadelphia, 1983.
Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem., 48(3), 1976, pp. 516-519.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list);
by ICP, it is approximately $10 (list).
B-262
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CYANIDES
Air Samples
Laboratory Method
Compound CAS Number
Barium Cyanide 542-62-1
Calcium Cyanide 592-01-3
Copper Cyanide 544-92-3
Cyanide 57-12-5
Cyanogen 460-19-5
Cyanogen Bromide 506-68-3
Cyanogen Chloride 506-77-4
Mercuric Cyanide 592-04-1
Nickel Cyanide 557-19-7
Potassium Cyanide 151-50-8
Potassium Silver Cyanide 506-61-6
Silver Cyanide 506-64-9
Sodium Cyanide 143-33-9
Zinc Cyanide 557-21-1
METHOD SUMMARY:
Analysis for the above cyanides in air can be performed by passage of a
known volume of air through a cellulose membrane filter and an impinger charged
with 0.1-norraal sodium hydroxide (in series), extraction of the filter with
sodium hydroxide and analysis of the two resulting solutions with a cyanide
ion-specific electrode and a pH/millivolt meter. This method does not identify
any specific cyanide compound, but measures the total cyanide content of the
air sample.
INTERFERENCES:
Sulfide ions irreversibly poison the electrode and may be removed by
addition of a small amount of cadmium carbonate to the solution. High concen-
trations of other ions that form insoluble silver salts will also cause the
electrode to malfunction, as will the presence of cations that form cyano-
coraplexes. Gaseous hydrogen cyanide is an interference.
QUALITY CONTROL:
Sample recovery should be determined and a method blank should be pro-
cessed with each set of 10 or fewer samples. Results of method-blank analyses
and sample recovery determinations should be used in the calculation of the
results.
EPA/TECHNICAL STATUS:
Method S250 is approved by the National Institute for Occupational Safety
and Health (NIOSH), and has been validated over the range of 2.6 to 9.7
milligrams cyanide per cubic meter, using a 90-liter air sample. Method P&CAM
B-263
-------
116 is classified as operational by NIOSH for use over the range of 0.013 to 13
milligrams per cubic meter. Precision and accuracy information is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 116; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S250; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
American Public Health Service, Methods of Air Sampling and Analysis, 2nd ed.,
Method 808; APHA: Washington, 1977^
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set R, Method S250; PB-262 403 (NTIS), U.S. DHEW: Cincinnati, December 1976.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $35 (list),
plus sampling costs.
B-264
-------
CYANIDES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Barium Cyanide 542-62-1
Calcium Cyanide 592-01-8
Copper Cyanide 544-92-3
Cyanide 57-12-5
Cyanogen 460-19-5
Cyanogen Bromide 506-68-3
Cyanogen Chloride 506-77-4
Hydrogen Cyanide 74-90-8
Mercuric Cyanide 592-04-1
Nickel Cyanide 557-19-7
Potassium Cyanide 151-50-8
Potassium Silver Cyanide 506-61-6
Silver Cyanide 506-64-9
Sodium Cyanide 143-33-9
Zinc Cyanide 557-21-1
METHOD SUMMARY:
Determination of the above cyanides in soil/sediment samples can be done
colorimetrically or by titrimetry. The cyanide in a 1-gram soil/sediment
sample is distilled from an acidic solution into sodium hydroxide. The cyanide
in the distillate is determined by either conversion to cyanogen chloride and
colorimetry or by titration with silver nitrate. Chlorination preceeding
distillation allows determination of total cyanide, including iron complexes.
This method does not identify any specific cyanide-containing compounds, but
measures the total cyanide content of the sample.
INTERFERENCES:
Samples should be preserved with sodium hydroxide after collection and
stored at 4°C. All standards and samples must have the same salt content.
QUALITY CONTROL:
A blank, duplicate, spiked sample, and a reference standard must be dis-
tilled and analyzed with each 10 samples.
EPA/TECHNICAL STATUS:
This method is in use in the CERCLA program and is approved for use under
the Resource Conservation and Recovery Act. No precision or accuracy informa-
tion is furnished.
B-265
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REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 9010: SW-846, U.S. EPA: Washington^
1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $43-63
(list).
B-266
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CYANIDES
Water Samples
Laboratory Method
Compound CAS Number
Barium Cyanide 542-62-1
Calcium Cyanide 592-01-8
Copper Cyanide 544-92-3
Cyanide 57-12-5
Cyanogen 460-19-5
Cyanogen Chloride 506-77-4
Hydrogen Cyanide 74-90-8
Mercuric Cyanide 592-04-1
Nickel Cyanide 557-19-7
Potassium Cyanide 151-50-8
Potassium Silver Cyanide 506-61-6
Silver Cyanide 506-64-9
Sodium Cyanide 143-33-9
Zinc Cyanide 557-21-1
METHOD SUMMARY:
Analysis of water samples for the above cyanides can be performed by
colorimetry, titrimetry, or potentiometry. The cyanide in the sample can be
released and converted to cyanogen chloride, which is determined colorimetri-
cally. Alternatively, the acidified sample can be heated and hydrocyanic acid
distilled into sodium hydroxide, and the resulting solution analyzed titrimetri-
cally, colorimetrically, or potentiometrically with a cyanide-specific elec-
trode. Titration is used for higher-level concentrations and colorimetry or
potentiometry is used for lower levels. These methods do not identify specific
cyanide-containing compounds, but measure the total cyanide content of the
sample.
INTERFERENCES:
In some instances, thiocyanates in the sample will cause a positive inter-
ference. Titration cannot be used with samples containing fatty acids. In all
methods, samples must be preserved with sodium hydroxide at the time of collec-
tion and stored at 4°C. Sulfides and oxidizing agents in the sample require
the addition of cadmium carbonate and ascorbic acid, respectively.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for use in
Clean Water Act and Resource Conservation and Recovery Act analyses. Precision
and accuracy information is furnished. The cyanogen chloride method has a
B-267
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limit of detection of approximately 1 milligram cyanide per liter. The dis-
tillation-only method has limits of detection of 1.0, 0.03, and 0.03 milligrams
cyanide per liter, respectively, depending on whether measurements are by
titrimetry, colorimetry, or ion-selective electrode.
REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 335.2, 335.3; EPA-600/4-79-020, U.S. EPA: Cincinnati, March
1979.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, Method D2036-82, ASTM: Philadelphia, 1983.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Method 9010; SW-846, U.S. EPA: Washington,
1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Cyanide," pp. IV-126 to IV-135; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
Alberta Environmental Centre, Methods Manual for Chemical Analysis of Water
and Wastes, "Cyanide;" Publication No. AECV81-M1, Alberta Environmental Centre,
Vegreville, Alberta, Canada, 1981.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 412A, 412B, 412C, 412D, 412E: APHA:
Washington, 1980.
COST INFORMATION:
Cost per sample for analysis by these methods is approximately $28-40
(list).
B-268
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FLUORIDES
Air Samples
Laboratory Method 1
Compound CAS Number
Antimony Trifluoride 7783-56-4
Beryllium Fluoride 7787-49-7
Ferric Fluoride 7783-50-8
Lead Fluoride 7783-46-2
Sodium Fluoride 7681-49-4
Zinc Fluoride 7783-49-5
METHOD SUMMARY:
Analysis for the above water-soluble particulate fluoride compounds in air
can be performed by filtration and use of an ion-selective electrode. After
high-volume glass-fiber filtration of air for 24 hours, the fluoride is
extracted from the filter and the fluoride concentration in the extract is
determined with a fluoride-specific electrode and an expanded-scale pH/milli-
volt meter. Five standard fluoride solutions should be used to calibrate the
instrument. This method does not identify the fluoride-containing compounds
present, but measures the total water-soluble particulate fluoride content of
the sample.
INTERFERENCES:
Polyvalent cations such as Si(IV), Fe(III), and Al(III) can interfere.
A Total Ionic Strength Activity Buffer (TISAB) is used to eliminate these
interferences.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved, but is used by Environment Canada. No
precision or accuracy information is furnished. The method is sensitive to
concentrations of fluoride above 10 nanograms per cubic meter of air.
REFERENCES:
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Method 23030; Alberta Environmental Centre: Vegreville, Alberta,
Canada, 1981.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.03, Methods D3269-79 (11) and D3270-80; ASTM: Philadelphia, 1983.
B-269
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $25-44
(list), plus sampling costs.
B-270
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FLUORIDES
Air Samples
Laboratory Method 2
Compound
Ammonium Bifluoride
Ammonium Fluoride
Beryllium Fluoride
Ferric Fluoride
Hydrogen Fluoride
Lead Fluoride
Sodium Bifluoride
Sodium Fluoride
Zinc Fluoride
CAS Number
1341-49-7
12125-01-8
7787-49-7
7783-50-8
7664-39-3
7783-46-2
1333-83-1
7681-49-4
7783-49-5
METHOD SUMMARY:
Analysis of air samples for the above fluorides can be performed spectro-
photometrically. The sample is collected in a bubbler containing hot (70°C)
sulfuric acid, which dissolves most interferences and releases the fluoride.
The fluoride is then trapped in a solution of 0.05-percent sulfamic acid. Any
nitrate present will react with the sulfamic acid and be converted to nitrogen
gas. Alizarin complexone, lanthanum nitrate buffer, acetone, and distilled
water are added, in that order, to the fluoride solution. The absorbance is
measured at 618 nm on a spectrophotometer, and the concentration is obtained
from a standard curve. This method does not identify the specific fluoride-
containing compounds present, but measures the total fluoride content of the
sample.
INTERFERENCES:
When the sampling procedure described is followed, all likely interfer-
ences are removed.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision or accuracy information is
not given.
REFERENCES:
"Spectrophotometric Determination of Atmospheric Fluorides" In Environmental
Pollutants-Selected Analytical Methods (SCOPE 6); W. Gallay, H. Egan, J. L.
Monkman, R. Jruhaut, P. W. West, G. Widmark, Eds.; Ann Arbor Science: Ann
Arbor, 1975, pp. 231-235.
B-271
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American Society for Testing and Materials, 1983 Annual Book of ASTM Standards.
Vol. 11.03, Method D3269 (10); ASTM: Philadelphia, 1983.'
COST INFORMATION:
No cost information has been obtained.
B-272
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FLUORIDES
Air Samples
Laboratory Method 3
Compound CAS Number
Ammonium Bifluoride 1341-49-7
Ammonium Fluoride 12125-01-8
Beryllium Fluoride 7787-49-7
Ferric Fluoride 7783-50-8
Hydrogen Fluoride 7664-39-3
Lead Fluoride 7783-46-2
Sodium Bifluoride 1333-83-1
Sodium Fluoride 7681-49-4
Zinc Fluoride 7783-49-5
METHOD SUMMARY:
The above fluoride compounds in air samples may be measured using an
ion-specific electrode. A known volume of air is drawn through midget impingers
containing 0.1-molar sodium hydroxide. The samples are diluted 1:1 with Total
Ionic Strength Activity Buffer (TISAB) followed by analysis using the fluoride-
ion specific electrode. An alternative sampling and preparation procedure
employs a device containing a membrane filter to collect particulate fluorides
and an alkali-impregnated cellulose pad for gaseous fluorides. The filter and
particulates are made alkaline and ashed, the residue fused, and the melt
dissolved; the gaseous fluoride is extracted from the cellulose pad with water.
The solutions are treated with TISAB and analyzed.
INTERFERENCES:
Hydroxide ion is the only significant interference; however, the addition
of TISAB eliminates the problem. Large amounts of polyvalent metal ions such
as aluminum may result in low readings.
QUALITY CONTROL:
A method blank and standards are processed along with the samples.
EPA/TECHNICAL STATUS:
The method with impinger sampling is an operational one as defined by the
National Institute for Occupational Health and Safety (NIOSH), with a lower
limit of detection of 0.009 milligrams of fluoride per cubic meter of air. The
method with filtration sampling is defined as proposed by NIOSH, with a lower
limit of 0.005 milligrams per cubic meter of air. No precision or accuracy
information is furnished.
B-273
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REFERENCES;
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 117; Publication No. 75-121, U.S. DREW: Cincinnati, 1974.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 1, Method P&CAM 212; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater. 15th ed., Method 413; APHA: Washington, 1977.
American Society for Testing and Materials, ASTM 1983 Annual Book of Standards,
Vol. 11.03, D3269-72 (11), D3269-80; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-274
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FLUORIDES
Water Samples
Laboratory Method 1
Compound CAS Number
Ammonium Bifluoride 1341-49-7
Ammonium Fluoride 12125-01-8
Ammonium Silicofluoride 16919-19-0
Antimony Trifluoride 7783-56-4
Beryllium Fluoride 7787-49-7
Ferric Fluoride 7783-50-8
Hydrogen Fluoride 7664-39-3
Lead Fluoride 7783-46-2
Sodium Bifluoride 1333-83-1
Sodium Fluoride 7681-49-4
Zinc Fluoride 7783-49-5
Zinc Silicofluoride 16871-71-9
Zirconium Potassium Fluoride 16923-95-8
METHOD SUMMARY:
Automated colorimetry may be used to analyze water samples for the above
fluoride compounds. The sample is distilled, the distillate is reacted with
alizarin fluorine blue-lanthanum reagent, and the resulting blue complex is
analyzed colorimetrically with an automated spectrophotometric analysis system.
The method does not identify any specific fluoride compound, but determines the
total fluoride content of the sample.
INTERFERENCES:
Interference by aluminum may be removed by addition of 8-hydroxyquinoline
and extraction with chloroform before analysis.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use in Clean Water Act analyses.
This method is applicable to fluoride concentrations of approximately 0.05 to
1.5 milligrams per liter. No precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 340.3; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 413E; APHA: Washington, 1980.
B-275
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list).
B-276
-------
FLUORIDES
Water Samples
Laboratory Method 2
Compound CAS Number
Ammonium Bifluoride 1341-49-7
Ammonium Fluoride 12125-01-8
Ammonium Silicofluoride 16919-19-0
Antimony Trifluoride 7783-56-4
Beryllium Fluoride 7787-49-7
Ferric Fluoride 7783-50-8
Hydrogen Fluoride 7664-39-3
Lead Fluoride 7783-46-2
Sodium Bifluoride 1333-83-1
Sodium Fluoride 7681-49-4
Zinc Fluoride 7783-49-5
Zinc Silicofluoride 16871-71-9
Zirconium Potassium Fluoride 16923-95-8
METHOD SUMMARY:
Potentiometry may be used to analyze water samples for the above fluorides.
A 50-milliliter sample is distilled as is and the distillate is analyzed with a
fluoride-selective electrode and a pH/mV meter. This method does not identify
any particular fluoride-containing compound, but measures the total fluoride
content of the sample.
INTERFERENCES:
A pH 5 buffer containing a strong chelating agent should be added to
prevent possible interferences for silicon, iron, aluminum, and pH.
QUALITY CONTROL:
Blanks and standards should be analyzed periodically.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use in Clean Water Act analyses and will
detect fluoride concentrations of approximately 0.1 to 1000 milligrams per
liter. Limited precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 340.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 413; APHA: Washington, 1977.
B-277
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toerican Society for Testing and Materials, 1983 Annual Book of ASTM Standards
Vol. 11.01, D1179-80; ASTM: Philadelphia, 19&T. " ''
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards
Vol. 11.02, D3868-79; ASTM: Philadelphia, 1983^ '
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards.
. 11.03, D3269 (11); ASTM: Philadelphia, 1983. '
Mberta Environmental Centre, Methods Manual for Chemical Analysis of Water and
Pastes, "Fluoride, Dissolved;" Publication No. AECV81-M1, Alberta Environmental
Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $28-38
(list).
B-278
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FLUORIDES
Water Samples
Laboratory Method 3
Compound CAS Number
Ammonium Bifluoride 1341-49-7
Ammonium Fluoride 12125-01-8
Ammonium Silicofluoride 16919-19-0
Antimony Trifluoride 7783-56-4
Beryllium Fluoride 7787-49-7
Ferric Fluoride 7783-50-8
Hydrogen Fluoride 7664-39-3
Lead Fluoride 7783-46-2
Sodium Bifluoride 1333-83-1
Sodium Fluoride 7681-49-4
Zinc Fluoride 7783-49-5
Zinc Silicofluoride 16871-71-9
Zirconium Potassium 16923-95-8
Fluoride
METHOD SUMMARY:
Spectrophotometry may be used to analyze water samples for the above
fluorides. A 300-milliliter sample is distilled, after pretreatment for
chlorine residues, and the distillate is reacted with zirconyl-SPADNS dye. The
resultant color loss is measured spectrophotometrically. This method does not
identify any particular fluoride-containing compound, but measures the total
fluoride content of the sample.
INTERFERENCES:
The SPADNS reagent is more tolerant of interfering materials than other
accepted fluoride reagents. No specific interferences are reported.
QUALITY CONTROL:
Blanks and standards must be analyzed routinely.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use in Clean Water Act analyses and is
applicable to samples containing approximately 0.1 to 2.5 milligrams of
fluoride per liter. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 340.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
B-279
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American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Methods 809, 810; APHA: Washington, 1977.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards
Vol. 11.01, Method D 1179-80; ASTM: Philadelphia, 1983.~'
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list).
B-280
-------
HYDRAZINES
Air Samples
Laboratory Method
Compound CAS Number
1,1-Dimethylhydrazine 57-14-7
Hydrazine 302-01-2
Methylhydrazine 60-34-4
METHOD SUMMARY:
The above hydrazines in air samples may be measured by gas chromatography.
A known volume of air is drawn through a tube containing sulfuric acid-coated
silica gel to trap the hydrazine compounds. The analytes are desorbed with
distilled water and treated with a reagent containing sodium acetate and fur-
fural. The resulting derivatives are extracted into ethyl acetate and analyzed
by gas chromatography with flame ionization detection (GC/FID).
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
A blank should be processed with the samples.
EPA/TECHNICAL STATUS:
This method is proposed by the National Institute for Occupational Safety
and Health (NIOSH) for use over the ranges of 0.002 to 60 milligrams hydrazine,
0.09 to 90 milligrams methylhydrazine, and 0.04 to 120 milligrams 1,1-dimethyl-
hydrazine per cubic meter, based on a 96-liter air sample. Precision and
accuracy information is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 1, Method P&CAM 248; Publication No. 77-157-A, U.S.
DHEW: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $85-100
(list).
B-281
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INORGANIC ACIDS
Air Samples
Laboratory Method
Compound CAS Number
Hydrochloric Acid 7647-01-0
Nitric Acid 7697-37-2
Phosphoric Acid 7664-38-2
Sulfuric Acid 7664-93-9
METHOD SUMMARY:
Inorganic acids in air, including hydrochloric, nitric, phosphoric, and
sulfuric acids, may be measured using ion chromatography. A known volume of
air is drawn through a silica gel tube, followed by analyte desorption in a
heated dilute sodium bicarbonate/sodium carbonate solution. Ion chromatography
is used for the analyses of the resulting solutions.
INTERFERENCES:
Possible interferences include sulfur dioxide for sulfuric acid, nitrogen
dioxide for nitric acid, and chlorine or hypochlorite ion for hydrochloric
acid.
QUALITY CONTROL:
Method blanks and standards are analyzed with the samples.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range (in milligrams per
cubic meter) of 0.14 to 14 for hydrochloric acid, using a 15-liter sample, 1.0
to 10 for nitric acid, and 0.5 to 2 for phosphoric acid and sulfuric acid,
using a 48-liter sample. Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 339; Publication No. 82-100, U.S. DHHS: August
1981.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-11, "Determination
of Anions by Ion Chromatography;" HASL-300, Environmental Measurements Labora-
tory, U.S. DOE: New York, 1983.
COST INFORMTION:
Cost per sample for analysis by this method is approximately $80 (list).
B-282
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IODIDES AND BROMIDES
Water Samples
Laboratory Method
Compound CAS Number
Antimony Tribromide 7789-61-9
Cadmium Bromide 7789-42-6
Lead Iodide 10101-63-0
Zinc Bromide 7699-45-8
METHOD SUMMARY:
Analysis of water samples for iodide and/or bromide ions from the above
compounds can be performed by determination of bromide or iodide ion concentra-
tions. The iodide ion concentration can be determined volumetrically, by
oxidation of iodide to iodate with bromine, reduction of the iodate with iodine,
and titration of the iodine with sodium thiosulfate. The combined iodide and
bromide ion concentration can be determined volumetrically, by oxidation to
iodate and bromate with hypochlorite, reduction of the resulting iodate and
bromate with iodide to form iodine, and titration of the resulting iodine with
sodium thiosulfate. Alternatively, iodide in the sample can be oxidized with
nitrous acid and extracted into carbon tetrachloride. The intensity of the
iodine color at 517 nanometers is then measured colorimetrically. Bromide ions
can be oxidized to bromine with chromium trioxide, and the resulting bromine is
extracted into carbon tetrachloride and measured spectrophotometrically at 417
nanometers. Additionally, an iodide-selective electrode and millivolt meter
can be used. These methods do not identify any specific bromide- or iodide-
containing compound, but measure the total iodide and/or bromide ion content of
the sample.
INTERFERENCES:
The volumetric method suffers interferences from iron, manganese, and
organics. Iron and manganese can be removed by precipitation and filtration,
and traces of residual iron can be masked by the addition of fluoride. Inter-
ferences from hydrocarbons in the colorimetric determination of bromide can be
removed by a pre-extraction with carbon tetrachloride. In the colorimetric
iodide determination, chloride and bromide ions interfere, and interferences
from sulfide ions can be removed by buffering the sample at a pH below 6.
These methods are designed for brackish water, sea water, and brines.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The volumetric method is suitable for
concentrations from 0.2 to 2000 milligrams iodide per liter and 5 to 6500
milligrams bromide per liter. The colorimetric methods are applicable to the
B-283
-------
range 0.2 to 2000 milligrams iodide per liter and 40 to 6500 milligrams bromide
per liter, while the iodide-selective electrode method is applicable to
concentrations from 1 to 2000 milligrams of iodide per liter. Precision and
accuracy information is furnished.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards
Vol. 11.02, D3869-79; ASTM: Philadelphia, 198l!'
COST INFORMATION:
Cost per sample for analysis by the titrimetric methods are approximately
$20-50 (list); by the ion-selective electrode method, approximately $10-19
(list).
B-284
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IRON
Air Samples
Laboratory Method 1
Compound
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Dextran
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
CAS Number
1185'
2944-
55483-
7705-
9004-
7783-
10421-
10028-
10045-
7758-
7720
7782-
-57-5
-67-4
-87-4
-08-0
-66-4
-50-8
-48-4
-22-5
-89-3
-94-3
-78-7
-63-0
METHOD SUMMARY:
Analysis for the above particulate iron compounds in air can be performed
by filtration of air and analysis of the filter medium for iron by X-ray
fluorescence spectrometry. The method is non-destructive, so that further
analyses may be performed on samples. The sample-collection time may be up to
8 hours, but analysis time is approximately 1 minute. The method measures
total iron present in the sample, and does not differentiate between chemical
compounds or iron valence states.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-
fiber filters are acceptable for use only if they are of the highest purity.
Cellulose membrane, cellulose fiber, polycarbonate membrane, and fluorocarbon
membrane filters are acceptable.
QUALITY CONTROL:
Attenuation corrections must be included in the calculation of results.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
method should be applicable to 0.01 to 1.0 micrograms of iron per cubic meter,
depending on sample size.
B-285
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REFERENCES:
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-09, "Trace Metals
by X-ray Fluorescence;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
Rhodes, J. R. ; Stout, J. A.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for In Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP 786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R. ; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6/10), 1972, pp. 922-927.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
$20 (bid), plus sampling costs.
B-286
-------
IRON
Air Samples
Laboratory Method 2
Compound
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Dextran
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
CAS Number
1185-
2944-
55488-
7705-
9004-
7783-
10421-
10028-
10045-
7758-
7720-
7782-
57-5
67-4
87-4
•08-0
•66-4
•50-8
•48-4
•22-5
89-3
94-3
•78-7
63-0
METHOD SUMMARY:
Analysis for the above particulate iron compounds in air samples may be
performed by flame atomic absorption (AA) spectrometric determination of iron.
A known volume of air is drawn through a membrane or glass-fiber filter. The
filter with the collected particulates is digested with nitric or nitric and
hydrofluoric acid, and an aliquot of the resulting solution is aspirated into
the AA spectrometer. This method does not identify any specific iron com-
pound, but measures the total iron content of the sample.
INTERFERENCES:
High nickel and silica concentrations may interfere.
QUALITY CONTROL:
A blank should be processed with every 10 samples. Standard solutions
should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 21 to 210
micrograms of iron per cubic meter in a 240-liter air sample. Precision infor-
mation is furnished. The limit of detection determined by Alberta Environment
is 0.05 micrograms iron per cubic meter of air.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
B-287
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Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual.
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE, New York, 1983.
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23540; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
B-288
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IRON
Air Samples
Laboratory Method 3
Compound
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Dextran
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
CAS Number
1185-
2944-
55488-
7705-
9004-
7783-
10421-
10028-
10045-
7758-
7720-
7782-
•57-5
67-4
87-4
08-0
•66-4
50-8
•48-4
22-5
•89-3
94-3
•78-7
•63-0
METHOD SUMMARY:
Analysis for the above iron-containing compounds in air may be performed
by inductively coupled plasma atomic emission spectroscopy (ICP). A known
volume of air is drawn through a cellulose ester membrane filter. The filter
is ashed with a mixture of nitric and perchloric acids followed by analysis by
ICP- This method does not identify any specific iron-containing compound, but
measures the total iron content of the sample.
INTERFERENCES;
No specific interferences are reported.
QUALITY CONTROL:
Method blanks, spikes, and standards are prepared and processed with the
samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute of Occupational
Safety and Health (NIOSH) for use over the range of 5 to 2000 micrograms of
iron per cubic meter for a 500-liter sample. Limited precision and accuracy
information is furnished.
REFERENCES:
U.S. Department of Health and Services, NIOSH Manual of Analytical Methods,
Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DHHS: Cincinnati, August
1981.
B-289
-------
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $10 (list),
plus sampling costs.
B-290
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IRON
Soil/Sediment Samples
Laboratory Method
Compound
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Dextran
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
CAS Number
1185-
2944-
55488-
7705-
9004-
7783-
10421-
10028-
10045-
7758-
7720-
7782-
57-5
67-4
87-4
08-0
66-4
50-8
•48-4
22-5
89-3
94-3
•78-7
63-0
METHOD SUMMARY:
Analysis of soil/sediment samples for the above iron compounds can be
performed by atomic spectrometric analysis for iron. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and analyzed by inductively
coupled plasma (ICP) or flame atomic absorption spectrometry (AA). Direct AA
is not recommended for low levels of iron. Alternatively, the metal can be
chelated with pyrrolidinedithiocarbamic acid, the resulting complex extracted
with chloroform, and the extract analyzed by AA. Analysis for iron in oily
samples may be performed by ICP after sample dilution with methyl isobutyl
ketone (MIBK) or xylene, using standards miscible with these solvents. These
methods do not identify any specific iron-containing compounds, but measure the
total iron content of the sample.
INTERFERENCES:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
QUALITY CONTROL;
Standards should be analyzed at least daily and a reference standard
should be analyzed weekly. At least 10 percent of the analyses should be
duplicates and/or standards.
EPA/TECHNICAL STATUS:
The ICP and direct AA methods are in use in the CERCLA program and are
approved for use in Clean Water Act analyses. Precision and accuracy informa-
tion is furnished.
B-291
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REFERENCES:
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and
Wastes, Method 236.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
Federal Register, _44(233), December 3, 1979, pp. 69559-69564.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina-
tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro-
scopy," pp. IV-99 to IV-124; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
Fassell, V. A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simul-
taneous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry," Anal. Chem. , ^3_(3), 1976, pp. 516-519.
American Public Health Association, Standard Methods for the Examination of
Water and Wastes, 15th ed., Methods 303A, 303B; APHA: Washington, 1980.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $20-30 (list);
by ICP, it is approximately $20 (list).
B-292
-------
IRON
Water Samples
Laboratory Method 1
Compound
CAS Number
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
1185-
2944-
55488-
7705-
7783-
10421-
10028-
10045-
7758-
7720-
7782-
•57-5
67-4
•87-4
08-0
50-8
48-4
•22-5
89-3
•94-3
78-7
•63-0
METHOD SUMMARY:
Analysis of water samples for the above iron compounds can be performed by
colorimetric or atomic spectrometric analysis for iron. Colorimetric analysis
is performed by addition of orthophenanthroline and measurement of the
absorbance at 510 nanometers, or by addition of bathophenanthroline to a sample
previously reduced with hydroxylamine hydrochloride, and measurement of the
absorbance at 533 nanometers. For atomic spectrometric analysis, a 100-milli-
liter sample is digested with nitric acid and hydrogen peroxide and analyzed by
inductively coupled plasma (ICP) or flame atomic absorption spectrometry (AA).
Furnace rather than flame AA is recommended for low levels of iron. Alterna-
tively, the metal can be chelated with pyrrolidinedithiocarbamic acid, the
resulting complex extracted with chloroform, and the extract analyzed by AA.
These methods do not identify any specific iron-containing compound, but
measure the total iron content of the sample.
INTERFERENCES:
For each matrix analyzed, it is necessary to
and/or interferences require standard addition or
performing direct atomic spectrometric analyses.
necessary to determine low levels of iron in some
be removed by extracting iron from a hydrochloric
ether and then extracting the ether with water to
water solution.
QUALITY CONTROL:
A reference standard should be analyzed weekly, and at least 10 percent of
the analyses should be duplicate samples and/or standards.
determine if matrix effects
serial dilution methods when
Background correction may be
samples. Interferences may
acid solution with diisopropyl
obtain an interference-free
B-293
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EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for Clean
Water Act analyses. Precision and accuracy information is furnished. For
direct flame AA analysis the detection limit is 20 micrograms per liter, the
sensitivity 120 micrograms per liter, and the optimum concentration range 0.3
to 10 milligrams per liter (APHA). The chelation-extraction AA procedure is
applicable over the range of 5 to 500 micrograms per liter (ASTM). The batho-
phenanthroline colorimetric method is suitable for the determination of low
levels of total iron (200 micrograms per liter and below), while the ortho-
phenanthroline colorimetric method can be used for the determination of total,
dissolved, and ferrous iron over the range of 0.05 to 3 milligrams per liter.
REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes. Method 236.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Technical Additions to Methods for
Chemical Analysis of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Cincinnati, 1982.
Federal Register, 44_(233), December 3, 1979, pp. 69559-69564.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Methods 303A, 303B; APHA: Washington, 1980.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.01, Methods D1068(A), D1068(B), D1068(C), D1068(D): ASTM: Philadelphia,
1983.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list);
by furnace AA, approximately $18-50 (list); by ICP, approximately $10 (list);
by colorimetric methods, approximately $20 (list).
B-294
-------
IRON
Water Samples
Laboratory Method 2
Compound
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
CAS Number
1185-
2944-
55488-
7705-
7783-
10421-
10028-
10045-
7758-
7720-
7782-
•57-5
67-4
•87-4
08-0
•50-8
•48-4
•22-5
89-3
•94-3
•78-7
•63-0
METHOD SUMMARY:
Analysis of water samples for the above iron-containing compounds can be
performed by spectrophotometric analysis for iron. A 50-milliliter sample is
treated with hydroxylamine hydrochloride, and the ferrous iron originally
present or formed by the hydroxylamine is reacted with 2,4,6-tripyridyl-s-
triazine (TPTZ). The intensity of the color of the iron-TPTZ complex formed is
measured and compared with that of standards. This method measures the total
iron content of the sample and is not specific for any particular iron-contain-
ing compound.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Duplicate and fortified samples should be processed in accordance with a
quality control program.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is applicable to samples in
the range of 0.05 to 2 milligrams iron per liter. Precision and accuracy
information is furnished.
REFERENCE:
Alberta Environmental Centre, Methods Manual for Chemical Analysis of Water and
Wastes, "Iron;" Publication No. AECV81-M1, Alberta Environmental Centre:
Vegreville, Alberta, Canada, 1981.
B-295
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $15-25
(list).
B-296
-------
LEAD
Air Samples
Laboratory Method 1
Compound
Lead
Lead Acetate
Lead Arsenate
CAS Number
Lead
Lead
Lead
Lead
Lead
Lead
Lead
Chloride
Fluoborate
Fluoride
Iodide
Nitrate
Phosphate
Stearate
Lead Subacetate
Lead Sulfate
Lead Sulfide
Lead Thiocyanate
7439-
301-
7784-
7645-
10102-
7758-
13814-
7783-
10101-
10099-
7446-
7428-
1072-
56189-
1335-
15739-
7446-
1314-
592-
92-1
04-2
40-9
25-2
•48-4
95-4
96-5
46-2
•63-0
74-8
•27-7
•48-0
•35-1
•09-4
32-6
•80-7
•14-2
87-0
•87-0
METHOD SUMMARY:
Atomic absorption spectrometric analysis (AA) for lead may be used for the
determination of the above particulate lead compounds in air samples. A known
volume of air is passed through a cellulose-membrane or glass-fiber filter.
The filter and collected particulates are wet-ashed and the resulting solution
is then analyzed by flame or furnace AA. This method does not identify any
specific lead-containing compound, but measures the total lead content of the
sample.
INTERFERENCES:
Acetate, carbonate, fluoride, iodide, and phosphate ions suppress absor-
bance if at concentrations ten times that of lead. The presence of EDTA (0.1
molar) will overcome this interference. Calcium and high levels of sulfate
ions may interfere. High levels of organic compounds in the sample may
necessitate the use of background correction techniques. Since flameless AA is
more prone to matrix effects than flame methods, the method of standard addi-
tions should be employed when flameless AA is used.
B-297
-------
QUALITY CONTROL:
One blank filter should be analyzed with each set of ten or fewer samples
and corrections for the blank must be made for each sample. At least five stan-
dards should be used for calibration.
EPA/TECHNICAL STATUS:
Method S341 has been validated over the range of 0.128 to 0.399 milligrams
lead per cubic meter in 180 liters of air and is approved by the National
Institute for Occupational Safety and Health (NIOSH). Method P&CAM 155 is a
NIOSH operational method for use over the range of 0.01 to 4 milligams per
cubic meter in 100 liters of air. Method P&CAM 173 is a NIOSH operational
method for use over the range of 42 to 840 micrograms per cubic meter, using a
240-liter sample. Method P&CAM 214 is proposed by NIOSH for use over the range
of 0.02 to 0.4 milligrams per cubic meter, using a 5-liter sample of air. The
APHA method uses flame AA and has a detection limit of 10 micrograms per cubic
meter for a 100-liter air sample and an optimum concentration range of up to
approximately 1 milligram per cubic meter. Alberta Environment has determined
that the limit of detection is 0.01 micrograms per cubic meter. Precision and
accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set 0, Method S341; PB-262 402 (NTIS), U.S. DHEW: Cincinnati, 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 155; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S341; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 214; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method S341; Publication No. 82-100, U.S. DHHS: Cincinnati,
August 1981.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Elemental Analysis by
Atomic Absorption Spectrometry," pp. IV-2 to IV-48; EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
B-298
-------
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-04, "Trace Metals
by Atomic Absorption;" HASL-300, Environmental Measurements Laboratory, U.S.
DOE: New York, 1983.
Alberta Environment, Method Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23541; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., Method 813; APHA: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20, plus
sampling costs; by furnace AA, it is approximately $18-50, plus sampling costs.
B-299
-------
LEAD
Air Samples
Laboratory Method 2
Compound
Lead
Lead Acetate
Lead Arsenate
CAS Number
Lead
Lead
Lead
Lead
Lead
Lead
Lead
Chloride
Fluoborate
Fluoride
Iodide
Nitrate
Phosphate
Stearate
Lead Subacetate
Lead Sulfate
Lead Sulfide
Lead Thiocyanate
7439-
301-
7784-
7645-
10102-
7758-
13814-
7783-
10101-
10099-
7446-
7423-
1072-
56189-
1335-
15739-
7446-
1314-
592-
•92-1
•04-2
•40-9
•25-2
•48-4
95-4
•96-5
46-2
•63-0
74-8
•27-7
48-0
35-1
09-4
32-6
•80-7
•14-2
87-0
87-0
METHOD SUMMARY:
Analysis for the above particulate lead compounds in air may be performed
by filtration of air and analysis of the filter deposit for lead by X-ray
fluorescence spectrometry. The method is non-destructive, so that further
analyses may be performed on samples. The method is sensitive to amounts of
lead above 4 micrograms with a precision of 60 percent at that level. The
sample-collection time may be up to 8 hours, but analysis time is only approxi-
mately 1 minute. The method measures total lead present in the sample, and
does not differentiate between chemical compounds or lead valence states.
INTERFERENCES:
Polyvinyl chloride (PVC) filters are unacceptable for sampling, and
glass-fiber filters are acceptable for use only if they are of the highest
purity. Cellulose membrane, cellulose fiber, polycarbonate membrane, and
fluorocarbon membrane filters are acceptable.
QUALITY CONTROL:
No quality control procedures are given.
B-300
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list).
Note: NIOSH Method 351 (filter collection, acid digestion, analysis by ICP) is
applicable. (Reference supplied by reviewer.)
B-435
-------
B. ORGANIC SUBSTANCES
B-436
-------
ACETATES
Air Samples
Laboratory Method
Compound CAS Number
iso-Amyl Acetate 123-92-2
sec-Amyl Acetate 626-38-0
Butyl Acetate 123-86-4
iso-Butyl Acetate 110-19-0
sec-Butyl Acetate 105-46-4
tert-Butyl Acetate 540-88-5
METHOD SUMMARY:
Analysis of air samples for the above acetate esters can be performed by
passage of the a known volume of air through a charcoal-tube filter, followed
by desorption of analytes with carbon disulfide and analysis of the resulting
solution by gas chromatography with flame ionization detection (GC/FID). The
method is capable of measuring much smaller amounts if the desorption effi-
ciency is adequate.
INTERFERENCES
High humidity severely decreases the capacity of the sampling apparatus.
QUALITY CONTROL:
The desorption efficiency must be determined over the range of analysis,
and a method blank should be processed with each 10 samples. The desorption
efficiency and blank results should be used in the calculation of the results.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and has been validated over the following ranges (milligrams
per cubic meter): 208 to 874 (iso-amyl acetate), 349 to 1460 (sec-amyl
acetate), 306 to 1280 (iso-butyl acetate). 478 to 2005 (sec-butyl acetate), 424
to 1780 (tert-butyl acetate), 352 to 1475 (butyl acetate), using a 10-liter air
sample. Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set D. Methods S31, S32, S44, S45, S46, S47; PB-245 935, U.S. DHEW: Washington,
1975.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 2, Methods S31, S32, S44, S45, S46, S47; Publication
No. 77-157-B, U.S. DHEW: Washington, 1977.
B-437
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
B-438
-------
ACID AND BASE/NEUTRAL EXTRACTABLE ORGANICS
Soil/Sediment Samples
Laboratory Method
Compound
Acenaphthene
Acenaphthylene
Aldrin
Anthracene
Benzidine
Benzo[a]anthracene
Benzo[b]fluoranthene
Benzo[k]fluoranthene
Benzo[ghi]perylene
Benzo[a]pyrene
a-BHC
6-BHC
Bis(2-chloroethoxy)-
methane
Bis(2-chloroethyl)-
ether
Bis(2-chloroisopropyl)-
ether
4-Bromophenyl Phenyl
Ether
Chrysene
Butyl Benzyl Phthalate
Chlordane
£-Chloro-m-cresol
2-Chloronaphthalene
2-Chlorophenol
4-Chlorophenyl Phenyl
Ether
ODD
DDE
DDT
Dibenz[a,h]anthracene
Di-n-butyl Phthalate
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
3,3'-Dichlorobenzidine
2,4-Dichlorophenol
Dleldrin
METHOD SUMMARY:
CAS Number Compound CAS Number
83-32-9 Diethyl Phthalate 84-66-2
208-96-8 2,4-Dimethylphenol 105-67-9
309-00-2 Dimethyl Phthalate 131-11-3
120-12-7 4,6-Dinitro-o-cresol 543-52-1
92-87-5 and salts
56-55-3 2,4-Dinitrophenol 51-28-5
205-99-2 2,4-Dinitrotoluene 121-14-2
207-08-9 2,6-Dinitrotoluene 606-20-2
191-24-2 Di-n-Octyl Phthalate 117-84-0
50-32-8 1,2-Diphenylhydrazine 122-66-7
319-85-7 Endosulfan Sulfate 1031-07-8
319-86-8 Endrin 72-20-8
111-91-4 Endrin Aldehyde 7421-93-4
Fluoranthene 206-44-0
111-44-4 Fluorene 86-73-7
Heptachlor 76-44-8
108-60-1 Heptachlor Epoxide 1024-57-3
Hexachlorobenzene 118-74-1
101-55-3 Hexachlorobutadiene 87-68-3
Hexachloroethane 67-72-1
218-01-9 Indeno[l,2,3,-cd]pyrene 193-39-5
85-68-7 Isophorone 78-59-1
57-74-9 Naphthalene 91-20-3
59-50-7 p-Nitroaniline 100-01-6
91-58-7 Nitrobenzene 98-95-3
95-57-8 2-Nitrophenol 88-75-3
7005-72-3 4-Nitrophenol 100-02-7
N-Nitrosodimethylamine 62-75-9
72-54-8 N-Nitrosodiphenylamine 86-30-6
72-55-9 N-Nitrosodi-_n-propylamine 621-64-7
50-29-3 Pentachlorophenol 87-86-5
53-70-3 Phenanthrene 85-01-8
84-74-2 Phenol 108-95-2
95-50-1 Polychlorinated 1336-36-3
541-73-1 Biphenyls
106-46-7 Pyrene 129-00-0
91-94-1 Toxaphene 8001-35-2
121-14-2 1,2,4-Trichlorobenzene 120-82-1
60-57-1 2,4,6'-Trichlorophenol 88-06-2
Simultaneous analysis for the above organic compounds in soil/sediment
samples may be performed by extraction and determination by gas chromatography/
mass spectrometry (GC/MS). A 1-gram portion of sample is mixed with surrogates
B-439
-------
and anhydrous sodium sulfate. The mixture is sonified with methylene chloride
and the supernatant is screened by gas chromatography with flame ionization
detection (GC/FID), in order to determine if extraction by the low-level method
is necessary. The extract is concentrated and a portion is analyzed by GC/MS
with a fused-silica capillary colum (FSCC). If screening yields negative or
low results, a 30-gram sample mixed with surrogates and anhydrous sodium
sulfate is extracted with methylene chloride/acetone and the extract is con-
centrated. A gel permeation chromatography (GPC) cleanup is optional. Acid
and most base/neutral analytes may be determined simultaneously since the
soil/sediment samples are extracted without pH adjustment.
QUALITY CONTROL;
The concentrate is analyzed using multiple internal standards, with
quantitative determination based on the internal standard specified in the
protocol. Mass abundance calibrations, internal standard responses, and
retention times must be monitored daily. The ratios of the response factors of
deuterated compounds to those of non-deuterated compounds must be between 0.8
and 1.2. The percent relative standard deviation for calibration check com-
pounds must be less than 30 percent. A system performance check must be per-
formed to assure that minimum average response factors are met before the
calibration curve is used. The same check must be performed each 12 hours to
assure the quality of the analytical system. A matrix spike and matrix-spike
duplicate must be performed once for each set of samples or once for every 20
samples of similar concentration and/or sample matrix, whichever is greater.
INTERFERENCES;
Interferences may be caused by contaminants in solvents, reagents, glass-
ware, and other sample processing equipment. These materials must be routinely
demonstrated to be free from laboratory interferences by processing and
analyzing reagent blanks. Matrix interferences may be caused by contaminants
that are coextracted from the sample. The extent of matrix interferences may
vary considerably from source to source.
EPA/TECHNICAL STATUS:
This method is in use in the CERCLA Contractor Laboratory Program and is
based on methods approved for use under the Clean Water Act and the Resource
Conservation and Recovery Act (RCRA). Precision and accuracy information is
furnished (EPA Methods 624, 625). The method detection limit is 1 to 10
micrograms per liter, except for diethylphthalate (22), benzidine (44), 3,3'-
dichlorobenzidine, polychlorinated biphenyls (30 to 40), 2,4-dinitrophenol
(42), and 2-methyl-4,6,-dinitrophenol (24).
REFERENCES:
U.S. Environmental Protection Agency, Invitation for Bid, "Organics Analysis,
Multi-Media, Multi-Concentration, GC/MS with Medium-Level GC Screen," Solicita-
tion Number WA84A-266; U.S. EPA: Washington, June 15, 1984.
B-440
-------
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. Longbottom; J. Lichtenburg, Eds.,
Methods 624, 625; EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
Plumb, R. H., Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. II. Available Laboratory Analytical Methods, pp. 111-93 to III-133, EPA-
600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas, 1984.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 8250, 8270; SW-846, U.S. EPA:
Washington, 1982.
U.S. Geological Survey, Methods for Determination of Organic Substances in
Water and Fluvial Sediments, Book 5, Laboratory Analysis, Chapter A4; Open-File
Report 82-1004, USGS: Denver, 1983.
COST INFORMATION:
Cost per sample for the GC screen is approximately $70-90 (list), $60
(bid); GC/MS analysis is approximately $450-495 (list), $230 (bid).
B-441
-------
ACID-EXTRACTABLE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
p_-Chloro-m-Cresol 59-50-7
2-Chlorophenol 95-57-8
2,4-Dichlorophenol 120-83-2
2,4-Dimethylphenol 105-67-9
4,6-Dinitro-o-cresol and salts 534-52-1
2,4-Dinitrophenol 51-28-5
2-Nitrophenol 88-75-5
4-Nitrophenol 100-02-7
Pentachlorophenol 87-86-5
Phenol 108-95-2
2,4,6-Trichlorophenol 88-06-2
METHOD SUMMARY:
Analysis for the above acid-extractable organic compounds may be performed
by gas chromatography/mass spectrometry (GC/MS). A 1-liter sample is fortified
with surrogates and extracted with methylene chloride at a pH below 2. A
portion of the extract is screened for organic compounds by gas chromatography
with flame ionization detection (GC/FID) to determine whether sample dilution
prior to extraction is required. If no dilution is required, then the extract
is dried, concentrated, and analyzed by GC/MS. If the screening reveals that
it is a medium-level sample, a 50-milliliter aliquot of the original sample is
diluted to 1 liter, surrogates are added, and the resulting solution is
extracted and analyzed as described. GC/MS analysis may be performed using a
fused silica capillary column (FSCC).
QUALITY CONTROL:
The concentrate is analyzed using multiple internal standards with and the
quantitative determinations are based on the internal standard specified in the
protocol. Mass abundance calibrations, internal standard responses, and reten-
tion times must be monitored daily. The ratios of the response factors of
deuterated compounds to those of non-deuterated compounds must be between 0.8
and 1.2. The percent relative standard deviation for calibration check com-
pounds must be less than 30 percent. A system performance check must be per-
formed to assure that minimum average response factors are met before the
calibration curve is used. The same check must be performed each 12 hours to
assure the quality of the analytical system. A matrix spike and matrix-spike
duplicate must be performed once for each set of samples or once for every 20
samples of similar concentration and/or sample matrix, whichever is greater.
INTERFERENCES:
Interferences may be caused by contaminants in solvents, reagents, glass-
ware, and other sample processing equipment. These materials must be routinely
B-442
-------
demonstrated to be free from laboratory interferences by processing and
analyzing reagent blanks. Matrix interferences may be caused by contaminants
that are coextracted from the sample. The extent of matrix interferences may
vary considerably from source to source.
EPA/TECHNICAL STATUS:
This method is currently in use in the CERCLA program. Precision and
accuracy information is furnished. The method detection limit is 1 to 4
micrograms per liter, except for 2,4-dinitrophenol (42 micrograms) and 4,6-
dinitro-o-cresol (26 micrograms).
REFERENCES:
U.S. Environmental Protection Agency, Invitation for Bid, "Organics Analysis,
Multi-Media, Multi-Concentration, GC/MS with Medium Level GC Screen," Solicita-
tion Number WA84A-266; U.S. EPA: Washington, June 15, 1984.
I
"Base/Neutrals and Acids - Method 625," Methods for Organic Chemical Analysis
for Municipal and Industrial Wastewater, Longbottom, J; Lichtenburg, J.; Eds.,
EPA-600/4-82-057, U.S. EPA, 1983.
Method 8250, 8270, Test Methods for the Evaluation of Solid Wastes, 2nd ed.,
U.S. EPA, SW-846, July 16, 1982.
Sauter, A. D.; Betowski, L. D.; Smith, T. R.; Strickler, V. A; Beimer, R. G.;
Colby, B. N.; Wilkenson, J. E. "Fused Silica Capillary Column GC/MS for the
Analysis of Priority Pollutants," J. High Resolut. Chromatogr. Chromatogr.
Comm.. ^, 1981, pp. 366-384.
COST INFORMATION:
Cost per sample for the GC screen is approximately $70-90 (list); $60
(bid); the GC/MS analysis is approximately $225-250 (list).
B-443
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ALIPHATIC ALDEHYDES
Air Samples
Laboratory Method
Compound CAS Number
Acetaldehyde 75-07-0
Chloral 75-87-6
Chloroacetaldehyde 107-20-0
Crotonaldehyde 4170-30-3
123-73-9
Glycidylaldehyde 765-34-4
METHOD SUMMARY:
Analysis for the above low—molecular-weight aldehydes in air can be per-
formed by gas chromatography. The aldehydes are collected in bisulfite-filled
impingers by sampling for 1 hour at 2 liters per minute. The bisulfite solu-
tion is then analyzed by gas chromatography with flame ionization detection
(GC/FID).
INTERFERENCES:
Alcohols, esters, and ketones may be partially collected and the corres-
ponding peaks may appear on the chromatogram.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information
is furnished.
REFERENCE:
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., M. Katz, Ed.; APHA: Washington, 1977, p. 300.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-90
(list), plus sampling costs.
B-444
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ALIPHATIC AMINES
Air Samples
Laboratory Method
Compound CAS Number
Butylamine 109-73-9
Diethylamine 109-89-7
Dimethylamine 124-40-3
Triethylamine 121-44-8
METHOD SUMMARY:
Gas chromatography may be used for the analysis of the above aliphatic
amines in air samples. The analysis is performed by passage of a known volume
of air through a silica-gel sampling device. The silica gel and adsorbed
amines are treated with sulfuric acid, a portion of the solution is made
alkaline with excess sodium hydroxide, and an aliquot of the alkaline solution
is analyzed by gas chromatography with flame ionization detection (GC/FID).
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
QUALITY CONTROL:
Desorption efficiency must be determined over the range of interest, and a
method blank should be processed with each 10 samples. The desorption effi-
ciency and the results of the method-blank analysis should be used in the cal-
culation of the results.
EPA/TECHNICAL STATUS:
This method is proposed by the National Institute for Occupational Safety
and Health (NIOSH), for use over the range of 1 to 2,400 milligrams per cubic
meter, for a 10-liter sample of air. Precision and accuracy information is
furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 221; Publication No. 77-157-A, U.S.
DHEW: Washington, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $80-90
(list), plus sampling costs.
B-445
-------
ALIPHATIC AMINES
Water Samples
Laboratory Method
Compound CAS Number
Butylamine 109-73-9
ijso-Butylamine 78-81-9
sec-Butylamine 513-49-5
13952-84-6
tert-Butylamine 75-64-9
Diethylamine 109-89-7
Dimethylamine 124-40-3
Monoethylamine 75-04-7
n-Propylamine 107-10-8
Trimethylamine 75-50-3
METHOD SUMMARY:
Analysis of water samples for the above amines can be performed by gas
chromatography (GC). A 1.5-microliter sample is injected directly into a gas
chromatograph with nitrogen-sensitive detection.
INTERFERENCES:
Water may interfere. This can be eliminated by lowering the GC column
temperature. The addition of ammonia to solutions before analysis suppresses
adsorption of amines on glass surfaces and on the column packing. Other inter-
ferences are not reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. The method can be used to detect amine concentrations as low as
0.03 parts per million for short-chain amines and 0.1 part per million for
other amines.
REFERENCE:
Dalene, M.; Mathiasson, L.; Jonsson, J. A. "Trace Analysis of Free Amines by
Gas-Liquid Chromatography," J. Chromatogr., 207, 1981, pp. 37-46.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60 (list).
B-446
-------
ALIPHATIC COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Acetaldehyde 75-07-0
Acetic Acid 64-19-7
Acetone 67-64-1
ijso-Butyl Alcohol 78-83-1
n-Butyl Alcohol 71-36-3
Ethyl Ether 60-39-7
Methanol 67-56-1
Methyl Ethyl Ketone 78-93-3
Methyl Isobuty Ketone 108-10-1
Propionic Acid 79-09-4
METHOD SUMMARY:
The above aliphatic compounds in water samples can be measured by steam
carrier gas chromatography with flame ionization detection (SCGC/FID). The
sample is analyzed directly, without any pretreatment, producing a chromatogram
with a signal-to-noise ratio large enough to permit quantitative analyses.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision or accuracy information is
not furnished. The limit of detection is approximately 20 to 60 micrograms per
liter.
REFERENCE:
Urano, K.; Ogura, K. ; Wada, H. "Direct Analytical Method for Aliphtic
Compounds in Water by Steam Carrier Gas Chromatography," Water Res., 15, 1981,
pp. 225-231.
COST INFORMATION:
No cost information has been obtained.
B-447
-------
ALKALOIDS
Water Samples
Laboratory Method
Compound CAS Number
Reserpine 50-55-5
Strychnine 57-24-9
METHOD SUMMARY:
Analysis for the above alkaloids in water samples can be performed by
high-performance liquid chromatography (HPLC). A sample is extracted with
chloroform/methanol or diethyl ether/methanol mixture, and the extract is
analyzed by HPLC with ultraviolet absorbance detection.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. The limit of detection for this method is 20 nanograms injected on
the column.
REFERENCE:
Verpoorte, R. ; Svendsen, A. B. "High-speed Liquid Chromatography of Alkaloids.
I," J. Chromatogr., 100, 1974, pp. 227-230.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $145 (list).
B-448
-------
ALKYL BENZENE SULFONATES
Water Samples
Laboratory Method 1
Compound CAS Number
Calcium Dodecylbenzene Sulfonate 26264-06-2
Dodecylbenzenesulfonic Acid 27176-87-0
Isopropanolamine Dodecylbenzene Sulfonate 42504-46-1
Sodium Dodecylbenzene Sulfonate 25155-30-0
Triethanolamine Dodecylbenzene Sulfonate 27323-41-7
METHOD SUMMARY:
Analysis for the above alkyl benzene sulfonates in water can be performed
by addition of an acidic methylene blue solution to an acidified 100-milliliter
sample, followed by serial extraction with chloroform. The chloroform extract
is then analyzed spectrophotometrically. This method measures methylene-blue
active substances, but does not specifically identify the methylene-blue active
substance(s) being measured. For such information, methods such as infrared
spectrometry or mass spectrometry should be used.
INTERFERENCES:
If potential interferences are present in the sample, pretreatment to
remove them is required. This includes boiling the acidified sample to near
dryness, addition of aqueous alkali solution and boiling, and finally extrac-
tion with 1-methyl heptylamine. Possible interferences include phosphorodi-
thioates (e.g., organophosphate pesticides), benzene sulfonates, thiocyanates,
picric acid, and alkyl sulfonates.
QUALITY CONTROL:
All glassware used must be free of scratches and etch marks, and should be
preconditioned by rinsing with chloroform. A blank should be processed with
each sample or set of samples. A quality control standard, near the midrange
of the calibration curve, should be analyzed with each set of samples and the
calibration factor should fall within the 95-percent confidence interval.
EPA/TECHNICAL STATUS:
This method is EPA-approved for the Clean Water Act. Precision informa-
tion is furnished. The method is applicable over the range from 0.03 to 3.5
milligrams per liter, using a 100-milliliter sample (ASTM). The minimum
detectable quantity of methylene-blue active substance(s) using this method is
10 micrograms.
REFERENCES:
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 512A; APHA: Washington, 1980.
B-449
-------
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards
Volume 11.02, D 2330-82; ASTM: Philadelphia, 1983, pp. 85-97. " "'
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Methylene Blue Active Substances;" Publication No. AECV81-M1~~
Alberta Environmental Centre, Vegreville, Alberta, Canada, 1981.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 425.1; EPA 600/4-79-020, U.S. EPA: Cincinnati, 1979.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-100
(list).
B-450
-------
ALKYL BENZENE SULFONATES
Water Samples
Laboratory Method 2
Compound CAS Number
Calcium Dodecylbenzene Sulfonate 26264-06-2
Dodecylbenzenesulfonic Acid 27176-87-0
Isopropanolamine Dodecylbenzene Sulfonate 42504-46-1
Sodium Dodecylbenzene Sulfonate 25155-30-0
Triethanolamine Dodecylbenzene Sulfonate 27323-41-7
METHOD SUMMARY:
Analysis of water samples for the above alkyl benzene sulfonates can be
performed using infrared spectrometry. A sample containing 10 to 25 milligrams
of surfactant is treated with activated carbon, the adsorbed surfactant is
desorbed with an alkaline benzene/methanol solution, the surfactants are
hydrolyzed, and the resulting acids are converted to amine salts. The infrared
absorptions due to the substituted benzene ring (9900 nm or 1010 cm ) and the
sulfonate group (9600 nm or 1041 cm~l) are measured. Quantification is made by
use of a calibration curve. This method measures the total amount of the above
alkyl benzene sulfonates in the sample, but cannot distinguish between linear
alkylbenzene sulfonates; it does distinguish alkylbenzene sulfonates from other
sulfonates.
INTERFERENCES:
Most natural interferences are removed in sample preparation. No specific
interferences are listed.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. No precision or accuracy information is
furnished. The method is suitable for samples containing at least 0.25 milli-
grams methylene-blue active substance per liter (USGS).
REFERENCES:
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed.; Method 512B; APHA: Washington, 1980.
U.S. Geological Service, Methods for the Determination of Organic Substances in
Water and Fluvial Sediments, Book 5, "Laboratory Analysis," Chapter A3; USGS:
Denver, Open-File Report 82-1004, 1983.
B-451
-------
COST INFORMATION:
Cost per sample for analyses by this method is approximately $75-85.
B-452
-------
AMINES
Water Samples
Laboratory Method
Compound CAS Number
Butylamine 109-73-9
Dipropylamine 142-84-7
Triethylamine 121-44-8
METHOD SUMMARY:
Analysis of water samples for the above alkylamines can be performed by
ion-pair chrotnatography. The amines are separated with naphthalene-2-sulfonate
as a counter-ion using high-performance liquid chromatography (HPLC) with
ultra-violet absorbance detection.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision or accuracy information is
not supplied.
REFERENCE:
Croramen, J.; Fransson, B.; Schill, G. "Ion-Pair Chromatography in the Low
Concentration Range by Use of Highly Absorbing Counter Ions," J. Chromatogr.,
142, 1977, pp. 283-297.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $125 (list).
B-453
-------
AMINES AND ALCOHOLS
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Aniline 62-53-3
n-Butyl Alcohol 71-36-3
Butylamine 109-73-9
sec-Butylamine 513-49-5
13952-84-6
Phenol 108-95-2
Pyridine 110-86-1
Quinoline 91-22-5
Thiophenol 108-98-5
Triethylatnine 121-44-8
METHOD SUMMARY:
The above compounds may be measured in soil/sediment samples by extrac-
tion, derivatization, and F-19 nuclear magnetic resonance (NMR). A sample is
extracted with dimethylformamide, treated with trifluoromethanesulfonyl
chloride, and the products analyzed by F-19 NMR. The method gives NMR shifts
for each derivative, but no quantitative results are given.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Shue, F. F.; Yen, T. F. "Trifluororaethanesulfonyl Chloride for Identification
of Oxygen, Nitrogen, and Sulfur Functional Groups by Fluorine-19 Nuclear
Magnetic Resonance Spectrometry," Anal. Ghent., 54, 1982, pp. 1641-1642.
COST INFORMATION:
No cost information has been obtained.
B-454
-------
AMINES AND OTHER NITROGEN COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Ammonium Fluoride 12125-01-8
Ammonium Oxalate 6009-70-7
5972-73-6
14258-49-2
Aniline 62-53-3
Benzidine 92-87-5
Butylamine 109-73-9
iso-Butylamine 78-81-9
£-Chloroaniline 106-47-8
Ethylenediamine 107-15-3
METHOD SUMMARY:
Analysis of water samples for the above amines and other nitrogen com-
pounds can be performed by spectrophotometry. Chloranil is added to a pH 9
buffered sample and the intensity of the color developed due to the formation
of a molecular or charge-transfer complex is monitored. Thirty minutes should
be allowed for color development at 65°C.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Some precision and accuracy information
is furnished. The working range of the method is approximately 1 milligram per
liter to 100 milligrams per liter.
REFERENCE:
Al-Ghabsha, T. S.; Rahim, S. A. "Spectrophotometric Determination of Micro-
gram Amounts of Amines with Chloranil," Anal. Chim. Acta., 85, 1976, pp.
189-194.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-35
(list).
B-455
-------
AROMATIC AMINES
Air Samples
Laboratory Method
Compound CAS Number
Aniline 62-53-3
p-Nitroaniline 100-01-6
METHOD SUMMARY:
Gas chromatography may be used for the analysis for the above aromatic
amines in air. A known volume of air is drawn through a tube containing silica
gel. The gel is treated with ethanol, and an aliquot of the resulting solution
is injected into a gas chromatograph equipped with a flame ionization detector
(GC/FID).
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
QUALITY CONTROL:
A method blank and standards are analyzed with the samples.
EPA/TECHNICAL STATUS;
This is an operational method as set forth by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 0.01 to 14
milligrams per sample. Precision and accuracy information is furnished.
REFERENCE:
U.S. Department of Health, Education and Welfare, NIOSH Manual of Analytical
Methods. Method P&CAM 168; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90 (list), ,
plus sampling costs.
B-456
-------
AROMATIC AMINES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Benzidine 92-87-5
3,3'-Dichlorobenzidine 91-94-1
3,3'-Dimethoxybenzidine 119-90-4
4,4'-Methylenebis- 101-14-4
(2-Chloroaniline)
METHOD SUMMARY:
Analysis of soil/sediment samples for the above aromatic amines can be
performed by high-performance liquid chromatography with electrochemical detec-
tion (HPLC/EC) and pre-column concentration. A 1- to 10-gram soil sample is
slurried in 100 to 1,000 milliliters water, and 20 milliliters of the resulting
solution are passed through a preconcentration column. The concentrated sample
is then flushed into the HPLC/EC and analyzed.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
A representative sample of the solids left after slurrying should be
processed to ascertain that extraction has been complete.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The method can detect concentrations above approximately 1 nanogram
per gram.
REFERENCE:
Rice J.; Kissinger, P. "Liquid Chromatography with Precolumn Sample Precon-
centration and Electrochemical Detection: Determination of Aromatic Amines in
Environmental Samples," Environ. Sci. Technol., 16(5), 1982, pp. 263-268.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130-155
(list).
B-457
-------
AROMATIC AMINES
Water Samples
Laboratory Method 1
Compound CAS Number
Benzidine 92-87-5
3,3'-Dichlorobenzidine 91-94-1
3,3'-Dimethoxybenzidine 119-90-4
4,4'-Methylenebis-
(2-Chloroaniline) 101-14-4
METHOD SUMMARY:
Analysis of water samples for the above aromatic amines can be performed by
high-performance liquid chromatography with electrochemical detection (HPLC/EC).
A 1- to 10-milliliter sample is filtered, concentrated on a preconcentration
column, and analyzed by reversed-phase HPLC/EC.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
A representative sample of the residue trapped in sample filtration should
be analyzed to ascertain that no analyte is adsorbed on the filtered material.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision and accuracy information is
furnished. The method is sensitive to low nanogram-per-liter concentrations.
REFERENCE:
Rice, J. R.; Kissinger, P. T. "Liquid Chromatography with Precolumn Sample
Preconcentration and Electrochemical Detection: Determination of Aromatic
Amines in Environmental Samples," Environ. Sci. Technol., 16^(5), 1982, pp.
263-268.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130-155
(list).
B-458
-------
AROMATIC AMINES
Water Samples
Laboratory Method 2
Compound CAS Number
4-Aminopyridine 504-24-5
Aniline 62-53-3
p-Nitroaniline 100-01-6
5-Nitro-o-Toluidine 99-55-8
o-Toluidine Hydrochloride 636-21-5
METHOD SUMMARY:
Analysis of water samples for the above aromatic amines can be performed
by diazotization and colorimetric measurement. A 35-milliliter water sample is
acidified with hydrochloric acid, sodium nitrite solution is added, and the
solution is allowed to stand for 5 minutes. A color reagent, either 8-amino-l-
hydroxy-naphthalene-3,6-disulfoni acid or N-(l-naphthyl)ethylenediamine, is
added to produce a cherry-red or purplish-red color, respectively, and the
intensity of the color is measured spectrophotometrically.
INTERFERENCES:
No interferences are reported. All glassware, including absorption cells,
should be cleaned frequently with hydrochloric acid.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
The method is not EPA-approved. No precision or accuracy information is
furnished. The method is sensitive to levels above approximately 0.1 milligrams
per liter in reagent-water samples.
REFERENCE:
Norwitz, G.; Keliher, P- N. "Spectrophotometric Determination of Aromatic
Amines by the Diazotization-Coupling Technique with 8-Amino-l-hydroxynaphtha-
lene-3,6-disulfonic acid and N-(l-Naphthyl)ethylenediamine as the Coupling
Agents," Anal. Chem., _54(4), 1982, pp. 807-809.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $24-30
(list).
B-459
-------
AROMATIC PRIMARY AMINES
Air Samples
Laboratory Method
Compound CAS Number
Aniline 62-53-3
3,3'-Dichlorobenzidine 91-94-1
3,3'-Dimethoxybenzidine 119-90-4
4,4'-Methylenebis 101-14-4
(2-Chloroaniline)
1-Naphthylamine 134-32-7
p-Nitroaniline 100-01-6
METHOD SUMMARY:
The above aromatic primary amines in air samples can be measured by gas
chromatography (GC). A 1-liter air sample is drawn through a bubbler contain-
ing 0.1 M hydrochloric acid. The resulting solution is then diluted with more
0.1 M hydrochloric, if necessary. Disodium tetraborate, heptafluorobutyryl
chloride, and cyclohexane are added. After shaking the mixture, an aliquot of
the cyclohexane fraction is analyzed by GC.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Limited precision and accuracy informa-
tion is furnished.
REFERENCE:
Meddle, D. W.; Smith, A. F. "Field Method for the Determination of Aromatic
Primary Amines in Air. Part I. Generation of Standard Atmospheres of Amines,"
Analyst, 106, 1981, pp. 1082-1087, 1094.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $105-150
(list), plus sampling costs.
B-460
-------
AROMATIC VOLATILE ORGANIC COMPOUNDS
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Benzene 71-43-2
Chlorobenzene 108-90-7
1,2-Dichlorobenzene 95-50-1
1,3-Dichlorobenzene 541-73-1
1,4-Dichlorobenzene 106-46-7
Ethylbenzene 100-41-4
Toluene 108-88-3
Xylene 1330-20-7
m-Xylene 108-38-3
o-Xylene 95-47-6
p-Xylene 106-42-3
METHOD SUMMARY:
Analysis for the above volatile aromatic organic compounds in soil/
sediment samples can be accomplished by gas chromatography. The sample is
dispersed in polyethylene glycol (PEG) or distilled-in-glass methanol
to dissolve the volatile organic compounds. A portion of this solution is
combined with water, purged with an inert gas onto a trap, and the trap back-
flushed into a temperature-programmed gas chromatograph with a photoionization
detector (GC/PID). Either internal or external standards are used for cali-
bration.
INTERFERENCES:
Samples should be collected in glass containers, sealed, and refrigerated
immediately. Contamination from the plumbing head of the trap and gas
chromatograph from previous injections and diffusion of volatile compounds
through the sample container seal can affect analytical results.
QUALITY CONTROL:
The plumbing head of the trap and gas chromatograph must be demonstrated
to be free of interferences by analysis of a method blank each time a set of
samples is processed or a change in reagents occurs. Field replicates, labora-
tory replicates, and fortified samples must be analyzed to demonstrate the
precision and accuracy of the method. In cases of doubt concerning the
identity of a peak in the chromatogram, confirmatory techniques, such as gas
chromatography/mass spectrometry (GC/MS) or second-column confirmation, should
be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
analyses (40 CFR, Part 261, Identification and Listing of Hazardous Wastes).
Precision and accuracy information is furnished.
B-461
-------
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 5030, 5020, 8020; SW-846,'
U.S. EPA: Washington, July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $100-115
(list); GC/MS confirmation is approximately $150-200 (list); second-column
confirmation is approximately $100-115 (list).
B-462
-------
AROMATIC VOLATILE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Benzene 71-43-2
Chlorobenzene 108-90-7
1,2-Dichlorobenzene 95-50-1
1,3-Dichlorobenzene 541-73-1
1,4-Dichlorobenzene 106-46-7
Ethylbenzene 100-41-4
Toluene 108-88-3
Xylene 1330-20-7
m-Xylene 108-38-3
o-Xylene 95-47-6
p-Xylene 106-42-3
METHOD SUMMARY:
Analysis of water samples for the above volatile aromatic organic com-
pounds can be performed by gas chromatography. A water sample is purged with
an inert gas onto a trap, and the trap is backflushed into a temperature-
programmed gas chromatograph with a photoionization detector (GC/PID). Either
internal or external standards are used for calibration.
INTERFERENCES:
Contamination from the plumbing head of the trap and the gas chromatograph
and diffusion of volatile compounds through the sample container seal can
affect analytical results.
QUALITY CONTROL:
Samples should be collected in glass containers, sealed and refrigerated
immediately. The plumbing head of the trap and the gas chromatograph must be
demonstrated to be free of interferences by the analysis of a method blank each
time a set of samples is processed or a change in reagents occurs. Field
replicates, laboratory replicates, and fortified samples must be analyzed to
demonstrate the precision and accuracy of the method. In cases of doubt con-
cerning the identity of a peak in the chromatogram, confirmatory techniques,
such as gas chromatography/mass spectrometry (GC/MS) or second-column confirma-
tion, should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
(RCRA) analyses (40 CFR, Part 261, Identification and Listing of Hazardous
Wastes). No precision or accuracy information is furnished.
B-463
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REFERENCES;
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 5030, 8020; SW-846, U.S.~
EPA: Washington, July 1982.
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, JT E^ Longbottom; J~. JT Lichtenberg; Eds.1
Method 602; EPA-600/4-82-057, U.S. EPA: Washington, July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $100-115
(list); GC/MS confirmation is approximately $150-200 (list); second column
confirmation is approximately $80 (list).
B-464
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0-ARYL CARBAMATE PESTICIDES
Water Samples
Laboratory Method
Compound CAS Number
Carbaryl 63-25-2
Mexacarbate 315-18-4
METHOD SUMMARY:
Analysis for the above 0-aryl carbamate pesticides in water samples can be
performed by a thin-layer chromatographic method. A 1-liter water sample is
extracted with dichloromethane, and the extract is dried, concentrated, and
cleaned up by Florisil® column chromatography. Fractions from the eluate are
concentrated, portions are separated by thin-layer chromatography, and the
carbamates are visualized by reaction with 2,6-dibromoquinone chlorimide.
Semi-quantitative measurement is made by visual comparison of the color inten-
sity with the color intensity of standards, and confirmation is established by
observation of color changes with pH.
INTERFERENCES:
Interferences by phenols may be overcome by the use of a different solvent
system.
QUALITY CONTROL:
Quality control charts should be used, and duplicate, spiked, and perfor-
mance evaluation samples should be analyzed regularly.
EPA/TECHNICAL STATUS:
This method is EPA-approved for National Pollutant Discharge Elimination
System (NPDES) analyses. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Benzidine, Chlorinated
Organic Compounds, Pentachlorophenol, and Pesticides in Water and Wastewater,
U.S. EPA: Washington, September 1978.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Supplement, "Selected Analytical Methods
Approved and Cited by the U.S. EPA," APHA: Washington, 1981, pp. S60, S73.
COST INFORMATION:
Cost information has not been obtained.
B-465
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BASE/NEUTRAL-EXTRACTABLE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound
CAS Number Compound
Acenaphthene
Acenaphthylene
Aldrin
Anthracene
Benzidine
Benzo[a]anthracene
Benzo[b]fluoranthene
Benzo[k]fluoranthene
Benzo[a]pyrene
Benzo[ghi]perylene
a-BHC
6-BHC
Bis(2-chloroethoxy)methane
Bis(2-chloroethyl)ether
Bis(2-chloroisopropyl)ether
4-Bromophenyl Phenyl Ether
Butyl Benzyl Phthalate
Chlordane
2-Chloronaphthalene
4-Chlorophenyl Phenyl Ether
Chrysene
4,4'-ODD
DDE
4,4'-DDT
Dibenz[a,h]anthracene
Di-n-butyl Phthalate
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
3,3'-Dichlorobenzidine
METHOD SUMMARY:
CAS Number
83-32-9 Dichloroethyl Ether 111-44-4
208-96-8 Dieldrin 60-57-1
309-00-2 Diethyl Phthalate 84-66-2
120-12-7 Dimethyl Phthalate 131-11-3
92-87-5 2,4-Dinitrotoluene 121-14-2
56-55-3 2,6-Dinitrotoluene 606-20-2
205-99-2 Di-n-octyl Phthalate 117-84-0
207-08-9 1,2-Dlphenylhydrazine 122-66-7
50-32-8 Endosulfan Sulfate 1031-07-8
191-24-2 Endrin
319-85-7 Endrin Aldehyde 7421-93-4
319-86-8 Fluoranthene 206-44-0
111-91-1 Fluorene 86-73-7
111-44-4 Heptachlor 76-44-8
108-60-1 Heptachlor Epoxide 1024-57-3
101-55-3 Hexachlorobenzene 118-74-1
85-68-7 Hexachlorobutadiene 87-68-3
57-74-9 Hexachloroethane 67-72-1
91-58-7 Indeno[l,2,3-cd]pyrene 193-39-5
7005-72-3 Isophorone 78-59-1
218-01-9 Naphthalene 91-20-3
72-54-8 p-Nitroaniline 100-01-6
Nitrobenzene 98-95-3
50-29-3 N-Nitrosodimethylamine 62-75-9
53-70-3 N-Nitrosodiphenylamine 86-30-6
84-74-2 N-Nitrosodi-n-propylamine 621-64-7
95-50-1 Phenanthrene 85-01-8
541-73-1 Polychlorinated Biphenyls 110-86-1
106-46-7 Pyrene 129-00-0
91-94-1 Toxaphene 8001-35-2
1,2,4-Trichlorobenzene 120-82-1
Analysis for the above organic compounds in water samples can be performed
by extraction followed by gas chromatography/mass spectrometry (GC/MS). A
1-milliliter sample is transferred into a vial and the pH is adjusted to 11.
The sample is extracted with methylene chloride and the methylene chloride
extract is screened for organic compounds by gas chromatography with a flame
ionization detector (GC/FID), in order to determine whether dilution will be
required for gas chromatographic/mass spectrometric (GC/MS) analysis. This
procedure is designed to screen at 100 milligrams per liter; in the absence of
interfering compounds. After dilution (as appropriate), samples that give
positive results in screening are analyzed by GC/MS. For samples that give
negative results in the GC/FID screening, a 1- to 2-liter sample is extracted
B-466
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at pH 11 with methylene chloride. The extract is dried and concentrated to
approximately 1 milliliter. For GC/MS analysis using a fused-silica capillary
column (FSCC), both the pH 11 extract and a pH 2 extract may be combined for
simultaneous chromatographic analysis of both acid and base/neutral extractable
organic compounds. The concentrate is analyzed using GC/MS with multiple
internal standards, and quantitative determinations are based on the response
factor of the nearest internal standard.
INTERFERENCES:
If emulsions form during the extraction step, a continuous-extraction
technique should be used.
QUALITY CONTROL;
Instrument performance is checked by minimum detection limit criteria and
ongoing monitoring of relative response factors, relative retention times,
internal standard response factors, stability of a 3-point calibration curve,
and performance of the gas chromatographic system. Specifications for instrument
tuning are given. Analytical performance is monitored by use of surrogates,
duplicate analyses, and fortified samples, and criteria for surrogate recoveries
are listed. The analytical system must be demonstrated to be free of interfer-
ences before analysis of any samples.
EPA/TECHNICAL STATUS;
This method is currently in use in the CERCLA program and is EPA-approved
for use in Clean Water Act analyses and analyses under the Resource Conserva-
tion and Recovery Act (RCRA). Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, GC Screen, GC/MS Analysis of Organic
Compounds, Invitation for Bid (Solicitation Number WA 82-A154); Exhibit D,
U.S. EPA: Washington, July 16, 1982.
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis for
Municipal and Industrial Wastewater, J. E. Longbottom; J. J. Lichtenberg; Eds.;
Method 625; EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 8250, 8270; SW-846, U.S. EPA:
Washington, 1982.
Sauter, A. D.; Betowski, L. D.: Smith, T. R. ; Strickler, V. A.; Beimer, R. G.;
Colby, B. N.; Wilkinson, J. E. "Fused Silica Capillary Column GC/MS for the
Analysis of Priority Pollutants," J. High Resolut. Chromatogr. Chromatogr.
Comm., 4, 1981, pp. 366-384.
B-467
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Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual.
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Methylene
Chloride Extracts of Aqueous Samples for Base/Neutral Compounds," pp. III-112
to III-117; EPA-600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas
1984.
U.S. Geological Survey, Methods for the Determination of Organic Substances in
Water and Fluvial Sediments, Book 5, "Laboratory Analysis," Chapter A3; USGS:
Denver, Open-File Report 82-1004, 1983.
COST INFORMATION:
Cost per sample for the GC screen is approximately $70-90 (list), $60
(bid); the GC/MS analysis is approximately $275-415 (list), $230 (bid).
B-468
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BASIC ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Aniline 62-53-3
£-Chloroaniline 106-47-8
1-Naphthylamine 134-32-7
2-Picoline 109-06-8
Pyridine 110-86-1
Quinoline 91-22-5
METHOD SUMMARY:
The above basic organic compounds in water samples can be determined by
gas chromatography with flame ionization detection (GC/FID). The sample is
passed through a cation-exchange resin to collect the organic bases, and the
resin is washed to remove the sorbed neutral and acidic compounds. The eluate
is concentrated by evaporation of solvent. An aliquot is injected into a GC
equipped with both a packed column and a fused-silica capillary column.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Kaczvinsky, J. R., Jr.; Saitoh, K.; Fritz, J. S. "Cation-Exchange Concentration
of Basic Organic Compounds from Aqueous Solution," Anal. Chem. 55(8), 1983, pp.
1210-1215.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $105-120.
B-469
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BENZAL CHLORIDE, BENZOTRICHLORIDE, AND BENZYL CHLORIDE
Air Samples
Laboratory Method
Compound CAS Number
Benzal Chloride 98-87-3
Benzotrichloride 98-07-7
Benzyl Chloride 100-44-7
METHOD SUMMARY;
Benzal chloride, benzotrichloride, and benzyl chloride in air samples
can be measured by gas chromatography with flame ionization detection (GC/FID).
The air is passed through a tube packed with Tenax-GC to adsorb the analytes,
which are desorbed with carbon tetrachloride. An aliquot is injected into the
GC/FID.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
The method is not EPA-approved. Precision or accuracy information is not
furnished.
REFERENCE:
Matsushita, H.; Kanno, S. "A Gas Chromatographic Determination of Benzotri-
chloride and Related Compounds in the Work Environment," Ind. Health, 17, 1979,
pp. 199-206.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90 (list),
plus sampling costs.
B-470
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BENZIDINE AND CONGENERS
Air Samples
Laboratory Method
Compound CAS Number
Benzidine 92-87-5
3,3'-Dichlorobenzidine 75-27-4
3,3'-Dimethoxybenzidine 119-90-4
3,3'-Dimethylbenzidine 119-93-7
METHOD SUMMARY:
Benzidine and the above congeners in particulate air samples can be
measured by high-performance liquid chromatography with electrochemical detec-
tion (HPLC/EC). Samples are collected on glass-fiber filters using a high-
volume air sampler. The filter is then extracted twice with chloroform. After
combining the extracts, the amines in the resulting solution are extracted into
1M sulfuric acid, the acid solution is neutralized, and the amines are
re-extracted into chloroform. After a series of dilutions with methanol and
concentration steps, the solution is buffered and then analyzed by HPLC/EC.
INTERFERENCES:
3,3'-Dimethylbenzidine and 3,3'-dimethoxybenzidine are not resolved
chromatographically.
QUALITY CONTROL:
Blank filters, spiked filters, and blind duplicate samples should be
analyzed with the rest of the samples.
EPA/TECHNICAL STATUS:
The method is not EPA-approved. Precision and accuracy information is
furnished. The detection limit is approximately 1 nanogram per cubic meter.
REFERENCE:
Riggin, R. M.; Howard, C. C. ; Scott, D. R. ; Hedgecoke, R. L. "Determination^of
Benzidine Related Congeners, and Pigments in Atmospheric Particulate Matter,"
J. Chromatogr. Sci., 2l_, 1983, pp. 321-325.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $15 (list),
plus sampling costs.
B-471
-------
BENZIDINE AND CONGENERS
Water Samples
Laboratory Method
Compound CAS Number
Benzidine 92-87-5
3,3'-Dimethoxybenzidine 119-90-4
3,3'-Dimethylbenzidine 119-93-7
METHOD SUMMARY:
Benzidine and the above congeners in water samples can be measured by
spectrophotofluorimetry (SPF). Wastewater samples are extracted with benzene,
the extract is cleaned up on an alumina column, the eluate is evaporated just
to dryness, and the residue is dissolved in methanol. The free amine in the
methanol solution is determined by SPF.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information are
furnished. The limit of detection is approximately 10 micrograms per liter.
REFERENCE:
Bowman, M. C.; King. J. R.; Holder, C. L. "Benzidine and Congeners: Analytical
Chemical Properties and Trace Analysis in Five Substrates," Intern. J. Environ.
Anal. Chem., _4, 1976, pp. 205-223.
COST INFORMATION:
Cost information has not been obtained.
B-472
-------
CARBAMATE AND UREA PESTICIDES
Water Samples
Laboratory Method
Compound CAS Number
Carbaryl 63-25-2
Carbofuran 1563-66-2
Diuron 330-54-1
Methomyl 16752-77-5
Mexacarbate 315-18-4
METHOD SUMMARY:
High-performance liquid chromatography (HPLC) can be used to determine the
above pesticides in water samples. A 1-liter sample is solvent-extracted with
methylene chloride and the extract is dried, concentrated, and analyzed by HPLC
with UV detection.
INTERFERENCES:
A Florisil® column cleanup procedure may be used when interferences are
present.
QUALITY CONTROL:
Laboratory reagent blanks must be analyzed to determine that reagents and
apparatus are free from interferences. Standard solutions must be checked
frequently for signs of degradation. The accuracy and precision of measure-
ments must be validated before analysis. At least 10 percent of the analyses
must be spiked samples, and duplicate samples should be analyzed periodically.
EPA/TECHNICAL STATUS:
This method is EPA-approved. Precision and accuracy information is
furnished. The method is sensitive to levels of analyte above two micrograms
per liter (USGS).
REFERENCES:
Pressley, T. ; Longbottom, J. The Determination of Carbamate and Urea Pesticides
in Industrial and Municipal Wastewater, Method 632; U.S. EPA: Cincinnati,
January 1932.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Determination of Carbamate
and Urea Pesticides in Industrial and Municipal Wastewater," pp. III-268 to III-
275; EPA-600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas, 1984.
B-473
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U.S. Geological Survey, Methods for the Determination of Organic Substances
in Water and Fluvial Sediments, Book 5, "Laboratory Analysis," Chapter A3;
USGS: Denver, Open-File Report 82-1004, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $155 to 180
(list).
B-474
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CARBAMATE PESTICIDES
Air Samples
Laboratory Method
Compound CAS Number
Carbaryl 63-25-2
Carbofuran 1563-66-2
METHOD SUMMARY:
Gas chromatography can be used for the analysis of air samples for the
above carbamate pesticides. A known volume of air is passed through a glass-
fiber, polyurethane foam, or composite filter, the sampling medium is Soxhlet-
extracted with hexane/diethyl ether, and the resulting solution is analyzed
with a gas chromatograph with a nitrogen-selective eletrolytic conductivity
detector or by chemical derivatization with alpha-bromo-2,3,4,5,6-pentafluoro-
toluene and analysis with a gas chromatograph with an electron-capture detector
(GC/ECD).
INTERFERENCES:
No interferences are listed.
QUALITY CONTROL:
Control limits for recovery must be established and recovery monitored.
Results for sets of samples processed with a fortified sample that gives
results that do not fall within control limits must be labeled as suspect.
EPA/TECHNICAL STATUS:
This method is not EPA-approved for use in any regulatory program.
Precision and accuracy information is furnished.
REFERENCES:
Sherraa, J.; Beroza, M. Manual of Analytical Methods for the Analysis of
Pesticides in Humans and Environmental Samples, Sections 8A and 8B; EPA-600/8-
80-038, U.S. Environmental Protection Agency: Research Triangle Park, North
Carolina, 1980.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Determination of Carbamate
Pesticides in Air," pp. III-293 to III-299; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $125-145
(list), plus sampling costs.
B-475
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CARBAMATE PESTICIDES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Carbofuran 1563-66-2
Mexacarbate 315-18-4
METHOD SUMMARY:
Analysis of soil/sediment samples for the above carbamate pesticides can
be performed by gas chromatography with electrolytic conductivity detection
(GC/ECD). A 50-gram sample is extracted with an acetone/aqueous sodium
chloride/aqueous sodium hydrogen carbonate solution and the extract is parti-
tioned with benzene. The solution is concentrated, cleaned up on a deactivated
Florisil column and the pesticides in the column eluate are determined by
GC/ECD.
INTERFERENCES:
No specific interferences are listed.
QUALITY CONTROL:
Recovery should be determined at 0.1 and/or 1.0 milligram-per-kilogram
fortification levels.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Determination of Carbamate
Pesticides in Soil," pp. III-276 to III-280; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $190 (list).
B-476
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CARBOXYLIC ACIDS
Water Samples
Laboratory Method
Compound CAS Number
Acetic Acid 64-19-7
Acrylic Acid 79-10-7
Fumaric Acid 110-17-8
Maleic Acid 110-16-7
METHOD SUMMARY:
Water samples can be analyzed for the above carboxylic acids by ion
exchange chromatography. The sample is analyzed by monitoring the eluates with
a UV detector at 210 nm, without pretreatment other than degassing.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
The method is not EPA-approved. No precison or accuracy information is
furnished.
REFERENCE:
Richards, M. "Separation of Mono- and Dicarboxylic Acids by Liquid Chromato-
graphy," J. Chromatogr., 115, 1975, pp. 259-261.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70 (list).
B-477
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CHLORINATED AND OTHER ORGANIC CONTAMINANTS
Water Samples
Laboratory Method
Compound CAS Number
Bis(2-Chloroethyl)ether 111-44-4
Chlorodibromomethane 124-48-1
1,4-Dichlorobenzene 106-46-7
Hexachlorobenzene 118-74-1
Hexachlorobutadiene 87-68-3
Pentachlorobenzene 608-93-5
Styrene 100-42-5
1,2,4-Trichlorobenzene 120-82-1
METHOD SUMMARY:
The above chlorinated organic contaminants in water samples can be
measured by gas chromatography/mass spectrometry (GC/MS). A one-liter sample
is passed through a closed-loop stripping system to purge the organics, which
are collected in carbon disulfide. A 2-microliter aliquot of the extract is
injected into a gas chromatograph equipped with a fused-silica capillary column.
Quantification is based on the ion current area of a single selected mass ion
of the mass spectrum.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Procedural blanks are analyzed and results are corrected for contaminants
in the blanks.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. This method is suitable for concentrations of analyte at the nano-
gram-per-liter level.
REFERENCE:
Coleman, W. E.; Munch, J. W.; Slater, R. W. ; Melton, R. G.; Kopfler, F. C.
"Optimization of Purging Efficiency and Quantification of Organic Contaminants
from Water Using a 1-liter Closed-Loop-Stripping Apparatus and Computerized
Capillary Column GC/MS," Environ. Sci. Technol., _L7(10), 1983, pp. 571-576.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $250-325
(list).
B-478
-------
CHLORINATED BENZENES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Hexachlorobenzene 118-74-1
Pentachloronitrobenzene 82-68-8
METHOD SUMMARY:
Hexachlorobenzene and pentachloronitrobenzene in soil samples can be
determined by gas chromatography with electron capture detection (GC/ECD). The
sample is mixed with water and shaken with toluene and isopropanol. The sol-
vent layer is separated from water and is washed twice with an aqueous sodium
sulfate solution, centrifuged, shaken with Nuchar-Attaclay, and filtered. The
filtrate is diluted, if necessary, and analyzed by GC/ECD. Compound identifi-
cation can be verified by gas chromatography/mass spectrometry (GC/MS).
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy informtion is
furnished for the compounds listed.
REFERENCE:
de Vos, R. H.; ten Noever de Brauw, M. C.; Olthof, P. D. A. "Residues of
Pentachloronitrobenzene and Related Compounds in Greenhouse Soils," Bull.
Environ. Contam. Toxicol., 11, 1974, pp. 567-571.
COST INFORMATION:
Cost per sample for the GC/ECD analysis is approximately $120-165 (list).
B-479
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CHLORINATED BENZENES
Air Samples
Laboratory Method
Compound CAS Number
Pentachlorobenzene 608-93-5
Pentachloronitrobenzene 82-68-8
METHOD SUMMARY:
Analysis for the above airborne chlorinated benzenes can be performed by
passage of 1000 liters of air through a polyurethane-foam sampling tube,
followed by Soxhlet extraction of the foam and analysis of the extract by gas
chromatography with electron capture detection (GC/ECD).
INTERFERENCES:
Phthalate esters and polychlorinated naphthalenes can interfere. Use of
non-TFE plastics must be avoided.
QUALITY CONTROL:
When concentration levels are high enough, confirmation of peak identifi-
cation is performed by gas chromatography/mass spectrometry (GC/MS). Solvents,
reagents, glassware, and polyurethane plugs must be shown to be free of interfer
ing artifacts. A field blank must be analyzed with each set of samples, and
both a quality control standard and a method blank should be analyzed with each
set of 5 to 15 samples.
EPA/TECHNICAL STATUS:
This method has been evaluated by the Environmental Protection Agency, but
is not approved for any specific regulatory program. No precision or accuracy
information is furnished. This method is applicable to a range from 1 nanogram
per cubic meter to 1000 nanograms per cubic meter.
REFERENCE:
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Waste Sites, Assignment 26, Appendix B; Contract 68-02-3168; U.S. EPA: Research
Triangle Park, North Carolina, May 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $115 (list),
plus sampling costs.
B-480
-------
CHLORINATED ETHERS AND OTHER COMPOUNDS
Water Samples
Laboratory Method
Compound
Bis(2-chloroethyl)ether
Bromoform
Chlorobenzene
Chlorodibromomethane
2-Chloroethyl Vinyl Ether
Chloroform
2-Chlorophenol
1,2-Dichlorobenzene
1,4-Dichlorobenzene
1,1-Dichloroethane
1,2-Dichloroethane
1,3-Dichloropropene
Ethylbenzene
Hexachlorobutadiene
Hexachloroethane
METHOD SUMMARY:
CAS Number Compound CAS Number
111-44-4 Isophorone 78-59-1
75-25-2 Naphthalene 91-20-3
108-90-7 N-Nitrosodimethylamine 62-75-9
124-48-1 N-Nitroso-di-n-propylamine 621-64-7
110-75-8 Phenol 108-95-2
67-66-3 1,1,2,2-Tetrachloroethane 79-34-5
95-57-8 Tetrachloroethylene 127-18-4
95-50-1 Toluene 108-88-3
106-46-7 1,2,4-Trichlorobenzene 120-82-1
75-34-3 1,1,1-Trichloroethane 71-55-6
107-06-2 1,1,2-Trichloroethane 79-00-5
542-75-6 Trichloroethylene 79-01-6
100-41-4 m-Xylene 108-38-3
87-68-3 o-Xylene 95-47-6
67-72-1 p-Xylene 106-42-3
Gas chromatography may be used to analyze water samples for the above
chlorinated ethers and other compounds. A 120-milliliter water sample is
extracted with methylene chloride. The extract is condensed, the solvent is
exchanged for hexane, and the sample is analyzed by gas chromatography with
electron capture detection (GC/ECD), flame ionization detection (GC/FID), or
Hall electrolytic conductivity detection (HECD).
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Triplicate samples should be analyzed. Standard solutions should be
extracted and analyzed. When the identification of a peak is in doubt, GC/MS
should be used for confirmation.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Otson, R.; Williams D. T. "Evaluation of a Liquid-Liquid Extraction Technique
for Water Pollutants," J. Chromatogr., 212, 1981, pp. 187-197.
B-481
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $110-215
(list), plus sampling costs.
B-482
-------
CHLORINATED HYDROCARBONS
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Benzotrichloride 98-07-7
Benzyl Chloride 100-44-7
ot-BHC 319-86-8
B-BHC 319-84-5
Y-BHC 319-85-7
2-Chloronaphthalene 91-58-7
1,2-Dichlorobenzene 95-50-1
1,3-Dichlorobenzene 541-73-1
1,4-Dichlorobenzene 106-46-7
Hexachlorobenzene 118-74-1
Hexachlorobutadiene 87-68-3
Hexachlorocyclopentadiene 77-47-4
Hexachloroethane 67-72-1
Lindane 59-89-9
1,2,4,5-Tetrachlorobenzene 95-94-3
1,2,4-Trichlorobenzene 120-82-1
METHOD SUMMARY:
Analysis for the above chlorinated hydrocarbons in soil/sediment samples
may be performed by extraction and gas chromatography. A soil/sediment sample
is extracted at neutral pH with dichloromethane, using either Soxhlet extrac-
tion or sonication, and the extract is dried, solvent-exchanged into hexane,
concentrated, and analyzed by gas chromatography with electron capture detec-
tion (GC/ECD) using either internal or external standards.
INTERFERENCES:
Contact with plastics must be avoided during collection, storage, and
processing of samples. Florisil® column cleanup may be required to eliminate
interferences.
QUALITY CONTROL:
An aliquot of each sample must be spiked with standards to determine
recovery and limits of detection. The analytical system must be demonstrated
to be free of interferences by analysis of a method blank with each set of
samples or change in reagents. Field and laboratory replicates and duplicate
samples should be analyzed to ascertain the precision and accuracy of the
method. In cases where the identification of a peak in the chromatogram is in
question, confirmatory techniques, such as gas chromatography/mass spectrometry
(GC/MS) or second-column confirmation, should be used.
B-483
-------
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
analyses (RCRA). No precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency-. Methods for Organic Chemical Analysis
of Municipal and Industrial WastewaterlJ~. J~i Longbottom; J~i J^ Lichtenberg;
Eds.; Method 612; EPA-600/4-82-059, U.S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8120; SW-846,~
U.S. EPA: Washington, 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $135-150
(list); the cost of a Florisil® column cleanup is approximately $35 (list).
B-484
-------
CHLORINATED HYDROCARBONS
Water Samples
Laboratory Method
Compound CAS Number
Benzotrichloride 98-07-7
Benzyl Chloride 100-44-7
a-BHC 319-86-8
fr-BHC 319-84-5
>-BHC 319-85-7
2-Chloronaphthalene 91-58-7
1,2-Dichlorobenzene 95-50-1
1,3-Dichlorobenzene 541-73-1
1,4-Dichlorobenzene 106-46-7
Hexachlorobenzene 118-74-1
Hexachlorobutadiene 87-68-3
Hexachlorocyclopentadiene 77-47-4
Hexachloroethane 67-72-1
Lindane 59-89-9
1,2,4,5-Tetrachlorobenzene 95-94-3
1,2,4-Trichlorobenzene 120-82-1
METHOD SUMMARY:
Analysis for the above chlorinated hydrocarbons in water can be performed
by extraction and gas chromatography. A sample of water is extracted with
dichlorome thane and the extract is dried, solvent-exchanged into hexane, con-
centrated, and analyzed by gas chromatography with electron capture deterring
(GC/ECD), using either internal or external standards.
INTERFERENCES :
Contact with pasties must be avoided in collection, storage, and process
ing of samples. Florisil®-column cleanup may be required to eliminate fnter-
QUALITY CONTROL:
An aliquot of each sample must be spiked with standards to determine
rpco"ory and limits of detection. The analytical system must be demonstrated
to be free of interferences by the analysis of a method-blank with each set of
samples or change in reagents. Field and laboratory replicates and duplicate
samples should be analyzed to ascertain the precision and accuracy of the
method. In C«S°P x;here identification of a peak in the chromatogram is in
question, confirmatory techniques, such as gas chromatography/mass spectrometry
or second-column confirmation, should be used.
B-485
-------
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
analyses (40 CFR, Part 261, Identification and Listing of Hazardous Wastes) and
for analyses for the Clean Water Act. Precision and accuracy information is
furnished.
REFERENCES;
U.S. Environmental Protection Agency: Methods for Organic Chemical Analysis
of Municipal and Industrial Wastewater, J. J. Longbottom; J. J. Lichtenburg;
Eds., Method 612; EPA-600/4-82-059, U.S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3510, 3520, 8120; SW-846, U.S. EPA:
Washington, July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $120-170
(list); GC/MS confirmation is approximately $150-200 (list); second-column
confirmation is approximately $80 (list).
B-486
-------
CHLORINATED PHENOXY ACID HERBICIDES
Soil/Sediment Samples
Laboratory Method 1
Compound
2,4-D Acid
2,4-D Esters
CAS Number
Dicamba
Dinoseb
2,4,5-T
2,4,5-T Amines
2,4,5-T Esters
2,4,5-TP Acid
2,4,5-TP Acid Esters
2,4,5-T Salts
94-
94-
94.
94-
1320-
1928-
1928-
1929-
2971-
25168-
53467-
1918-
88-
93-
2008-
93-
2545-
61792-
1928-
25168-
93-
32534-
13560-
75-7
•11-1
79-1
•80-4
18-9
•38-7
61-6
73-3
•38-2
•26-7
11-1
00-9
•85-7
76-5
•46-0
79-8
•59-7
•07-2
-47-8
•15-4
•72-1
•95-5
99-1
METHOD SUMMARY:
Analysis for the above chlorinated herbicides in soil/sediment samples may
be performed by extraction and gas chromatography. A soil/sediment sample
equivalent to a 50-gram dry mass is acidified and extracted with acetone
followed by diethyl ether. The combined extracts are heated with aqueous
potassium hydroxide, and the aqueous solution is washed with diethyl ether.
The aqueous solution is then acidified and extracted with diethyl ether. The
diethyl ether extract is dried, concentrated, and treated with diazomethane,
and the solution of methyl esters is analyzed by gas chromatography with an
electron capture detector (GC/ECD), using either internal or external standards
for quantification.
INTERFERENCES:
Samples must be collected in glass containers, and all contact with
plastics should be avoided during sample collection, storage, and processing.
Organic acids and phenols can interfere, and all glassware and glass wool
should be acid-washed, and all sodium sulfate should be acidified before use.
B-487
-------
QUALITY CONTROL:
The analytical system must be demonstrated to be free of interferences by
analysis of a method blank with each set of samples and/or change in reagents.
Laboratory and field replicates should be processed to ascertain the precision
of sampling and analysis, and fortified samples should be analyzed to validate
the accuracy of the analysis. Where doubt exists concerning the identification
of a peak in the chromatogram, confirmatory techniques, such as gas chromato-
graphy/mass spectrometry (GC/MS) and second-column confirmation, should be
used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
sample analyses (40 CFR, Part 261, Identification and Listing of Hazardous
Wastes). No precision or accuracy information is furnished.
REFERENCES;
American Society for Testing and Materials, 1933 Annual Book of ASTM Standards,
Vol. 11.02, D3478-79; ASTM: Philadelphia, 1983, pp. 151-157.
American Society for Testing and Materials, ASTM Standards on Chromatography,
D-3478-79; ASTM: Philadelphia, 1981, pp. 440-447.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 8150; SW-846, U.S. EPA: Washington,
July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $155-230
(list).
B-488
-------
CHLORINATED PHENOXY ACID HERBICIDES
Soil/Sediment Samples
Laboratory Method 2
Compound CAS Number
2,4-D Acid 94-75-7
2,4-D Esters 94-11-1
94-79-1
94-80-4
1320-18-9
1928-38-7
1928-61-6
1929-73-3
2971-38-2
25168-26-7
53467-11-1
Dicamba 1918-00-9
Dinoseb 88-85-7
2,4,5-T 93-76-5
2,4,5-T Amines 2008-46-0
2,4,5-T Esters 93-79-8
2545-59-7
61792-07-2
1928-47-8
25168-15-4
2,4,5-TP Acid 93-72-1
2,4,5-TP Acid Esters 32534-95-5
2,4,5-T Salts 13560-99-1
METHOD SUMMARY:
Analysis of soil/sediment samples for the above chlorinated phenoxy acid
herbicides can be performed by extraction, derivatization, and analysis by gas
chroraatography with electron capture detection (GC/ECD). A 25-gram sample is
acidified and extracted with acetone/hexane, the extract is dried, solvent-
exchanged into benzene, treated with boron trifluoride/methanol, and cleaned up
by silica column chromatography. The resulting solution is analyzed by GC/ECD.
INTERFERENCES:
No interferences are listed.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
B-489
-------
REFERENCES;
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual.
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Sediment
Samples for Chlorinated Phenoxy Acid Acid Herbicides by Acetone-Hexane Extrac-
tion," pp. III-318 to III-321; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Geological Survey, Methods for the Determination of Organic Substances in
Water and Fluvial Sediments, Book 5, "Laboratory Analysis," Chapter A3; USGS^
Denver , Open-File Report, 82-1004, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $170-200
(list).
B-490
-------
CHLORINATED PHENOXY ACID HERBICIDES
Soil/Sediment Samples
Laboratory Method 3
Compound CAS Number
2,4-D Acid 94-75-7
2,4-D Esters 94-11-1
94-79-1
94-80-4
1320-18-9
1928-38-7
1928-61-6
1929-73-3
2971-38-2
25168-26-7
53467-11-1
Dicamba 1918-00-9
Dinoseb 88-85-7
2,4,5-T 93-76-5
2,4,5-T Amines 2008-46-0
2,4,5-T Esters 93-79-8
2545-59-7
61792-07-2
1928-47-8
25168-15-4
2,4,5-TP Acid 93-72-1
2,4,5-TP Acid Esters 32534-95-5
2,4,5-T Salts 13560-99-1
METHOD SUMMARY:
Analysis of soil/sediment samples for the above chlorinated phenoxy acid
herbicides can be performed by high-performance liquid chromatography (HPLC).
A 20-gram sample is acidified and extracted with dichloromethane, the dichloro-
methane is evaporated, and the residue is hydrolyzed with methanolic potassium
hydroxide. The resulting solution is extracted with methylene chloride to
remove organic interferences, the solution is acidified, the solvent is evapor-
ated, the residue is dissolved in methanol, and the resulting solution is
cleaned up by reversed-phase column chromtography. The resulting solution is
then analyzed by high performance liquid chromatography (HPLC) with UV detec-
tion at 285 nanometers.
INTERFERENCES:
No interferences are listed.
QUALITY CONTROL:
No quality control procedures are provided.
B-491
-------
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Sediment
Samples for Chlorinated Phenoxy Acid Acid Herbicides by Acetone-Hexane Extrac-
tion," pp. III-318 to III-321; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $210 (list).
B-492
-------
CHLORINATED PHENOXY ACID HERBICIDES
Water Samples
Laboratory Method 1
Compound
2,4-D Acid
2,4-D Esters
CAS Number
Dicamba
Dinoseb
2,4,5-T
2,4,5-T Amines
2,4,5-T Esters
2,4,5-TP Acid
2,4,5-TP Acid Esters
2,4,5-T Salts
94-
94-
94-
94-
1320-
1928-
1928-
1929-
2971-
25168-
53467-
1918-
88-
93-
2008-
93-
2545-
61792-
1928-
25168-
93-
32534-
13560-
-75-7
•11-1
-79-1
•80-4
•18-9
•38-7
•61-6
•73-3
•38-2
•26-7
•11-1
•00-9
•85-7
•76-5
•46-0
79-8
•59-7
•07-2
•47-8
•15-4
72-1
•95-5
99-1
METHOD SUMMARY:
Analysis of water samples for the above chlorinated herbicides can be
performed by extraction and chromatographic analysis. A water sample is
extracted at pH 2 with diethyl ether, the extract is heated with aqueous
potassium hydroxide, and the aqueous solution is washed with diethyl ether,
acidified, and extracted with diethyl ether. The diethyl ether extract is
dried, concentrated, and treated with diazomethane. The resulting solution of
methyl esters is analyzed by gas chromatography with an electron capture
detector (GC/ECD), using either internal or external standards for quantifi-
cation.
INTERFERENCES:
Grab samples must be collected in glass containers, and all contact with
plastics should be avoided in sample collection, storage, and processing.
Organic acids and phenols can interfere, and all glassware and glass wool
should be acid-washed and all sodium sulfate acidified before use.
B-493
-------
QUALITY CONTROL:
The analytical system must be demonstrated to be free of interferences by
analysis of a method blank with each set of samples and/or change in reagents.
Laboratory and field replicates should be processed to ascertain the precision
of sampling and analysis, and fortified samples should be analyzed to validate
the accuracy of the analysis. Where doubt exists concerning the identification
of a peak in the chromatogram, confirmatory techniques, such as gas chromato-
graphy/mass spectrometry (GC/MS) and second-column confirmation, should be
used.
EPA/TECHNICAL STATUS;
This method is EPA-approved for Resource Conservation and Recovery Act
(RCRA) sample analyses. Precision and accuracy information is furnished.
Detection limits (ASTM, 1983) are 20 nanograms per liter for 2,4-D acid and 5
nanograms per liter for 2,4,5-T and 2,4,5-TP acid.
REFERENCES:
American Society for Testing and Materials, ASTM Standards on Chromatography,
D-3478-79; ASTM: Philadelphia, 1981, pp. 440-447.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, ASTM: Philadelphia, 1983, pp. 151-157.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 8150; SW-846, U.S. EPA: Washington,
July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $155-230
(list).
B-494
-------
CHLORINATED PHENOXY ACID HERBICIDES
Water Samples
Laboratory Method 2
Compound
2,4-D Acid
2,4-D Esters
CAS Number
Dicamba
Dinoseb
2,4,5-T
2,4,5-T Amines
2,4,5-T Esters
2,4,5-TP Acid
2,4,5-TP Acid Esters
2,4,5-T Salts
94-
94-
94-
94-
1320-
1928-
1928-
1929-
2971-
25168-
53467-
1918-
88-
93-
2008-
93-
2545-
61792-
1928-
25168-
93-
32534-
13560-
•75-7
11-1
•79-1
80-4
•18-9
38-7
•61-6
73-3
38-2
26-7
•11-1
00-9
•85-7
76-5
•46-0
79-8
•59-7
•07-2
•47-8
15-4
•72-1
•95-5
99-1
METHOD SUMMARY:
Analysis of water samples for the above chlorinated phenoxy acid herbi-
cides can be performed by gas chromatography. A 1-liter sample is acidified
and extracted with chloroform; the extract is dried, concentrated, solvent-
exchanged into methanol, and the herbicide residues are converted to methyl
esters with a boron trifluoride/methanol reagent. The methyl esters are
extracted into benzene, the extract is cleaned up with a Florisil column, and
the resulting solution is analyzed by gas chromatography with electron capture
detection (GC/ECD).
INTERFERENCES:
No interferences are listed.
QUALITY CONTROL;
No quality control procedures are provided.
B-495
-------
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCES:
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Sediment
Samples for Chlorinated Phenoxy Acid Acid Herbicides by Acetone-Hexane Extrac-
tion," pp. III-318 to III-321; EPA-600/S4-84-038, U.S. Environmental Protection
Agency: Las Vegas, 1984.
U.S. Geological Survey, Methods for the Determination of Organic Substances in
Water and Fluvial Sediments,Book 5,"Laboratory Analysis," Chapter A3; USGS:
Denver, Open-File Report 82-1004, 1983.
Environment Canada, Analytical Methods Manual, Inland Waters Directorate, Water
Quality Branch, Ottowa, Ontario, Canada, 1973.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $170-200
(list).
B-496
-------
Compound
Aldicarb
Aldrin
a-BHC
B-BHC
Y-BHC
Carbaryl
Carbofuran
Chlordane
DDE
DDT
Diazinon
Dieldrin
Endosulfan
METHOD SUMMARY:
CHLORINATED PESTICIDES
Air Samples
Laboratory Method
CAS Number
116-
309-
319-
319-
319-
63-
1563-
57-
72-
50-
333-
60-
115-
•06-3
•00-2
•84-6
•85-7
•86-8
•25-2
•66-2
74-9
•55-9
•29-3
-41-5
•57-1
-29-7
Compound
a-Endosulfan
B-Endosulfan
Endrin
Endrin Aldehyde
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Lindane
Malathion
Methomyl
Methyl Parathion
Parathion
Toxaphene
CAS Number
959-
33213-
72-
7421-
76-
1024-
118-
58-
121-
16752-
298-
56-
8001-
•98-8
65-9
•20-8
93-4
•44-8
57-3
•74-1
89-9
•75-5
77-5
•00-0
38-2
35-2
Analysis of air samples for the above pesticides can be performed by gas
chromatography. The pesticides are collected on polyurethane foam by sampling
air with a calibrated sampling device; the polyurethane foam is Soxhlet-
extracted and the extract is cleaned up, concentrated, and analyzed by gas
chromatography. Organochlorine pesticides are measured by gas chromatography
with electron-capture detection (GC/ECD), organophosphorus pesticides by gas
chromatography with flame photometric detection (GC/FPD), and carbamate pesti-
cides by either gas chromatography with Hall electrolytic conductivity detec-
tion (GC/HECD) in the N-mode, or derivatization and GC/ECD. Confirmation of
peak identification can be performed by gas chromatography/mass spectrometry
(GC/MS).
INTERFERENCES:
Extracts to be analyzed for organochlorine pesticides should be cleaned up
by alumina column chromatography; the presence of polychlorinated biphenyls
(PCBs) may require cleanup by silicic acid column chromatography. Analysis for
organophosphorus pesticides must be performed without column chromatographic
cleanup, and extracts to be analyzed for carbamate pesticides should be cleaned
up by silica-gel column chromatography.
QUALITY CONTROL:
The collection efficiency and desorption efficiency of the sampling device
must be demonstrated by multiple tests before sampling begins. The sampling
system must be calibrated before use.
B-497
-------
EPA/TECHNICAL STATUS:
This method is not EPA-approved, but has undergone EPA evaluation. No
precision or accuracy information is furnished.
REFERENCES;
U.S. Environmental Protection Agency, Manual of Analytical Methods for the
Analysis of Pesticides in Humans and Environmental Samples; EPA-600/8-80-038,
U.S. EPA: Research Triangle Park, North Carolina, 1980.
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Waste Sites, Assignment 26, Appendix B; Contract 68-02-3168;~~
U.S. EPA: Research Triangle Park, North Carolina, May 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $135-220
(list), plus sampling costs.
B-498
-------
CHLORINATED PHENOLS
Air Samples
Laboratory Method
Compound CAS Number
2,4-Dichlorophenol 120-83-2
Pentachlorophenol 87-86-5
2,4,5-Trichlorophenol 95-95-4
2,4,6-Trichlorophenol 88-06-2
METHOD SUMMARY:
Analysis of an air sample for the above airborne chlorinated phenols is
performed by passage of 1000 liters of air through a polyurethane-foam sampling
tube, followed by Soxhlet extraction of the foam, and analysis of the extract
by gas chromatography with electron capture detection (GC/ECD). When concen-
tration levels are high, confirmation of peak identification can be performed
by gas chromatography/mass spectrometry (GC/MS).
INTERFERENCES:
Phthalate esters and polychlorinated naphthalenes can interfere, and use
of non-TFE plastics must be avoided.
QUALITY CONTROL:
Solvents, reagents, glassware, and polyurethane plugs must be shown to be
free of interfering artifacts. A field blank must be analyzed with each set of
samples, and both a quality control standard and a method blank should be
analyzed with each set of 5 to 15 samples.
EPA/TECHNICAL STATUS:
This method has been evaluated by the Environmental Protection Agency, but
is not approved for any specific regulatory program. No precision or accuracy
information is furnished. This method is applicable to concentrations of 1 to
1000 nanograms per cubic meter.
REFERENCE:
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Waste Sites, Assignment 26, Appendix B; Contract 68-02-3168, U.S. EPA,
U.S. EPA: Research Triangle Park, North Carolina, May 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $115 (list);
the cost of GC/MS confirmation is approximately $150-200 (list). Sampling
costs are additional.
B-499
-------
CHLORINATED PHENOLS
Water Samples
Laboratory Method
Compound CAS Number
2,4-D Acid 94-75-7
Hexachlorophene 70-70-4
Pentachlorophenol 87-86-5
2,4,5-T-Acid 93-76-5
2,3,4,6-Tetrachlorophenol 58-90-2
2,4,6-Trichlorophenol 25167-82-2
METHOD SUMMARY:
The above chlorinated phenols in water samples can be measured by gas
chromatography with electron capture detection (GC/ECD). The sample is passed
through a strongly basic anion-exchange resin bed, then the phenols are
extracted with benzene (containing an internal standard), and derivatized into
the corresponding methyl ethers. The extract, containing the methyl ethers, is
analyzed by GC/ECD and the results are compared to standards.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The detection limits for the different
substances range from 0.001-0.1 parts per billion in one liter of water. No
precision or accuracy information is furnished.
REFERENCES:
Renberg, L. "Ion Exchange Technique for the Determination of Chlorinated
Phenols and Phenoxy Acids in Organic Tissue, Soil, and Water," Anal. Chem.,
46^(3), 1974, pp. 459-461.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $155-180
(list).
B-500
-------
CHLOROBENZENES
Air Samples
Laboratory Method
Compound CAS Number Range (mg/m3)
Pentachlorobenzene 608-93-5 0.008-22
1,2,4,5-Tetrachlorobenzene 95-95-4 0.003-31
1,2,4-Trichlorobenzene 120-82-1 0.002-100
METHOD SUMMARY:
Gas chromatography can be used for the analysis of the above chloroben-
zenes in air. A known volume of air is drawn through a 2-stage sampler
consisting of a Teflon fiber mat filter followed by a tube containing 2
sections of Amberlite XAD-2 resin sorbent. The analyte from the filter and 2
sorbent sections is desorbed separately with hexane. The resulting solutions
are analyzed with a gas chromatograph with electron capture detection (GC/ECD).
INTERFERENCES:
Separation of 1, 2, 3,5-tetrachlorobenzene and 1,2,4,5-tetrachlorobenzene is
not possible using this method.
QUALITY CONTROL;
Method blanks and standards must be analyzed with the samples.
EPA/TECHNICAL STATUS:
This method has been accepted by the National Institute for Occupational
Safety and Health (NIOSH) for use over the ranges listed above (in a 10- to 12-
liter sample). Precision and accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods,
Vol. 7, Method P&CAM 343; Publication No. 82-100, U.S. DHHS: Cincinnati, August
1981.
COST INFORMATION:
Cost per sample for analyses by this method is approximately $90 (list),
plus sampling costs.
B-501
-------
B-CHLOROETHERS
Air Samples
Laboratory Method
Compound CAS Number
Bis(2-chloroethoxy) Methane 111-91-1
Bis(2-chloroethyl) Ether 111-44-4
Bis(2-chloroisopropyl) Ether 108-60-1
2-Chloroethyl Vinyl Ether 110-75-8
METHOD SUMMARY:
The above 6-chloroethers in air samples can be measured by gas chromato-
graphy/mass spectrometry (GC/MS). The samples are collected by drawing air
through two tubes packed with Tenax GC, which are both desorbed with methanol.
An aliquot of the resulting solution is then analyzed by GC/MS.
INTERFERENCES:
Chloroethyl vinyl ether and chloroethyl ethyl ether have the same reten-
tion time and thus are not separatable by use of the GC/MS.
QUALITY CONTROL:
Tubes spiked in the field and control tubes are handled in the same manner
as samples.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The limit of detection is 0.7 micrograms per cubic meter.
REFERENCE:
Sherman, P. L.; Kemmer, A. M.; Metacalfe, L.; Toy, H. D. Environmental Monitor-
ing Near Industrial Sites: g-Chloroethers; EPA-560/6-78-003, U.S. Environ-
mental Protection Agency: Washington, June 1978.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $250-335
(list), plus sampling costs.
B-502
-------
CRESOLS
Air Samples
Laboratory Method
Compound CAS Number
Cresol 1319-77-3
m-Cresol 108-39-4
£-Cresol 95-48-7
p-Cresol 106-44-5
METHOD SUMMARY:
Analysis of air samples for the above cresols can be performed by passage
of a known volume of air through a silica-gel tube trap, followed by desorption
with acetone and analysis of the resulting solution by gas chromatography with
flame ionization detection (GC/FID).
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
QUALITY CONTROL:
A method blank must be processed and the desorption efficiency calculated
for each set of samples. The results for the samples must be corrected accord-
ingly.
EPA/TECHNICAL STATUS;
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 10 to 42 milligrams per
cubic meter for a 20-liter air sample. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set L, Method S167; PB-250 159 (NTIS), U.S. DHEW: Washington, January 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S167; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
B-503
-------
DINITROBENZENES
Air Samples
Laboratory Method
Compounds CAS Number
Dinitrobenzene (mixed) 25154-54-5
m-Dinitrobenzene 99-65-0
o-Dinitrobenzene 528-29-0
£-Dinitrobenzene 100-25-4
METHOD SUMMARY:
The above dinitrobenzenes in air samples may be measured by high-perfor-
mance liquid chromatography (HPLC). A known volume of air is drawn through a
mixed cellulose ester membrane filter connected in series to a midget bubbler
containing 10 milliliters of ethylene glycol. After collection of the sample,
the filter is placed in the bubbler flask and 5 milliliters of methanol are
added. The resulting solution is analyzed by HPLC with UV detection.
INTERFERENCES:
Any compound that has the same retention time as dinitrobenzene will
interfere.
QUALITY CONTROL:
Since no internal standard is used in this method, standard solutions must
be analyzed at the same time as the samples. A correction for the blank must
be made for each sample.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.42 to 2.4 milligrams per
cubic meter, using a 90-liter sample. Precision and accuracy information is
furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S214; Publication No. 78-175, U.S. DREW:
Cincinnati, 1978.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $100-110
(list), plus sampling costs.
B-504
-------
DINITROTOLUENES
Air Samples
Laboratory Method
Compounds CAS Number
Dinitrotoluene 25321-14-6
2,4-Dinitrotoluene 121-14-2
2,6-Dinitrotoluene 606-20-2
METHOD SUMMARY:
Analysis of air for the above dinitrotoluenes can be performed by sampling
with silica gel tubes, desorption with carbon tetrachloride, and gas chroraato-
graphic (FID) analysis. The method differentiates between dinitrotoluene
isomers.
INTERFERENCES:
No interferences' are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Hunt, R. I.; Neubauer, N. R. ; Picone, R. F. "An Improved Procedure for Sampling
and Analysis of Dinitrotoluene Vapor Concentrations in Workplace Air,"
Am. Ind. Hyg. Assoc. J., _41(8), 1980, pp. 592-594.
COST INFORMATION:
Cost per sample for this analysis is approximately $70-90 (list), plus
sampling costs.
B-505
-------
DIURON AND PYRETHRINS
Air Samples
Laboratory Method
Compounds CAS Number
Diuron 330-54-1
Pyrethrins 121-29-9
121-21-1
METHOD SUMMARY:
Diuron and pyrethrins in air can be determined by high-performance liquid
chromatography (HPLC). The sample is collected in a low-volume system using
polyurethane foam as a trapping medium. The foam is Soxhlet extracted with
5-percent ethyl ether in hexane, the extract is concentrated in a rotary
evaporator, and an aliquot is analyzed by reversed-phase HPLC with UV detection.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. No precision or accuracy information for
the analyses is furnished.
REFERENCE;
Lewis, R. G.; MacLeod, K. E. "Portable Sampler for Pesticides and Semivolatile
Industrial Organic Chemicals in Air," Anal Chem., 54, 1982, pp. 310-315.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $165 (list),
plus sampling costs.
B-506
-------
EXPLOSIVES
Water Samples
Laboratory Method
Compounds CAS Number
Dinitrotoluene 25321-14-6
Nitroglycerine 55-63-0
METHOD SUMMARY:
The above explosives in water samples can be measured by single-sweep
polarography. The substances are extracted from the water into a suitable
solvent, which is then evaporated. The analyte is determined by polarography
with an appropriate supporting electrolytic solution, either directly or by the
standard addition method.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. The method is for use over the range of 5 micrograms to 5 milligrams
of analyte per liter.
REFERENCE:
Whitnack, G. C. "Single-Sweep Polarographic Techniques Useful in Micropollu-
tion Studies of Ground and Surface Waters," Anal. Chem., ^7(4), 1975, pp.
618-621.
COST INFORMATION:
Cost information has not been obtained.
B-507
-------
Compound
Acrylonitrile
Bis(2-Chloroethyl) Ether
Bromoform
Carbon Bisulfide
Carbon Tetrachloride
Chlorobenzene
Chloroform
1,2-Dichlorobenzene
1,4-Dichloroenzene
Ethylene Dibromide
METHOD SUMMARY:
FUMIGANTS
Air Samples
Laboratory Method
CAS Number Compound CAS Number
107-13-1 Hydrogen Cyanide 74-90-8
111-44-4 Methyl Bromide 74-83-9
75-25-2 Methyl Chloride 74-87-3
75-15-0 Methylene Chloride 75-09-2
56-23-5 Phosphine 7803-51-2
108-90-7 Propylene Bichloride 78-87-5
67-66-3 Tetrachloroethylene 127-18-4
95-50-1 1,1,1-Trichloroethane 71-55-6
106-46-7 Trichloroethylene 79-01-6
106-93-4
Gas chromatography may be used to analyze air for the above fumigants. A
bubbler, charged with 1-butanol, n-pentane, or in-xylene is used to collect the
analyte, and the resulting solution is analyzed by gas chromatography with
flame ionization detection (GC/FIB).
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Berck, B. "Determination of Fumigant Gases by Gas Chroraatography," J. Agric.
Food Chem. , J_3(4). 1965, pp. 373-377.
COST INFORMATION:
Cost per sample of analysis by this method is approximately $60-90 (list),
plus sampling costs.
B-508
-------
GASEOUS CONTAMINANTS
Air Samples
Laboratory Method
Compound CAS Number
Acetonitrile 75-05-8
Benzene 71-43-2
Cyclohexane 110-82-7
1,2-Dichlorobenzene 95-50-1
Dichlorodifluoromethane 75-71-8
1,2-Dichloroethane 107-06-2
Furan 10-00-9
Methyl Ethyl Ketone 78-93-3
Vinyl Chloride 75-01-4
METHOD SUMMARY:
The above gaseous contaminants in air samples can be determined by long-
path laser absorption spectrometry. Measurements are performed using a 50-
centimeter cell with sodium chloride windows. The response of the sample to
the laser is received by a pyroelectric detector, amplified, and the data
treated by computer.
INTERFERENCES:
The number and absorption characteristics of other substances in the
sample affect the determination of each particular substance.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Limited precision and accuracy information
is furnished. The detection limit varies with the composition of the sample,
but is generally in the parts-per-million range.
REFERENCES:
Green, B. D. ; Steinfeld, J. I. "Monitoring Complex Trace-Gas Mixtures by Long-
Path Laser Absorption Spectrometry," Proc. Soc. Photo-Opt. Instrum. Eng., 99,
1977, pp. 32-38.
Green, B. D. ; Steinfeld, J. I. "Laser Absorption Spectroscopy: Method for
Monitoring Complex Trace Gas Mixtures," Environ. Sci. Technol., J_0(2), 1976,
pp. 1134-1138.
B-509
-------
COST INFORMATION:
No cost information has been obtained.
B-510
-------
HALOGENATED, AROMATIC, AND OTHER COMPOUNDS
Air Samples
Laboratory Method
Compound CAS Number Compounds CAS Number
Acetaldehyde 75-07-0 1,2-Dichlorobenzene 95-50-1
Acetic Acid 64-19-7 1,4-Dichlorobenzene 106-46-7
Acetic Anhydride 108-24-7 1,1-Dichloroethane 75-34-3
Acetone 67-64-1 1,2-Dichloroethane 107-06-2
Acetonitrile 75-05-8 1,1-Dichloroethylene 156-60-5
Acetophenone 98-86-2 1,2-Dichloroethylene
Acrolein 107-02-8 1,1-Dimethylhydrazine 57-14-7
Acrylonitrile 107-13-1 Epichlorohydrin 106-89-8
Allyl Alcohol 107-18-6 Ethyl Acetate 141-78-6
Allyl Chloride 107-05-1 Ethyl Acrylate 140-88-5
Aniline 62-53-3 Toluene 108-88-3
Benzene 71-43-2 1,2,4-Trichlorobenzene 120-82-1
Benzoic Acid 65-85-0 1,1,1-Trichloroethane 71-55-6
Bis(2-Chloroethyl) Ether 111-44-4 1,1,2-Trichloroethane 79-00-5
Butyl Acetate 123-86-4 Trichloroethylene 79-01-6
n-Butyl Alcohol 71-36-3 Vinyl Chloride 75-01-4
Carbon Tetrachloride 56-23-5 Xylene 1330-20-7
Chlorobenzene 108-90-7 m-Xylene 108-38-3
Chloroethane 75-00-3 o-Xylene 95-47-6
Chloroform 67-66-3 £-Xylene • 106-42-3
Cumene
METHOD SUMMARY:
Analysis for the above halogenated and aromatic compounds in air can be
performed by passage of 25 to 80 liters of air through a Tenax© sorbent tube,
followed by thermal desorption of the analytes into a temperature-programmed
gas chromatograph with mass spectrometric detection (GC/MS).
INTERFERENCES:
Sorbent contaminants represent the primary source of interferences, and
sorbent plugs should be pre-extracted and packaged to prevent contamination
both before and after sampling. The sorbent should be Soxhlet-extracted with
methanol, and then with pentane, for 24 hours, and dried under helium before
use. Decomposition of analyte due to ultraviolet radiation has been reported.
QUALITY CONTROL:
Analysis of duplicate samples should agree within 20 percent. One method
blank must be processed with each set of 20 or fewer samples, and a blank
sampling cartridge should be analyzed after each analysis of a sample with
heavy organic loading. If method blanks show any peaks, the results must be
adjusted accordingly. A field blank should be analyzed with each set of 20 or
fewer samples, and a laboratory control standard must be processed with each
B-511
-------
set of 20 or fewer samples and give results within 20 percent of the actual
concentration.
EPA/TECHNICAL STATUS:
This method is not EPA-approved for any regulatory program, but has been
evaluated by the EPA. No precision or accuracy information is furnished. The
method is applicable from a level of 2 micrograms per cubic meter. Break-
through volumes are reported by Brown and Purnell.
REFERENCES:
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Wastes Sites, Assignment No. 26, Appendix A; Contract 68-02-3168, U.S. EPA:"
Research Triangle Park, North Carolina, 1982.
Schlitt, H.; Knoeppel, H.; Versino, B.; Peil, A.; Schauenburg, H.; Visers, H.
In Sampling and Analysis of Toxic Organics in the Atmosphere; ASTM STP 721,
American Society for Testing and Materials: Philadelphia, 1980, pp. 22-35.
Brooks J.; West, D. Portable Miniature Sampler for Potential Airborne Carcino-
gens in Microenvironments, Phase 1; Development; EPA-600/2-80-026, U.S. EPA,
1980.
Pellizzari, E. D. ; Carpenter, B. H. ; Bunch, J. E.; Sawicki, E. "Collection and
Analysis of Trace Organic Vapor Pollutants in Ambient Atmospheres," Environ.
Sci. Technol., _9(6), 1975, pp. 556-560.
Brown, R. H.; Purnell, C. J. "Collection and Analyses of Trace Organic Vapor
Pollutants in Ambient Atmospheres," J. Chromatogr. 178, 1979, pp. 79-90.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $250-325
(list), plus sampling costs.
B-512
-------
HALOGENATED COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Bromoform 75-25-2
Carbon Tetrachloride 56-23-5
Chlorobenzene 108-90-7
Chlorodibromomethane 124-48-1
Chloroform 67-66-3
Dichlorobromomethane 75-27-4
Methylene Chloride 75-09-2
Methyl Iodide 74-88-4
1,1,2,2-Tetrachloroethane 79-34-5
Trichloroethylene 79-01-6
METHOD SUMMARY:
The above halogenated compounds in water samples can be measured by gas
chromatography (GC). The analytes are collected from the water by a purge and
trap apparatus, then desorbed directly into the GC instrument. The effluent
from the GC column is split to be monitored by both a flame ionization detector
(FID) and a microwave emission detector, which is element-selective and can
distinguish the different halogens.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. Limits of detection range from 54 to 280 nanograms of analyte per
liter of water.
REFERENCE:
Quimby, B. D. ; Delaney, M. F. ; Uden, P. C. ; Barnes, R. M. "Determination of
Trihalomethanes in Drinking Water by Gas Chromatography with a Microwave Plasma
Emission Detector," Anal. Chem., 5^(7), 1979, pp. 875-880.
COST INFORMATION:
Cost information has not been obtained.
B-513
-------
HALOGENATED VAPORS
Air Samples
Laboratory Method
Compound CAS Number
Carbon Tetrachloride 56-23-5
Trichloromonofluoromethane 75-69-4
METHOD SUMMARY:
Analysis of air for carbon tetrachloride and trichloromonofluorome thane
can be performed by gas chromatography. A sample is pressurized, the analytes
are condensed with liquid nitrogen, and the sample is evacuated into a gas
chromatograph with electron capture detection (GC/ECD). Calibration is by the
exponential dilution method.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The lower limit of detection without pre-
concentration is 10 microliters per cubic meter for carbon tetrachloride and 2
microliters per cubic meter for trichloromonofluoromethane. No precision or
accuracy information is furnished.
REFERENCE:
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-07, "Chromatographic
Determination of SF^ , CC^F, CC14, and ^0," HASL-300, Environmental Measurement
Laboratory, U.S. DOE: New York, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70, plus
sampling costs.
B-514
-------
HALOGENATED VOLATILE ORGANIC COMPOUNDS
Soil/Sediment Samples
Laboratory Method
Estimated Detection
Limit (yg/L)
Compound CAS Number (SW-846, EPA)
Benzyl Chloride 100-44-7 0.20
Bromoform 75-25-2
Chloral 75-87-6
Chloroacetaldehyde 107-20-0
Chlorobenzene 108-90-7 0.25
Chloroethane 75-00-3 0.52
2-Chloroethyl Vinyl Ether 110-75-8 0.13
Chloroform 67-66-3 0.05
Chloromethyl Methyl Ether 107-30-2
Dichlorobenzene (mixed) 25321-22-6 0.24
1,2-Dichlorobenzene 95-50-1 0.15
1,3-Dichlorobenzene 541-73-1 0.32
1,4-Dichlorobenzene 106-46-7 0.24
Dichlorobromomethane 75-27-4 0.10
Dichlorodifluoromethane 75-71-8 1.81
1,1-Dichloroethane 75-34-3 0.07
1,2-Dichloroethane 107-06-2 0.03
1,1-Dichloroethylene 75-35-4 0.13
1,2-trans-Dichloroethylene 156-60-5 0.10
1,2-Dichloropropane 78-87-5 0.04
l,3-cis_-Dichloropropene 26952-23-8 0.20
1,3-trans-Dichloropropene 542-75-6 0.34
Methyl Bromide 74-83-9 1.18
Methyl Chloride 74-87-3 0.08
Methylene Bromide 74-95-3
Methylene Chloride 75-09-2 0.25
1,1, 1,2-Tetrachloroethane 630-20-6
1,1,2,2-Tetrachloroethane 79-34-5 0.03
Tetrachloroethylene 127-18-4 0.03
1,1,1-Trichloroethane 71-55-6 0.03
1,1,2-Trichloroethane 79-00-5 0.02
Trichloroethylene 79-01-6 0.12
Trichloromonofluoromethane 75-69-4
Vinyl Chloride 75-01-4 0.18
METHOD SUMMARY:
Analysis of soil/sediment samples for the above halogenated compounds can be
performed by gas chromatography. A solid sample, dispersed in methanol or
polyethylene glycol, is purged with an inert gas onto a sorbent trap, and the^
trap is heated and backflushed into a gas chromatograph equipped with an elec-
tron capture detector (GC/ECD). Either internal or external standards may be
used for quantification.
B-515
-------
INTERFERENCES:
Sample contact with plastics during collection, storage, or processing
must be avoided.
QUALITY CONTROL:
The analytical system must be demonstrated to be free of interferences
through analysis of a method blank each time a set of samples is processed or a
change in reagents occurs. Field replicates, laboratory replicates, and forti-
fied samples must be analyzed to demonstrate the precision and accuracy of the
method. In cases of doubt regarding the identity of a peak in the chromato-
gram, confirmatory techniques such as gas chromatography/mass spectrometry
(GC/MS) or second-column confirmation should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use under the Resource Conservation and
Recovery Act (RCRA). Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom; J. J. Lichtenberg, Eds.,
Method 601; EPA-600/4-82-059, U.S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 8010, 5020, 5030; SW-846, U.S. EPA:
Washington, July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $80-145
(list).
B-516
-------
HALOGENATED VOLATILE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound
Benzyl Chloride
Bromoform
Chloral
Chloroacetaldehyde
Chlorobenzene
Chloroethane
2-Chloroethyl Vinyl Ether
Chloroform
Chloromethyl Methyl Ether
Dichlorobenzene (mixed)
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
Dichlorobromomethane
Dichlorodifluoromethane
1,1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethylene
1,2-trans-Dichloroethylene
1,2-Dichloropropane
1,3-cis-Dichloropropene
1,3-trans-Dichloropropene
Methyl Bromide
Methyl Chloride
Methylene Bromide
Methylene Chloride
1,1,1,2-Tetrachloroethane
1,1,2,2-Tetrachloroethane
Tetrachloroethylene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethylene
Trichloromonofluoromethane
Vinyl Chloride
METHOD SUMMARY:
CAS Number
100-
75-
75-
107-
108-
75-
110-
67-
107-
25321-
95-
541-
106-
75-
75-
75-
107-
75-
156-
78-
26952-
542-
74-
74-
74-
75-
630-
79-
127-
71-
79-
79-
75-
75-
•44-7
25-2
•87-6
•20-0
•90-7
00-3
•75-8
66-3
•30-2
22-6
•50-1
73-1
•46-7
27-4
•71-8
•34-3
-06-2
•35-4
-60-5
•87-5
•23-8
•75-6
•83-9
•87-3
-95-3
•09-2
-20-6
•34-5
-18-4
•55-6
•00-5
•01-6
-69-4
•01-4
Method Detection
Limit (yg/L)
(SW-846, EPA)
0.20
0.25
0.52
0.13
0.05
0.24
0.15
0.32
0.24
0.10
1.81
0.07
0.03
0.13
0.10
0.04
0.20
0.34
1.18
0.08
0.25
0.03
0.03
0.03
0.02
0.12
0.18
Analysis of water samples for the above volatile organic compounds can be
performed by gas chromatography. A water sample is purged with an inert gas
onto a trap and the trap is heated and backflushed into a gas chromatograph
with an electron capture detector (GC/ECD), using either internal or external
standards for quantification. Alternatively, the sample can be extracted with
isooctane and the resulting solution analyzed by GC/ECD.
B-517
-------
INTERFERENCES:
Contact of the samples with plastics during collection, storage, or pro-
cessing must be avoided. The analytical system must be demonstrated to be free
of interferences by the analysis of a method blank each time a set of samples
is processed or a change in reagents occurs.
QUALITY CONTROL:
Field replicates, laboratory replicates, and fortified samples must be
analyzed to determine the precision and accuracy of the method. In cases of
doubt regarding the identity of a peak on the chromatogram, confirmatory
techniques such as gas chromatography/mass spectrometry (GC/MS) or second-
column confirmation should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use under the Federal Water Pollution
Control Act and the Resource Conservation and Recovery Act (40 CFR, Part 261,
Identification and Listing of Hazardous Waste). Precision and accuracy infor-
mation is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 8010, 5030; SW-846; U.S. EPA:
Washington, July 1982.
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom; J. J. Lichtenberg; Eds.,
Method 601; EPA-600/4-82-059, U.S. EPA: Cincinnati, 1982.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D3973-80; ASTM: Philadelphia, 1983^
COST INFORMATION:
Cost per sample for analysis by this method is approximately $115 (list).
B-518
-------
Compound
Acetaldehyde
Acetone
Acetophenone
Acrolein
Allyl Chloride
Aniline
Bis(Chloromethyl) Ether
Bis(2-Chloroisopropyl)
Ether
Bromoform
iso-Butylamine
Butyric Acid
Carbon Tetrachloride
Chlorobenzene
Chloroform
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,2-Dichloroethane
1,1-Dichloroethylene
1,2-Dichloropropane
Dichloropropene
1,2:3,4-Diepoxybutane
Diethyl Phthalate
Dimethylamine
Dimethyl Phthalate
Epichlorohydrin
Ethyl Acetate
Ethylbenzene
METHOD SUMMARY:
HAZARDOUS ORGANIC EMISSIONS
Air Samples
Laboratory Method
CAS Number Compound CAS Number
75-07-0 Ethylene Dibromide 106-93-4
Ethyl Ether 60-29-7
98-86-2 Glycidylaldehyde 765-34-3
107-02-8 Hexachlorobutadiene 87-68-3
107-05-1 Hexachloroethane 67-72-1
62-53-3 Methanol 90-80-5
542-88-1 Methyl Bromide 74-83-9
108-60-1 Methyl Chloride 74-87-3
Methylene Bromide 74-95-3
75-25-2 Methyl Chloride 75-09-2
78-81-9 Methyl Methacrylate 80-62-6
107-92-6 Nitric Oxide 10102-43-9
56-23-5 Nitrogen Dioxide 10102-44-0
108-90-7 N-Nitrosodiethylamine 55-18-5
67-66-3 N-Nitrosodimethylamine 62-75-9
95-50-1 Pentachloroethane 76-01-7
541-73-1 Phenol 108-95-2
107-06-2 Phosgene 75-44-5
75-34-5 Propylene Oxide 75-56-9
78-87-5 Pyridine 110-86-1
26952-23-8 1,1,1,2-Tetrachloroethane 630-20-6
1464-53-5 1,1,2,2-Tetrachloroethane 79-34-5
84-66-2 Tetrachloroethylene 127-18-4
124-40-3 Toluene 108-88-3
131-11-3 1,1,1-Trichloroethane 71-55-6
106-89-8 Trichloroethylene 79-01-6
141-78-6 Vinyl Chloride 75-01-4
100-41-4
Analysis of air for the above organic compounds can be performed by gas
chromatography/mass spectrometry (GC/MS). Air is pumped through a Tenax®
cartridge, the cartridge is desorbed into a liquid nitrogen trap, and the
sample is released into the GC/MS instrument by rapidly heating the trap.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
With each batch of samples, two or three sampling cartridges should be
processed as blanks.
B-519
-------
EPA/TECHNICAL STATUS:
Sampling precision and accuracy information for some compounds is given.
Breakthrough volumes are given or estimated for some compounds.
REFERENCE;
Krost, K.; Pellizzari, E. D.; Walburn, S. G.; Hubbard, S. A. "Collection and
Analysis of Hazardous Organic Emissions," Anal. Chem., 54(4), 1982, pp. 810-
817.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $250-325
(list), plus sampling costs.
B-520
-------
HAZARDOUS COMPOUNDS
Air Samples
Laboratory Method
Compound CAS Number
2-Acetylaminofluorene 53-96-3
Benzidine 92-87-5
3,3'-Dichlorobenzidine 91-94-1
Diethylstilbestrol 56-53-1
3,3'-Dimethoxybenzidine 119-90-4
3,3'-Dimethylbenzidine 119-93-7
1-Naphthylamine 134-32-7
2-Naphthylamine 91-59-8
METHOD SUMMARY:
The above hazardous compounds in air samples can be measured by gas
chromatography with electron capture detection (GC/ECD). The sample is
collected on an air filter. The procedure for removal of the compounds from
the filter is not specified. The sample is partitioned between an aqueous acid
solution and benzene. The two phases are treated separately by pH adjustments
and additonal extraction steps to eventually produce three fractions; a
phenolic fraction containing estrogens (diethylstilbestrol), a neutral fraction
containing acetylaminofluorene hydrolyzed to 2-aminofluorene, and a basic
fraction containing the amines. The residues are converted to their penta-
fluoropropionyl derivatiives before GC/ECD analysis.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The limit of detection is not specified, but the method is designed
for analysis at the sub- to low- parts-per-billion range.
REFERENCE:
Bowman, M. C. "Trace Analysis: A Requirement for Toxicological Research with
Carcinogens and Hazardous Substances," J. Assoc. Off. Anal. Chem. , 6_1(5), 1978,
pp. 1253-1262.
B-521
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $150-240
(list) (est.)«
B-522
-------
HAZARDOUS COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
2-Acetylaminofluorene 53-96-3
Benzidine 92-87-5
3,3'-Dichlorobenzidine 91-94-1
Diethylstilbestrol 56-53-1
3,3'-Dimethoxybenzidine 119-90-4
3,3'-Dimethylbenzidine 119-93-7
1-Naphthylamine 134-32-7
2-Naphthylamine 91-59-8
METHOD SUMMARY:
The above hazardous compounds in water samples can be measured by gas
chromatography with electron capture detection (GC/ECD). The sample is acidi-
fied and then extracted with benzene. The two phases are treated separately by
pH adjustments and additional extraction steps to eventually produce three
fractions: a phenolic fraction containing estrogens (diethylstilbestrol), a
neutral fraction containing acetylaminofluorene hydrolyzed to 2-aminofluorene,
and a basic fraction containing the amines. The residues are converted
to their pentafluoropropionyl derivatives before the GC/ECD analysis.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The limit of detection is not specified, but the method is designed
for analysis at the sub- to low- parts-per-billion range.
REFERENCE:
Bowman, M. C. "Trace Analysis: A Requirement for Toxicological Research with
Carcinogens and Hazardous Substances," J. Assoc. Off. Anal. Chem., ^_U5), 1978,
pp. 1253-1262.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $150-240
(list) (est.).
B-523
-------
HERBICIDES
Air Samples
Laboratory Method
Compound CAS Number
2,4-D Esters 94-11-1
94-79-1
94-80-4
1320-18-9
1928-38-7
1928-61-6
1929-73-3
25168-26-7
53467-11-1
2971-38-2
2,4,5-T Esters 93-79-8
2545-59-7
61792-07-2
1928-47-8
25168-15-4
METHOD SUMMARY:
Analysis for the above airborne herbicides is performed by passage of
1000 liters of air through a polyurethane-foara sampling tube, followed by
Soxhlet extraction of the foam, and analysis of the extract by gas chromato-
graphy with electron capture detection (GC/ECD). When concentration levels are
high, confirmation of peak identification is performed by gas chromatography/
mass spectrometry (GC/MS).
INTERFERENCES:
Phthalate esters and polychlorinated naphthalenes can interfere, and use
of non-TFE plastics must be avoided.
QUALITY CONTROL:
Solvents, reagents, glassware, and polyurethane plugs must be shown to be
free of interfering artifacts. A field blank must be analyzed with each set of
samples, and both a quality control standard and a method blank should be
analyzed with each set of 5 to 15 samples.
EPA/TECHNICAL STATUS:
This method has been evaluated by the Environmental Protection Agency, but
is not approved for any specific regulatory program. No precision or accuracy
information is furnished. This method is applicable to a range from 1 nanogram
to 1000 nanograms per cubic meter.
B-524
-------
REFERENCE;
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Waste Sites, Assignment 26, Appendix B; Contract 68-02-3168, U.S. EPA: Research
Triangle Park, North Carolina, May 1982.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $115 (list);
the cost of GC/MS confirmation is approximately $150-200 (list). Sampling
costs are additional.
B-525
-------
HYDROCARBON ODORANTS
Air Samples
Laboratory Method
Compound CAS Number
Benzene 71-43-2
Ethylbenzene 100-41-4
Isoprene 78-79-5
Toluene 108-88-3
m-Xylene 108-38-3
o-Xylene 95-47-6
p-Xylene 106-42-3
METHOD SUMMARY:
The above hydrocarbon odorants in air samples can be measured by gas
chromatography (GC). The sample is collected by cold trapping with liquid
nitrogen and undergoes a pre-column concentration step before analysis.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
detection limits are 0.1 to 5.5 micrograms per cubic meter.
REFERENCE:
Hoshika, Y.; Nihei, Y.; Muto, G. "Pattern Display for Characterization of
Trace Amounts of Odorants Discharged from Nine Odour Sources," Analyst, 106,
1981, pp. 1187-1202.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $105-120
(list).
B-526
-------
LOW-MOLECULAR-WEIGHT ALIPHATIC AMINES
Air Samples
Laboratory Method
Compound CAS Number
Butylamine 109-73-9
iso-Butylamine 78-81-9
sec-Butylamine 513-49-5
13852-84-6
tert-Butylamine 75-64-9
Diethylamine 109-89-7
Dimethylamine 124-40-3
Trimethylamine 75-50-3
METHOD SUMMARY:
The above low-molecular-weight aliphatic amines in air samples can be
measured by gas chromatography with nitrogen-phosphorus detection (GC/NPD). A
known volume of air is passed through a prepared SEP-PAK C^Q cartridge to
collect the analyte which is then desorbed with methanol:water (1:1). The pH
of the eluant is adjusted, the solution is brought to volume, and an aliquot is
analyzed by GC/NPD.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precison and accuracy information is
furnished. The limit of detection is 9 micrograms per cubic meter.
REFERENCE:
Kuwata, K.; Akiyama, E.; Yamazaki, Y.; Yamasaki, H.; Kuge, Y.; Kiso, Y. "Trace
Determination of Low Molecular Weight Aliphatic Amines in Air by Gas Chromato-
graphy," Anal. Chem., 55, 1983, pp. 2199-2201.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $175 (list).
B-527
-------
LOW-MOLECULAR-WEIGHT HALOGENATED HYDROCARBONS
Water Samples
Laboratory Method
Compound CAS Number
Bromoform 75-25-2
Chlorodibromomethane 124-48-1
Chloroform 67-66-3
Tetrachloroethylene 127-18-4
1,1,1-Trichloroethane 71-55-6
METHOD SUMMARY:
Gas chromatography may be used to measure the above low-molecular-weight
halogenated hydrocarbons in water samples. A 5-milliliter sample is extracted
with 1 milliliter of isooctane, and an aliquot of the organic phase is analyzed
in a gas chromatograph with an electron capture detector (GC/ECD).
INTERFERENCES:
Volatile compounds that are extractable and responsive to electron capture
detection may interfere, as may impurities in the extracting solvent.
QUALITY CONTROL:
Blanks and standards should be analyzed with the samples.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. The applicable concentration range for
trihalomethanes is 1 to 200 micrograms per liter. Precision and accuracy
information is furnished.
REFERENCE;
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D 3973-80; ASTM: Philadelphia, 1983, pp. 145-150.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $100 (list),
plus sampling costs.
B-528
-------
MERCAPTANS
Air Samples
Laboratory Method
Compound CAS Number
Methyl Mercaptan 74-93-1
Thiophenol 108-98-5
METHOD SUMMARY:
Analysis of air samples for the above mercaptans can be performed by
colorimetry. A sample is taken, either manually or automatically, by passage
of a known volume of air through a bubbler charged with a mercuric acetate/
acetic acid solution. The resulting solution is treated with an acidic solu-
tion of ferric chloride and N,N-dimethyl-£-phenylenediamine hydrochloride.
After 30 minutes the absorbance of the resulting solution at 500 nanometers is
measured with a spectrophotometer. This method measures the total mercaptan
content of the sample, and does not identify any particular compound.
INTERFERENCES:
Other sulfur-containing compounds, including hydrogen sulfide, can give
positive results. The mercuric acetate used must be free of mercurous ion or
turbidity will result.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is suitable for measurement
of atmospheric concentrations of mercaptans below 195 micrograms per cubic
meter. The minimum detectable amount of methyl mercaptan is 0.04 micrograms
per milliliter of absorbing solution. The minimum detectable concentration is
1.95 micrograms methyl mercaptan per cubic meter, using a 240-liter sample. No
precision or accuracy information is furnished.
REFERENCES:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.03, D2913-75; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list).
B-529
-------
METHYLAMINES
Air Samples
Laboratory Method
Compound CAS Number
Dimethylamine 124-40-3
Monomethylamine 74-89-5
Trimethylamine 75-50-3
METHOD SUMMARY:
The above methylamines in air samples can be measured by collection of the
sample on an activated charcoal trap and analysis by gas chromatography with
alkali flame ionization detection (GC/AFID).
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method has been evaluated by a single laboratory and is not EPA-
approved. No precision or accuracy information is furnished. The method is
suitable for concentration levels of analyte greater than approximately 10
micrograms per cubic meter -
REFERENCE:
Fuselli, S.; Benedetti, G.; Mastrangeli, R. "Determination of Methylamines in
Air Using Activated Charcoal Traps and Gas Chromatographic Analysis with an
Alkali Flame Detector (AFID)," Atmos. Environm., 2^(12), 1982, pp. 2943-2946.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $120-130
(list), plus sampling costs.
B-530
-------
N-METHYLCARBAMATES
Water Samples
Laboratory Method
Compound CAS Number
Carbaryl 63-25-2
Carbofuran 1563-66-2
Mercaptodimethur 2032-65-7
METHOD SUMMARY:
Analysis of water samples for the above N-methylcarbamate pesticides can
be performed by derivatization and gas chromatography with electron-capture
detection (GC/ECD). The sample is acidified to pH 3 to 4, and the pesticides
are extracted into methylene chloride. The extract is washed with potassium
carbonate, dried, and concentrated. Ten-percent methanolic potassium hydroxide
is used for hydrolysis, and the pentafluorobenzyl bromide derivatives are
prepared. The derivatives are cleaned up and separated by silica-gel micro-
column chromatography, by eluting the column three times, each time with a
different eluant. The eluates are analyzed by GC/ECD.
INTERFERENCES:
Carbamate phenols are removed in the potassium carbonate wash step.
Determination of mexacarbate and aminocarb is not possible with this method.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved for any regulatory program. Precision and
accuracy information for the overall analysis and the cleanup step is fur-
nished .
REFERENCE:
Coburn, J. A.; Ripley, B. D.; Chau, A. S. Y. "Analysis of Pesticide Residues
by Chemical Derivatization. II. N-Methylcarbamates in Natural Water and
Soils," J. Assoc. Off. Anal. Chem., 59(1), 1976, pp. 188-196.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $160-185
(list).
B-531
-------
NAPHTHYLAMINES
Air Samples
Laboratory Method
Compound CAS Number
1-Naphthylamine 134-32-7
2-Naphthylamine 91-59-8
METHOD SUMMARY:
The above naphthylamines in air samples may be measured by gas chromato-
graphy. A three-stage sampler consisting of a high-efficiency glass fiber
filter and two beds of silica gel is used to collect the naphthylamine. The
analyte is desorbed with a solution of acetic acid in 2-propanol, and an
aliquot of this solution is injected into a gas chromatograph with flame ioni-
zation detection (GC/FID).
INTERFERENCES:
The retention time of 1-nitronaphthalene is between those of 1- and 2-
naphthylamine and interferes with their determinations.
QUALITY CONTROL:
A method blank should be run with samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH), for use over the range of 4 to 70 micrograms per
cubic meter for a 50-liter sample. The detection limit is 0.01 micrograms per
sample. Precision information is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method P&CAM 264; Publication No. 78-175, U.S.DREW:
Cincinnati, 1978.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list) plus sampling costs.
B-532
-------
NITRILES
Water Samples
Laboratory Method
Compound CAS Number
Acetonitrile 75-05-8
Acrylonitrile 107-13-1
Benzonitrile 100-47-0
METHOD SUMMARY:
Analysis for the above nitriles in water samples can be performed by
direct injection of 3 to 5 microliters of the sample into a gas chromatograph
with a flame ionization detector (GC/FID), utilizing either temperature-
programmed or isothermal operation.
INTERFERENCES:
Samples should be quick-frozen if not analyzed immediately, and sample pH
should be adjusted to 7 at the time of collection.
QUALITY CONTROL:
Standard solutions should be regarded as unstable and stored in a freezer.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. It has undergone inter-laboratory
evaluation and extensive review, and shows a precision of 3 to 10 percent over
the range of 10 to 60 milligrams per liter. The detection limit is approximately
1 milligram per liter.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D 3371-79; ASTM: Philadelphia, 1983, pp. 162-164.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-90
(list).
B-533
-------
NITROAROMATIC COMPOUNDS AND BENZONITRILE
Air Samples
Laboratory Method
Compound CAS Number
Benzonitrile 100-47-0
£-Dinitrobenzene 100-25-4
Nitrobenzene 98-95-3
METHOD SUMMARY:
The above nitroaromatic compounds in air samples can be measured by gas
chromatography. Sensitivites for specific compounds vary widely with the type
of detector used; the electron capture detector is quite effective for nitro-
benzene and £-dinitrobenzene. Analysis of benzonitrile requires a flame ioni-
zation detector.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
A reference standard must be run just before and after each group of
samples.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Mitchell, J.; Deveraux, H.D. "Determination of Traces of Organic Compounds in
the Atmosphere: Role of Detectors in Gas Chromatography," Anal. Chim. Acta.,
100, 1978, pp. 45-52.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-90 (list)
with the FID, and approximately $80-100 (list) with the ECD, plus sampling
costs.
B-534
-------
NITROAROMATICS
Water Samples
Laboratory Method
Compound CAS Number
Dinitrobenzenes, Mixed 25154-54-5
m-Dinitrobenzene 99-65-0
o-Dinitrobenzene 528-29-0
£-Dinitrobenzene 100-25-4
Dinitrotoluene 25321-14-6
2,4-Dinitrotoluene 121-14-2
2,6-Dinitrotoluene 606-20-2
Nitrotoluene 1321-12-6
5-Nitro-o-Toluidine 99-55-8
Toluene 108-88-3
sym-Trinitrobenzene 99-35-4
METHOD SUMMARY:
Water samples may be analyzed for the above nitroaromatics by gas chro-
matography with flame ionization detection (GC/FID). A 20-milliliter sample is
extracted with diethyl ether, the extract is dried, concentrated, and analyzed
using an internal standard. Identification of components is confirmed by gas
chromatography/mass spectrometry (GC/MS).
INTERFERENCES;
No specific interferences are reported. Complex wastewater matrices
require the use of fused-silica capillary column GC/FID.
QUALITY CONTROL:
The GC/FID should be calibrated twice daily, precision should be deter-
mined by analysis of multiple samples, and accuracy measured by analysis of
fortified samples.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Spanggord, R. J.; Gibson, B. W.; Keck, R. G.; Thomas, D. W. "Effluent
Analysis of Wastewater Generated in the Manufacture of 2,4,6-Trinitrotoluene.
1. Characterization Study," Environ. Sci. Technol., 16^(4), 1982, pp. 229-232.
B-535
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $110-155
(list), excluding the GC/MS confirmation.
B-536
-------
NITROAROMATICS AND CYCLIC KETONES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Dinitrobenzenes, Mixed 25154-54-5
Dinitrotoluene 25321-14-6
2,4-Dinitrotoluene 121-14-2
2,6-Dinitrotoluene 606-20-2
Isophorone 78-59-1
1,4-Naphthoquinone 130-15-4
Nitrobenzene 98-95-3
METHOD SUMMARY:
Analysis of soil/sediment samples for the above nitroaromatics and cyclic
ketones can be performed by gas chromatography. A soil/sediment sample is
extracted with methylene chloride at neutral pH, using Soxhlet extraction or
sonication, and the extract is dried, concentrated, and analyzed by gas
chromatography with electron capture detection (GC/ECD) or flame ionization
detection (GC/FID), using either internal or external standards for quantifi-
cation.
INTERFERENCES:
The use of plastics in collection, storage, or processing of samples must
be avoided.
QUALITY CONTROL:
An aliquot of each sample must be spiked to determine the detection limits
and recovery, and a method blank should be analyzed with each set of samples or
change in reagents. Field and laboratory replicates and duplicate samples
should be analyzed to demonstrate the sensitivity and accuracy of the method.
When doubt exists about the identification of a peak in the chromatogram,
confirmatory methods, such as gas chromatography/mass spectrometry (GC/MS) or
second-column confirmation, should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for the Resource Conservation and Recovery Act
(RCRA). No precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom: J. J. Lichtenberg, Eds.,
"Nitroaromatics and Isophorone" Method 609; EPA-600/4-82-057, U.S. EPA:
Cincinnati, 1982.
B-537
-------
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8090; SW-846, U.S. EPA~-
Washington, July 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $120-130
(list).
B-538
-------
NITROAROMATICS AND CYCLIC KETONES
Water Samples
Laboratory Method
Compound CAS Number
Dinitrobenzene, Mixed 25154-54-5
1,4-Naphthoquinone 130-15-4
METHOD SUMMARY:
Analysis for the above nitroaromatics and cyclic ketones in water samples
can be performed by gas chromatography. A water sample is extracted with
methylene chloride, and the extract is dried, concentrated, and analyzed by gas
chromatography with flame ionization detection (GC/FID) or with electron
capture detection (GC/ECD).
INTERFERENCES:
Use of plastics during collection, storage, or processing of samples must
be avoided.
QUALITY CONTROL:
An aliquot of each sample must be spiked to determine the detection limits
and recovery, and a method blank should be analyzed with each set of samples or
change in reagents. Field and laboratory replicates and duplicate samples
should be analyzed to demonstrate the sensitivity and accuracy of the method.
When doubt exists about the identification of a peak in the chromatogram,
confirmatory methods, such as gas chromatography/mass spectrometry (GC/MS) or
second-column confirmation, should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for the Resource Conservation and Recovery Act
(40 CFR, Part 261, Identification and Listing of Hazardous Wastes). No
precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom; J. J. Lichtenberg, Eds.,
Method 609; EPA-600/4-82-057, U.S. EPA: Cicinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8090; SW-846, U.S. EPA:
Washington, July 1982.
B-539
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $110-160
(list).
B-540
-------
NITROGENOUS DRUGS
No Matrix Given
Laboratory Method
Compound CAS Number
Methapyrilene 91-80-5
Nicotine 54-11-5
Phenacetin 62-44-2
METHOD SUMMARY:
Analysis for the above nitrogenous drugs can be performed by gas chromato-
graphy with both flame-ionization and nitrogen-selective rubidium silicate bead
alkali flame ionization detectors. The drugs are chromatographed with a
caffeine internal standard on a 3-percent OV-17 column with a temperature
program of 100°C to 250°C at 4° per minute.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are furnished.
EPA/TECHNICAL STATUS:
This method is not EPA-approved for use in any regulatory program. No
precision or accuracy information is given.
REFERENCE:
Baker, J. K. "Identification and Chemical Classification of Drugs Based on the
Relative Response of a Nitrogen Selective Detector and a Flame Ionization
Detector in Gas Chromatographic Analysis," Anal. Chem. , 49_(7), 1977, pp.
906-908.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $180 (list),
plus sample preparation.
B-541
-------
NITROPHENOLS
Water Samples
Laboratory Method
Compound CAS Number
Nitrophenol, Mixed 25154-55-6
2-Nitrophenol 88-75-5
3-Nitrophenol 554-84-7
4-Nitrophenol 100-02-7
METHOD SUMMARY:
The above nitrophenols in water samples can be measured by high-performance
liquid chromatography (HPLC). The samples are adjusted to pH 2, and the nitro-
phenols are collected on mixed XAD-4/8 macroreticular resins. After extraction,
concentration, and isolation from interferences, the nitrophenols are analyzed
by HPLC with a UV detector.
INTERFERENCES:
The sample extract is isolated from interfering neutral hydrophobic
organic compounds by retention on cesium silicate and elution with methanol.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision or accuracy information is
not furnished.
REFERENCE:
Graham, J. A. In Trace Analysis Vol. I, J. F. Lawrence, Ed.; Academic Press:
New York, 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $205-240
(list).
B-542
-------
N-NITROSAMINES
Air Samples
Laboratory Method
Compound CAS Number
N-Nitrosodi-N-butylamine 924-16-3
N-Nitrosodiethylamlne 55-18-5
N-Nitrosodimethylamine 62-75-9
N-Nitrosodiphenylamine 86-30-6
N-Nitrosodi-N-propylamine 621-64-7
N-Nitrosopiperidine 100-75-4
N-Nitrosopyrrolidine 930-55-2
METHOD SUMMARY:
The above N-nitrosamines in air samples can be measured by gas chromato-
graphy/mass spectrometry (GC/MS). The samples are collected with trapping
concentrators and cartridges. The cartridges are then pre-eluted to remove
interfering compounds. After the nitrosamines are eluted they are analyzed by
GC/MS using selective ion monitoring.
INTERFERENCES:
Interfering compounds trapped on the cartridges during sampling are
removed by the pre-elution step.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Marano, R. S.; Updegrove, W. S.; Machen, R.C. "Determination of Trace Levels
of Nitrosamines in Air by Gas Chromatography/Low-Resolution Mass Spectrometry,'
Anal. Chem., 54, 1982, pp. 1947-1951.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $250-325
(list), plus sampling costs.
B-543
-------
N-NITROSAMINES
Water Samples
Laboratory Method 1
Compound CAS Number
N-Nitrosodiethylamine 55-18-5
N-Nitrosodimethylamine 62-75-9
N-Nitrosopiperidine 100-75-4
N-Nitrosopyrrolidine 930-55-2
METHOD SUMMARY:
The above N-nitrosamines in water samples can be measured on a gas
chromatograph interfaced with a Thermal Energy Analyzer (GC-TEA). The sample
is passed through a carbonaceous adsorbent. The nitrosamines are eluted with
dichloromethane and analyzed by GC-TEA. This method was designed for the
analysis of tap water.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE;
Kimoto, W.; Dooley, C. J.; Carre, J.; Fiddler, W. "Nitrosamines in Tap Water
After Concentration by a Carbonaceous Adsorbent," Water Res., 1_5(9), 1981, pp.
1099-1106.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $150-210
(list).
B-544
-------
N-NITROSAMINES
Water Samples
Laboratory Method 2
Compound CAS Number
N-Nitrosodi-n-butylamine 924-16-3
N-NitrosodieFhylamine 55-18-5
N-Nitrosodimethylamine 62-75-9
N-Nitrosopiperidine 100-75-4
N-Nitrosodi-n-propylamine 621-64-7
METHOD SUMMARY:
The above N-nitrosamines in water samples can be measured on a gas
chromatography with an N-nitroso compound-specific thermal energy analysis
detector (GC/TEA). The samples are collected in brown bottles and stored at
4°C. The sample is extracted three times with methylene chloride, and the
extracts are combined and dried, concentrated, and analyzed by GC/TEA or
HPLC/TEA. A high-performance liquid chromatograph (HPLC) equipped with TEA
detection may also be used for the analysis.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Accuracy information is furnished. The
detection limit for N-nitrosodimethylamine and N-nitrosodiethylamine is about
0.002 micrograms per liter.
REFERENCES:
Fine, D. H.; Rounbehler, D. P- "N-Nitroso Compounds in Water" In Identifica-
tion and Analysis of Organic Pollutants in Water, Ch. 17; L. H. Keith, Ed.;
Ann Arbor Science: Ann Arbor, 1976.
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom, J. J. Lichtenburg, Eds.:
Method 607; U.S. EPA: Cincinnati, 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $150-295
(list).
B-545
-------
NITROSO COMPOUNDS
No Matrix Given
Laboratory Method
Compound CAS Number
N-Nitroso-N-Ethylurea 759-73-9
N-Nitroso-N-Methylurea 684-93-5
N-Nitroso-N-Methylurethane 615-53-2
METHOD SUMMARY:
High-pressure liquid chromatography (HPLC) may be used to measure the
above nitroso compounds. The sample must first be extracted and concentrated.
The extract is hydrolyzed in dilute hydrochloric acid to give nitrite. The
nitrite is reacted with naphthylethylenediamine to give a colored dye, which is
analyzed by HPLC. The extraction and concentration steps are not necessary
when large amounts of nitroso compounds are present. This method does not
identify any specific compound, but is specific to all compounds which hydro-
lyze in dilute hydrochloric acid to yield nitrite. This method is capable of
sensitivities of 0.5 nanomoles of injected nitrosamides and may be used for
analysis for nitriles, nitrosamides, nitrocarbamates, and alkylnitrites.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCES:
Singer, G. M.; Singer S. S.; Schmidt, D. G. "A Nitrosamide-Specific Detector
for use with High-Pressure Liquid Chromatography," J. Chromatogr., 133, 1977,
pp. 59-66.
Heyns, K.; Roper H. "Analysis of N-Nitroso Compounds. II. Separation and
Quantitative Determination of N-Nitroso-N-alkylureas and N-Nitroso-N-alkylur-
ethans by High-Speed High-Pressure Liquid Chromatography," J. Chromatogr., 93_,
1974, pp. 429-439, (German).
B-546
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $125-215
t) •
(list),
B-547
-------
N-NITROSO COMPOUNDS
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
N-Nitrosodi-n-butylaraine 924-16-3
N-Nitrosodiethylamine 55-18-5
N-Nitrosodiphenylamine 86-30-6
N-Nitrosodi-n-butylamine 924-16-3
N-Nitrosodi-n-propylaraine 621-64-7
N-Nitrosopiperidine 100-75-4
N-Nitrosopyrrolidine 930-55-2
METHOD SUMMARY:
The above N-nitroso compounds in soil/sediment samples can be measured by
chemiluminescence. The sample is extracted with methylene chloride, the
extract is filtered and then partitioned with water for back-extraction of
nitrites. The extract is dried and concentrated. Analysis is by hydrobromic
acid-catalyzed denitrosation and subsequent detection of the evolved nitric
oxide by its chemiluminescent reaction with ozone. This method is not specific
for a particular N-nitroso compound, but measures the total N-nitroso group
content of the sample.
INTERFERENCES:
N-Alkylnitrites interfere if not removed. If water is present in the
extract during analysis, the detector signal will be severely reduced.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The limit of detection is, on the average, 100 nanograms of N-
nitroso compound per kilogram of soil.
REFERENCE:
Drescher, G. S.; Frank, C. W. "Estimation of Extractable N-Nitroso Compounds
at the Parts-per-Billion Level," Anal. Chem., 50(14), 1978, pp. 2118-2121.
COST INFORMATION:
Cost information has not been obtained.
B-548
-------
NON-HALOGENATED VOLATILE ORGANIC COMPOUNDS
Soil/Sediment Samples
Laboratory Method
Compounds CAS Number
Acetonitrile 75-05-8
Acrolein 107-02-8
Acrylamide 79-06-1
Acrylonitrile 107-13-1
Carbon Bisulfide 75-15-0
Methyl Ethyl Ketone 78-93-3
Methyl Isobutyl Ketone 108-10-1
Paraldehyde 123-63-7
METHOD SUMMARY:
Analysis for the above volatile organic compounds in soil/sediment samples
can be performed by gas chromatography- A soil/sediment sample is dispersed in
methanol or polyethylene glycol, the solution is purged with an inert gas onto
a trap, and the trap is backflushed into a temperature-programmed gas chromato-
graph with flame ionization detection (GC/FID). Either internal or external
standards are used for quantification.
INTERFERENCES:
Samples should be collected in glass containers and immediately sealed and
refrigerated.
QUALITY CONTROL:
The analytical system must be demonstrated to be free of interferences by
analysis of a method blank each time a set of samples is processed or a change
in reagents occurs. Field replicates, laboratory replicates, and fortified
samples must be analyzed to demonstrate the precision and accuracy of the
method. In cases of doubt concerning the identity of a peak in the chroraato-
gram, confirmatory techniques, such as gas chromatography/mass spectrometry
(GC/MS) or second-column confirmation, should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
(RCRA) sample analyses. Limited precision and accuracy information is furnished
(Method 603).
REFERENCES:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed. , Methods 5020, 5030, 8015, 8030; SW-846,
U.S. EPA: Washington, July 1982.
B-549
-------
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis
of Municipal and Industrial Wastewater, J. E. Longbottom, J. J. Lichtenberg.
Eds., Method 603; EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-125
(list).
B-550
-------
NON-HALOGENATED VOLATILE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compounds CAS Number
Acetonitrile 75-05-8
Acrolein 107-02-8
Acrylamide 79-06-1
Acrylonitrile 107-13-1
Carbon Disulfide 75-15-0
Methyl Ethyl Ketone 78-93-3
Methyl Isobutyl Ketone 108-10-1
Paraldehyde 123-63-7
METHOD SUMMARY:
Analysis of water samples for the above volatile organic compounds can be
performed by gas chromatography. A water sample is purged with an inert gas
onto a Tenax® trap, and the trap is backflushed into a temperature-programmed
gas chromatograph with a flame ionization detector (GC/FID). Either internal
or external standards are used for calibration.
INTERFERENCES:
Samples should be collected in glass containers, sealed, and refrigerated
immediately.
QUALITY CONTROL:
The analytical system must be demonstrated to be free of interferences by
the analysis of a method blank each time a set of samples is processed or a
change in reagents occurs. Field replicates, laboratory replicates, and forti-
fied samples must be analyzed to demonstrate the precision and accuracy of the
method. In cases of doubt concerning the identity of a peak in the chromato-
gram, confirmatory techniques, such as gas chromatography/mass spectrometry
(GC/MS) or second-column confirmation, should be used.
EPA/TECHNICAL STATUS;
This method is EPA-approved for Clean Water Act and Resource Conservation
and Recovery Act (RCRA) sample analyses. Precision and accuracy information is
furnished (Method 603). The method detection limit for acrolein is 0.6 yg per
liter and for acrylonitrile is 0.5 yg per liter.
REFERENCES:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste^
Physical/Chemical Methods, 2nd ed., Methods 5020, 5030, 8015, 8030; SW-846,
U.S. EPA: Washington, July 1982.
B-551
-------
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis
of Municipal and Industrial Wastewater, J. E. Longbottom; J. J. Lichtenberg,
Eds., Method 603: EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-115
(list).
B-552
-------
METHOD SUMMARY:
NON-VOLATILE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound
Benzyl Chloride
Captan
Chlorpyrifos
Diazinon
Dichlobenil
Dichlone
Dichlorovos
2,4-Dimethylphenol
p_-Dinitrobenzene
£-Dinitrobenzene
Disulfoton
Ethion
Kelthane
Kepone
Malathion
Methoxychlor
Methyl Parathion
Mevinphos
Nitrotoluene
Parathion
Propargite
Quinoline
Resorcinol
Trichlorfon
CAS Number
100-
133-
2921-
333-
1194-
117-
62-
105-
528-
100-
298-
563-
115-
143-
121-
72-
298-
7786-
1321-
56-
2312-
91-
108-
52-
•44-7
•06-2
•88-2
41-9
•65-6
80-6
•73-7
67-9
•29-0
•25-4
•04-4
•12-2
•32-2
•50-0
•75-5
43-5
•00-0
•24-7
•12-6
38-2
•35-8
•22-5
•46-3
•68-6
Analysis of water samples for the above non-volatile organic compounds can
be performed by gas chromatography/mass spectrometry (GC/MS). A 1.0-liter
sample is serially extracted at acidic and basic pH. The base/neutral extract
is obtained by extraction of the sample with methylene chloride at pH 11. The
remaining aqueous solution is extracted with methylene chloride at pH 2 to
obtain the acidic extract. The two fractions are each concentrated in a Kuderna-
Danish apparatus and analyzed by GC/MS.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
Fortified samples should be analyzed to determine recovery and measurement
precision.
B-553
-------
EPA/TECHNICAL STATUS:
This method is not EPA-approved, but is a modification of EPA Method 625,
which is approved. This method will detect concentrations as low as approxi-
mately 0.2 milligrams per liter. Precision information is furnished.
REFERENCE:
Spingarn, N. E.; Northington, D. J.; Pressely, T. "Analysis of Non-Volatile
Organic Hazardous Substances by GC/MS," J. Chromatogr. Sci., 20, December 1982,
pp. 571-574.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $320-490
(list).
B-554
-------
ORGANIC ACIDS
Water Samples
Laboratory Method 1
Compound CAS Number
Acetic Acid 64-19-7
Butyric Acid 107-92-6
Formic Acid 64-18-6
Propionic Acid 79-09-4
METHOD SUMMARY:
The above organic acids of low molecular mass (i.e., C^ to C^~) can be
determined in water by gas chromatography. The acids are converted to their
benzyl esters and injected into a gas chromatograph equipped with a flame
ionization detector (GC/FID). This method is used over the range of 1.0 to 2.5
milligrams of acid per liter in a 10-milliliter water sample.
INTERFERENCES:
High concentrations of acids other than those to be determined will .
interfere.
QUALITY CONTROL:
Standards are analyzed along with the samples.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Bethge, P. 0.; Lindstrom, K. "Determination of Organic Acids of Low Relative
Molecular Mass (Ci to 04) in Dilute Aqueous Solutions," Analyst, 9£(2), 1974,
pp. 137-142.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $90 (list),
plus sampling costs.
B-555
-------
ORGANIC ACIDS
Water Samples
Laboratory Method 2
Compound CAS Number
Acetic Acid 64-19-7
Benzoic Acid 65-85-0
Ethylenediamine- 60-00-4
tetraacetic Acid
Phenol 108-95-2
Phthalic Anhydride 85-44-9
METHOD SUMMARY:
Analysis of water samples for the above organic acids can be performed by
ion chromatography. Separation is achieved by use of a cross-linked dextran
geltype cation exchanger and a tetramethylammonium chloride eluent, and detection
is by use of a flow-cell-equipped spectrophotometer or by derivatization and
determination as the hydroxamic acid. Aromatic acids are detected directly,
while ethylenediaminetetraacetic acid is detected as the cobalt complex, and
aliphatic acids are derivatized.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved for any regulatory program. It has been
used to separate aqueous standard solutions. No precision or accuracy infor-
mation is furnished.
REFERENCE:
Tokunaga, Y.; Waki, H.; Ohashi, S. "Elution Behavior of Organic Acids in Donnan
Exclusion Chromatography," J. Liq. Chromatogr. , (>(2), 1983, pp. 271-280.
COST INFORMATION:
No cost information has been obtained.
B-556
-------
Compound
Acenaphthene
Acetaldehyde
Acetone
Acetonitrile
Aniline
Benzene
Benzonitrile
Butyric Acid
Cresol
m-Cresol
o-Cresol
£-Cresol
2,4-Dimethylphenol
Ethylbenzene
Fluorene
METHOD SUMMARY:
CAS Number
ORGANIC COMPOUNDS
Water Samples
Laboratory
Compound
CAS Number
83-
75-
67-
75-
62-
71-
100-
107-
1319-
108-
95-
106-
105-
100-
86-
32-9
07-0
64-1
05-8
53-3
43-2
•47-0
92-6
77-3
39-4
•48-7
•44-5
67-9
•41-4
•73-7
Furan 110-00-9
Methacrylonitrile 126-98-7
Methyl Ethyl Ketone 78-93-3
Methyl Isobutyl Ketone 108-10-1
Naphthalene 91-20-3
Phenol 85-01-8
Propanenitrile 107-12-0
Pyridine 110-86-1
Quinoline 91-22-5
Styrene 100-42-5
Toluene 108-88-3
Xylene 1330-20-7
m-Xylene 108-38-3
o-Xylene 95-47-6
p-Xylene 106-42-3
Analysis of water samples for the above organic compounds can be performed
by gas chromatography/mass spectrometry (GC/MS). A sample is purged with inert
gas through a Tenax® trap and the trap is thermally desorbed into a gas chromato-
graph/mass spectrometer (GC/MS) for characterization and measurement of the
volatile components of the sample. The sample is then extracted with Freon TF,
and the extract is concentrated, fractionated, and the fractions analyzed by
GC/MS. Gas chromatography/Fourier transform infrared spectrometry (GC/FTIR)
can be used to aid in identification of compounds as needed.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
Blanks should be used to monitor materials used in purification. All
equipment and reagents should be demonstrated to be free of interferences
before being used in this method. The GC/MS system must be calibrated daily,
and a twelve-component reference compound solution is used to evaluate the
performance of the GC/MS each day.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The lower limit of detection is 0.1
microgram per liter. Precision information is furnished.
B-557
-------
REFERENCE;
Pellizzari, E. D.; Castillo, N. P.; Willis, S.; Smith, D.; Bursey, J. T.,
"Identification of Organic Components in Aqueous Effluents from Energy-Related
Processes," Measurement of Organic Pollutants in Water and Wastewater, C. E.
Van Hall, Ed.; STP 686, American Society for Testing and Materials: Philadelphia
1979. pp. 256-274.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $250-325
(list).
B-558
-------
ORGANIC VAPORS
Air Samples
Laboratory Method
Compound CAS Number
iso-Butyl Alcohol 78-83-1
Chloroform 67-66-3
Ethyl Acrylate 140-88-5
Ethylbenzene 100-41-4
Ethyl Ether 60-29-7
Methylene Chloride 75-09-2
Pyridine 110-86-1
Tetraethyl Lead 78-00-2
1,1,2-Trichloroethane 79-00-5
METHOD SUMMARY:
Analysis for the above organic vapors in air can be performed by gas
chromatography. Air samples are collected by aspirating 2 to 50 liters of air
through activated charcoal sampling tubes, followed by desorption of the analytes
with carbon disulfide (ethyl acetate for ethyl ether and methylene chloride for
pyridine) and analysis of the resulting solution by gas chromatography with
flame ionization detection (GC/FID).
INTERFERENCES:
High humidity can greatly reduce the adsorptive capacity of the charcoal.
Peak superimposition can be overcome by changes in gas chromatography columns
or operating conditions. No specific interferences are reported.
QUALITY CONTROL:
Desorption efficiency must be determined for each set of samples and must
be above 75 percent. Field blanks must be processed with each set of samples.
Calculations should include the desorption efficiency. The collecting system
must be tested for breakthrough with each sample, and if breakthrough has
occurred, results should not be used.
EPA/TECHNICAL STATUS:
This method has been approved by the National Institute for Occupational
Safety and Health (NIOSH), and has been validated by that agency. Precision
and accuracy information is furnished.
REFERENCE:
American Society for Testing and Materials, ASTM Standards on Chromatography,
D 3686-78, D 3687-78; ASTM: Philadelphia, 1981, pp. 537-555.
B-559
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
B-560
-------
ORGANOCHLORINE AND ORGANOPHOSPHORUS PESTICIDES
Water Samples
Laboratory Method
Compounds
Aldrin
a-BHC
B-BHC
6-BHC
Captan
Chlordane
Chlorpyrifos
ODD
DDE
DDT
2,4-D Esters
Diazinon
Dieldrin
Dimethoate
Disulfoton
a-Endosulfan
6-Endosulfan
Endrin
METHOD SUMMARY:
CAS Number
Compound
CAS Number
309-
319-
319-
319-
133-
57-
2921-
72-
72-
50-
94-
94-
94-
1320-
1928-
1928-
1929-
2971-
25168-
53467-
333-
60-
60-
298-
959-
33213-
72-
00-2
84-6
85-7
86-8
06-2
74-9
88-2
54-8
55-9
29-3
11-1
79-1
•80-4
18-9
38-7
•61-6
73-3
•38-2
•26-7
•11-1
•41-5
•57-1
•51-5
•04-4
98-8
65-9
•20-8
Heptachlor 76-
Heptachlor Epoxide 1024-
Hexachlorobenzene 118-
Hexachlorohexahydro-endo, 465-
endo-dimethanonaphthalene
Kelthane
Kepone
Lindane
Malathion
Methoxychlor
Methyl Parathion
Mevinphos
Naled
Pentachloronitrobenzene
Phorate
Polychlorlnated
Biphenyls
2,4,5-T Esters
Toxaphene
115-
143-
58-
121-
72-
298-
7786-
300-
82-
298-
11097-
11096-
1336-
12674-
11104-
11141-
53469-
12672-
93-
2545-
61792-
1928-
25168-
8001-
•44-8
•57-3
•74-1
•73-6
32-2
•50-0
89-9
•75-5
•43-5
•00-0
•34-7
•76-5
•68-8
•02-2
•69-1
•82-5
•36-3
•11-2
•28-2
•16-5
•21-9
•29-6
•79-8
•59-7
•07-2
•47-8
•15-4
•35-2
Gas chromatography may be used for the analysis of water samples for
the above organochlorine and organophosphorus pesticides. A 500-milliliter
sample is extracted with methylene chloride and the extract is dried, con-
centrated, separated into fractions on a deactivated silica-gel column, and the
fractions analyzed by gas chromatography, using an electron capture detector
(GC/ECD) for organochlorine compounds and a flame photometric detector (GC/FPD)
for organophosphorus compounds.
INTERFERENCES:
Organochlorine pesticide-containing samples must be refrigerated at 2° to
4°C and analyzed within 1 week. Organophosphorus pesticide-containing samples
must be frozen immediately after collection and analyzed within 4 days.
B-561
-------
QUALITY CONTROL:
Reagent blanks and standards should be analyzed with each sample or set of
samples. Further confirmatory techniques, such as gas chromatography/mass
spectrometry or thin-layer chromatography, should be used when uncertainty
exists concerning the identity of a compound.
EPA/TECHNICAL STATUS:
This method has been evaluated in an EPA study, but is not EPA-approved
for any regulatory program. Precision and accuracy information is furnished.
REFERENCES:
American Society for Testing and Materials, ASTM Standards on Chromatography,
D 3086-79; ASTM: Philadelphia, 1981, pp. 326-349.
U.S. Environmental Protection Agency, Manual of Analytical Methods for the
Analysis of Pesticides in Humans and Environmental Samples, Section 10, EPA-600/
8-80-038, U.S. EPA: Cincinnati, June 1980.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $150-215
(list).
B-562
-------
ORGANOCHLORINE PESTICIDES
Water Samples
Laboratory Method
Compounds CAS Number Compound CAS Number
Aldrin 309-00-2 Dieldrin 60-57-1
a-BHC 319-84-6 Endosulfan H5_29-7
B-BHC 319-85-7 Endrin 72-20-8
6-BHC 319-86-8 Heptachlor 76-44-8
Captan 133-06-2 Heptachlor Epoxide 1024-57-3
Chlordane 57-74-9 Lindane 58-89-9
ODD 72-54-8 Methoxychlor 72-43-5
DDE 72-55-9 Pentachloronitrobenzene 82-68-8
DDT 50-29-3 Toxaphene 8001-35-2
METHOD SUMMARY:
The above organochlorine pesticides in water samples may be measured by
gas chromatography. The sample is extracted with methylene chloride or ethyl
ether/hexane (15/85), interferences are removed if necessary, and the extract
is analyzed by gas chromatography with electron capture, microcoulometric, or
electrolytic conductivity detection.
INTERFERENCES:
Reagents and glassware can cause discrete artifacts or elevated baselines.
Polychlorinated aromatics, phthalate esters, and organophosphate pesticides may
interfere. Interferences can be minimized by such treatments as liquid-liquid
partitioning, macro and micro chromatography, and thin-layer chromatography.
QUALITY CONTROL:
When the volume of sample permits, one set of duplicates and one spiked
sample should also be analyzed as a quality control check.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method sensitivity limit (ASTM)
ranges from 1 to 10 nanograms per liter for single-component pesticides, and 50
to 1000 nanograms per liter for multi-component pesticides, using a 1-liter
sample. Precision and accuracy information is furnished.
REFERENCES;
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D 3086-79; ASTM: Philadelphia, 1983, pp. 178-201.
B-563
-------
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Water Samples
for Organochlorine Pesticides/Polychlorinated Biphenyls," EPA-600/54-84-038,
pp. III-186'
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130-175
(list).
B-564
-------
ORGANOCHLORINE PESTICIDES AND PCB's
Compound
Aldrin
a-BHC
g-BHC
6-BHC
Chlordane
DDD
DDE
DDT
Dieldrin
Endosulfan
a-Endosulfan
B-Endosulfan
Endosulfan Sulfate
Endrin
Endrin Aldehyde
Heptachlor
Heptachlor Epoxide
Kepone
Lindane
Methoxychlor
Polychlorinated
Biphenyls
Toxaphene
METHOD SUMMARY:
Soil/Sediment Samples
Laboratory Method 1
CAS Number
309-
319-
319-
319-
57-
72-
72-
50-
60-
115-
959-
33213-
1031-
72-
7421-
76-
1024-
143-
58-
72-
1336-
12674-
11104-
11141-
53469-
12672-
11097-
11096-
8001-
00-2
84-6
85-7
86-8
74-9
•54-8
55-9
29-3
•57-1
•29-7
•98-8
•65-9
•07-8
•20-8
93-4
•44-8
•57-3
•50-0
•89-9
•43-5
•36-3
•11-2
•28-2
•16-5
•21-9
•29-6
•69-1
•82-5
•35-2
Detection Limit
0.004
0.004
0.006
0.004
0.014
0.012
0.004
0.012
0.002
0.014
0.004
0.066
0.006
0.023
0.004
0.083
0.009
0.176
0.24
Analysis of soil/sediment samples for the above organochlorine pesticides
and PCB's can be performed by gas chromatography. A soil/sediment sample is
extracted at neutral pH with dichloromethane, hexanelacetone (1/1), or other
designated solvent mixture and the extract is dried, cleaned up on a Florisil®
column using appropriate elution mixtures, solvent-exchanged into hexane if
necessary, concentrated, and analyzed by gas chromatography with electron-
capture detection (GC/ECD). C-uantification is performed using either external
or internal standards, and an aliquot of each sample is spiked to determine
recovery and detection limits.
* From Method 8080 (U.S. EPA); ug/liter of liquid extract,
B-565
-------
INTERFERENCES:
Phthalate esters interfere, so that all contact with non-Teflon® plastics
should be avoided. Elemental sulfur interferes and can be removed by treatment
with mercury or copper.
QUALITY CONTROL:
The gas chromatographic system must be demonstrated to be free of inter-
ferences by analysis of a method blank with each set of samples or change in
reagents. Laboratory replicates, field replicates, and duplicate samples
should be processed and analyzed to ascertain the precision and accuracy of the
method. Where doubt exists concerning the identification of a peak in the
chromatogram, confirmatory techniques, such as gas chromatography/mass spectro-
metry (GC/MS) or second-column confirmation, should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved under the Clean Water Act and the Resource
Conservation and Recovery Act (RCRA) and is in use in the CERCLA program.
Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Invitation for Bid, "Organics Analysis,
Multi-Media, Multi-Concentration, GC/MS with GC Screen," Solicitation Number
WA84A-266; U.S. EPA; Washington, June 15, 1984.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3510, 3520, 8080; SW-846, U.S. EPA:
Washington, July 1982.
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, Method 608; EPA-600/4-82-057, U.S. EPA:
Washington, 1982.
U.S. Environmental Protection Agency, Methods for Benzidine, Chlorinated Organic
Compounds, Pentachlorophenol, and Pesticides in Water and Wastewater, U.S. EPA:
Cincinnati, 1978, pp. 7-24.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol.
Ill, Available Laboratory Analytical Methods, "Analysis of Sediment Samples for
Polychlorinated Biphenyls," pp. III-202 to III-210; EPA-600/84-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
ASTM STP 573, American Society for Testing and Materials, Philadelphia, 1975,
p. 206.
B-566
-------
COST INFORMATION:
Cost per sample for the GC screen is approximately $90-150 (list) $60
(bid); the cost of GC/MS confirmation is approximately $150-200 (list) $137-
177 (bid); the cost of second-column confirmation is approximately $8o'(list)
B-567
-------
ORGANOCHLORINE PESTICIDES AND PCB's
Soil/Sediment Samples
Laboratory Method 2
Compound CAS Number
Aldrin 309-00-2
DDE 72-55-9
DDT 50-29-3
Heptachlor 76-44-8
Hexachlorobenzene 118-74-1
Hexachlorohexahydro- 465-73-6
endo, endo-dimethano-
naphthalene
Polychlorinated Biphenyls 1336-36-3
(PCB's) 12674-11-2
53469-21-9
11104-28-2
12672-29-6
11141-16-5
11097-69-1
11096-82-5
METHOD SUMMARY:
The above organochlorine pesticides and polychlorinated biphenyls in
soil/sediment samples can be measured by gas chromatography with electron-
capture detection (GC/ECD). The sample, with water added, is extracted with
acetone, concentrated, partitioned into water, extracted with petroleum ether,
then dried and concentrated. The extract is added to an alumina column, which
is eluted with petroleum ether. The concentrated eluate is added to a silica
gel column, which is also eluted with petroleum ether. After concentration and
removal of sulfur, the sample is analyzed by capillary column GC/ECD. When
different eluents are used in the columns, additional organochlorine pesticides
can be determined.
INTERFERENCES:
PCB's can interfere with analysis for heptachlor, aldrin, and DDT.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The limit of detection is 0.01 milligrams of analyte per kilogram
of soil/sediment, on a dry-weight basis.
B-568
-------
REFERENCE:
Wegman, R. C. C.; Hofstee, A. W. M. "Determination of Organochlorines in River
Sediment by Capillary Gas Chromatography," Water Res., 16, 1982, pp. 1265-1272.
COST INFORMATION:
Cost per sample for this analysis is approximately $180-200 (list).
B-569
-------
Compound
Aldrin
a-BHC
6-BHC
6-BHC
Chlordane
ODD
DDE
DDT
Dieldrin
Endosulfan
a-Endosulfan
B-Endosulfan
Endosulfan Sulfate
Endrin
Endrin Aldehyde
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Lindane
Polychlorinated
Biphenyls
ORGANOCHLORINE PESTICIDES AND PCB's
Water Samples
Laboratory Method 1
CAS Number
Toxaphene
METHOD SUMMARY:
309-
319-
319-
319-
57-
72-
72-
50-
60-
115-
959-
33213-
1031-
72-
7421-
76-
1024-
118-
58-
1336-
12674-
11104-
11141-
53469-
12672-
11097-
11096-
8001-
00-2
•84-6
•85-7
86-8
74-9
•54-8
55-9
29-3
57-1
29-7
98-8
65-9
07-8
•20-8
93-4
•44-8
•57-3
•74-1
89-9
36-3
•11-2
•28-2
•16-5
•21-9
29-6
69-1
82-5
•35-2
Detection Limit
(Mg/L)* _
0.004
0.003
0.006
0.009
0.011
0.004
0.004
0.004
0.002
0.014
0.014
0.004
0.066
0.006
0.023
0.003
0.083
0.004
Analysis for the above organochlorine pesticides and polychlorinated
biphenyls in water samples can be performed by gas chromatography. A 1-liter
portion of sample is mixed with surrogates and extracted with methylene chlor-
ide at a pH of 5 to 9, using a separatory funnel or a continuous extractor.
The extract is dried, solvent-exchanged to hexane, and concentrated. Cleanup
techniques are optional. A portion of the extract is screened by gas chromato-
graphy with an electron capture detector (GC/ECD). The presence of pesticides
is qualitatively confirmed by a second column or by gas chromatography/mass
spectrometry (GC/MS). If the screening results are positive, a 50-milliliter
portion of the sample is diluted to 1 liter prior to extraction. The extract
* From EPA Method 608
B-570
-------
is then analyzed as described above. Quantification is accomplished on a
packed column, whereas confirmation can be on either a packed column or a
capillary column.
INTERFERENCES:
Interferences may be caused by contaminants in solvents, reagents, glass-
ware, and other sample processing equipment. These materials must be routinely
demonstrated to be free from laboratory interferences by analyzing reagent
blanks. Matrix interferences may be caused by contaminants that are coextracted
from the sample. The extent of matrix interferences may vary considerably from
source to source.
QUALITY CONTROL:
Pesticides are analyzed by a two-column confirmatory technique. The
analytes must be quantified by packed column GC. The extract is analyzed using
external standards with at least 3 concentrations. All single-peak pesticides
may be in one calibration mixture provided that a 25-percent or greater resolu-
tion can be achieved between each compound. All multicomponent standards must
be in separate calibration solutions except Aroclors 1016/1260. Both columns
used for analysis must meet the same quality control requirements: Prior to
sample analysis, analyte retention time windows must be established for com-
pound identification. DDT and endrin degradation must not exceed 5 percent and
10 percent, respectively- DDT must elute at greater than 12 minutes when
injected onto the packed column. The retention time shift for dibutyl chloren-
date during 8 hours of analysis must not exceed 2 percent relative difference
(RPD) for packed column analysis and 0.3 percent for FSCC analysis.
EPA/TECHNICAL STATUS:
This method is in use in the CERCLA program and is approved for use under
the Resource Conservation Recovery Act and the Clean Water Act. Precision and
accuracy information is furnished (ASTM STP 573 and D 3086-79 and EPA Methods
608 and 8080).
REFERENCES;
U.S. Environmental Protection Agency, Invitation for Bid, "Organics Analysis,
Multi-Media, Multi-Concentration, GC/MS with Medium Level GC Screen," Solicita-
tion Number WA84A-266; U.S. EPA: Washington, DC, June 15, 1984.
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom, J. J. Lichtenberg,
Eds., Method 608; EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
Pressley, T. A.; Longbottom, J. E. "The Determination of Organohalide Pesti-
cides and PCBs in Industrial and Municipal Wastewater," Method 617; EPA-600/4-
82-006, U.S. EPA: Cincinnati, 1982, 35 pp.
B-571
-------
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste.
Physical/Chemical Methods, 2nd ed., Methods 3510, 3520, 8080; SW-846, U.S. EPA
Washington, 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $125-150
(list).
B-572
-------
ORGANOPHOSPHORUS AND CARBAMATE INSECTICIDES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Carbofuran 1563-66-2
Dichlorvos 62-73-7
Methomyl 16752-77-5
Trichlorfon 52-68-6
METHOD SUMMARY:
Analysis for the above compounds in soil/sediment samples can be performed
by gas chromatography. The analyte is extracted from the soil, cooled to
precipitate water and waxes, and analyzed by GC with an alkali flame ionization
detector (GC/AFID). On-column acetylation with acetic anhydride is used for
trichlorfon. Mass spectrometry (MS) is used to confirm GC results.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Holland, P. T. "Routine Methods for Analysis of Organophosphorus and Carbamate
Insecticides in Soil and Ryegrass," Pestic. Scl., 8, 1977, pp. 354-358.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $125-170
(list); the cost of GC/MS confirmation is approximately $150-200 (list).
B-573
-------
ORGANOPHOSPHORUS COMPOUNDS
Air Samples
Laboratory Method
Compound CAS Number
Chlorpyrifos 2921-88-2
Diazlnon 333-41-5
Dichlorvos 62-73-7
Malathion 121-75-5
Methyl Parathion 298-00-0
Parathion 56-38-2
METHOD SUMMARY:
Analysis for the above airborne organophosphorus compounds can be performed
by passage of 1000 liters of air through a polyurethane-foam sampling tube,
followed by Soxhlet extraction of the foam, and analysis of the extract by gas
chromatography with electron capture detection (GC/ECD). When concentration
levels are high enough, confirmation of peak identification can be performed by
gas chromatography/mass spectrometry (GC/MS).
INTERFERENCES:
Phthalate esters and polychlorinated naphthalenes can interfere, and use
of non-TFE plastics must be avoided.
QUALITY CONTROL:
Solvents, reagents, glassware, and polyurethane plugs must be shown to be
free of interfering artifacts. A field blank must be analyzed with each set of
samples, and both a quality control standard and a method blank should be
analyzed with each set of 5 to 15 samples.
EPA/TECHNICAL STATUS:
This method has been evaluated by the Environmental Protection Agency, but
is not approved for any specific regulatory program. The method is applicable
to a range from 50 nanograms per cubic meter to 1000 nanograms per cubic meter.
No precision or accuracy information is furnished.
REFERENCE:
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Waste Sites, Assignment 26, Appendix B, Contract 68-02-3168; U.S. EPA: Research
Triangle Park, North Carolina, May 1982.
B-574
-------
HOST INFORMATION:
Cost per sample for analysis by this method is approximately $115 (list):
the cost for GC/MS confirmation is approximately $150-200 (list). Sampling
costs are additional.
B-575
-------
ORGANOPHOSPHORUS PESTICIDES
Air Samples
Laboratory Method
Compound CAS Number
Chlorpyrifos 2921-88-2
Coumaphos 56-72-4
Diazinon 333-41-5
Dichlorvos 62-73-7
Disulfoton 298-04-4
Guthion 86-50-0
Malathion 121-75-5
Methyl Parathlon 298-00-0
Mevinphos 7786-34-7
Naled 300-76-5
Phorate 298-02-2
METHOD SUMMARY:
Analysis of air for the above organophosphorus pesticides can be performed
by highvolume air sampling, followed by Soxhlet extraction of the analyte from
the sampling medium and concentration and analysis of the resulting solution by
gas chromatography with flame photometric detection (GC/FPD).
INTERFERENCES:
Elemental sulfur can interfere with the determination, but can be removed
by the addition of copper powder.
QUALITY CONTROL:
Retention time efficiency of standards must be determined for each pesticide
to be analyzed by at least 6 replicate tests.
EPA/TECHNICAL STATUS;
This method is not EPA-approved, but the gas chromatographic analysis
applied to water and wastewater extracts is approved under NPDES. Precision
and accuracy information is furnished.
REFERENCES:
Sherma, J.; Beroza, M. Manual of Analytical Methods for the Analysis of
Pesticides in Humans and Environmental Samples, Section 8B; EPA-600/8-80-038,
U.S. Environmental Protection Agency: Research Triangle Park, North Carolina,
1980.
B-576
-------
Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual,
Vol. IH» Available Laboratory Analytical Methods, "Determination of Organo-
phosphorus Pesticides in Air," EPA-600/S4-84-038, pp. III-247 to III-250: U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $165 (list),
plus sampling costs.
B-577
-------
Compound
Chlorpyrifos
Coumaphos
Diazinon
Dichlorvos
Dimethoate
Disulfoton
Ethion
Guthion
Malathion
Mevinphos
Naled
Parathion
Phorate
ORGANOPHOSPHORUS PESTICIDES
Soil/Sediment Samples
Laboratory Method
CAS Number
2921
56
333
62
60
298
563
86
121-
7786
300-
56
298
-88-2
-72-4
-41-5
-73-7
-51-5
-04-4
-12-2
-50-0
-75-5
-34-7
-76-5
-38-2
-02-2
Estimated
Detection
Limit (yig/L)
0.3*
1.5*
0.012**
0.1*
0.20*
1.5*
0.3*
0.015**
0.15*
METHOD SUMMARY:
Gas chromatography can be used to analyze soil/sediment samples for the above
organophosphorus pesticides. A soil/sediment sample is extracted at neutral pH
with dichloromethane or with hexane-isopropanol, and the extract is dried, con-
centrated, and analyzed by gas chromatography using a nitrogen/phosphorus
detector (GC/NPD), a flame photometric detector (GC/FPD), or (as applicable) a
halogenspecific detector (GC/HSD).
INTERFERENCES:
The use of Florisil® column or silica-gel column cleanup is not recom-
mended for removal of interferences, but the use of GC/HSD for naled and
dichlorvos, or of GC/FPD, minimizes the effects of the presence of many
interferents. Elemental sulfur can interfere with GC/FPD.
QUALITY CONTROL:
Either internal or external standards may be used for quantification, and an
aliquot of each sample must be spiked to determine recoveries and detection
limits. The analytical system must be demonstrated to be free of interferences
by the analysis of a method blank with each set of samples or change in reagents.
Field laboratory replicates should be processed and analyzed to assess the
precision of the sampling and analysis methods. Fortified samples should be
* As cited in Method 622
** As cited in Method 614
B-578
-------
analyzed to ascertain the accuracy of the analysis. In cases where uncertainty
exists concerning the identification of a peak in the chromatogram, confirmatory
techniques, such as gas chromatography/mass spectrometry (GC/MS) or second-
column confirmation, should be used.
EPA/TECHNICAL STATUS:
This method is EPA-approved for the Resource Conservation and Recovery Act
(RCRA) sample analyses. Precision and accuracy information is furnished.
REFERENCES:
Pressley, T. A.; Longbottom, J. E. "The Determination of Organophosphorous
Pesticides in Industrial and Municipal Wastewater," Method 614; U.S. EPA:
Cincinnati, 1982, 21 pp.
Pressley, T. A.; Longbottom, J. E. "The Determination of Organophosphorous
Pesticides in Industrial and Municipal Wastewater," Method 622; U.S. EPA:
Cincinnati, 1982, 35 pp.
U.S. Environmental Protection Agency, Test Methods for Evaluating of Solid
Waste: Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8140; SW-846,
U.S. EPA: Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Determination of Organo-
phosphorus Pesticides in Air," EPA-600/S4-84-038, pp. III-247 to III-250; U.S.
Environmental Protection Agency: Las Vegas, 1984.
Tonan, J. A. Design and Development Branch, U.S. EPA, Toxicant Analysis
Center, Private Communication to Edward Kantor, U.S. EPA-EMSL, Las Vegas,
Nevada.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $165-210
(list).
B-579
-------
ORGANOPHOSPHORUS PESTICIDES
Water Samples
Laboratory Method 1
Estimated
Detection
Compound CAS Number Limit (ug/L)
Chlorpyrifos 2921-88-2 0.3*
Coumaphos 56-72-4 1.5*
Diazinon 333-41-5 0.012**
Dichlorvos 62-73-7 0.1*
Dimethoate 60-51-5
Disulfoton 298-04-4 0.20*
Guthion 86-50-0 1.5*
Malathion 121-75-5
Mevinphos 7786-34-7 0.3*
Naled 300-76-5
Parathion 56-38-2 0.015**
Phorate 298-02-2 0.15*
METHOD SUMMARY:
Analysis for the above organophosphorus pesticides in water samples can be
performed by gas chromatography. A water sample is extracted at neutral pH
with methylene chloride, and the extract is dried, concentrated, and analyzed
by gas chromatography using a nitrogen/phosphorus detector (GC/NPD), a flame
photometric detector (GC/FPD), or (as applicable) a halogen-specific detector
(GC/HSD).
INTERFERENCES:
The use of Florisil® column or silica-gel column cleanup is not recom-
mended for removal of interferences, but the use of GC/HSD for naled and
dichlorvos, or of GC/FPD, minimizes the effects of the presence of many inter-
ferents. Elemental sulfur can interfere with GC/FPD.
QUALITY CONTROL:
Either internal or external standards may be used for quantification, and an
aliquot of each sample must be spiked to determine recoveries and detection
limits. The analytical system must be demonstrated to be free of interferences
by analysis of a method blank with each set of samples or with each change in
reagents, and field and laboratory replicates should be processed and analyzed
to assess the precision of the sampling and analysis methods. Fortified samples
should be analyzed to ascertain the accuracy of the analysis. In cases where
uncertainty exists concerning the identification of a peak in the chromatogram,
confirmatory techniques, such as gas chromatography/mass spectrometry (GC/MS)
or second-column confirmation, should be used.
*As cited in Method 622
**As cited in Method 614
B-580
-------
EPA/TECHNICAL STATUS:
This method is EPA-approved for the Resource Conservation and Recovery Act
(RCRA) and the Clean Water Act. Precision and accuracy information is
furnished.
REFERENCES:
Pressley, T. A.; Longbottom, J. E., "The Determination of Organophosphorous
Pesticides in Industrial and Municipal Wastewater," Method 614; U.S. EPA:
Cincinnati, 1982, 21 pp.
Pressley, T. A.; Longbottom, J- E., "The Determination of Organophosphorous
Pesticides in Industrial and Municipal Wastewater," Method 622; U.S. EPA:
Cincinnati, 1982, 35 pp.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed. , Methods 3510, 3520, 8140; SW-846; U.S. EPA:
Washington, 1982.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Determination of Organo-
phosphorus Pesticides in Air," EPA-600/S4-84-038, pp. III-247 to III-250; U.S.
Environmental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $165-210
(list).
B-581
-------
ORGANOPHOSPHORUS PESTICIDES
Water Samples
Laboratory Method 2
Compound CAS Number
Coumaphos 56-72-4
Diazinon 333-41-5
Dichlorvos 62-73-7
0,0-Diethyl 0-Pyrazinyl
Phosphorothioate 297-97-2
Dimethoate 60-51-5
Disulfotos 298-04-4
Ethion 563-12-2
Mevinphos 7786-34-7
Parathion 56-38-2
Phorate 298-02-2
Trichlorfon 57-68-6
METHOD SUMMARY:
The above organophosphorus pesticides in water samples can be measured by
gas chromatography (GC) with phosphorus-selective flame thermionic detection.
In most instances, the sample is extracted with chloroform, and cleanup, if
necessary, is performed by passing the solvent containing the analyte through a
Nuchar® carbon column, and eluting with chloroform. Coumaphos and dichlorvos
require an alternative cleanup procedure because they are retained on Nuchar.
The eluate is solvent-exchanged with acetone or ethanol, and the resulting
solution is analyzed by GC.
INTERFERENCES:
Volatile nitrogen-containing compounds may cause false peaks if they are
present in sufficient concentration.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Accuracy information is furnished. The
limit of detection is approximately 0.1 microgram per liter.
REFERENCE:
Askew, V.; Ruzicka, J. H.; Wheals, B. B. "A General Method for Determination
of Organophosphorus Pesticide Residues in River Waters and Effluents by Gas,
Thin-layer, and Gel Chromatography," Analyst, 94, 1969, pp. 275-283.
B-582
-------
COST INFORMATION:
(list).
Cost per sample for analysis by this mPt-VmH ,-„
). method is approximately $195-235
B-583
-------
PARTICULATE AROMATIC HYDROCARBONS
Air Samples
Laboratory Method
Compound CAS Number
Anthracene 120-12-7
Benzo[a]anthracene 56-55-3
Benzene 71-43-2
Benzo[b]fluoranthene 205-99-2
Benzo[k]fluoranthene 207-08-9
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
ODD 72-54-8
DDE 72-55-9
DDT 50-29-3
Dibenz[a,b]anthracene 53-70-3
Fluoranthene 206-44-0
Fluorene 86-73-7
Naphthalene 91-20-3
Phenanthrene 85-01-8
Polychlorinated Biphenyls
(Aroclor 1260) 11096-82-5
Pyrene 129-00-0
METHOD SUMMARY:
The above particulate aromatic hydrocarbons in air samples may be measured
by high-performance liquid chromatography (HPLC). The particulates are collected
on a glass-fiber filter, then extracted ultrasonically in the presence of
silica powder. The hydrocarbons in the extract are separated by HPLC on a
column of Porasil II with a nonpolar solvent, and the absorbance is measured by
a UV detector at 254 nm.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Replicates and a blank should be processed.
EPA/TECHNICAL STATUS:
This method is classified as proposed by the National Institute for
Occupational Safety and Health (NIOSH). The minimum detection limit for
benzofa]pyrene is approximately 3.3 nanograms per cubic meter of air, using
a 1500-cubic meter sample. Precision and accuracy information is furnished.
B-584
-------
gFERENCE:
J.S. Department of Health, Education and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol 1, Method P&CAM 206; Publication No. 77-157-A, U.S. DREW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $150 (list).
B-585
-------
PESTICIDE RESIDUES
Air Samples
Laboratory Method
Compound CAS Number
Aldrin 309-00-2
a-BHC 319-84-6
6-BHC 319-85-7
Carbaryl 63-25-2
Carbofuran 1563-66-2
ODD 72-54-8
DDE 72-55-9
DDT 50-29-3
Diazinon 333-41-9
Dieldrin 60-57-1
Endrin 72-20-8
Ethion 563-12-2
Heptachlor Epoxide 1024-57-3
Lindane 58-89-9
Malathion 121-75-5
Mercaptodimethur 2032-65-7
Methyl Parathion 298-00-0
Mexacarbate 315-18-4
Parathion 56-38-2
METHOD SUMMARY:
Gas chromatography may be used for the analysis of the above chlorinated,
organophosphate, and N-methyl carbamate insecticides in air. A known volume of
air is drawn through an impinger containing 100 milliliters of ethylene glycol,
followed by extraction of the resulting solution with methylene chloride and
fractionation of the extract on silica gel. The fraction containing chlori-
nated compounds is analyzed with a gas chromatograph equipped with an elec-
tron-capture detector (GC/ECD); the fraction containing phosphate compounds is
analyzed with a gas chromatograph equipped with a flame photometric detector
(GC/FPD). The carbamates are derivatized with pentafluoropropionic anhydride,
and the products are analyzed with a gas chromatograph equipped with an elec-
tron capture detector (GC/ECD).
INTERFERENCES:
Lindane may elute in Fractions I and II, but can be resolved and quantified
in both. Diazinon, if present in Fraction III, would co-elute with carbaryl
under the conditions used. The derivatization step will effectively remove
this interference.
QUALITY CONTROL:
Method blanks and standards are prepared and processed along with the
samples.
B-586
-------
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE;
Sherma, J.; Shafik, T. M. "A Multiclass, Multiresidue Analytical Method for
Determining Pesticide Residues in Air," Arch. Environ. Contam. Toxicol 3m
1975, pp. 55-71. ~" ' - ''
COST INFORMATION;
Cost per sample for analysis by this method is approximately $115-180
(list), plus sampling costs.
B-587
-------
PESTICIDES
Water Samples
Laboratory Method 1
Compound CAS Number
Aldrin 309-00-2
a-BHC 319-84-6
B-BHC 319-85-7
6-BHC 319-86-8
Captan 133-06-2
DDE 72-55-9
DDT 50-29-3
Dichlorvos 62-73-7
Dieldrin 60-57-1
Parathion 56-38-2
Diethyl-p-nitrophenyl 311-45-5
Phosphate
a-Endosulfan 959-98-8
B-Endosulfan 33213-65-9
Endrin 72-20-8
Ethion 563-12-2
Heptachlor 76-44-8
Heptachlor Epoxide 1024-57-3
Lindane 58-59-9
Methoxychlor 72-43-5
Methyl Parathion 298-00-0
Parathion 56-38-2
METHOD SUMMARY:
The above pesticides in water samples can be measured by gas chromato-
graphy with electron capture detection (GC/ECD). For good quantitative per-
formance, the column, OV-17, a phenyl methyl silicone, should be saturated with
microgram quantities of the compounds to be separated.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
B-588
-------
REFERENCE:
Leoni, V.; Puccettl, G. "Gas-Liquid Chromatography of Pesticides on OV-17
Stationary Phase," J. Chromatogr.. 43, 1969, pp. 388-391?
COST INFORMATION;
Cost per sample for analysis by this method is approximately $70-100
(list).
B-589
-------
PESTICIDES
Water Samples
Laboratory Method 2
Compound CAS Number
Aldrin 309-00-2
DDE 72-55-9
Dieldrin 60-57-1
Endrin 72-20-8
Heptachlor 76-44-8
Heptachlor Epoxide 1024-57-3
Hexachlorohexahydro- 465-73-6
dimethanonaphthalene
Malathion 121-75-5
Methyl Parathion 298-00-0
Parathion 56-38-2
METHOD SUMMARY:
The above pesticides in water samples can be measured by gas chromato-
graphy with electron capture detection (GC/ECD). A hexane extract of the water
sample is applied to an alumina column. An elution solvent is added in small
increments, and each resulting eluate fraction is analyzed separately, allowing
adequate resolution of the peaks in the chromatogram.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision and accuracy information is
furnished for most compounds.
REFERENCE:
Law, L. M.; Goerlitz, D. F. "Microcolumn Chromatographic Cleanup for the
Analysis of Pesticides in Water," J. Assoc. Off. Anal. Chem. , 5_3,(6), 1970, pp.
1276-1286.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $135-150
(list).
B-590
-------
PHENOLIC COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
2-Chlorophenol 95-57-8
Cresol 1319-77-3
m-Cresol 108-39-4
o-Cresol 95-48-7
£-Cresol 106-44-5
2,4-Dichlorophenol 120-83-2
2,6-Dichlorophenol 87-65-0
Phenol 108-95-2
METHOD SUMMARY:
Analysis for the above phenols, methylphenols (cresols), and mono- and di-
chlorophenols in water may be performed by direct injection of 1 to 3 microliters
of the sample into a gas chromatograph with a flame ionization detector (GC/FID).
INTERFERENCES:
Suspended particulate matter may cause problems, and interferences by
co-eluting compounds should be removed by an appropriate preliminary separation
technique. In strongly alkaline samples, salt formation may be a problem, and
pH adjustment may be required.
QUALITY CONTROL:
Three microliters of distilled water should be injected into the gas
chromatograph between sample injections. Triplicate determinations of each
sample should be performed.
EPA/TECHNICAL STATUS:
The method is applicable over the range of 1 to 80 milligrams per liter
and has undergone single-laboratory evaluation. The method is not EPA-approved.
Single-operator precision information is available (ASTM).
REFERENCES:
Kirshen, N.A. "The Analysis of Phenols in Water by Direct Aqueous Injection,"
In Varian Instruments at Work, No. 66, October 1982.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards.
Volume 11.02, D 2580-80; ASTM: Philadelphia, 1981, pp. ^8 ^10.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-90 (list).
B-591
-------
PHENOLICS
Air Samples
Laboratory Method
Compound
Ammonium Picrate
p-Chloro-m-cresol
2-Chlorophenol
Cresol
m-Cresol
£-Cresol
£-Cresol
2,4-Dichlorophenol
2,6-Dichlorophenol
2,4-Dimethylphenol
4,6-Dinitro-o-cresol
CAS Number
131-
59-
95-
1319-
108-
95-
106-
120-
87-
105-
534-
74-8
50-7
57-8
77-3
39-4
48-7
44-5
83-2
65-0
67-9
52-1
89-5
4,6-Dinitro-o-cyclohexyl- 131
phenol
Dinitrophenol 25550-58-7
METHOD SUMMARY:
Compound CAS Number
2,4-Dinitrophenol 51-28-5
2,5-Dinitrophenol 329-71-5
2,6-Dinitrophenol 573-56-8
Nitrophenol, Mixed 25154-55-6
m-Nitrophenol 554-84-7
o-Nitrophenol 88-75-5
p-Nitrophenol 100-02-7
Pentachlorophenol 87-86-5
Phenol 108-95-2
2,3,4,6-Tetrachlorophenol 58-90-2
Trichlorophenol 25167-82-2
2,4,5-Trichlorophenol 95-95-4
2,4,6-Trichlorophenol 88-06-2
Xylenol 1300-71-6
Analysis of air for the above phenolic compounds can be performed spectro-
photometrically. The phenolics present in approximately 1000 liters of air are
collected on a fiberglass filter with a high-volume sampler at 28 liters per
minute. The filter medium should be wet with sodium hydroxide. The phenolics
are Soxhlet-extracted from the filter medium with benzene, and the resulting
solution is extracted with sodium hydroxide, acidified, and distilled. The
phenolics present in the distillate are determined by spectrophotometry. This
method does not identify the phenolic compounds present, but measures the total
phenolic content of the sample.
INTERFERENCES:
Any color or turbidity in the sample that carries through the distillation
step can interfere. Sulfur compounds and certain metal ions interfere. The
addition of copper sulfate to the alkaline solution of phenols will stabilize
the solution.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The distillation/colorimetric portion of
the method is approved for use in Clean Water Act analyses. The method is
sensitive to levels above approximately 80 micrograms per cubic meter for the
recommended sample size. Precision and accuracy information is furnished.
B-592
-------
REFERENCES;
American Public Health Association, "Tentative Method of Analysis for Phenols
in the Atmosphere (Gas Chromatographic Method)," Methods of Air Sampling and
Analysis, M. Katz, Ed., Method 121; APHA: Washington, 1972, PP. 328-332.
Mohler E. P.; Jacob, L. N. "Determination of Phenolic-Type Compounds in Water
and Industrial Waste Waters, Anal. Chem., 29^(9), 1957, pp. 1369-1374.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $85-100
(list), plus sampling costs.
B-593
-------
PHENOLICS
Water Samples
Laboratory Method
Compound CAS Number
p_-Chloro-m-cresol 59-50-7
2-Chlorophenol 95-57-8
Cresol 1319-77-3
m-Cresol 108-39-4
o-Cresol 95-48-7
2,4-Dichlorophenol 120-83-2
2,6-Dichlorophenol 87-65-0
2,5-Dinitrophenol 329-71-5
2,6-Dinitrophenol 573-56-8
2-Nitrophenol 88-75-5
3-Nitrophenol 554-84-7
Pentachlorophenol 87-86-5
Phenol 108-95-2
2,3,4,6-Tetrachlorophenol 58-90-2
Trichlorophenol 25167-82-2
2,4,5-Trichlorophenol 95-95-4
2,4,6-Trichlorophenol 88-06-2
METHOD SUMMARY:
The above phenolic compounds in water samples can be measured photometri-
cally. After acid distillation, the phenolics in the sample are reacted with
4-amino-antipyrine at a pH of 10 + 0.2 in the presence of potassium ferricyanide.
The antipyrine dye may be extracted from the aqueous solution into chloroform
and the absorbance measured at 460 nm, or the absorbance can be measured directly
in the aqueous solution at 505, 510, or 520 nm. The extraction method provides
20-fold lower detection. The analysis may be performed manually or with a
Technicon AutoAnalyzer (or equivalent). A similar procedure uses 3-methyl-2-
benzothiolinone hydrazene hydrochloride (MBTH) as the color reagent and eerie
ammonium sulfate as an oxidant. This procedure is performed at pH 4 and the
color is measured at 520 or 490 nm. This method does not identify the specific
phenolic compounds present, but measures the total phenolic content of the
sample. The result should be considered as a minimum value.
INTERFERENCES:
Sulfur compounds, oxidizing agents, oil and tar may interfere. While
phenol-decomposing bacteria, reducing substances, and strongly alkaline condi-
tions may also interfere, provisions have been incorporated in the method to
minimize their effects. Phenolic compounds that have a substituent in the para
position usually do not produce color, unless the para substituent is a carboxyl,
halogen, hydroxyl, methoxyl or sulfonic acid group.
B-594
-------
QUALITY CONTROL;
A standard and a blank must be prepared and the results should be used in
the calculations.
EPA/TECHNICAL STATUS:
These methods are approved for SDWA and NPDES analyses. Limits of detec-
tion are: for the 4-aminoantipyridine methods 5 micrograms per liter if the
chloroform extraction is performed, 50 to 100 micrograms per liter if it is not,
and 2 micrograms per liter for the automated method; for the MBTH methods, 2
micrograms per liter if the extraction is performed and 50 micrograms per liter
if it is not. Precision and accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and WAstes, Methods 420.1, 420.2, 420.3; EPA-600/4-79-020, U.S. EPA:
Washington, 1979.
American Public Health Association, Standard Methods for the Examination of
Water and Wastewater, 15th ed., Method 510; APHA: Washington, 1981 pp. 508-513.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D 1783-80, ASTM: Philadelphia, 1983 pp. 202-207.
U.S. Geological Survey, Methods for the Determination of Organic Substances in
Water and Fluvial Sediments, Book 5, "Laboratory Analysis," Chapter A3; USGS:
Denver, Open-File Report 82-1004, 1983.
Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water
and Wastes, "Phenolics;" Publication No. AECV81-M1; Alberta Environmental
Centre: Vegreville, Alberta, Canada, 1981.
COST INFORMATION:
Cost information has not been obtained.
B-595
-------
PHENOLS
Soil/Sediment Samples
Laboratory Method
Detection
Limit
Compound CAS Number (yg/L)*
£-Chloro-m-cresol 59-50-7 0.36
2-Chlorophenol 95-57-8 0.31
2,4-Dichlorophenol 120-83-2 0.39
2,6-Dichlorophenol 87-65-0
2,4-Dimethylphenol 105-67-9 0.32
4,6-Dinitro-o-cresol
and salts 534-52-1 16.0
4,6-Dinitro-o-cyclohexyl- —
phenol 131-89-5
Dinitrophenol 25550-58-7 13.0
2,4-Dinitrophenol 51-28-5 13.0
2-Nitrophenol 88-75-5 0.45
4-Nitrophenol 100-02-7 2.8
Pentachlorophenol 87-86-5 7.4
Phenol 108-95-2 0.14
2,3,4,6-Tetrachlorophenol 58-90-2
2,4,6-Trichlorophenol 88-06-2 0.64
METHOD SUMMARY:
Analysis of soil/sediment samples for the above phenols can be performed
by gas chromatography. A soil/sediment sample is extracted at pH 2 with
methylene chloride, and the extract is dried, concentrated, and analyzed by gas
chromatography with either a flame ionization detector (GC/FID) or an electron
capture detector (GC/ECD).
INTERFERENCES:
Use of plastics in collection, storage, or processing of samples must be
avoided.
QUALITY CONTROL:
An aliquot of each sample must be spiked to determine the detection limits
and recovery, and a method blank should be analyzed with each set of samples or
change in reagents. Field and laboratory replicates and duplicate samples
should be analyzed to demonstrate the sensitivity and accuracy of the method.
When doubt exists about the identification of a peak in the chromatogram,
confirmatory methods, such as gas chroraatography/mass spectrometry (GC/MS) or
second-column confirmation, should be used.
* As listed in Method 604 (EPA)
B-596
-------
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
(40 CFR, Part 261, Identification and Listing of Hazardous Wastes) sample
analyses. No precision or accuracy information is furnished.
REFERENCES:
Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater,
J. E. Longbottom, J. J. Lichtenberg, Eds., Method 604;" EPA-600/4-82-057, U.S.
EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8040: SW-846, U.S. EPA:
Washington, July 1982.
U.S. Environmental Protection Agency, Development and Application of Test
Procedures for Specific Organic Toxic Substances in Wastewaters. Category
3-Phenols, Report for EPA Contract 68-03-2625.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $105-160
(list).
B-597
-------
PHENOLS
Water Samples
Laboratory Method
Detection
Limit
Compound CAS Number (yg/L)*
p-Chloro-m-cresol 59-50-7 0.36
2-Chlorophenol 95-57-8 0.31
2,4-Dichlorophenol 120-83-2 0.39
2,6-Dichlorophenol 87-65-0
2,4-Dimethylphenol 105-67-9 0.32
4,6-Dinitro-o-cresol
and salts 534-52-1 16.0
4,6-Dinitro-£-cyclohexyl
phenol 131-89-5
Dinitrophenol 25550-58-7 13.0
2,4-Dinitrophenol 51-28-5 13.0
2-Nitrophenol 88-75-5 0.45
4-Nitrophenol 100-02-7 2.8
Pentachlorophenol 87-86-5 7.4
Phenol 108-95-2 0.14
2,3,4,6-Tetrachlorophenol 58-90-2
2,4,6-Trichlorophenol 88-06-2 0.64
METHOD SUMMARY:
Analysis of water samples for the above phenols can be performed by gas
chromatography. A water sample is extracted at pH 2 with methylene chloride
and the extract is dried, concentrated, and analyzed by gas chromatography with
either a flame ionization detector (GC/FID) or an electron capture detector
(GC/ECD).
INTERFERENCES:
The use of plastics in collection, storage, or processing of samples must
be avoided.
QUALITY CONTROL:
An aliquot of each sample must be spiked to determine the detection limits
and recovery, and a method blank should be analyzed with each set of samples or
change in reagents. Field and laboratory replicates and duplicate samples
should be analyzed to demonstrate the sensitivity and accuracy of the method.
When doubt exists about the identification of a peak in the chromatogram,
confirmatory methods, such as gas chromatography/mass spectrometry (GC/MS) or
second-column confirmation, should be used.
*As cited in Method 604.
B-598
-------
EPA/TECHNICAL STATUS:
This method is EPA-approved for Resource Conservation and Recovery Act
(40 CFR, Part 261, Identification and Listing of Hazardous Wastes) sample
analyses. No precision or accuracy information is furnished.
REFERENCES:
Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater,
J. E. Longbottom, J. J. Lichtenberg, Eds., Method 604; EPA-600/4-82-057, U.S.
EPA: Cinncinati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8040; SW-846, U.S. EPA:
Washington, July 1982.
U.S. Environmental Protection Agency, Development and Application of Test
Procedures for Specific Organic Toxic Substances in Wastewaters. Category
3-Phenols, Report for EPA Contract 68-03-2625.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $105-160
(list).
B-599
-------
PHENOLS AND OTHER COMPOUNDS
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Chlorambucil 305-03-3
Daunomycin 20830-81-3
Melphalan 148-82-3
Methomyl 16752-77-5
Mitomycin C 50-07-7
5-Nitro-o-toluidine 99-55-8
Reserplne 50-55-5
Streptozotocin 18883-66-4
Thiram 137-26-8
Warfarin 81-81-2
METHOD SUMMARY:
Analysis for the above phenols and other compounds may be performed by
high-performance liquid chromatograpy (HPLC). The sample is extracted with
diethyl ether and the extract is analyzed by solvent-programmed reversed-phase
HPLC with UV detection at 254 nm.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
Method blanks should be processed with each set of samples or change in
operating conditions or matrix. Field and laboratory replicates should be
analyzed and fortified samples should be processed and analyzed.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precison or accuracy information is
furnished.
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste;
Physical/Chemical Methods, 2nd ed., Method 8320; SW-846, U.S. EPA: Washington,
1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130-175
(list).
B-600
-------
PHENOLS AND OTHER COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Chlorambucil 305-03-3
Daunomycin 20830-81-3
Melphalan 148-82-3
Methomyl 16752-77-5
Mitomycin C 50-07-7
5-Nitro-o-toluidine 99-55-8
Reserpine 50-55-5
Streptozotocin 18883-66-4
Thiram 137-26-8
Warfarin 81-81-2
METHOD SUMMARY:
Analysis for the above phenols and other compounds in water samples can be
performed by high-performance liquid chromatograpy (HPLC). A water sample is
extracted with diethyl ether, and the extract is analyzed by solvent-programmed
reversephase HPLC with UV detection at 254 nm.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
A method blank should be processed with each set of samples or change in
operating conditions or sample matrix. Fortified samples, field replicates,
and laboratory replicates should be processed and analyzed.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precison or accuracy information is
furnished.
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed. , Method 8320; SW-846, U.S. EPA: Washington,
19827
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130-175
(list).
B-601
-------
PHTHALATE ESTERS
Soil/Sediment Samples
Laboratory Method
Detection
Limit
Compound CAS Number (ug/L)*
Bis(2-Ethylhexyl) Phthalate 117-81-7 2.0
Di-n-butyl Phthalate 84-74-2 0.36
Diethyl Phthalate 84-66-2 0.49
Dimethyl Phthalate 113-11-3 0.29
Di-n-octyl Phthalate 117-84-0 3.0
METHOD SUMMARY:
Analysis of soil/sediment samples for the above phthalate esters can be
performed by gas chromatography. The sample is extracted at neutral pH with
methylene chloride, the solvent exchanged, and the resulting solution is analyzed
by gas chromatography (GC), using either an electron-capture detector (ECD) or
a flame-ionization detector (FID).
INTERFERENCES:
Use of plastics in sampling or sample processing must be avoided.
QUALITY CONTROL:
A reagent blank should be processed each time a change in analytical
conditions occurs or with each new set of samples. Field and laboratory repli-
cates and fortified samples should be analyzed to validate the analytical
results.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use under the Clean Water Act and the
Resource Conservation and Recovery Act (RCRA). Precision and accuracy informa-
tion is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom, and J. J. Lichtenberg,
Eds., Method 606; EPA 600/4-82-057, U. S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 8060; SW-846; U.S. EPA: Washington,
1982.
* As cited in Method 606.
B-602
-------
COST INFORMATION;
Cost per sample for analysis by this method is approximately $90-145
• )•
(list)
B-603
-------
PHTHALATE ESTERS
Water Samples
Laboratory Method
Detection
Limit
Compound CAS Number (yg/L)*
Bis(2-Ethylhexyl) Phthalate 117-81-7 2.0
Di-n-butyl Phthalate 84-74-2 0.36
Diethyl Phthalate 84-66-2 0.49
Dimethyl Phthalate 113-11-3 0.29
Di-n-octyl Phthalate 117-84-0 3.0
METHOD SUMMARY:
Analysis of water samples for the above phthalate esters can be performed
by gas chromatography. The sample is extracted at neutral pH with methylene
chloride, and the extract is analyzed by gas chromatography (GC), using either
an electron-capture detector (ECD) or a flame-ionization detector (FID).
INTERFERENCES:
Use of plastics in sampling or sample processing must be avoided.
QUALITY CONTROL:
A reagent blank should be processed each time a change in analytical
conditions occurs or with each new set of samples. Field and laboratory repli-
cates and fortified samples should be analyzed to validate the analytical
results.
EPA/TECHNICAL STATUS:
This method is EPA-approved for use under the Clean Water Act and the
Resource Conservation and Recovery Act (RCRA). Precision and accuracy informa-
tion is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom, and J. J. Lichtenberg,
Eds., Method 606; EPA 600/4-82-057, U. S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 8060; SW-846: U.S. EPA: Washington,
1982.
*As cited in Method 606.
B-604
-------
COST INFORMATION:
Cost per sample for analysis by this method is approximately $90-145
(list).
B-605
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 1
Compound CAS Number
Benzo[k]fluoranthene 207-08-9
Benzofajpyrene 50-32-8
METHOD SUMMARY:
Analysis of air for benzo[ajpyrene (BaP) and benzo[k]fluoranthene (BkF)
can be performed by high-volume glass-fiber filtration of air for 24 hours,
followed by cyclohexane Soxhlet extraction for 6 hours, extract concentration,
and fluorimetric or high-performance liquid chromatographic (HPLC) determina-
tion of BaP and BkF.
INTERFERENCES:
BaP and BkF are separated from potentially interfering organic compounds
by chromatography on alumina.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. The detection limit for BaP and BkF is 0.01 nanograms per cubic
meter of air-
REFERENCES:
Alberta Environmental Centre, Manual of Methods for the Analysis of Atmospheric
Pollutants, Methods 21515, 21516; Alberta Environmental Centre: Vegreville,
Alberta, Canada, 1981.
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol.
Ill, Available Laboratory Analytical Methods, "Analysis of Air for Polycyclic
Aromatic Hydrocarbons," pp. III-414 to III-420; EPA-600/S4-84-038, U.S. Environ-
mental Protection Agency: Las Vegas, 1984.
COST INFORMATION:
Cost per sample for analysis for this method is approximately $85-160
(list).
B-606
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 2
Compound CAS Number
Benzo[a]anthracene 56-55-3
Benzo[b]fluoranthene 205-99-2
Benzo[k]fluoranthene 207-08-9
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Dibenz[a,h]anthracene 53-70-3
7,12-Dimethylbenz[a]anthracene 57-97-6
Fluoranthene 206-44-0
3-Methylcholanthrene 56-49-5
Pyrene 129-00-0
METHOD SUMMARY:
Analysis of air for the above polycyclic aromatic hydrocarbons can be per-
formed by high-volume glass-fiber filtration of approximately 200 cubic meters
of air, followed by Soxhlet extraction of the filter with methylene chloride,
solvent-exchange into isooctane, and analysis of the resulting solution by
high-performance liquid chromatography (HPLC) with ultraviolet-absorbance or
fluorescence detection, or by gas chromatography with flame-ionization detec-
tion (GC/FID), or with peak-trapping followed by ultraviolet spectrophotometric
analysis of the individual peaks.
INTERFERENCES;
Extensive sample cleanup is usually not required, but the isooctane
extract may be extracted with phosphoric acid in dimethylsulf oxide, and the
resulting solution may be purified by column chromatography.
QUALITY CONTROL;
When doubt exists regarding the identification of peaks in the chromato-
gram, detection at two wavelengths or gas chromatography/mass spectrometry
(GC/MS) can be used to confirm tentative identifications.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished. The method can measure levels above approximately 1 microgram per
cubic meter.
REFERENCES:
Thomas, R. S.; Lao, R. C.; Wang, D. T.; Robinson, D.; Sakuma, T. In Carcino-
jenesis, Vol. 3: Polynuclear Aromatic Hydrocarbons; P. W. Jones and R. I.
Freudenthal, Eds.; Raven Press: New York, 1978, pp. 9 19.
B-607
-------
McElroy, F. C.; Searl, T. D.; Brown R. A. In Trace Organic Analysis: A New
Frontier in Analytical Chemistry, National Bureau of Standards Special Publica-
tion 519. 1978, pp. 7-18.
Das, B. S.; Thomas, G. H. In Trace Organic Analysis; A New Frontier in
Analytical Chemistry, National Bureau of Standards Special Publication 519,
1979, pp. 41-56.
COST INFORMATION:
Cost per sample for analysis by HPLC is approximately $155-175 (list), plus
sampling costs; by GC/FID, approximately $115 (list), plus sampling costs.
Cost information for the U.V. spectrometrty peak-trapping method has not been
obtained.
B-608
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 3
Compound CAS Number
Anthracene 120-12-7
Fluoranthene 206-44-0
Phenanthrene 85-01-8
Pyrene 129-00-0
METHOD SUMMARY:
Analysis for the above airborne polycyclic aromatic hydrocarbons is per-
formed by passage of 1000 liters of air through a polyurethane-foam sampling
tube, followed by Soxhlet extraction of the foam and analysis of the extract by
gas chromatography with electron capture detection (GC/ECD). When concentration
levels are high enough, confirmation of peak identification can be performed by
gas chromatography/mass spectrometry (GC/MS).
INTERFERENCES:
Phthalate esters and polychlorinated naphthalenes can interfere, and use
of non-TFE plastics must be avoided.
QUALITY CONTROL:
Solvents, reagents, glassware, and polyurethane plugs must be shown to be
free of interfering artifacts. A field blank must be analyzed with each set of
samples, and both a quality control standard and a method blank should be
analyzed with each set of 5 to 15 samples.
EPA/TECHNICAL STATUS:
This method has been evaluated by the Environmental Protection Agency, but
is not approved for any specific regulatory program. This method is applicable
to a range from 50 to 1000 nanograms per cubic meter. Precision and accuracy
information is furnished.
REFERENCE:
U.S. Environmental Protection Agency, Guidelines for Air Monitoring at Hazardous
Waste Sites, Appendix B, Assignment 26; Contract 68-02-3168, U.S. EPA: Research
Triangle Park, North Carolina, May 1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $115 (list):
the cost for GC/MS confirmation is approximately $150-200 (list). Sampling
costs are additional.
B-609
-------
POLYCYLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 4
Compound CAS Number
Anthracene 120-12-7
Benzo[a]anthracene 56-55-3
Benzo[k]fluoranthene 207-08-9
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Dibenz[a,h]anthracene 53-70-3
Fluoranthene 206-44-0
Fluorene 86-73-7
Phenanthrene 85-01-8
Pyrene 129-00-0
METHOD SUMMARY:
Analysis of air for the above polycyclic aromatic hydrocarbons can be
performed by passage of approximately 200 cubic meters of air through a sampling
train with a glass-fiber filter, followed by cyclohexane Soxhlet extraction of
the filter, concentration of the extract and analysis by high-performance liquid
chromatography (HPLC) with ultraviolet or fluorescence detection.
INTERFERENCES:
Use of two wavelengths for absorbance detectors can eliminate some inter-
ference and/or co-elution problems.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
The method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Thomas, R. S.; Lao, R. C.; Wang, D. T.; Robinson, D.; Sakuma, T. In Carcino-
genesis, Vol. 3: Polynuclear Aromatic Hydrocarbons; P- W. Jones and R. I.
Freudenthal, Eds.; Raven Press: New York, 1978, pp. 9-19.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $160-180
(list), plus sampling costs.
B-610
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 5
Compound CAS Number
Benz[c]acridine 225-51-4
Benzo[a]anthracene 56-55-3
Benzo[b]fluoranthene 205-99-2
Benzo[k]fluoranthene 207-08-9
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Fluoranthene 206-44-0
Pyrene 129-00-0
METHOD SUMMARY:
The above polycyclic aromatic hydrocarbons in air samples may be measured
spectrophotometrically. The analytes are collected on a filter and extracted
with benzene. Internal standards are added, the extract is concentrated, and a
portion of the concentrate is injected into a gas chromatograph (GC). The poly-
nuclear aromatic hydrocarbons and the internal standards are trapped individually
as they elute from the GC column, and each compound is measured by UV
spectrophotometry.
INTERFERENCES:
Any compound with similar GC retention time as one of the analytes or
internal standards, and any compound with a similar UV absorption spectrum as
one of the analytes will interfere.
QUALITY CONTROL;
A filter blank should be processed, and its value used in the calculation of
the results. Also, appropriate corrections must be made based on the recovery of
the internal standard.
EPA/TECHNICAL STATUS;
This method is classified as operational by the National Institute of Occupa-
tional Safety and Health (NIOSH) for use over the range of 2 to 1,000 raicrograms
of each compound per cubic meter of air, with a 0.5-liter sample. No precision
or accuracy information is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 183; Publicaton No. 77-157-A, U.S. DHEW:
Cincinnati, 1977.
B-611
-------
COST INFORMATION:
Cost information has not been obtained.
B-612
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 6
Compound CAS Number
Benzofa]anthracene 56-55-3
Benzo[k]fluoranthene 207-08-9
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Fluoranthene 206-44-0
Pyrene 129-00-0
METHOD SUMMARY:
The above polycyclic aromatic hydrocarbons in air samples may be measured
spectrophotometrically. The analyte is collected on a filter and extracted
with benzene. The hydrocarbons are separated on an alumina column with a
n-pentanediethyl ether mixture as eluting solvent. The collected fractions
are analyzed by UV spectrophotometry.
INTERFERENCES:
Any substance that hinders the separation or absorbs radiation at the same
wavelengths as the analytes will interfere.
QUALITY CONTROL:
The recovery should be determined, and a blank should be processed with
each group of samples. The recovery and the value of the blank should be used
in the calculation of the results.
EPA/TECHNICAL STATUS:
This method has been classified as operational by the National Institute
of Occupational Safety and Health (NIOSH) for use over the range of 0 to 3
milligrams of benzene-soluble polycyclic aromatic hydrocarbons per cubic meter.
Precision or accuracy information is not furnished.
PFERENCE :
U.S. Department of Health, Education and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 184; Publicaton No.77-157-A, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $90-105
(list), plus sampling costs.
B-613
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 7
Compound CAS Number
Benzo[a]anthracene 56-55-3
Benzo[b]fluoranthene 205-99-2
Benzofkjfluoranthene 207-08-9
Benzo[a]pyrene 50-32-8
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Dibenzo[a,h]anthracene 53-70-3
Dibenzo[a,i]pyrene 189-55-9
Fluoranthene 206-44-0
lndeno[l,2,3-cd]pyrene 193-39-5
Phenanthrene 85-01-8
Pyrene 129-00-0
METHOD SUMMARY:
The above polycyclic aromatic hydrocarbons In particulate air samples can
be measured by liquid chromatography (LC). Samples are collected in a specially
designed baghouse. An aliquot of the collected particulates is Soxhlet-extracted
with methylene chloride. Sample cleanup involves concentration, solvent exchangq
to cyclohexane, liquid-liquid partition between cyclohexane and nitromethane,
and a final concentration step. Analysis is by LC with fluorescence wavelength
programming. Also described are a gas chromatographic method and a sequential
(reversed-phase) LC method, with specific sample extraction and cleanup pro-
cedures for each.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Internal standards are specified.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
May, W. E.; Wise, S. A. "Liquid Chromatographic Determination of Polycyclic
Aromatic Hydrocarbons in Air Particulate Extracts," Anal. Chem., 56, 1984, pp.
225-232.
B-614
-------
COST INFORMATION;
Cost per sample for analysis by this method is approximately $195 (list),
plus sampling costs.
B-615
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Air Samples
Laboratory Method 8
Compound CAS Number
Acenaphthene 83-32-9
Anthracene 120-12-7
Benzo[a]pyrene 50-32-8
Fluorene 86-73-7
METHOD SUMMARY:
The above polycyclic aromatic hydrocarbons in particulate air samples can
be measured by synchronous luminescence spectroscopy. The samples are collected
either in high-volume samplers or on filter papers.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision or accuracy information is
not furnished. The detection limit is approximately 7 micrograms of analyte per
cubic meter of air.
REFERENCE:
Vo-Dinh, T. "New Luminescence Techniques Simplify Air Analysis," InTech,
28,(5), 1981, pp. 45-48.
COST INFORMATION:
Cost information has not been obtained.
B-616
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Soil/Sediment Samples
Laboratory Method 1
Compound CAS Number
Acenaphthene 83-32-9
Acenaphthylene 208-96-8
Anthracene 120-12-7
Benzo[a]anthracene 56-55-3
Benzo[b]fluoranthene 207-08-9
Benzo[k]fluoranthene 205-99-2
Benzo[a]pyrene 50-32-8
Benzo[ghi]perylene 191-24-2
Chrysene 218-01-9
Dibenzo[a,h]anthracene 53-70-3
Dibenzo[a,i]pyrene 189-55-9
Fluorene 86-73-7
Indeno[l,2,3-cd]pyrene 193-39-5
3-Methylcholanthrene 56-49-5
Phenanthrene 85-01-8
pyrene 129-00-0
METHOD SUMMARY:
Analysis of soil/sediment samples for the above polycyclic aromatic hydro
carbons can be performed by gas chromatography. A soil/sediment sample is
Soxhlet-extracted or sonicated at neutral pH with dichloromethane, and the
extract is dried, concentrated, and analyzed by gas chromatography with flame
ionization detection (GC/FID), using internal or external standards for quanti
fication. Confirmation of compound identification can be accomplished by gas
chromatography/mass spectrometry (GC/MS).
INTERFERENCES:
A silica-gel column cleanup procedure may be required to eliminate inter-
ferences, and some samples may require further cleanup procedures.
QUALITY CONTROL:
ssrisrs ,
Field and laboratory replicates, fortified
should be processed to ascertain 'he precision an c cu racy
°
cases where doubt exists .regarding the ^J^°^hy?maB8 spectrometry
gram, confirmatory techniques, such as gas cnromaLug v
(GC/MS) and secondcolumn confirmation, should be used.
B-617
-------
EPA/TECHNICAL STATUS;
This method is EPA-approved for analyses under the Resource Conservation
and Recovery Act (RCRA). No precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, Method 610; EPA 600/4-82-057, U.S. EPA:
Washington, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste;
Physical/Chemical Methods, 2nd ed., Methods 3540, 3550, 8100, 8310;
SW-846, U.S. EPA: Washington, 1982.
U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures
Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-14, "Determination
of Polynuclear Aromatic Hydrocarbons in Sediments;" HASL-300, Environmental
Measurements Laboratory, U.S. DOE: New York, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $120 (list);
the cost of a silica-gel column cleanup is approximately $25-35 (list).
B-618
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Soil/Sediment Samples
Laboratory Method 2
Compound CAS Number
Acenaphthene 83-32-9
Anthracene 120-12-7
Dibenz[a,h]anthracene 53-70-3
7,12-Dimethyl-
benz[a]anthracene 57-97-6
Fluorene 86-73-7
Naphthalene 91-20-3
Phenanthrene 85-01-8
METHOD SUMMARY:
Analysis for the above fluorescent organic compounds in soil/sediment
samples can be performed by gas chromatography (GC) with fluorescence detection.
A flame photometric detector is modified with quartz fiber optics to achieve
the necessary instrumental configuraion.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. The analytical technique has a sub-nanogram sensitivity and high
selectivity. Limits of detection are provided.
REFERENCE:
Thomas, L. C.; Adams, A. K. "Detection of Fluorescent Compounds by Modified
Flame Photometric Gas Chromatography Detectors," Anal. Chem. , 54/14), 1982, pp.
2597-2599.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $135-180
(list).
B-619
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Soil/Sediment Samples
Laboratory Method 3
Compound CAS Number
Anthracene 120-12-7
Benzo[a]anthracene 56-55-3
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Fluoranthene 206-44-0
Fluorene 86-73-7
Phenanthrene 85-01-8
Pyrene 129-00-0
METHOD SUMMARY:
The above polycycllc aromatic hydrocarbons in sediment samples may be
measured by gas chromatography- The wet sample is dewatered by washing with
raethanol and then extracted with methylene chloride/methanol (2:1) using a
ball-mill tumbler or a shaker table. The extracts and methanol washes are
combined and filtered into a separatory funnel. The methanol is partitioned
into water. The methanol/water solution is extracted into methylene chloride.
The extracts are filtered, then separated into saturated and unsaturated hydro-
carbons by silica gel adsorption chromatography, and the resulting solutions
are analyzed by gas chromatography with flame ionization detection (GC/FID)
using a capillary column.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Recovery internal standards should be added and the results used in
calculations. A reagent blank, reagent spike, GC internal standard, and GC
calibration standard should also be used.
EPA/TECHNICAL STATUS:
This method is not EPA-approved and has no status as an ASTM standard
method. Individual hydrocarbons can be quantified in the parts-per-billion
range. Precision information is furnished.
REFERENCE:
American Society for Testing and Materials, "Proposed Test Method for Hydro-
carbons in Marine Sediments," 1983 Annual Book of ASTM Standards, Vol. 11.02,
(no method number), ASTM: Philadelphia, 1983, pp. 963-969.
B-620
-------
COST INFORMATION:
(list)
Cost per sample for analysis by this method is approximately $150-195
.).
B-621
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Soil/Sediment Samples
Laboratory Method 4
Method
Detection
Compound CAS Number Limit (pg/1)
Acenaphthene 83-32-9 1.8
Acenaphthylene 208-96-8 2.3
Anthracene 120-12-7 0.66
Benzo[a]anthracene 56-55-3 0.013
Benzo[b]fluoranthene 205-99-2 0.018
Benzo[k]fluoranthene 207-08-9 0.017
Benzo[ghi]perylene 191-24-2 0.076
Benzo[a]pyrene 50-32-8 0.023
Chrysene 218-01-9 0.15
Dibenz[a,h]anthracene 53-70-3 0.030
Fluoranthene 206-44-0 0.21
Fluorene 86-73-7 0.21
Indeno[1,2,3-cd]
pyrene 193-39-5 0.043
Naphthalene 91-20-3 1.8
Phenanthrene 85-01-8 0.64
Pyrene 129-00-0 0.27
METHOD SUMMARY;
Analysis of soil/sediment samples for the above polycyclic aromatic hydro-
carbon compounds (PAHs) can be performed by high-performance liquid chromatography
(HPLC). A 10- to 100-gram sample is spiked with a radiolabeled PAH and refluxed
with ethanolic potassium hydroxide. The resulting solution is centrifuged, the
liquid is extracted with isooctane, and the isooctane solution is concentrated
by evaporation. The solution is solvent-exchanged into toluene and the toluene
solution is cleaned up by Florisil column chromatography, dimethyl sulfoxide
partitioning and Sephadex LH-20 chromatography. The cleaned extract is then
analyzed by HPLC with ultraviolet absorbance and fluorescence detection.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Recovery of radiolabeled PAH compounds should be measured and sample results
corrected accordingly.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
B-622
-------
REFERENCES;
Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Sediment
Samples for Polycyclic Aromatic Hydrocarbons," pp. III-395 to III-401: EPA-
600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas, 1984.
Dunn, B. P.; Armour R. J. "Sample Extraction and Purification for Determina-
tion of Polycyclic Aromatic Hydrocarbons by Reversed-Phase Chromatography"
Anal. Chem.. Vol. 52, No. 13 (1980), pp. 2027-2031.
COST INFORMATION:
Cost information has not been obtained.
B-623
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Water Samples
Laboratory Method 1
Method
Detection
Compound CAS Number Limit (ug/1)
Acenaphthene 83-32-9 1.8
Acenaphthylene 208-96-8 2.3
Anthracene 120-12-7 0.66
Benzo[a]anthracene 56-55-3 0.013
Benzo[b]fluoranthene 205-99-2 0.018
Benzo[k]fluoranthene 207-08-9 0.017
Benzo[ghi]perylene 191-24-2 0.076
Benzo[a]pyrene 50-32-8 0.023
Chrysene 218-01-9 0.15
Dibenz[a,h]anthracene 53-70-3 0.030
Fluoranthene 206-44-0 0.21
Fluorene 86-73-7 0.21
Indeno[l,2,3-cd]
pyrene 193-39-5 0.043
Naphthalene 91-20-3 1.8
Phenanthrene 85-01-8 0.64
Pyrene 129-00-0 0.27
METHOD SUMMARY:
Analysis of water samples for the above polycyclic aromatic hydrocarbons
can be performed by high-performance liquid chromatography (HPLC). A one-liter
sample is extracted with methylene chloride, the extract solution is concentrated,
and the solvent is exchanged into cyclohexane. An optional silica-gel cleanup
procedure removes high levels of interferences. The solvent is then exchanged
into acetonitrile and the resulting solution is analyzed by gradient reverse-phase
HPLC with ultraviolet absorbance and fluorescent detection.
INTERFERENCES:
Other polycyclic aromatic compounds besides those listed may interfere.
QUALITY CONTROL:
A minimum of ten percent of all samples should be fortified and analyzed
in duplicate.
EPA/TECHNICAL STATUS:
This method is EPA-approved for Clean Water Act analyses. Precision and
accuracy information is furnished.
B-624
-------
REFERENCES:
U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater. Method 610; EPA 600/4-82-057, U.S. EPA:
Cincinnati, 1982.
Plumb, R- H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol.
Ill, Available Laboratory Analytical Methods, " Analysis for Polycyclic Aromatic
Hydrocarbons in Water Samples," pp. III-386 to III-394, EPA-600/S4-84-038, U.S.
Environmental Protection Agency: Las Vegas, 1984.
U.S. Geological Survey, Methods for the Determination of Organic Substanes in
Water and Fluvial Sediment, Book 5, "Laboratory Analysis," Chpater A3; USGS:
Denver, Open-File Report 82-1004, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $175-255
(list).
B-625
-------
POLYCYLIC AROMATIC HYDROCARBONS
Water Samples
Laboratory Method 2
Compound CAS Number
Acenaphthene 83-32-9
Acenaphthylene 208-96-8
Anthracene 120-12-7
Benzo[a]anthracene 56-55-3
Benzofbjfluoranthene 205-99-2
Benzo[k]fluoranthene 207-08-9
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Dibenz[a,h]anthracene 53-70-3
Dibenz[a,i]pyrene 189-55-9
Fluoranthene 206-44-0
Fluorene 86-73-7
Indeno[l,2,3-cd]
pyrene 193-39-5
3-Methylcholanthrene 56-49-5
Phenanthrene 85-01-8
Pyrene 129-00-0
METHOD SUMMARY:
Water samples can be analyzed for the above polycyclic aromatic hydro-
carbons by gas chromatography. A water sample is Soxhlet- or ultrasonically
extracted at neutral pH with dichloromethane, and the extract is dried, con-
centrated and analyzed by gas chromatography with flame ionization detection
(GC/FID), using internal or external standards.
INTERFERENCES:
A silica-gel column cleanup procedure may be required to eliminate inter-
ferences, and some samples may require further cleanup procedures.
QUALITY CONTROL:
An aliquot of each sample is spiked with standards and analyzed to deter-
mine recovery and sensitivity. The gas chromatographic system must be demon-
strated to be free of interferences by the analysis of a method blank with each
set of samples or each change in reagents. Field and laboratory replicates,
fortified samples, and duplicate samples should be processed to ascertain the
precision and accuracy of the method. In cases where some doubt exists regard-
ing the identification of peaks in the chromatogram, confirmatory techniques,
such as gas chromatography/mass spectrometry (GC/MS) and second-column confirm-
ation, should be used.
B-626
-------
EPA/TECHNICAL STATUS:
This method is EPA-approved for the Resource Conservation and Recovery Act
(RCRA) sample analyses. No precision or accuracy information is furnished.
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. 2nd ed., Methods 3510, 3520, 8100, 8130; SW-846,
U.S. EPA: Washington, July 1982.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $110-120
(list); the cost of a silica-gel column cleanup is approximately $25-35 (list).
B-627
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Water Samples
Laboratory Method 3
Compound CAS Number
Acenaphthene 83-32-9
Anthracene 120-12-7
Dibenz[a,h]anthracene 53-70-3
7,12-Diraethyl-
benz[a]anthracene 57-97-6
Fluorene 86-73-7
Naphthalene 91-20-3
Phenanthrene 85-01-8
METHOD SUMMARY:
Analysis of water samples for the above polycyclic aromatic hydrocarbons
can be performed by extraction and gas chromatography (GC) with fluorescence
detection. A flame photometric detector is modified with quartz fiber optics
to achieve the necessary instrumental configuration.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. The analytical technique has a sub-
nanogram sensitivity and high selectivity. No precision or accuracy informa-
tion is furnished. Limits of detection are provided.
REFERENCE:
Thomas, L. C.; Adams, A. K. "Detection of Fluorescent Compounds by Modified
Flame Photometric Gas Chromatography Detectors," Anal. Chem., 54_(14), 1982, pp.
2597-2599.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $125-135
(list).
B-628
-------
POLYCYCLIC AROMATIC HYDROCARBONS
Water Samples
Laboratory Method 4
Compound CAS Number
Benzo[a]anthracene 56-55-3
Benzo[b]fluoranthene 205-99-2
Benzo[k]fluoranthene 207-08-9
Benzo[ghi]perylene 191-24-2
Benzo[a]pyrene 50-32-8
Chrysene 218-01-9
Dibenz[a,h]anthracene 53-70-3
7,12-Dimethylbenz[a]anthracene 57-97-6
Fluoranthene 206-44-0
3-Methylcholanthrene 56-49-5
Pyrene 129-00-0
METHOD SUMMARY:
Analysis of water for the above polycyclic aromatic hydrocarbons can be
performed by extraction of a 3-liter sample with methylene chloride, solvent-
exchange into isoocatane, and analysis of the resulting solution by high-
performance liquid chromatography (HPLC) with ultraviolet absorbance and/or
fluorescence detection, by gas chromatography with flame-ionization detection
(GC/F1D), or by gas chromatography with peak-trapping followed by ultraviolet
spectrophotometric analysis of the individual peaks.
INTERFERENCES:
Extensive sample cleanup is usually not required, but the isooctane
extract may be extracted with phosphoric acid in dimethylsulfoxide, and the
resulting solution may be purified by column chromatography.
QUALITY CONTROL:
When doubt exists regarding the identification of peaks in the chromato-
gram, detection at two wavelengths or gas chromatography/mass spectroraetry
(GC/MS) can be used to confirm tentative identifications.
EPA/TECHNICAL STATUS:
The method is not EPA-approved. The method can measure levels above
approximately 1 micrograra per liter. Precision and accuracy information is
furnished.
REFERENCES:
Thomas, R. S.; Lao, R. C.; Wang, D. T.; Robinson, D.; Sakuma, T. In Carcino-
genesis. Vol. 3; Polynuclear Aromatic Hydrocarbons, P- W. Jones and
R- I. Freudenthal, Eds.; Raven Press: New York, 1978, pp. 9-19.
B-629
-------
McElroy, F. C.; Searl, T. D.; Brown R. A. In Trace Organic Analysis; A New
Frontier in Analytical Chemistry, National Bureau of Standards Special Publica-
tion 519, 1978, pp. 7-18.
Das, B. S.; Thomas, G. H. In Trace Organic Analysis: A New Frontier in
Analytical Chemistry, National Bureau of Standards Special Publication 519,
1978, pp. 41-56.
COST INFORMATION:
Cost per sample for analysis by the HPLC method is approximately $155-175
(list); by GC/FID, approximately $115 (list). Cost information for the UV
spectrometry peak-trapping method has not been obtained.
B-630
-------
PRIMARY AND SECONDARY AMINES
Soil/Sediment Samples
Laboratory Method
Compound CAS Number
Diethylamine 109-89-7
Dimethylamine 124-40-3
Dipropylamine 142-84-7
Ethylenediamine 107-15-3
Monoethylamine 75-04-7
Monomethylamine 74-89-2
n-Propylamine 107-10-8
METHOD SUMMARY:
Analysis of soil/sediment samples for the above primary and secondary
amines can be performed by distillation of a mixture of a 10-gram sample, 70
milliliters of 50-percent sodium hydroxide, and 100 milliliters of water,
followed by formation of the pentafluorobenzoyl derivatives of the amines in the
distillate, and analysis of the resulting solution by gas chromatography with a
nitrogen/phosphorus detector (GC/NPD). Analysis of the extract can also be
performed by gas chromatography/mass spectrometry (GC/MS).
INTERFERENCES:
Excess derivatizing agent should be used, and chlorinated solvents can
cause a reversible loss of sensitivity in the detector.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved and has not undergone interlaboratory
evaluation. The method is sensitive to levels over 1 milligram per gram.
No precision or accuracy information is furnished.
REFERENCE:
Ripley, B. D.; French, B. J.; Edgington, L. V. "Gas Chromatographic Determina-
tion of Primary and Secondary Amines as Pentafluorobenzamide Derivatives," J.
Assoc. Off. Anal. Chem.. 65(5), 1982, pp. 1066-1072.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $158-180
(list).
B-631
-------
PRIMARY AND SECONDARY AMINES
Water Samples
Laboratory Method
Compound CAS Number
Diethylamine 109-89-7
Dimethylamine 124-40-3
Dipropylamine 142-84-7
Ethylenediamine 107-15-3
Monoethylamine 75-04-7
Monomethylamine 74-89-2
n-Propylamine 107-10-8
METHOD SUMMARY:
Analysis of water samples for the above primary and secondary amines can
be performed by alkaline distillation of a 100-milliliter sample, followed by
formation of the pentafluorobenzoyl derivatives of the amines in the distillate,
and analysis of the resulting solution by gas chromatography with a nitrogen/phos
phorus detector (GC/NPD). Analysis of the extract can also be performed by gas
chromatography/mass spectrometry (GC/MS).
INTERFERENCES;
Excess derivatizing agent should be used, and chlorinated solvents can
cause a reversible loss of sensitivity in the detector.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved and has not undergone interlaboratory
evaluation. The method is sensitive to levels over 1 milligram per liter of
sample. No precision or accuracy information is furnished.
REFERENCE:
Ripley, B. D.; French, B. J.; Edgington, L. V. "Gas Chromatographic Determina-
tion of Primary and Secondary Amines as Pentafluorobenzamide Derivatives," J.
Assoc. Off. Anal. Chem., 6X5), 1982, pp. 1066-1072.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $158-180
(list).
B-632
-------
SUBSTITUTED NITRILES AND TETRANITROMETHANE
Water Samples
Laboratory Method
Compound CAS Number
Acetone Cyanohydrin 75-86-5
Cyanogen Bromide 506-68-3
Propanedinitrile 109-77-3
Tetranitromethane 509-14-8
METHOD SUMMARY:
Analysis for the above compounds in water samples can be performed
by chemiluminescence. A sample is made alkaline and treated with hydrogen
peroxide and luminol. The resulting chemiluminescence is monitored by a
spectrofluorimeter. This method does not identify any specific compound, but
gives a positive response for any substance that is chemiluminescent after the
above treatment.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished. Relative intensities of chemiluminescence are provided.
REFERENCE;
Yurow, H. W.; Sass, S. "Detection of Various a-Substituted Nitriles and Gem-
Halonitroalkanes by Chemiluminescence," Anal. Chim. Acta., 77_, 1975, pp.
324-326.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $55-95
(list).
B-633
-------
SULFUR-CONTAINING GASES
Air Samples
Laboratory Method
Compound CAS Number
Hydrogen Sulfide 7783-06-4
Methylmercaptan 74-93-1
METHOD SUMMARY:
The above sulfur-containing compounds in air samples can be measured by
gas chromatography. A Teflon® column and a flame-photometric detector are
used.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. This method is suitable for concentra-
tions in the approximate range of 1.5 to 150 milligrams analyte per cubic
meter. No precision or accuracy information is furnished.
REFERENCE:
de Souza, T. L. C.; Lane, D. C.; Bhatia, S. P- "Analysis of Sulfur-Containing
Gases by Gas-Solid Chromatography on a Specially Treated Porapak QS Column
Packing," Anal. Chem., 47, 1975, pp. 543-545.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $135 (list),
plus sampling costs.
B-634
-------
THIOIC ACID ESTER PESTICIDES
Water Samples
Laboratory Method
Compound CAS Number
Diuron 330-54-1
Methomyl 16752-77-5
METHOD SUMMARY:
Analysis of water samples for diuron and methomyl can be performed by
reverse-phase high-performance liquid chromatography (HPLC). A water sample is
serially extracted with three 60-milliliter portions of methylene chloride,
the extract is solvent-exchanged into one milliliter of acetonitrile, and the
resulting acetonitrile solution is analyzed by gradient-elution HPLC with UV
detection at 254 nm. Additional sample cleanup, for samples with solids or
high levels of interferences, can be performed before analysis by use of a
SEP-PAK® cartridge.
INTERFERENCES:
Methomyl undergoes hydrolysis at high pH; sample pH should be adjusted to
6 to 8 within four hours of sampling, and the samples should be kept refrigerated.
QUALITY CONTROL;
A minimum of ten percent of all analyses should be fortified samples.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Environmental Protection Agency, Test Methods for Nonconventional Pesticides
Chemicals Analysis of Industrial and Municipal Wastewater. Method 109; EPA
440/1-83/079-C, U.S. EPA: Cincinnati, 1983, PB 83176636.
E.I. duPont de Nemours & Co, Inc, "Determination of Houston Plant Pesticides,
High Performance Liquid Chromatography (HPLC) Methods," Method W28.303(R);
Houston, Texas, 29 April 1980.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $140-205
(list).
B-635
-------
THIOUREAS AND OTHER COMPOUNDS
Soil/Sediment Samples
Laboratory Method
Compound
N-Nitroso-N-
methylurea
N-Phenylthiourea
Thioacetamide
Thiosemicarbazide
Thiourea
Trypan Blue
CAS Number
684-93-5
103-85-5
62-55-5
79-19-6
62-56-6
72-57-1
Compound CAS Number
l-Acetyl-2-thiourea 591-08-2
Azaserine 115-02-6
l-(o-Chlorophenyl) 5344-82-1
thiourea
Crotonaldehyde 123-73-9
4170-30-3
Diethylstilbestrol 56-53-1
Epinephrine 51-43-4
Ethylenethiourea 96-45-7
a-Naphthylthiourea 86-88-4
METHOD SUMMARY:
Analysis of soil/sediment samples for the above thioureas and other com-
pounds can be performed by extraction and high-performance liquid chromatography
(HPLC). The sample is extracted with diethyl ether and analyzed by reverse-
phase HPLC with UV detection at 254 nm, using an acetonitrile/water mobile
phase.
INTERFERENCES;
No specific interferences are reported.
QUALITY CONTROL:
A method blank should be processed with each set of samples or each change
in operating conditions or sample matrix. Field and laboratory replicates and
fortified samples should be analyzed.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Method 8330; SW-846, U.S. EPA: Washington,
1982.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130-205
(list).
B-636
-------
TRACE ORGANIC CONTAMINANTS
Water Samples
Laboratory Method
Compound
Acenaphthene
Acetophenone
Anthracene
Benzole Acid
Benzonitrile
Benzyl Chloride
Bis(2-ethyhexyl)
Phthalate
Chlorobenzene
2-Chlorophenol
o-Cresol
Cumene
1,2-Dichlorobenzene
METHOD SUMMARY:
CAS Number
83-32-9
98-86-2
120-12-7
65-85-0
100-47-0
100-44-7
117-81-7
108-90-7
95-57-8
95-48-7
98-82-8
95-50-1
Compound
CAS Number
1,4-Dichlorobenzene 106-46-7
Diethyl Phthalate 84-66-2
Dimethyl Phthalate 131-11-3
Ethylbenzene 100-41-4
Fluorene 86-73-7
Methyl Methacrylate 80-62-6
Naphthalene 91-20-3
Nitrobenzene 98-95-3
Phenol 108-95-2
Quinoline 91-22-5
1,2,4,5-Tetrachlorobenzene 95-94-3
2,4,6-Trichlorophenol 88-06-2
Analysis of water samples for the above organic compounds can be performed
by gas chromatography. The organic compounds can be concentrated by sorption
on a small column of macroreticular resin and eluted; the eluate can then be
concentrated and analyzed by gas chroraatography with flame-ionization detection
(GC/FID). A 1-liter sample is passed through a column of XAD resin at 30 to 50
milliliters per minute, and the resin is eluted with diethyl ether. The ether
solution is dried, concentrated, and analyzed by GC/FID. Gas chromatography/
mass spectrometry (GC/MS) can be used for identity confirmation.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE:
Junk, G. A.; Richard, J. J.; Grieser, M. D.; Witiak, D.; Witiak, J. L.;
Arguello, M. D.; Vick, R.; Svec, H. J.: Fritz, J. S.; Calder, G. V. "Use of
Macroreticular Resins in the Analysis of Water For Trace Organic Contaminants,"
Ji Chromatogr.. 99. 1974, pp. 745-762.
B-637
-------
COST INFORMATION;
Cost per sample for analysis by this method is approximately $110 (list);
the cost of GC/MS confirmation is approximately $150-200 (list).
B-638
-------
VOLATILE ALCOHOLS AND OTHER ORGANIC COMPOUNDS
Water Samples
Laboratory Method
Compound
Acetaldehyde
Acetone
Acetonitrile
Acetophenone
Acrylonitrile
Benzene
Bis(2-Chloroethyl) Ether
Butyl Acetate
iso-Butyl Acetate
sec-Butyl Acetate
tert-Butyl Acetate
Crotonaldehyde
1,2-Dichloroethane
1,2-Dichloropropane
METHOD SUMMARY:
CAS Number Compound CAS Number
75-07-0 1,4-Dioxane 123-91-1
67-64-1 Epichlorohydrin 106-89-8
75-05-8 Ethyl Acetate 141-78-6
98-86-2 Ethylbenzene 100-41-4
107-13-1 Ethylene Oxide 75-21-8
71-43-2 Isophorone 78-59-1
111-44-4 Methanol 67-56-1
123-86-4 Methyl Ethyl Ketone 78-93-3
110-19-0 Methyl Isobutyl Ketone 108-10-1
105-46-4 Paraldehyde 123-63-7
540-88-5 2-Picoline 109-06-8
123-73-9 Propylene Oxide 75-56-9
4170-30-3 Toluene 108-88-3
107-06-2 Vinyl Acetate 108-05-4
78-87-5 ^-Xylene 106-42-3
Analysis of water samples for the above alcohols and other volatile com-
pounds can be performed by gas chromatography with flame ionization detection
(GC/FID). The method involves direct injection of 10 microliters of sample.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
The method may not be suitable for simultaneous analysis for organic
compounds with similar functionalities, and the qualitative identification of
peaks in the chromatogram should be confirmed by a multicolumn approach or
other techniques.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method has undergone interlaboratory
evaluation for samples containing only alcohols under the American Society for
Testing and Materials. Precision and accuracy information is furnished.
REFERENCES:
American Society for Testing and Materials, Annual Book of ASTM Standards, Part
31, Water; ASTM: Philadelphia, 1978, pp. 834-838, pp. 672-680.
B-639
-------
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D 2908-74 (1980), D 3695-78; ASTM: Philadelphia, 1983, pp. 50-58,
241-248.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-80
(list).
B-640
-------
VOLATILE CARBONYL COMPOUNDS
Water Samples
Laboratory Method
Compound CAS Number
Acetaldehyde 75-07-0
Acetone 67-64-1
Acrolein 107-02-8
Crotonaldehyde 123-73-9
4170-30-3
Formaldehyde 50-00-0
Furfural 98-01-1
Methyl Ethyl Ketone 78-93-3
Methyl Isobutyl Ketone 108-10-1
METHOD SUMMARY:
Analysis for the above low-molecular-weight carbonyl compounds can be
performed by derivatization and gas chromatography. A sample containing
approximately 0.5 millimoles of carbonyl compounds is added to a solution of
pentafluorophenylhydrazine in methanol and allowed to stand overnight. The
resulting solution is then analyzed by gas chromatography with electron capture
detection (GC/ECD).
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method can detect amounts of
derivatives of about 0.01 nanograms and above. No precision or accuracy
information is furnished.
REFERENCE;
Hoshika, Y.; Muto, G. "Sensitive Gas Chromatographic Determination of Lower
Aliphatic Carbonyl Compounds as their Pentaf luorophenylhydrazones," J_.
Chromatogr., 152, 1978, pp. 224-227.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $90-105
(list).
B-641
-------
VOLATILE CHLORINATED ALIPHATIC HYDROCARBONS
Water Samples
Laboratory Method
Compound CAS Number
Carbon Tetrachloride 56-23-5
Chloroform 67-66-3
Hexachlorobutadiene 87-68-3
Hexachloroethane 67-72-1
Pentachloroethane 76-01-7
1,1,1,2-Tetrachloroethane 630-20-6
1,1,2,2-Tetrachloroethane 79-34-5
Tetrachloroethylene 127-18-4
1,1,1-Trichloroethane 71-55-6
Trichloroethylene 79-01-6
METHOD SUMMARY:
The above volatile chlorinated aliphatic hydrocarbons in water samples can
be measured using gas chromatography with electron capture detection (GC/ECD).
The water sample is extracted with n-pentane; the extract is dried with anhy-
drous sodium sulfate and analyzed by temperature-programmed GC/ECD.
INTERFERENCES;
Chlorobromomethanes and laboratory contaminants may interfere; however,
the method provides instrumental conditions to minimize their effects.
QUALITY CONTROL;
Standard solutions should be freshly prepared each week.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
method is suitable for concentrations of 0.01 to 10 micrograms per liter.
REFERENCE:
Deetman, A. A.; Demeulemeester, P-; Garcia, M.; Hauck, G.; Hollies, J. I.;
Krockenberger, D.; Palin, D. E.; Prigge, H. ; RohrSchneider, L.; Schmidhammer,
L. "Standardization of Methods for the Determination of Traces of Some Volatile
Chrorinated Aliphatic Hydrocarbons in Air and Water by Gas Chromatography"
Anal. Chim. Acta., 82^, 1976, pp. 1-17.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $100-145
(list).
B-642
-------
VOLATILE ORGANIC ACIDS
Water Samples
Laboratory Method
Compound CAS Number
Acetic Acid 64-19-7
Butyric Acid 107-92-6
iso-Butyric Acid 79-31-2
Propionic Acid 79-09-4
METHOD SUMMARY:
Analysis of water samples for the above volatile organic acids can be
performed by gas chromatography. A 10-milliliter sample is mixed with solid
metaphosphoric acid and centrifuged to remove suspended solids. The superna-
tant is then analyzed by gas chromatography with flame ionization detection
(GC/FID).
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL;
Standard addition methods may be required. No other quality control
procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision and accuracy information is
furnished.
REFERENCE;
Narkis, N. ; Henfeld-Furie, S. "Direct Analytical Procedure for Determination
of Volatile Organic Acids in Raw Municipal Wastewater," Water Research, 12,
1978, pp. 437-446.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $70-80
(list).
B-643
-------
VOLATILE ORGANIC COMPOUNDS
Air Samples
Laboratory Method 1
Compound CAS Number
Acetic Acid 64-19-7
Acetone 67-64-1
Benzene 71-43-2
Butyl Acetate 123-86-4
Butyric Acid 107-92-6
^so-Butyric Acid 79-31-2
Ethyl Acetate 141-78-6
Methyl Ethyl Ketone 78-93-3
Propionic Acid 79-09-4
Styrene 100-42-5
Toluene 108-88-3
Xylene 1330-20-7
m-Xylene 108-38-3
£-Xylene 95-47-6
p-Xylene 106-42-3
METHOD SUMMARY:
Analysis for the above volatile organics in air is performed by passage of
0.75 to 2 liters of air through a Tenax® sampling cartridge, followed by
thermal desorption of the analytes into a temperature-programmed gas chromato-
graph with flame ionization detection (GC/FID). Sampling cartridges should be
conditioned at 200°C for at least 2 hours before use.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
In case of uncertainty about the identification of peaks, gas chromato-
graphy/mass spectrometry (GC/MS) or second-column techniques should be used for
confirmation. A fortified sample should be analyzed and standards should be
analyzed in triplicate.
EPA/TECHNICAL STATUS;
This method is used by Environment Canada, but is not EPA-approved. No
precision or accuracy information is furnished. The detection limit for most
of the compounds is 4 micrograms per cubic meter.
B-644
-------
REFERENCES;
Alberta Environmental Centre, Methods Manual for Chemical Analysis of
Atmospheric Pollutants; N.C. Das, Ed., Method 17070; Alberta Environmental
Centre: Vegreville, Alberta, Canada, 1981.
Holzer, G.; Shanfield, H. ; Zlatkis, A.; Bertsch, W.; Juarez, P.; Mayfield, H.;
Liebich, H. M. "Collection and Analysis of Trace Organic Emissions from Natural
Sources," J_. Chromatogr., 142, 1977, pp. 755-764.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $60-80
(list), plus sampling costs.
B-645
-------
Compound
Acetic Acid
Acetone
Benzene
Butyl Acetate
Butyric Acid
iso-Butyric Acid
Carbon Tetrachloride
Chlorobenzene
Chloroform
Dichlorobenzene (Mixed)
1,1-Dichloroethane
1,2-Dichloroe thane
Dichloropropane
1,3-Dichloropropene
Ethyl Acetate
Hexachlorobutadiene
Methyl Ethyl Ketone
METHOD SUMMARY:
VOLATILE ORGANIC COMPOUNDS
Air Samples
Laboratory Method 2
CAS Number Compound CAS Number
64-19-7 Methyl Isobutyl Ketone 108-10-1
67-64-1 Pentachlorobenzene 608-93-5
71-43-2 Propionic Acid 79-09-4
123-86-4 Styrene 100-42-5
107-92-6 1,1,2,2-Tetrachloroethane 79-34-5
79-31-2 Tetrachloroethylene 127-18-4
56-23-5 Toluene 108-88-3
108-90-7 1,1,1-Trichloroethane 71-55-6
67-66-3 1,1,2-Trichloroethane 79-00-5
25321-22-6 Trichloroethylene 79-01-6
75-34-3 Vinyl Acetate 108-05-4
107-06-2 Vinyl Chloride 75-01-4
26638-19-7 Xylene 1330-20-7
542-75-6 m-Xylene 108-38-3
141-78-6 _o-Xylene 95-47-6
87-68-3 £-Xylene 106-42-3
78-93-3
Analysis of air for the above volatile organic compounds can be performed
by gas chromatography/mass spectrometry (GC/MS). A known volume of air is
sampled through a Tenax® GC cartridge, the cartridge is thermally desorbed, and
the analytes are collected in a liquid-nitrogen-cooled nickel capillary trap
and introduced into a gas chromatograph for analysis by GC/MS.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are provided.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision and accuracy information is
furnished. The estimated detection limits (nanograms per cubic meter) for the
following compounds are: benzene, 100; carbon tetrachloride, 250; chloro-
benzene, 2.10; chloroform, 200; 1,2-dichloroethane, 32; tetrachloroethylene,
2.5; 1,1,1-trichloroethane, 66; trichloroethylene, 10; and tetrachlorethylene
2.5.
B-646
-------
REFERENCES;
Plumb, R. H. Characterization of Hazarodous Waste Sites; A Methods Manual,
Vol. III> Available Laboratory Analytical Methods, "Analysis of Air Samples for
Volatile Organics," pp. 111-46 to 111-55; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
Pellizzari, E. D. "Analysis for Organic Vapor Emissions near Industrial and
Chemical Waste Disposal Sites," Environ. Sci. Technol., J^(ll), 1982, pp. 781-
785.
Krost, K. J.; Pellizzari, E. D. ; Walburn, S. G. ; Hubbard, S. A. "Collection
and Analysis of Hazardous Organic Emissions," Anal. Chem., J>4(4), 1982, pp.
810-817.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $150-325
(list).
B-647
-------
Compound
Acetone
Acrolein
Acrylonitrile
Benzene
Bromoform
Carbon Disulfide
Carbon Tetrachloride
Chlorobenzene
Chlorodibromomethane
Chloroethane
2-Chloroethyl Vinyl Ether
Chloroform
Dichlorobromomethane
Dichlorodifluoromethane
1,1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethylene
1,2-trans-Dichloroethylene
Dichloropropane
1,2-Dichloropropane
1,3-Dichloropropene
METHOD SUMMARY:
VOLATILE ORGANIC COMPOUNDS
Soil/Sediment Samples
Laboratory Method
CAS Number Compound
CAS Number
67-64-1 Ethylbenzene 100-41-4
107-02-8 Methyl Bromide 74-83-9
107-13-1 Methyl Chloride 74-87-3
71-43-2 Methylene Chlorine 75-09-2
75-25-2 Methyl Ethyl Ketone 78-93-3
75-15-0 Methyl Isobutyl Ketone 108-10-1
56-23-5 N-Nitrosodi-n-butylamine 924-16-3
108-90-7 !N-Nitrosodiethylamine 55-18-5
124-48-1 N-Nitrosodimethylamine 62-75-9
75-00-3 Styrene 100-42-5
110-75-8 1,1,1,2-Tetrachloroethane 630-20-6
67-66-3 1,1,2,2-Tetrachloroethane 79-34-5
75-27-4 Tetrachloroethylene 127-18-4
75-71-8 Toluene 108-88-3
75-34-3 1,1,1-Trichloroethane 71-55-6
107-06-2 1,1,2-Trichloroethane 79-00-5
75-35-4 Trichloroethylene 79-01-6
156-60-5 Trichloromonofluoromethane 75-69-4
26638-19-7 Vinyl Acetate 108-05-4
78-87-5 Vinyl Chloride 75-01-4
542-75-6 o-Xylene 95-47-6
Analysis for the above volatile organic compounds in soil/sediment samples
can be performed by gas chromatography. A 3-gram sample of solid waste is
extracted with hexadecane and screened by gas chromatography with flame ioniza-
tion detection (GC/FID). If screening results are positive, another measured
portion of the sample is dispersed in tetraglyme. A portion of the tetraglyme
mixture is combined with water in a specially designed purging chamber, and an
inert gas is bubbled through the solution at ambient temperature to transfer
the volatile organics onto a Tenax® sorbent. The sorbent is then heated and
the desorbed compounds are backflushed into a gas chromatograph/mass spectrom-
eter (GC/MS). If screening results are negative, a 10-gram sample is combined
with 10 milliliters of organic-free water and purged at 55°C onto a Tenax® trap.
The trap is heated and the desorbed compounds are backflushed into the GC/MS.
INTERFERENCES:
The tetraglyme must be free of low-molecular-weight impurities before
use, and peroxide formation should be prevented during storage by the addition
of 2,6-di-tert-butyl-4-methyl phenol. Peroxides may be removed from the tetra-
glyme by passage through an activated alumina column.
B-648
-------
QUALITY CONTROL;
The analytical system must be demonstrated to be free of impurities. Use
of tubing, thread sealant, or components made of plastics other than TFE (e g
Teflon©) must be avoided. Instrumental performance is checked by minimum
detection limit criteria, ongoing monitoring of relative response factors
relative retention times, internal standard response factors, stability of a 3-
point calibration curve, and performance of the gas chromatograph. Specifica-
tions for instrument tuning are given. Analytical performance is monitored by
use of surrogates, duplicate analyses, and fortified samples. Criteria for
surrogate recoveries are given.
EPA/TECHNICAL STATUS:
This method is in use in the CERCLA program and is based on a method in
use in the analyses of samples under the Clean Water Act. No precision or
accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Methods of Organic Chemical Analysis of
Municipal and Industrial Wastewater; J. E. Longbottom, J. J. Lichtenberg, Eds.,
Method 624; EPA 600/4-82-057, U.S. EPA: Cincinnati, 1982.
U.S. Environmental Protection Agency, GC jtcreen, GC/MS Analysis of Organic
Compounds, Exhibit D; Invitation for Bid (Solicitation Number WA 82-A54), U.S.
EPA: Washington, July 16, 1982.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Wastes:
Physical/Chemical Methods, 2nd ed., Method 8240; SW-846, U.S. EPA: Washington,
1982.
Plumb, R. H. Characterization of Hazarodous Waste Sites: A Methods Manual,
Vol. Ill, Available Laboratory Analytical Methods, "Analysis of Air Samples for
Volatile Organics," pp. 111-46 to 111-55; EPA-600/S4-84-038, U.S. Environmental
Protection Agency: Las Vegas, 1984.
Budde, W. L. ; Eichelberger, J. W. An EPA Manual for Organics Analysis Using
Gas Chromatography-Mass Spectrometry, pp. 26-35; EPA-600/8-79-006, U.S.
Environmental Protection Agendy, Cincinnati, 1979.
COST INFORMATION;
Cost per sample for the GC screen is approximately $90-115 (list), $60
(bid); the GC/MS analysis is approximately $170-250 (list), $115 (bid).
B-649
-------
Compound
Acetaldehyde
Acetone
Acrolein
Acrylonitrile
Allyl Alcohol
Allyl Chloride
Amyl Acetate
Benzene
Benzonitrile
Benzyl Chloride
Bromoform
Butyl Acetate
Carbon Bisulfide
Carbon Tetrachloride
Chlorobenzene
Chlorodibromomethane
Chloroethane
2-Chloroethyl Vinyl Ether
Chloroform
Crotonaldehyde
Cyclohexane
Dichlorobromomethane
Dichlorodifluoromethane
1,1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethylene
METHOD SUMMARY:
VOLATILE ORGANIC COMPOUNDS
Water Samples
Laboratory Method
CAS Number Compound CAS Number
75-07-0 1,2-trans-Dichloroethylene 156-60-5
67-64-1 Dichloropropane 26638-19-7
107-02-8 1,2-Dichloropropane 78-87-5
107-13-1 1,3-Dichloropropene 542-75-6
107-18-6 Ethylene Dibromide 106-93-4
107-05-1 Ethylbenzene 100-41-4
628-63-7 Furfural 98-01-1
71-43-2 Isoprene 78-79-5
100-47-0 Methyl Bromide 74-83-9
100-44-7 Methyl Chloride 74-87-3
75-25-2 Methylene Chloride 75-09-2
123-86-4 Methyl Ethyl Ketone 78-93-3
75-15-0 Methyl Methacrylate 80-62-6
56-23-5 Methyl Isobutyl Ketone 108-10-1
108-90-7 N-Nitrosodi-n-butylamine 924-16-3
124-48-1 N-Nitrosodiethylamine 55-18-5
75-00-3 N-Nitrosodimethylamine 62-75-9
110-75-8 Styrene 100-42-5
67-66-3 1,1,1,2-Tetrachloroethane 630-20-6
123-73-9 1,1,2,2-Tetrachloroethane 79-34-5
4170-30-3 Tetrachloroethylene 127-18-4
110-82-7 Toluene 108-88-3
75-27-4 1,1,1-Trichloroethane 71-55-6
75-71-8 1,1,2-Trichloroethane 79-00-5
75-34-3 Trichloroethylene 79-01-6
107-06-2 Trichloromonofluoromethane 75-69-4
75-35-4 Vinyl Acetate 108-05-4
Vinyl Chloride 75-01-4
o-Xylene 95-47-6
Analyses for the above volatile organic compounds in water samples can be
performed by gas chromatography/mass spectrometry (GC/MS). An inert gas is
bubbled through a 5-milliliter sample contained in a specially-designed purging
chamber at ambient temperature. The purgeables are efficiently transferred
from the aqueous phase to the vapor phase. The vapors are swept through a
sorbent column where the purgeables are trapped. After purging is completed,
the sorbent column is heated and backflushed with the inert gas to desorb the
purgeables onto a gas chromatographic column. The gas chromatogaph is
temperature-programmed to separate the purgeables which are then determined
with a mass spectrometer.
B-650
-------
INTERFERENCES;
Inpurities in the purge gas, organic compound out-gassing from the plumb-
ing ahead of the trap, and solvent vapors in the laboratory account for the
majority of contamination problems. The analytical system must be demonstrated
to be free from laboratory contaminants under the conditions of the analysis by
analzying reagent blanks. Samples can be contaminated by diffusion of organics
through the septum seal during storage and handling. Contamination can also
occur whenever high-level and low-level samples are analyzed sequentially.
QUALITY CONTROL;
The vapor is analyzed using multiple internal standards with quantitative
determinations based on the internal standards specified in the protocol. Mass
abundance calibrations, internal standard responses, and retention times must
be monitored daily. The ratio of the response factors of deuterated compounds
to that of non-deuterated ones must be between 0.8 and 1.2. The percent rela-
tive standard deviation for calibration check compounds must be less than 30
percent. A system performance check must be performed to assure that minimum
average response factors are met before the calibration curve is used. The
same check must be performed each 12 hours to assure the quality of the analyti-
cal system. A matrix spike and matrix-spike duplicate must be performed once
for each case of samples, once for every 20 samples of similar concentration
and/or sample matrix, whichever is greater.
EPA/TECHNICAL STATUS:
This method is in use in the CERCLA program and is based on a method in
the Clean Water Act. No precision or accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency, Invitation for Bid, "Organics Analysis,
Multi-Media, Multi-Concentration, GC/MS with Medium Level GC Screen," Solici-
tation Number WA8AA-266; U.S. EPA: Washington, June 15, 1982.
U.S. Environmental Protection Agency, Methods of Organic Chemical Analysis of
Municipal and Industrial Wastewater, J. E. Longbottom, J. J. Lichtenberg, Eds.,
Method 624; EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
COST INFORMATION;
Cost per sample for the GC screen is approximately $90-115 (list); $60
(bid); the cost of the GC/MS analysis is approximately $170-250 (list), $115
(bid).
B-651
-------
VOLATILE ORGANICS
Water Samples
Laboratory Method 1
Compound CAS Number
Acetone 67-64-1
Benzene 71-43-2
Bis(2-chloroethyl) Ether 111-44-4
n-Butyl Alcohol 71-36-4
Chloroform 67-66-3
1,4-Dioxane 123-91-1
Ethyl Ether 60-29-7
Tetrachloroethylene 127-18-4
Tetrahydrofuran 109-99-9
Toluene 108-88-3
Trichloroethylene 79-01-6
Xylene 1330-20-7
METHOD SUMMARY:
The above volatile organics in water samples can be measured by gas
chromatography/mass spectrometry (GC/MS). Samples are stored in refrigerated
125-milliliter zero-headspace glass containers after collection. The volatile
organics are stripped from a 100-milliliter sample in a stirred stripping
flask. The headspace gases are purged with nitrogen, and the volatiles are
removed from the gas stream by passage through an adsorbent column. The vola-
tiles are thermally desorbed from the column material and flushed through a
separate loop into the GC column for temperature-programmed analysis.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision or accuracy information is
not furnished.
REFERENCE:
De Walle, F. B.; Chian, E. S. K. "Detection of Trace Organics in Well Water
Near a Solid Waste Landfill," J. Am. Water Works Assn., April 1981, pp. 206-
211.
B-652
-------
COST INFORMATION;
Cost per sample for analysis by this method is approximately $250-325
(list).
B-653
-------
VOLATILE ORGANICS
Water Samples
Laboratory Method 2
Compound CAS Number
Acetaldehyde 75-07-0
Acetone 67-64-1
Benzene 71-43-2
ii-Butyl Alcohol 71-36-4
Chloroform 67-66-3
Ethyl Acetate 141-78-6
Ethyl Ether 60-29-7
Methanol 67-56-1
Methylene Chloride 75-09-2
Methyl Ethyl Ketone 78-93-3
Toluene 108-88-3
METHOD SUMMARY:
The above volatile organics in water samples can be determined by gas
chromatography with flame ionization detection (GC/FID). The sample is gas-
stripped by passing helium across the water sample, and the organics are
adsorbed onto a sorbent such as Tenax GC and then thermally desorbed into the
GC instrument.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished.
REFERENCE:
Kuo, P. P. K.; Chian, E. S. K.; De Walle, F. B.; Kim, J. H. "Gas Stripping,
Sorption, and Thermal Desorption Procedures for Preconcentrating Volatile Polar
Water-Soluble Organics from Water Samples for Analysis by Gas Chromatography,"
Anal. Chem., _49(7), 1977, pp. 1023-1029.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $60-90
(list).
B-654
-------
VOLATILE ORGANIC SOLVENTS
Air Samples
Laboratory Method 1
Detection
Limit
Compound CAS Number (mg/sample)
Acetone 67-64-1
Benzene 71-43-2 0.01
Carbon Tetrachloride 56-23-5 0.20
Chloroform 67-66-3 o! 10
1,2-Dichloroethane 107-06-2 0.05
1,4-Dioxane 123-91-1 0.05
Methylene Chloride 75-09-2 0.05
Methyl Ethyl Ketone 78-93-3 0.01
Styrene 100-42-5 0.10
Tetrachloroethylene 127-18-4 0.06
Toluene 108-88-3 0.01
1,1,1-Trichloroethane 71-55-6 0.05
1,1,2-Trichloroethane 79-00-5 0.05
Trichloroethylene 79-01-6 0.05
Xylene 1330-20-7 0.02
METHOD SUMMARY:
Gas chromatography can be used for the analysis of air for the above
volatile organic solvents. A known volume of air is drawn through a charcoal
tube. The trapped compounds are desorbed with carbon disulfide and an aliquot
of the resulting solution is injected into a gas chromatograph equipped with
flame ionization detection (GC/FID).
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
Any compound having the same retention time as the analyte will interfere.
Second-column confirmation is recommended.
QUALITY CONTROL;
A method blank should be prepared along with samples.
EPA/TECHNICAL STATUS:
This method is used by the National Institute for Occupational Safety and
Health (NIOSH). Detections limits are listed above. Limited precision and
accuracy information is furnished.
B-655
-------
REFERENCES;
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., M. Katz, Ed., APHA: Washington, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 127; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 127; Publication No. 75-121, U.S. DHEW: Cincinnati, 1975.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
B-656
-------
VOLATILE ORGANIC SOLVENTS
Air Samples
Laboratory Method 2
Compound CAS Number
Acetone 67-64-1
n-Butyl Alcohol 71-36-3
Ethyl Acetate 141-78-6
Methyl Ethyl Ketone 78-93-3
Methyl Isobutyl Ketone 108-10-1
Toluene 108-88-3
METHOD SUMMARY:
Gas chromatography is used to determine concentrations of the above
volatile organic solvents in air. The airborne solvents are sorbed onto an
activated charcoal sampling tube, and desorbed into a carbon disulfide-water
two-phase mixture. Each phase is analyzed separately by gas chromatography
with flame ionization detection. The carbon disulfide-water mixture should be
refrigerated after collection to prevent losses.
INTERFERENCES:
An alternate gas chromatographic column is necessary if toluene is to be
determined separately.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The method is sensitive to concentra-
tions of above approximately 0.3 milligrams per cubic meter. Limited precision
and accuracy information is furnished.
REFERENCE:
Langvardt, P. W.; Melcher, R. G. "Simultaneous Determination of Polar and Non-
Polar Solvents in Air Using a Two-Phase Desorption From Charcoal," Am. Ind.
Hyg. Assoc. J., 40, 1979, pp. 1006-1012.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
B-657
-------
WEAK ACIDS
Water Samples
Laboratory Method
Compound CAS Number
Benzole Acid 65-85-0
Phenol 108-95-2
Phosphoric Acid 7664-38-2
Resorcinol 108-46-3
METHOD SUMMARY:
Weak-acid anions from the above compounds in water samples can be deter-
mined by catalytic thermometric titrimetry. To a sample containing 0.1 milli-
mole of weak acid anion, 4 milliliters dimethyl sulfoxide and 2 milliliters
acrylonitrile are added. The sample solution is then titrated with 0.5 M
potassium hydroxide in 2-propanol, at a rate of 0.2 milliliters per minute.
The endpoint is indicated by a sharp rise in temperature from the exothermic
polymerization of acrylonitrile. This method does not identify any specific
weak acid or anion, but indicates total sample content of substances that can
initiate the polymerization of acrylonitrile.
INTERFERENCES;
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. No precision or accuracy information is
furnished.
REFERENCE:
Greenhow, E. J.; Shafi, A. A. "The Determination of Weak Acids in Aqueous
Solution by Catalytic Thermometric Titrimetry," Talanta, 23, 1976, pp. 73-76.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-45
(list).
B-658
-------
XYLENES
Air Samples
Laboratory Method 1
Compound CAS Number
Xylene 1330-20-7
m-Xylene 108-38-3
o-Xylene 95-47-6
p-Xylene 106-42-3
METHOD SUMMARY:
The above xylenes in air can be measured by gas chromatography. The
analysis is performed by passage of a known volume of air through a charcoal-
tube sampling device, followed by desorption of the analyte with carbon disul-
fide and analysis of the resulting solution by gas chromatography with flame
ionization detection (GC/FID). The method is capable of measurement of much
lower levels if the desorption efficiency is adequate.
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
QUALITY CONTROL:
Desorption efficiency must be determined over the range of interest, and a
method blank should be processed with each 10 samples. The desorption effi-
ciency and the results of the method-blank analysis should be used in the cal-
culation of the results.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health and has been validated over the range of 220 to 870 milligrams per
cubic meter in a 12-liter sample. Precision and accuracy information is
furnished.
REFERENCES;
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set U, Method S318, PB-262 405 (NTIS), U.S. DHEW: Washington, December 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S318; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
B-659
-------
XYLENES
Air Samples
Laboratory Method 2
Compound CAS Number
Xylene 1330-20-7
m-Xylene 108-38-3
o-Xylene 95-47-6
p-Xylene 106-42-3
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentra-
tion of the above xylenes in air samples. The absorbance at 13030, 13510,
and/or 12580 nm (768, 740, and/or 795 cm ) for the in-, o^-, and p- isomer,
respectively, is measured, using a 10-meter path length cell. Air can be
sampled in a Saran or Mylar© plastic bag; approximately 5 liters of the sample
are drawn into an evacuated cell. Continuous monitoring of air flowing through
the cell is possible if the spectrometer is set to one particular wavelength.
Some vapors can be adsorbed on silica gel and quantitatively desorbed into the
absorption cell later. Tentative qualitative identification of compounds can
be made based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample which absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter path-length cell, is 43 milligrams per cubic meter, or 10 parts per
million for each of the isomers. No precision or accuracy information is
furnished.
REFERENCE:
American Public Health Association, In Methods of Air Sampling and Analysis,
2nd ed., "Infrared Absorption Spectrometry," M. Katz, Ed. APHA: Washington,
1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list).
B-660
-------
APPENDIX C
Contents
C-i
-------
CAUTION
The following information is presented in each volume containing the
appendices to the report "Analytical Methods for CERCLA Hazardous Substances."
The Method Descriptions presented in Appendix A and Appendix B are not
intended to be critical reviews of analytical methods, but comprise an
annotated bibliography. The Method Descriptions are only brief summaries of
the information contained in the references being described. Efforts were
purposely made to avoid speculation about applications of methods to analytes
or circumstances not documented by a reference. There is an Index/Table of
Contents following the Report text, which tells the name for each substance
used throughout the Report. See the text of the report for a detailed descrip-
tion of the contents of the Method Descriptions and for the reasons for the
preparation of the appendices and report.
The cost figures furnished for each method are presented following the
Method Descriptions, and should not be used as a price list. For a discussion
of the factors involved in determining the cost figures cited, see the text of
the report. These facts are presented to ensure that the information presented
in the appendices is clearly defined and that what is not intended to be
included is outlined.
C-ii
-------
CONTENTS
The F Waste Streams ~
Page
F001 Spent Halogenated Solvents £_!
F002 Spent Halogenated Solvents !!!.'!.'.* C-l
F003 Spent Non-Halogenated Solvents C-l
F004 Spent Non-Halogenated Solvents C-2
F005 Spent Non-Halogenated Solvents C-2
F006 Electroplating Wastewater Sludges C-2
F007 Electroplating Cyanide Bath Solutions C-2
F008 Cyanide Electroplating Plating Bath Sludges C-3
F009 Cyanide Electroplating Cleaning Bath Solutions C-3
F010 Metal Heat Treating Quenching Bath Sludges C-3
F011 Metal Heat Treating Spent Cyanide Solutions C-3
F012 Metal Heat Treating Wastewater Treatment Sludges C-3
F013 Aluminum Chemical Conversion Coating Wastewater Sludges C-3
The K Waste Streams
K001 Wood Preservation Wastewater Treatment Sludge C-6
K002 Chrome Yellow/Orange Production Wastewater Treatment Sludge .... C-6
K003 Molybdate Orange Production Wastewater Treatment Sludge C-6
K004 Zinc Yellow Production Wastewater Treatment Sludge. ... C-6
K005 Chrome Green Production Wastewater Treatment Sludge C-6
K006 Chrome Oxide Green production Wastewater Treatment Sludge C-6
K007 Iron Blue Production Wastewater Treatment Sludge C-6
K008 Chrome Oxide Green Production Oven Residues C-7
K009 Distillation Bottoms from Acetaldehyde Production C-7
K010 Distillation Side Cuts from Acetaldehyde Production C-7
K011 Bottom Stream from Acrylonitrile Production C-7
K013 Acetonitrile Column Bottom Stream in Acrylonitrile Production . . . C-7
K014 Acetonitrile Purification Column Bottoms in Acrylonitrile
Production C-7
K015 Still Bottoms from Benzyl Chloride Production C-8
KOI6 Heavy Distillation Residues from Carbon Tetrachloride Production. . C-8
K017 Purification Column Still Bottoms in Epichlorohydrin Production . . C-8
KOI8 Fractionation Column Heavy Ends in Ethyl Chloride Production. . . . C-8
K019 Distillation Heavy Ends in Ethylene Dichloride Production C-8
K020 Vinyl Chloride Distillation Heavy Ends in Vinyl Chloride
Production c~8
K021 Spent Antimony Catalyst from Fluoromethanes Production C-9
K022 Distillation Bottom Tars from Phenol Production C-9
K023 Distillation Light Ends from Phthalic Anhydride Production C-9
K024 Distillation Bottoms from Phthalic Anhydride Production C-9
C-iii
-------
CONTENTS (Continued)
K025 Distillation Bottoms from Nitration of Benzene
K026 Stripping Still Tails from Methyl Ethyl Pyridine Production . . .
K027 Centrifuge/Distillation Residues from Toluene Diisocyanate
Production
K028 Spent Hydrochlorinator Catalyst from 1,1,1-TCE Production ....
K029 Stream Stripper Waste from 1,1,1-TCE Production
K030 Heavy Ends from Production of Trichloroethylene/Perchloroethylene
K031 Salts Generated in Production of MSMA and Cacodylic Acid
K032 Wastewater Treatment Sludge from Chlordane Production
K033 Wastes from Cyclopentadiene Chlorination in Chlordane Production.
K034 Filter Solids from Chlordane Production
K035 Creosote Production Wastewater Treatment Sludges
K036 Still Bottoms from Disulfoton Production
K037 Wastewater Treatment Sludges from Disulfoton Production
K038 Wastewater from Phorate Production
K039 Filter Cake from Phorate Production
K040 Wastewater Treatment Sludge from Phorate Production
K041 Wastewater Treatment Sludge from Toxaphene Production
K042 Heavy Ends from 2,4,5-T Production
K043 2,6-Dichlorophenol Waste from 2,4-D Production
K044 Wastewater Treatment Sludges from Explosive Processing
K045 Spent Carbon from Treatment of Explosive-Containing Wastewater. .
K046 Wastewater Treatment Sludges from Processing of Lead-Based
Initiators
K047 Pink/Red Water from TNT Operations
K048 DAF Float from Petroleum Refining
K049 Stop Oil Emulsions from Petroleum Refining
K050 Heat Exchanger Sludge from Petroleum Refining
K051 API Separator Sludge
K052 Leaded Tank Bottoms from Petroleum Refining
K060 Lime Sludge from Caking
K061 Steel Production Dust/Sludge Emissions
K062 Spent Pickle Liquor
K069 Lead Smelting Dust/Sludge Emissions
K071 Muds from Mercury-Cell Chlorine Production
K073 Chlorinated Hydrocarbons from Chlorine Production
K083 Aniline Extraction Distillation Bottoms
K084 Arsenic Veterinary Pharmaceutical Wastewater Treatment Sludges. .
K085 Chlorobenzene Distillation Column Bottoms
K086 Washes and Sludges from Production of Ink from Lead- and
Chromium-Containing Pigments
K087 Tar Sludge from Coking
K093 Distillation Light Ends from Phthalic Anhydride Production. . . .
K094 Distillation Bottoms from Phthalic Anhydride Production
K095 Distillation Bottoms from 1,1,1-Trichloroethane Production. . . .
K096 Heavy Ends from 1,1,1-Trichloroethane Production
K097 Vacuum Stripper Discharge from Chlordane Production
K098 Wastewater from Toxaphene Production
C-iv
-------
CONTENTS (Continued)
K099 Wastewater from 2,4-D Production C-16
K100 Leachate from Lead Smelting Dust/Sludge ............. C-16
K101 Distillation Residues from Arsenic Veterinary Pharmaceuticals . . C-16
K102 Activated Carbon Residues from Production of Arsenic Veterinary
Pharmaceuticals C-l 6
K103 Residues from Extraction in Production of Aniline C-16
K104 Wastewater from Nitrobenzene/Aniline Production C-l 7
K105 Aqueous Stream from Chlorobenzene Production C-l 7
K106 Sludge from Mercury Cell Chlorine Production C-l 7
C-v
-------
Appendix C
The F and K Waste Streams under the Resource Conservation and Recovery Act
of 1976 (RCRA)*
* From Federal Register," 48(102), 25 May 1983, pp. 23597-23601.
C-l
-------
Use of this Appendix - Each specific waste stream has references listed to
compounds of interest and to methods which are generally applicable to poten-
tial components of that stream. For references to specific compounds, the
consensual name used in the text is furnished and a notation of "Appendix A" as
the location of the reference is given. For references to multi-compound
methods, the name of the method and the location, as "Appendix B", is provided.
This listing is not complete or exhaustive, and individual waste streams will
have different characteristics. The sources of information used to compile the
contents of this Appendix were: Background Document, Resource Conservation and
Recovery Act, Subtitle C - Identification and Listing of Hazardous Waste, U.S.
EPA Office of Solid Waste, 14 November 1980, 853 pp. and The Condensed Chemical
Dictionary, Eighth ed., Van Nostrand, NY, 1972.
C-2
-------
Waste Streams
Reference
FQOl;
The following spent halogenated solvents
used in degreasing and sludges from the
recovery of these solvents in degreasing
operations:
(a)
(b)
(c)
(d)
(e)
(f)
F002:
Tetrachloroethylene
Trichloroethylene
Methylene Chloride
1,1,1-Trichloroethane
Carbon Tetrachloride
Chlorinated Fluorocarbons
The following spent halogenated solvents
and the still bottoms from the recovery
of these solvents:
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
F003:
Tetrachloroethylene
Methylene Chloride
Trichloroethylene
1,1,1-Trichloroethane
Chlorobenzene
1,1,2-Trichloro-l, 2,2-trifluoroethane
o-Dichlorobenzene
Trichlorofluoromethane
The following spent non-halogenated
solvents and the still bottoms from the
recovery of these solvents:
(a) Xylene
(b) Acetone
(c) Ethyl Acetate
(d) Ethylbenzene
(e) Ethyl Ether
(f) Methyl Isobutyl Ketone
(g) n-Butyl Alcohol
(h) Cyclohexanone
(i) Methanol
See Tetrachloroethylene, Appendix A
See Trichloroethylene, Appendix A
See Methylene Chloride, Appendix A
See 1,1,1-Trichloroethane, Appendix A
See Carbon Tetrachloride, Appendix A
See Trichloromonofluoromethane, Appendix A
See Dichlorodifluoromethane, Appendix A
See Tetrachloroethylene, Appendix A
See Methylene Chloride, Appendix A
See Trichloroethylene, Appendix A
See 1,1,1-Trichloroethane, Appendix A
See Chlorobenzene, Appendix A
See 1,2-Dichlorobenzene, Appendix A
See Trichloromonofluoromethane, Appendix A
See Xylene, Appendix A
See Acetone, Appendix A
See Ethyl Acetate, Appendix A
See Ethylbenzene, Appendix A
See Ethyl Ether, Appendix A
See Methyl Isobutyl Ketone, Appendix A
See n-Butyl Alcohol, Appendix A
See Cyclohexanone, Appendix A
See Methanol, Appendix A
(continued)
C-3
-------
Waste Streams
Reference
F004;
The following spent non-halogenated
solvents and the still bottoms from the
recovery of these solvents:
(a) Cresols/Cresylic Acid
(b) Nitrobenzene
F005:
The following spent non-halogenated
solvents and the still bottoms from the
recovery of these solvents:
(a)
(b)
(c)
(d)
(e)
F006:
Toluene
Methyl Ethyl Ketone
Carbon Bisulfide
Isobutanol
Pyridine
See Cresol, Appendix A
See Nitrobenzene, Appendix A
See Toluene, Appendix A
See Methyl Ethyl Ketone, Appendix A
See Carbon Bisulfide, Appendix A
See iso-Butyl Alcohol, Appendix A
See Pyridine, Appendix A
Wastewater treatment sludges from electro-
plating operations except from the follow-
ing processes:
(1) sulfuric acid anodizing of aluminum;
(2) tin plating on carbon steel;
(3) zinc plating (segregated basis) on
carbon steel;
(4) aluminum or zinc-aluminum plating on
carbon steel;
(5) cleaning/stripping associated with
tin, zinc and aluminum plating on
carbon steel; and
(6) chemical etching and milling of
aluminum.
See Aluminum, Appendix B
See Cadmium, Appendix B
See Chromium, Appendix B
See Cyanides, Appendix B
See Nickel, Appendix B
F007;
Spent cyanide plating bath solutions from
electroplating operations (except for
precious metals electroplating spent
cyanide plating bath solutions).
See Cyanides, Appendix B
(continued)
C-4
-------
Waste Streams Reference
F008:
plating bath sludges from the bottom of See Cyanides, Appendix B
plating baths from electroplating opera-
tions where cyanides are used in the
process (except for precious metals
electroplating plating bath sludges).
F009:
Spent stripping and cleaning bath solutions See Cyanides, Appendix B
from electroplating operations where cyanides
are used in the process (except for precious
metals electroplating spent stripping and
cleaning bath solutions).
F010:
Quenching bath sludge from oil baths from See Cyanides, Appendix B
letal heat treating operations where
cyanides are used in the process (except
for precious metals heat treating quenching
batch sludges) .
Spent cyanide solutions from salt bath pot See Cyanides, Appendix B
cleaning from metal heat treating operations
(except for precious metals heat treating
spent cyanide solutions from salt bath pot
cleaning) .
F012:
Quenching wastewater treatment sludges from See Cyanides, Appendix B
tetal heat treating operations where cyanides
are used in the process (except for precious
metals heat treating quenching wastewater
treatment sludges).
F01J:
Wastewater treatment sludges from the See Aluminum, Appendix B
chemical conversion coating of aluminum. See Aluminum Sulfate, Appendix A
(continued)
C-5
-------
Waste Streams
Reference
K001;
Bottom sediment sludge from the treatment
of wastewaters from wood preserving processes
that use creosote and/or pentachlorophenol.
K002;
Wastewater treatment sludge from the
production of chrome yellow and orange
pigments.
K003:
Wastewater treatment sludge from the
production of molybdate orange pigments.
See Pentachlorophenol, Appendix A
See Creosote, Appendix A
See Phenols, Appendix B
See Chromium, Appendix B
See Lead Chromate, Appendix A
See Chromium, Appendix B
See Lead Chromate, Appendix A
K004;
Wastewater treatment sludge from the
production of zinc yellow pigments.
See Chromium, Appendix B
See Zinc, Appendix B
K005:
Wastewater treatment sludge from the
production of chrome green pigments.
K006;
Wastewater treatment sludge from the
production of chrome oxide green pigments
(anhydrous and hydrated).
K007:
Wastewater treatment sludge from the
production of iron blue pigments.
See Chromium, Appendix B
See Chromium, Appendix B
See Chromium, Appendix B
See Iron, Appendix B
See Potassium Bichromate, Appendix A
(continued)
C-6
-------
Waste Streams
Reference
K008:
Oven residue from the production of chrome
oxide green pigments.
K009:
Distillation bottoms from the production of
acetaldehyde from ethylene.
R010:
Distillation side cuts from the production
of acetaldehyde from ethylene.
1011:
>m stream from the wastewater stripper
he production of acrylonitrile.
KOI 3:
Bottom stream from the acetonitrile column
in the production of acrylonitrile.
KQU:
Bottoms from the acetonitrile purification
column in the production of acrylonitrile.
See Chromium, Appendix B
See Nitrates and Sulfates, Appendix B
See Nitrate Ions, Appendix B
See Acetaldehyde, Appendix A
See Chloroform, Appendix A
See Methyl Chloride, Appendix A
See Formaldehyde, Appendix A
See Formic Acid, Appendix A
See Methylene Chloride, Appendix A
See Paraldehyde, Appendix A
See Acetaldehyde, Appendix A
See Acetaldehyde, Appendix A
See Acetonitrile, Appendix A
See Acrylamide, Appendix A
See Acrylonitrile, Appendix A
See Chloroform, Appendix A
See Chloromethane, Appendix A
See Cyanides, Appendix B
See Formaldehyde, Appendix A
See Formic Acid, Appendix A
See Methylene Chloride, Appendix A
See Paraldehyde, Appendix A
See Acetonitrile, Appendix A
See Acrylamide, Appendix A
See Acrylonitrile, Appendix A
See Cyanides, Appendix B
See Acetonitrile, Appendix A
See Cyanides, Appendix B
See Acrylonitrile, Appendix A
(continued)
C-7
-------
Waste Streams
Reference
KOI 5:
Still bottoms from the distillation of
benzyl chloride.
KOI 6;
Heavy ends or distillation residues from
the production of carbon tetrachloride.
KOI 7:
Heavy ends (still bottoms) from the
purification column in the production of
epichlorohydrin.
KOI 8;
Heavy ends from the fractionation column in
ethyl chloride production.
KOI 9:
Heavy ends from the distillation of ethylene
dichloride in ethylene dichloride production.
K020:
Heavy ends from the distillation of vinyl
chloride in vinyl chloride monomer production.
See Benzotrichloride, Appendix A
See Benzyl Chloride, Appendix A
See Toluene, Appendix A
See Chlorobenzene, Appendix A
See Carbon Tetrachloride, Appendix A
See Hexachloroethane, Appendix A
See Hexachlorobutadiene, Appendix A
See Hexachlorobenzene, Appendix A
See Tetrachloroethylene, Appendix A
See Epichlorohydrin, Appendix A
See Chloroethane, Appendix A
See 1,2-Dichloroethane, Appendix A
See Trichloroethylene, Appendix A
See Carbon Tetrachloride, Appendix A
See Chloroform, Appendix A
See 1,1,2-Trichloroethane, Appendix A
See 1,1,2,2-Tetrachloroethane, Appendix A
See 1,1-Dichloroethylene, Appendix A
See 1,1,1-Trichloroethane, Appendix A
See Carbon Tetrachloride, Appendix A
See Chloroform, Appendix A
See 1,1,2-Trichloroethane, Appendix A
See 1,1,2,2-Tetrachloroethane, Appendix
See 1,1-Dichloroethylene, Appendix A
See 1,1,1-Trichloroethane, Appendix A
See Vinyl Chloride, Appendix A
(continued)
C-8
-------
Waste Streams
Reference
K021/.
Aqueous spent antimony catalyst waste from
fluoromethanes production.
See Antimony, Appendix B
See Chloroform, Appendix A
See Carbon Tetrachloride, Appendix A
K022:
Distillation bottom tars from the production
of phenol/acetone from cumene.
K023:
Distillation light ends from the production of
phthalic anhydride from naphthalene.
K024:
lillation bottoms from the production of
aalic anhydride from naphthalene.
R025:
Distillation bottoms from the production of
nitrobenzene by the nitration of benzene.
R026:
Stripping still tails from the production
of methyl ethyl pyridines.
See Phenol, Appendix A
See Acetone, Appendix A
See Cumene, Appendix A
See Polycyclic Aromatic Hydrocarbons,
Appendix B
See Vanadium Pentoxide, Appendix A
See Phthalic Anhydride, Appendix A
See Naphthalene, Appendix A
See 1,4-Naphthoquinone, Appendix A
See Vanadium Pentoxide, Appendix A
See Phthalic Anhydride, Appendix A
See Naphthalene, Appendix A
See Phthalate Esters, Appendix B
See Sulfuric Acid, Appendix A
See Nitric Acid, Appendix A
See Benzene, Appendix A
See Nitrobenzene, Appendix A
See m-Dinitrobenzene, Appendix A
See 2\4-Dinitrotoluene, Appendix A
See Paraldehyde, Appendix A
See 2-Picoline, Appendix A
See Pyridine, Appendix A
(continued)
C-9
-------
Waste Streams
Reference
K027;
Centrifuge and distillation residues
from toluene diisocyanate production.
K028:
Spent catalyst from the hydrochlorinator
reactor in the production of 1,1,1-
trichloroethane.
K029:
Waste from the product steam stripper in
the production of 1,1,1-trichloroethane.
K030:
Column bottoms or heavy ends from the
combined production of trichloro-
ethylene and perchloroethylene.
K031:
By-product salts generated in the production
of MSMA and cacodylic acid.
K032:
Wastewater treatment sludge from the
production of chlordane.
See Phosgene, Appendix A
See Hydrochloric Acid, Appendix A
See Toluenediamine, Appendix A
See Toluene Diisocyanate, Appendix A
See Chloroform, Appendix A
See 1,2-Dichloroethane, Appendix A
See 1,1-Dichloroethylene, Appendix A
See 1,1,1,2-Tetrachloroethane, Appendix A
See 1,1,2,2-Tetrachloroethane, Appendix A
See 1,1,1-Trichloroethane, Appendix A
See Chloroform, Appendix A
See 1,2-Dichloroethane, Appendix A
See 1,1-Dichloroethylene, Appendix A
See 1,1,1,2-Tetrachloroethane, Appendix A
See 1 ,1,2,2-Tetrachloroethane, Appe
See 1,1,1-Trichloroethane, Appendix A
See Chloroethane, Appendix A
See Hexachloroethane, Appendix A
See Hexachlorobenzene, Appendix A
See 1,1,2,2-Tetrachlorobenzene, Appendix A
See Arsenic, Appendix B
See Chlordane, Appendix A
See Hexachlorocyclopentadiene, Appendix A
(continued)
C-10
-------
Waste Streams
Reference
K033:
Wastewater and scrub water from the
chlorination of cyclopentadiene in the
production of chlordane.
K034;
Filter solids from the filtration of
hexachlorocyclopentadiene in the production
of chlordane.
K035:
Wastewater treatment sludges generated
in the production of creosote.
K036;
Still bottoms from toluene reclamation
Distillation in the production of disulfoton.
K037:
Wastewater treatment sludges from the
production of disulfoton.
K038:
Wastewater from the washing and stripping of
phorate production.
K039:
Filter cake from the filtration of diethyl-
phosphorodithioic acid in the production of
phorate.
See Chlordane, Appendix A
See Hexachlorocyclopentadiene, Appendix A
See Chlordane, Appendix A
See Hexachlorocyclopentadiene, Appendix A
See Heptachlor, Appendix A
See Creosote, Appendix A
See Phenol, Appendix A
See Polycyclic Aromatic Hydrocarbons,
Appendix B
See Disulfoton, Appendix A
See Hydrochloric Acid, Appendix A
See Toluene, Appendix A
See Disulfoton, Appendix A
See Hydrochloric Acid, Appendix A
See Disulfoton, Appendix A
See Formaldehyde, Appendix A
See Hydrochloric Acid, Appendix A
See Phorate, Appendix A
See Disulfoton, Appendix A
See Hydrochloric Acid, Appendix A
See Phorate, Appendix A
(continued)
C-ll
-------
Waste Streams
Reference
K040;
Wastewater treatment sludge from the
production of phorate.
K041;
Wastewater treatment sludge from the
production of toxaphene.
K042;
Heavy ends or distillation residues from
the distillation of tetrachlorobenzene in
the production of 2,4,5-T.
K043:
2,6-Dichlorophenol waste from the production
of 2,4-D.
K044;
Wastewater treatment sludges from the
manufacturing and processing of explosives.
K045;
Spent carbon from the treatment of wastewater
containing explosives.
K046:
See Disulfoton, Appendix A
See Hydrochloric Acid, Appendix A
See Phorate, Appendix A
See Toxaphene, Appendix A
See £-Dichlorobenzene, Appendix A
See Hexachlorobenzene, Appendix A
See Tetrachlorobenzene, Appendix A
See 2,4-Dichlorophenol, Appendix A
See 2,6-Dichlorophenol, Appendix A
See 2,4,6-Trichlorophenol, Appendix A
See sym-Trinitrobenzene, Appendix A
See Lead, Appendix B
See sym-Trinitrobenzene, Appendix A
See Lead, Appendix B
Wastewater treatment sludges from the manufac- See Lead, Appendix B
turing, formulation and loading of lead-based
initiating compounds.
K047:
Pink/red water from TNT operations.
See sym-Trinitrobenzene, Appendix A
(continued)
C-12
-------
Waste Streams
Reference
R048:
Dissolved air flotation (DAF) float from
the petroleum refining industry.
K049:
Slop oil emulsion solids from the petroleum
refining industry.
K050:
Heat exchanger bundle cleaning sludge from
the petroleum refining industry.
K051:
API separator sludge from the petroleum
refining industry.
K052:
•^^^^•M
ft
,k bottoms (leaded) from the petroleum
ining industry.
K060;
Ammonia still lime sludge from coking
operations.
See Chromium, Appendix B
See Lead, Appendix B
See Chromium, Appendix B
See Lead, Appendix B
See Chromium, Appendix B
See Lead, Appendix B
See Chromium, Appendix B
See Lead, Appendix B
See Chromium, Appendix B
See Lead, Appendix B
See Cyanides, Appendix B
See Naphthalene, Appendix A
See Phenolic Compounds, Appendix B
See Phenolics, Appendix B
See Polycyclic Aromatic Hydrocarbons,
Appendix B
K061:
Emission control dust/sludge from the primary
production of steel in electric furnaces.
See Cadmium, Appendix B
See Chromium, Appendix B
See Lead, Appendix B
(continued)
C-13
-------
Waste Streams
Reference
K062;
Spent pickle liquor from steel finishing
operations.
K069;
Emission control dust/sludge from secondary
lead smelting.
K071:
Brine purification muds from the mercury
cell process in chlorine production, where
separately prepurified brine is not used.
K073:
Chlorinated hydrocarbon waste from the
purification step of the diaphragm cell
process using graphite anodes in chlorine
production.
See Chromium, Appendix B
See Sulfuric Acid, Appendix A
See Hydrochloric Acid, Appendix A
See Lead, Appendix B
See Phosphoric Acid, Appendix A
See Cadmium, Appendix B
See Chromium, Appendix B
See Lead, Appendix B
See Mercury, Appendix B
K083;
Distillation bottoms from aniline extrac-
tion.
K084;
Wastewater treatment sludges generated
during the production of veterinary
Pharmaceuticals from arsenic or organic-
arsenic compounds.
See Carbon Tetrachloride, Appendix A
See Chloroform, Appendix A
See Dichloroethylene, Appendix A
See Hexachloroethane, Appendix A
See 1,1,2,2-Tetrachloroethane, Appendix
See Tetrachloroethene, Appendix A
See Trichloroethane, Appendix A
See Aniline, Appendix A
See Diphenylamine, Appendix A
See Nitrobenzene, Appendix A
See Chlorobenzene, Appendix A
See Arsenic, Appendix B
(continued)
C-14
-------
Waste Streams
Reference
K085:
Distillation or fractionation column bottoms
from the production of chlorobenzenes.
K08j;
Solvent washes and sludges, caustic washes
and sludges, or water washes and sludges
from cleaning tubs and equipment used in
the formulation of ink from pigments,
driers, soaps, and stabilizers containing
chromium and lead.
K087;
Decanter tank tar sludge from coking opera-
tions .
K093:
light ends from the production
anhydride from ortho-xylene.
K094:
Distillation bottoms from the production of
phthalic anhydride from ortho-xylene.
See Benzene, Appendix A
See Chlorine, Appendix A
See Dichlorobenzene, Appendix A
See Chromates, Appendix B
See Chromium, Appendix B
See Hexavalent Chromium, Appendix B
See Lead, Appendix B
See Phenol, Appendix A
See Naphthalene, Appendix A
See Phthalate Esters, Appendix B
See Phthalic Anhydride, Appendix A
See o-Xylene, Appendix A
See Phthalate Esters, Appendix B
See Phthalic Anhydride, Appendix A
See o-Xylene, Appendix A
K095:
Distillation bottoms from the production of
1,1,1 -trichloroethane.
KQ96:
Heavy ends from the heavy ends column from
the production of a,a,a-trichlorethane,
1,1,1.
See 1,1,1-Trichloroethane, Appendix A
See 1,1,1-Trichloroethane, Appendix A
(continued)
C-15
-------
Waste Streams
Reference
K097;
Vacuum stripper discharge from the chlordane
chlorinator in the production of chlordane.
K098:
Untreated process wastewater from the
production of toxaphene.
K099:
Untreated wastewater from the production of
2,4-D.
K100;
Waste leaching solution from acid leaching
of emission control dust/sludge from secondary
lead smelting. (Components of this waste
are identical with those of K069.)
KL01:
See Chlordane, Appendix A
See Toxaphene, Appendix A
See Toxaphene, Appendix A
See 2,4-D, Appendix A
See Lead, Appendix B
See Cadmium, Appendix B
See Chromium, Appendix B
Distillation tar residues from the distilla-
tion of aniline-based compounds in the pro-
duction of veterinary Pharmaceuticals from
arsenic or organo-arsenic compounds.
K102:
Residue from the use of activated carbon
for decolorization in the production of
veterinary pharmaceuticals from arsenic or
organo-arsenic compounds.
K103:
Process residues from aniline extraction
from the production of aniline.
See Arsenic, Appendix B
See Aniline, Appendix A
See Arsenic, Appendix B
See Aniline, Appendix A
See Nitrobenzene, Appendix A
(continued)
C-16
-------
Waste Streams
Reference
1004;
Combined wastewater streams generated from
nitrobenzene/aniline chlorobenzenes.
K105:
Separated aqueous stream from
the reactor product washing step in the
production of chlorobenzenes.
See Ammonia, Appendix A
See Aniline, Appendix A
See Chlorobenzene, Appendix A
See Nitrobenzene, Appendix A
See Benzene, Appendix A
See Chlorine, Appendix A
See Chlorobenzene, Appendix A
See Dichlorobenzene, Appendix A
See Hexachlorobenzene, Appendix A
See Pentachlorobenzene, Appendix A
See Tetrachlorobenzene, Appendix A
See Trichlorobenzene, Appendix A
See 2,4,6-Trichlorophenol, Appendix A
Wastewater treatment sludge from the
rcury cell process in chlorine
See Mercury, Appendix B
C-17
-------
|