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 ------- ISOPROPANOLAMINE DODECYLBENZENESULFONATE (CAS Number 42504-46-1) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Anionic Detergents," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Alkyl Benzene Sulfonates," Appendix B. A-693 ------- ISOSAFROLE (CAS Number 120-58-1) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-694 ------- KELTHANE (CAS Number 115-32-2) RQ: 4.54 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. A-695 ------- KEPONE (CAS Number 143-50-0) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for kepone. The analysis can be performed by high-volume filtration of air with glass-fiber filters, extraction of the analyte from the glass-fiber filter with methanol/ benzene (1/1, v/v), filtration to remove glass fibers, concentration or dilu- tion (as necessary), and analysis by gas chromatography with electron capture detection (GC/ECD). An alternative procedure involves sample collection on a membrane filter with a backup impinger containing dilute sodium hydroxide, dissolution of the kepone on the filter in benzene/methanol (1/1, v/v), acidi- fication of the sodium hydroxide solution with sulfuric acid, and extraction of the kepone in it with benzene, followed by analysis of both solutions by GC/ECD. INTERFERENCES: Mirex in the air sample may generate some kepone when it reacts with the sodium hydroxide in the impinger. QUALITY CONTROL: Confirmation of the identity of chromatographic peaks may be accomplished by use of a second column, an electrolytic conductivity detector or mass spectrometer. Use of spiked standard reference materials helps assure the validity of analytical results. A-696 ------- EPA/TECHNICAL STATUS; This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 2 to 1000 micrograms per cubic meter of air in a 480-liter sample. The limit of detection is estimated to be below 0.1 nanograms per cubic meter by NIOSH. The limit of quantification reported in the EPA reference below is 0.1 nanograms per cubic meter. Precision and accuracy information is furnished. REFERENCES: Hodgson, D. W.; Kantor, E. J.; and Mann, J. B. "Analytical Methodology for the Determination of Kepone® Residues in Fish, Shellfish, and Hi-Vol Air Filters," Arch Environm. Contam. Toxicol., _7, 1978, pp. 99-112. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 225; Publication No. 77-157A, U.S. DHEW: Washington, 1977. U.S. Environmental Protection Agency, Manual of Analytical Methods for the Analysis of Pesticides in Humans and Environmental Samples, Section 5.A.5.a. EPA-600/8-80-038, U.S. EPA: Washington, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $115-170 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Organochlorine Pesticides and PCB's," Appendix B. Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. A-697 ------- LASIOCARPINE (CAS Number 303-34-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method METHOD SUMMARY: Colorimetric analysis can be used to determine lasiocarpine in water samples. The sample is made basic and extracted with chloroform. Sodium sulfate is used to remove water from the combined extracts, which are then evaporated to dryness. The residue is mixed with an oxidation reagent, heated, mixed with diglyme and acetic acid, heated again, mixed with Ehrlich reagent and heated. The solution will change color in the presence of lasiocarpine, and the intensity of the color is measured with a portable spectrometer. This method is not specific for lasiocarpine. INTERFERENCES: Alkaloids and compounds having an unsaturated basic moiety may also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: No sensitivity data are supplied. REFERENCE: Mattocks, A.; "Spectrophotometric Determination of Unsaturated Pyrrolizidine Alkaloids," Anal. Chem., 39(4), 1967, pp. 443-447- A-698 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $90-150 (list). Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-699 ------- LINDANE (CAS Number 58-89-9) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for lindane. The analysis is performed by passage of a known volume of air through a glass fiber filter connected in series to a midget bubbler containing isooctane. An aliquot of the resulting solution is injected into a gas chromatograph equipped with an electrolytic conductivity detector. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: Method blanks and standards should be prepared and analyzed with the samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 0.28 to 1.66 milligrams per cubic meter in a 90-liter sample. Precision and accuracy information is furnished. A-700 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T. Method S290; PB-262 404 (NTIS). U.S. DREW: Washington, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S290; Publication No. 77-157-C, U.S. DREW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $100 (list), plus sampling costs. See also: "Chlorinated Pesticides," Appendix B. See also: "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. Water Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. See "Pesticides," Appendix B. A-701 ------- MALATHION (CAS Number 121-75-5) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. See "Cholinesterase-Inhibiting Compounds," Appendix B. See "Organophosphorus Pesticides," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for malathion. The analysis is performed by passage of a known volume of air through a glass fiber filter sampling device, followed by desorption of the analyte with isooctane and analysis of the resulting solution by gas chromato- graphy with flame photometric detection (GC/FPD). 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 every 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 (NIOSH), and validated over the range of 8.0 to 35 milligrams per cubic meter in a 106-liter sample. Precision and accuracy information is furnished. A-702 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set 1, Method S370; PB-271 712 (NTIS), U.S. DREW: Washington, December 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 3, Method S370; Publication No. 77-157-C, U.S. DHEW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-120 (list), plus sampling costs. See also: "Chlorinated Pesticides," Appendix B. See also: "Organophosphorus Compounds," Appendix B. See also: "Organophosphorus Pesticides," Appendix B. See also: "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organophosphorus Pesticides," Appendix B. See "Pesticides," Appendix B. A-703 ------- MALEIC ACID (CAS Number 110-16-7) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Carboxylic Acids," Appendix B. A-704 ------- MALEIC ANHYDRIDE (CAS Number 108-31-6) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Note: NIOSH Method S302 (bubbler collection, analysis by HPLC) is applicable, (Reference provided by reviewer.) See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-705 ------- MALEIC HYDRAZIDE (CAS Number 123-33-1) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Maleic hydrazide in soil samples can be determined by colorimetry. The maleic hydrazide is hydrolyzed in water with zinc and alkali to yield hydrazine. The hydrazine is then distilled and determined colorimetrically using p- dimethylaminobenzaldehyde. ~~ INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: The method is not EPA-approved. Precision and accuracy information is not furnished. The method can detect levels of maleic hydrazide below 1 milligram per kilogram of sample. A-706 ------- REFERENCE: Freed, V- H. "Determination of Herbicides and Plant Growth Regulators," In The Physiology and Biochemisty of Herbicides, Ch. 2; L. J. Audus, Ed.; Academic Press: New York, 1964, pp. 39-71. COST INFORMATION; Cost per sample for analysis by this method is approximately $50-55 (list). Water Samples Laboratory Method A-707 ------- MELPHALAN (CAS Number 148-82-3) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, Water Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, A-708 ------- MERCAPTODIMETHUR (CAS Number 2032-65-7) RQ: 4.54 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "N-Methylcarbamates," Appendix B. A-709 ------- METHACRYLONITRILE (CAS Number 126-98-7) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Field analysis for methacrylonitrile in air may be performed by use of a detector tube. A 1-liter air sample is collected and analyzed with a hand- operated bellows pump and a methacrylonitrile gas detector tube (Draeger® 67 30101, or equivalent). A positive result is indicated by a color change in the tube from yellow to red, as the analyte reacts with a chromate compound, mercury (II), and methyl red. INTERFERENCES: Other cyanide compounds and hydrogen sulfide will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 3 to 30 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes," 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-710 ------- Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Compounds," Appendix B. A-711 ------- METHANOL (CAS Number 67-56-1) RQ: 2270 kg SAFETY INFORMATION: Flash point 52°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Organic Vapors," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for methanol, The analysis is performed by passage of 5 liters of air through a silica gel sampling tube, followed by desorption of the analyte with water 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 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 (NIOSH), and validated over the range of 140 to 540 milligrams methanol per cubic meter in a 5-liter sample of air. A variation utilizing a A-712 ------- larger sampling tube and intended for use in high humidity or for large concen- trations of methanol is classified as operational by NIOSH for the range of 135 to 534 milligrams methanol per cubic meter in a 5-liter sample. The method is capable of measurement of much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set E, Method S59; PB-246 148 (NTIS), U.S. DHEW: Washington, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 2, Method S59; Publication No. 77-157-B, U.S. DHEW: Washington, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 1, Method P&CAM 247; Publication No. 77-157-A, U.S. DHEW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of methanol in air samples. The absorbance at 9450 nm (1058 cm~l) is measured, using a 10-meter pathlength 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 that absorb infrared radiation at the wavelength of interest will interfere. QUALITY CONTROL: No quality control procedures are given. A-713 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. The sensitivity of the method, using a 10-meter pathlength cell, is 8 milligrams per cubic meter or 5 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B, See "Volatile Organics," Appendix B. A-714 ------- METHAPYRILENE (CAS Number 91-80-5) RQ: 2270 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method No Matrix Given Laboratory Method See "Nitrogenous Drugs," Appendix B. A-715 ------- METHOMYL (CAS Number 16752-77-5) RQ: 454 kg SAFETY INFORMATION: Methomyl is highly toxic, orally or inhaled as dust. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Chlorinated Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus and Carbamate Insecticides, Appendix B. See "Phenols and Other Compounds," Appendix B. Water Samples Laboratory Method See "Carbamate and Urea Pesticides," Appendix B. See "Phenols and Other Compounds," Appendix B. See "Thioic Acid Ester Pesticides," Appendix B. A-716 ------- METHOXYCHLOR (CAS Number 72-43-5) RQ: 0.454 kg SAFETY INFORMATION: Exhibits chronic toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Note: NIOSH Method S371 (filter collection, isooctane extraction, analyses by gas chromatography with electrolytes conductively detection) is applicable, (Reference provides by reviewer.) Soil/Sediment Samples Laboratory Method See "Organochlorine Pesticides and PCB's," Appendix B. Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. See "Pesticides," Appendix B. A-717 ------- 2-METHYLAZIRIDINE (CAS Number 75-55-8) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Substituted Nitriles," Appendix B. A-718 ------- METHYL BROMIDE (CAS Number 74-83-9) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Field analysis of air for methyl bromide may be performed by use of a detector tube. A 0.2- to 0.5-liter air sample is collected and analyzed with a hand-operated bellows pump and a methyl bromide gas detector tube (Draeger® 67 28211, or equivalent). A positive result is indicated by a color change in the tube from pale gray to brown, as the analyte reacts with fuming sulfuric acid, permanganate, and jj-anisidine. INTERFERENCES; Other halogenated hydrocarbons will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 10 to 400 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes," 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-719 ------- Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Analysis for methyl bromide in air may be performed by passage of 60 liters of air through a Tenax® cold trap (at -15°C) followed by desorption of the analyte from the trap into a gas chromatograph with a flame-ionization detector (GC/FID). INTERFERENCES: Any compound having the same retention time as methyl bromide will inter- fere. 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 above approximately 1 microgram per cubic meter. Precision and accuracy information is furnished. REFERENCE: Dumas, T. "Trapping Low Levels of Methyl Bromide in Air or as Residues at Ambient and Lower Temperatures for Gas Chromatography," J. Assoc. Off. Anal. Chem., 65/4), 1982, 913-915. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Fumigants," Appendix B. A-720 ------- Air Samples Laboratory Method 2 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for methyl bromide. 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 disulfide 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 10 samples. The desorption efficiency and the results of the method-blank analysis 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 validated over the range of 35 to 50 milligrams per cubic meter in an 11-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J, Method S372; PB-263 959 (NTIS), U.S. DHEW: Washington, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S372; Publication No. 77-157-C, U.S. DHEW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximatley $70-90 (list), plus sample costs. Air Samples Laboratory Method 3 METHOD SUMMARY; Infrared absorption spectrometry can be used to determine the concentra- tion of methyl bromide in air samples. The absorbance at 3360 (2976 cm~^) is measured using a 10-meter pathlength cell. Air can be sampled in a Saran or A-721 ------- 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 'that 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 pathlength cell, is 200 milligrams per cubic meter or 50 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Fumigants," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method A-722 ------- METHYL CHLORIDE (CAS Number 74-87-3) RQ: 0.454 kg SAFETY INFORMATION: Flash point: gas. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Methyl chloride in air samples can be measured by gas chromatography. A known volume of air is drawn through activated charcoal to trap the analyte. The methyl chloride is desorbed from the charcoal with methylene chloride or methanol, and an aliquot is injected into a gas chromatograph equipped with a flame ionization detector (GC/FID). INTERFERENCES: Any compound that has the same retention time as methyl chloride will interfere. QUALITY CONTROL: One method blank should be prepared with every 10 samples collected. Standards should be analyzed along with samples. EPA/TECHNICAL STATUS: Method S29 is validated by the National Institute for Occupational Safety and Health (NIOSH), for use over the range of 122 to 459 milligrams per cubic meter for an 8-hour time-weighted average with a 1.5-liter air sample and 2.96 to 1202 milligrams per cubic meter for a peak concentration with a 0.5-liter air sample. Method P&CAM 201 is proposed by NIOSH for use over the range of 2 A-723 ------- to 1600 milligrams per cubic meter with a 10-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 200; Publication No. 77-157-A, U.S. DREW: Washington, 1977- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, Method S99; Publication No. 78-175, U.S. DHEW: Washington, 1978. U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods Set 2, Method S99; PB-271 464 (NTIS), U.S. DHEW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximatley $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY; Infrared absorption spectrometry can be used to determine the concentra- tion of methyl chloride in air samples. The absorbance at 3350 nm (2985 cm~^) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 650 milligrams per cubic meter or 30 parts per million. No precision or accuracy information is furnished. A-724 ------- REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, D.C., 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Fumigants," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-725 ------- METHYL CHLOROCARBONATE (CAS Number 79-22-1) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-726 ------- 3-METHYLCHOLANTHRENE (CAS Number 56-49-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Polycyclic Aromatic Hydrocarbons," Appendix B. Soil/Sediment Samples Laboratory Method See "Polycyclic Aromatic Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Polycyclic Aromatic Hydrocarbons," Appendix B. A-727 ------- 4,4'-METHYLENEBIS(2-CHLOROANILINE) (CAS Number 101-14-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Aromatic Primary Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: 4,4'-Methylenebis(2-chloroaniline) in air samples may be measured by high- performance liquid chromatography (HPLC). A known volume of air is drawn through a glass-fiber filter followed by a bed of silica gel to collect the aerosol and vapor forms of the analyte, which is then desorbed with methanol. An aliquot of the resulting solution is analyzed by HPLC. INTERFERENCES: Some amines interfere. High humidity may interfere with the collection efficiency of the silica gel. QUALITY CONTROL: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with each set of 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 3 to 200 micrograms per cubic meter in a 50-liter air sample. Precision information is furnished. A-728 ------- REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 1, Method P&CAM 236; Publication No. 77-157-A, U.S. DREW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. See also: "Aromatic Primary Amines," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Amines," Appendix B. Water Samples Laboratory Method See "Aromatic Amines," Appendix B. A-729 ------- METHYLENE BROMIDE (CAS Number 74-95-3) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of methylene bromide in air samples. The absorbance at 8380 nm (1193 cm"1) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 75 milligrams per cubic meter or 5 parts per million. No precision or accuracy information is furnished. A-730 ------- REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. A-731 ------- METHYLENE CHLORIDE (CAS Number 75-09-2) RO' 454 ks SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard '—" information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Field analysis of air for methylene chloride may be performed by use of a detector tube. A 1-liter air sample is collected and analyzed with a hand- operated bellows pump and a methylene chloride gas detector tube (Draeger® 67 24601, or equivalent). A positive result is indicated by a color change from white to brownish-green in the indicating layer of the tube. The test is based on cleavage of methylene chloride by sulfuric acid, followed by reaction with iodine pentoxide, selenium dioxide, and fuming sulfuric acid. INTERFERENCES: Other halogenated hydrocarbons, organic compounds, and carbon monoxide also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 350 to 7000 milli- grams per cubic meter for the sample size above. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-732 ------- Soil/Sediment Samples Field Method See "Volatile Species," Appendix B, Water Samples Field Method See "Volatile Species," Appendix B, Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for methyl- ene chloride. 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 disulfide and analysis of the resulting solution by gas chromato- graphy 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 every 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 (NIOSH), and validated over the range of 1700 to 7100 milligrams per cubic meter in an 1-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J. Method S329; PB-263 959 (NTIS), U.S. DHEW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S329; 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. A-733 ------- Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of methylene chloride in air samples. The absorbance at 13100 nm (763 cm"1-) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 7 milligrams per cubic meter or 2 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximatley $75-85 (list), plus sampling costs. See also: "Fumigants," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. See also: "Organic Vapors," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. A-734 ------- Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B, See "Volatile Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-735 ------- METHYL ETHYL KETONE (CAS Number 78-93-3) RQ: 454 kg SAFETY INFORMATION: Flash point 16°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Acetone and Methyl Ketones," Appendix B. See "Organic Vapors," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for methyl ethyl ketone. 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 disulfide and analysis of the resulting solution by gas chromato- graphy 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 every 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 Insitute for Occupational Safety and Health (NIOSH), and validated for the range of 380 to 1240 milligrams per A-736 ------- cubic meter using a 10-liter sample. The method is capable of measurement of much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set A, Method S3; PB-245 850 (NTIS), U.S. DREW: Washington, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2., Method S3; Publication No. 77-157-B, U.S. DHEW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of methy ethyl ketone in air samples. The absorbance at 8520 nm (1174 cm"-'-) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 15 milligrams per cubic meter or 5 parts per million. No precision or accuracy information is furnished. A-737 ------- REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION; Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Gaseous Contaminants," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-738 ------- METHYL ETHYL KETONE PEROXIDE (CAS Number 1338-23-4) RQ: 4.54 kg SAFETY INFORMATION: Can undergo explosive decomposition. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Methyl ethyl ketone peroxide in air samples can be measured spectrometri- cally. A known volume of air is drawn through a midget impinger containing dimethyl phthalate. An aliquot of this solution is combined with diphenyl- carbohydrazide color reagent and the mixture is heated. The color intensity is determined on a spectrometer at 565 nm. INTERFERENCES: Other peroxides or any strong oxidant could interfere with the procedure. Most ketones will cause positive interference at high levels while substances that cause decomposition of peroxide will decrease the measured value. QUALITY CONTROL: A method blank and standards are processed along 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 0.31 to 3.1 milligrams per cubic meter in a 250-liter sample. Precision and accuracy information is furnished. A-739 ------- REFERENCE; U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol. 6, Method P&CAM 331; Publication No. 80-125, U.S. DHHS: Washington, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $40-60 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-740 ------- METHYL HYDRAZINE (CAS Number 60-34-4) RQ= 4-54 kg SAFETY INFORMATION: Flash point below 80°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography can be used for the analysis of air samples for methyl hydrazine. 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 disulfide and analysis of the resulting solution by gas chromato- graphy 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 every 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 (NIOSH), and validated over the range of 0.17 to 0.8 milligrams per cubic meter in a 10-liter sample. Precision and accuracy information is furnished. A-741 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set K, Method S149; PB-254 227, U.S. DREW: Washington, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtyical Methods, 2nd ed., Vol. 3, Method S149; Publication No. 77-157-C, U.S. DREW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Hydrazines," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-742 ------- METHYL IODIDE (CAS Number 74-88-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for methyl iodide. The analysis is performed by passage of 50 liters of air through a charcoal-tube sampling device, followed by desorption of the analyte with carbon disulfide 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: Desorption efficiency must be determined over the range of interest, and a method-blank should be processed with every 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 (NIOSH), and validated over the range of 17 to 52 milligrams per cubic meter using a 50-liter sample. The method is capable of measurement of A-743 ------- much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S98; Publication No. 77-157-B, U.S. DREW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Halogenated Compounds," Appendix B. A-744 ------- METHYL ISOBUTYL KETONE (CAS Number 108-10-1) RQ: 2270 kg SAFETY INFORMATION; Flashpoint 64°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Acetone and Methyl Ketones," Appendix B. See "Organic Vapors," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Methyl isobutyl ketone in air samples can be measured by gas chromatography. A known volume of air is drawn through a charcoal tube, the analyte is desorbed from the charcoal with carbon disulfide, and an aliquot of the resulting solu- tion 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 every 10 samples. ERA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and has been validated over the range of 208 to 836 milli- grams per cubic meter and 188 to 790 milligrams per cubic meter using 10-liter samples. Precision and accuracy information is furnished. A-745 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods Vol. 3, Method S178; Publication No. 77-157-C, U.S. DREW: Cincinnati, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set A, Method S18; PB-245 850 (NTIS), U.S. DHEW: Cincinnati, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S18; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Volatile Organic Solvents," Appendix B. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of methyl isobutyl ketone in air samples. The absorbance at 8520 nm (1174 cm"1) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 40 milligrams per cubic meter or 10 parts per million. No precision and accuracy information is furnished. A-746 ------- REFERENCE; American Public Health Association, "Infrared Absorption Spectroscopy." In Methods of Air Sampling and Analysis. 2nd ed., M. Katz, Ed.; APHA: Washington, 19//, pp. 79-84. COST INFORMATION; Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-747 ------- METHYL ISOCYANATE (CAS Number 624-83-9) RQ: 45.4 kg SAFETY INFORMATION: Flash point 19°F. Exhibits toxicity (inhalation). CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-748 ------- METHYL MERCAPTAN (CAS Number 74-93-1) RQ: 45.4 kg SAFETY INFORMATION: Flash point: 0°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Field analysis for methyl mercaptan in air may be performed by use of a detector tube. A 1-liter air sample is collected and analyzed with a hand- operated bellows pump and a mercaptan gas detector tube (Draeger® CH 20801, or equivalent). A positive result is indicated by a color change in the tube from white to yellowish-brown, as the analyte reacts with a sulfur solution and a copper (II) compound. INTERFERENCES: Propyl mercaptan, ethyl mercaptan, and hydrogen sulfide will also give positive results. High concentrations of ammonia or amines will cause a pale blue color and will prevent the determination of methyl mercaptan. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 40 to 200 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger ® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburghh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-749 ------- See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B, See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Mercaptans," Appendix B. See "Sulfur-Containing Gases," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-750 ------- METHYL METHACRYLATE (CAS Number 80-62-6) RQ: 454 kg SAFETY INFORMATION: Flash point 50°F. May polymerize upon exposure to ultraviolet light. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for methyl methacrylate in air may be performed by use of a detector tube. A 1-liter air sample is collected and analyzed with a hand- operated bellows pump and a methyl methacrylate gas detector tube (Draeger® 67 28171, or equivalent). A positive result is indicated by a color change in the tube from yellow to blue, as the analyte reacts with palladium molybdate. INTERFERENCES: Ethylene, carbon monoxide, and hydrogen sulfide will also change the tube color. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 200 to 2000 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105: National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger ® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-751 ------- See also: "Volatile Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Methyl methacrylate in air samples can be measured using gas chromato- graphy. A known volume of air is drawn through a tube containing XAD-2 resin. The analyte is desorbed with carbon disulfide and an aliquot of the extract is injected into a gas chromatograph equipped with a flame ionization detector (GC/FID). INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: A method blank is processed for every 10 samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH) and validated over the range of 193 to 725 milligrams per cubic meter in a 3-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 S43; Publication No. 80-125, U.S. DHHS: Washington 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. A-752 ------- Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of methyl methacrylate in air samples. The absorbance at 8550 nm (1169 cm ) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 5 milligrams per cubic meter or 1 part per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Trace Organic Contaminants," Appendix B. See "Volatile Organic Compounds," Appendix B. A-753 ------- N-METHYL-N'-NITRO-N-NITROSOGUANIDINE (CAS Number 70-25-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-754 ------- METHYL PARATHION (CAS Number 298-00-0) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. Air Samples Laboratory Method See "Chlorinated Pesticides," Appendix B. See "Organophosphorus Compounds," Appendix B. See "Organophosphorus Pesticides," Appendix B. See "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Pesticides," Appendix B. A-755 ------- METHYLTHIOURACIL (CAS Number 56-04-2) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-756 ------- MEVINPHOS (CAS Number 7786-34-7) RQ: 4.54 kg SAFETY INFORMATION: Exhibits toxicity (oral, inhalation). CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography can be used to analyze air samples for mevinphos. A known volume of air is drawn through a tube containing Chromosorb 102. The analyte is desorbed with toluene and the resulting solution is injected into a gas chromatograph equipped with a flame photometric detector (GC/FPD). INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: One method blank is processed for every 10 samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH) and validated over the range of 0.0270 to 0.145 milligrams per cubic meter in a 240-liter sample. Precision and accuracy information is furnished. A-757 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods. Vol 6, Method S296; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980.'' COST INFORMATION: Cost per sample for analysis by this method is approximately $80-120 (list), plus sampling costs. See also: "Organophosphorus Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organophosphorus Pesticides," Appendix B. A-758 ------- MEXACARBATE (CAS Number 315-18-4) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Carbamate Pesticides," Appendix B. Water Samples Laboratory Method See "Carbamate and Urea Pesticides," Appendix B, See "0-Aryl Carbamate Pesticides," Appendix B. A-759 ------- MITOMYCIN C (CAS Number 50-07-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, Water Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, A-760 ------- MONOETHYLAMINE (CAS Number 75-04-7) RQ: 454 kg SAFETY INFORMATION; Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Amines: Triethylamine and Other Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for mono- ethylamine. The analysis is performed by passage of a known volume of air through a silica gel tube sampling device, followed by desorption of the analyte with 0.1 M sulfuric acid. The resulting solution is made alkaline and an aliquot injected into a gas chromatograph with a flame ionization detector (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 every 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 (NIOSH), and validated over the range of 7.4 to 31.8 milligrams per cubic meter using a 30-liter sample. The method is capable of measurement of A-761 ------- much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Mthods for Set K, Method S144; PB-254 227 (NTIS), U.S. DREW: Cincinnati, 1976. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Primary and Secondary Amines," Appendix B. Water Samples Laboratory Method See "Aliphatic Amines," Appendix B. See "Primary and Secondary Amines," Appendix B. A-762 ------- MONOMETHYLAMINE (CAS Number 74-89-5) RQ: 45.4 kg SAFETY INFORMATION: Flash point: gas. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Amines: Triethylamine and Other Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Ion chromatography may be used for the analysis of air samples for mono- methylamine. A known volume of air is drawn through a tube containing silica gel and spiked with concentrated hydrochloric acid to stabilize the amine. The monomethylamine is extracted from the silica gel with deionized, distilled water and analyzed by ion chromatography using an electrolytic conductivity detector. INTERFERENCES: Large amounts of organic amines or ammonia can reduce the capacity of the sorbent. QUALITY CONTROL: One method blank is processed for every 10 samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH) and validated over the range of 6.24 to 28.1 milligrams per cubic meter in a 24-liter sample. Precision and accuracy information is furnished. A-763 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol 6, Method S148; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-90 (list), plus sampling costs. See also: "Methylamines," Appendix B. Soil/Sediment Samples Laboratory Method See "Primary and Secondary Amines," Appendix B. Water Samples Laboratory Method See "Primary and Secondary Amines," Appendix B. A-764 ------- NALED (CAS Number 300-76-5) RQ: 4.54 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. Air Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organophosphorus Pesticides," Appendix B. A-765 ------- RQ: 45.4 kg SAFETY INFORMATION: NAPHTHALENE (CAS Number 91-20-3) CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Naphthalene in air can be measured titrimetrically. A system of bubblers removes ammonia and collects the sample in picric acid. The sample is filtered and an aliquot is titrated with a standard sodium hydroxide solution. (This method is described in Jacobs, M. B. The Chemistry of Industrial Poisons, Hazards and Solvents, 2nd ed.; Interscience: New York, 1949, p. 550, and is summarized in the reference given below.) INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: No sensitivity information is furnished. REFERENCE: Quantitative Analysis of Gaseous Pollutants; Ruch, W. E., Ed.; Ann Arbor- Humphrey Science: Ann Arbor, 1970, p. 161. COST INFORMATION: Cost per sample for analysis by this method is approximately $10-18 (list), plus sampling costs. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B, A-766 ------- Air Samples Laboratory Method METHOD SUMMARY: Analysis of air samples for naphthalene can be performed by passing a known volume of air through a charcoal-tube sampling apparatus, followed by desorption from the charcoal with carbon disulfide and analysis of the resulting solution by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: High humidity severely limits the capacity of the sampling apparatus. QUALITY CONTROL: A method blank should be processed with each set of 10 or fewer samples. The desorption efficiency of the procedure must be determined and the results corrected accordingly. EPA/TECHNICAL STATUS: This procedure is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 19 to 85 milligrams per cubic meter for a 200-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T, Method S292; PB-263 404 (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 S292; 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. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Particulate Aromatic Hydrocarbons," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. A-767 ------- Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. See "Trace Organic Contaminants," Appendix B. A-768 ------- NAPHTHENIC ACID (CAS Number 1338-24-5) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-769 ------- 1,4-NAPHTHOQUINONE (CAS Number 130-15-4) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Nitroaromatics and Cyclic Ketones," Appendix B. Water Samples Laboratory Method See "Nitroaromatics and Cyclic Ketones," Appendix B. A-770 ------- 1-NAPHTHYLAMINE (CAS Number 134-32-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Aromatic Primary Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Aromatic Primary Amines," Appendix B. See "Hazardous Compounds," Appendix B. See "Naphthylamines," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Basic Organic Compounds," Appendix B. See "Hazardous Compounds," Appendix B. A-771 ------- 2-NAPHTHYLAMINE (CAS Number 91-59-8) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. "CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Hazardous Compounds," Appendix B. See "Naphthylamines," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Hazardous Compounds," Appendix B. A-772 ------- a-NAPHTHYLTHIOUREA (CAS Number 86-88-4) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: a-Naphthylthiourea in air samples can be determined by high-performance liquid chromatography (HPLC). The sample is collected using a polytetrafluoro- ethylene (Teflon®) filter. Methanol is used as the eluant, and the sample is analyzed by HPLC with UV detection. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method has been validated by the National Institute of Occupational Safety and Health (NIOSH) for use over the range of 0.128 to 0.76 milligrams analyte per cubic meter of air- Precision and accuracy information is furnished, A-773 ------- REFERENCE: U.S. Department of Health and Human Services NIOSH Research Report: Development and Validation of Methods for Sampling and Analysis of Workplace Toxic Substances; Publication No. 80-133, U.S. DHHS, 1980. COST INFORMATION: Cost per sample for anlaysis by this method is approximately $110 (list), plus sampling costs. Note: NIOSH Method S276 describes the above procedure in greater deatil. (Reference provided by reviewer.) Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method A-774 ------- NICOTINE AND SALTS (CAS Number 54-11-5) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Nicotine in air samples can be measured by gas chromatography. A known volume of air is drawn through a tube containing XAD-2 resin. The nicotine is desorbed from the resin with ethyl acetate, and an aliquot of the resulting solution is analyzed by gas chromatography with alkali flame ionization detec- tion (GC/AFID). INTERFERENCES: Any compound that is collected by the XAD-2, is eluted and has the same retention time as nicotine under the given operating conditions is an inter- ferent. QUALITY CONTROL: Desorption efficiency must be determined over the range of interest. A method blank should be processed with every 10 samples. 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 0.30 to 1.20 milligrams per cubic meter in a 100-liter sample. Precision and accuracy information is furnished. A-775 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 3, Method S293; Publication No. 77-157-C, U.S. DREW: Cincinnati, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T, Method S293; PB-262 404 (NTIS), U.S. DHEW: Cincinnati, 1976. COST INFORMATION: Cost per sample for analysis by this method is approximately $130 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method METHOD SUMMARY: Nicotine in water samples can be measured by gas chromatography (GC) with nitrogen-selective detection. Ammonium hydroxide must be added to all nicotine solutions to prevent adsorption of nicotine on glass and other materials out- side the gas chromatograph. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Accuracy and limited precision informa- tion is furnished. The limit of detection is approximately 0.3 to 0.7 micro- grams per liter. REFERENCE: Grubner, 0.; First, M. W.; Huber, G. L. "Gas Chromatographic Determination of Nicotine in Gases and Liquids with Suppression of Adsorption Effects " Anal. Chem., 52, 1980, pp. 1755-1758. A-776 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $115 (list) plus sampling costs. No Matrix Given Laboratory Method See "Nitrogenous Drugs," Appendix B. A-777 ------- Ł-NITROANILINE (CAS Number 100-01-6) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Aromatic Primary Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatic Amines," Appendix B. Air Samples Laboratory Method Note: NIOSH Method S7 (filter collection, extraction with isopropanol, analysis by HPLC) is applicable. (Reference provided by reviewers.) See also: "Aromatic Amines," Appendix B. See also: "Aromatic Primary Amines," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. A-778 ------- NITROBENZENE (CAS Number 98-95-3) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Organic Vapors," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. See "Nitro Compounds," Appendix B. No Matrix Given Field Method See "Nitro Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of nitrobenzene in air samples. The analysis is performed by passage of a known volume of air through a silica gel tube, desorption of the adsorbed substances with methanol, 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: The efficiency of desorption must be determined and results corrected accordingly. A method blank should be processed with each set of 10 or less samples• A-779 ------- 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 3 to 12 milligrams per cubic meter in a 55-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S217; Publication No. 77-157-C, U.S. DREW: Cincinnati, 1977. U.S. Department of Health, Educationand Welfare, NIOSH Analytical Methods for Set P, Method S217; PB-258 434 (NTIS), U.S. DHEW: Cincinnati, 1976. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Nitroaromatic Compounds and Benzonitrile," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Nitroaromatics and Cyclic Ketones," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. A-780 ------- NITROGLYCERIN (CAS Number 55-63-0) RQ: 4.54 kg SAFETY INFORMATION: Explosive. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for nitro- glycerin. The analysis can be performed by passage of a known volume of air through a tube of Tenax® adsorbent, desorption of the adsorbed substances with ethyl alcohol, and analysis of the resulting solution by gas chromatography with electron capture detection (GC/ECD). INTERFERENCES: There are no reported interferences. QUALITY CONTROL: A method blank should be analyzed with each set of 10 or fewer samples. Percent recovery must be determined and, if less than 95 percent, results should be corrected accordingly. EPA/TECHNICAL STATUS: The method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 0.6 to 3.2 milligrams per cubic meter. A related NIOSH method is proposed for use over the range of 0.1 to 100 milligrams per cubic meter in a 10-liter sample of air. Precision and accuracy information is furnished. A-781 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set P, Method S216; PB-256 434 (NTIS), U.S. DREW: Washington, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 203; Publication No. 77-157-A, U.S. DHEW: Washington, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S216; Publication No. 77-157-C, U.S. DHEW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $80 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Explosives," Appendix B. A-782 ------- NITROPHENOL, MIXED (CAS Number 25154-55-6) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitrophenols," Appendix B. A-783 ------- 2-NITROPHENOL (CAS Number 88-75-5) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard ~~ information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phenols," Appendix B. Water Samples Laboratory Method See "Acid Extractable Organic Compounds," Appendix B. See "Nitrophenols," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. A-784 ------- 3-NITROPHENOL (CAS Number 554-84-7) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitrophenols," Appendix B. See "Phenolics," Appendix B. A-785 ------- 4-NITROPHENOL (CAS Number 100-02-7) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phenols," Appendix B. Water Samples Laboratory Method See "Acid Extractable Organic Compounds," Appendix B. See "Nitrophenols," Appendix B. See "Phenols," Appendix B. A-786 ------- 2-NITROPROPANE (CAS Number 79-46-9) RQ: 0.454 kg SAFETY INFORMATION: Flash point 75°F. Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: 2-Nitropropane in air samples can be measured spectrometrically. A known volume of air is passed through a midget fritted bubbler containing 10 milli- liters of concentrated sulfuric acid. The resulting solution is heated in a water bath and cooled. Resorcinol reagent is added, and the sample is heated in a water bath again. The absorbance of the red-blue solution is read at a wavelength of 560 nm. (This method is described in Jones, L. R. Am. Ind. Hyg. Assoc. , 24. 1963, p. 11, and summarized in the reference given below.) INTERFERENCES: Most secondary aliphatic nitroparaffins and halogenated nitroparaffins will interfere with this analysis. QUALITY CONTROL: No quality control procedures are given., SENSITIVITY: This method is suitable for 2-nitropropane concentrations above approxi- mately 4 milligrams per cubic meter. REFERENCE: Quantitative Analysis of Gaseous Pollutants; Ruch, W. E., Ed.; Ann Arbor- Humphrey Science: Ann Arbor, MI, 1970, p. 174. COST INFORMATION: Cost per sample for analysis by this method is approximately $45-75 (list). Soil/Sediment Samples Field Method A-787 ------- Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography can be used to measure 2-nitropropane in air samples. A known amount of air is drawn through a sampling tube containing Chromosorb® 106. The 2-nitropropane is desorbed with ethyl acetate, and an aliquot of the resulting solution is injected into a gas chromatograph with flame ionization detection (GC/FID). INTERFERENCES: Any compound with the same retention time as 2-nitropropane is an inter- ferent. QUALITY CONTROL: A blank should be run with each batch of samples. EPA/TECHNICAL STATUS: This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 3 to 36 milligrams for a 3-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 P&CAM 272; Publication NO. 78-175, U.S. DHEW: Cincinnati, 1978. COST INFORMATION: Cost per sample for analysis by this method is approximatley $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of 2-nitropropane in air samples. The absorbance at 11750 nm (851 cm'1) is measured, using a 10-meter pathlength 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 A-788 ------- 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 that 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 pathlength cell, is 40 milligrams per cubic meter or 10 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association," Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-789 ------- N-NITROSODI-n-BUTYLAMINE (CAS Number 924-16-3) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "N-Nitrosamines," Appendix B. Soil/Sediment Samples Laboratory Method See "N-Nitroso Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "N-Nitrosamines," Appendix B. See "Volatile Organic Compounds," Appendix B. A-7 90 ------- N-NITROSODIETHANOLAMINE (CAS Number 1116-54-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-791 ------- N-NITROSODIETHYLAMINE (CAS Number 55-18-5) RQ: 0.454 kg SAFETY INFORMATION; Potentially carconogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Hazardous Organic Emissions," Appendix B. See "N-Nitrosamines," Appendix B. Soil/Sediment Samples Laboratory Method See "N-Nitroso Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "N-Nitrosamines," Appendix B. See "Volatile Organic Compounds," Appendix B. A-792 ------- N-NITROSODIMETHYLAMINE (CAS Number 62-75-9) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Air can be analyzed for the presence of N-nitrosodimethylamine by cryogenic or ambient-temperature trapping of analyte from a known volume of air on a Tenax® cartridge, followed by thermal desorption and analysis by capillary- column temperature-programmed gas chromatography/mass spectrometry (GC/MS). INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.0015 to 30 micrograms per cubic meter in a 150-liter air sample. Precision and accuracy information is furnished. A-793 ------- REFERENCES: Erickson, M.D. Monthly Technical Progress Report No. 32, EPA Contract 68-02-2767, Research Triangle Institute for U.S. EPA EMSL, Research Triangle Park, NC, May 1980. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 252; Publication No. 77-175-A, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $265-335 (list), plus sampling costs. Note: NIOSH Method 299 is also aplicable. See also: "Hazardous Organic Emissions," Appendix B. See also: "N-Nitrosamines," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "N-Nitrosamines," Appendix B. See "Volatile Organic Compounds," Appendix B. A-794 ------- N-NITROSODIPHENYLAMINE (CAS Number 86-30-6) RQ: 45.4 kg SAFTEY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "N-Nitrosamines," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "N-Nitroso Compounds," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B, A-795 ------- N-NITROSODI-n-PROPYLAMINE (CAS Number 621-64-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazat information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "N-Nitrosamines," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "N-Nitroso Compounds," Appendix B. Water Samples Laboratory Method See "N-Nitrosamines," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Base/Neutral Extractable Organic Compounds," Appendix B. A-796 ------- N-NITROSO-N-ETHYLUREA (CAS Number 759-73-9) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method No Matrix Given Laboratory Method See "Nitroso Compounds," Appendix B. A-797 ------- N-NITROSO-N-METHYLUREA (CAS Number 684-93-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. ~~ CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method No Matrix Given Laboratory Method See "Nitroso Compounds," Appendix B. A-798 ------- N-NITROSO-N-METHYLURETHANE (CAS Number 615-53-2) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B Water Samples Laboratory Method No Matrix Given Laboratory Method See "Nitroso Compounds," Appendix B. A-799 ------- N-NITROSOMETHYLVINYLAMINE (CAS Number 4549-40-0) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazarc information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-800 ------- N-NITROSOPIPERIDINE (CAS Number 100-75-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "N-Nitrosamines," Appendix B. Soil/Sediment Samples Laboratory Method See "N-Nitroso Compounds," Appendix B. Water Samples Laboratory Method See "N-Nitrosamines," Appendix B. A-801 ------- N-NITROSOPYRROLIDINE (CAS Number 930-55-2) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "N-Nitrosaraines," Appendix B. Soil/Sediment Samples Laboratory Method See "N-Nitroso Compounds," Appendix B. Water Samples Laboratory Method See "N-Nitrosamines," Appendix B. A-802 ------- NITROTOLUENE (CAS Number 1321-12-6) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Nitro Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Analysis for nitrotoluene in air can be performed by passage of 20 liters of air through a silica gel tube, followed by desorption of the analyte with methanol and analysis of the resulting solution by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: High humidity severely decreases the efficiency of the sampling apparatus. QUALITY CONTROL: The desorption efficiency must be determined over the range of use, a method blank processed with each set of samples, and the desorption efficiency and blank results used in the calculation of the results. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), has been reviewed and evaluated by that agency, and vali- dated over the range of 11 to 58 milligrams per cubic meter, using a 20-liter sample size. It is capable of measuring much smaller amounts if desorption efficiency is adequate. Precision and accuracy information is furnished. A-803 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set Q, Method S223, PB-258 435 (NTIS), U.S. DHEW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S223; 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. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitroaromatics," Appendix B. See "Non-Volatile Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. A-804 ------- 5-NITRO-o-TOLUIDINE (CAS Number 99-55-8) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatic Amines," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, Water Samples Laboratory Method See "Aromatic Amines," Appendix B. See "Nitroaromatics," Appendix B. See "Phenols and Other Compounds," Appendix B A-805 ------- OCTAMETHYLPYROPHOSPHORAMIDE (CAS Number 152-16-9) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-806 ------- PARAFORMALDEHYDE (CAS Number 30525-89-4) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Aldehydes," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-807 ------- PARALDEHYDE (CAS Number 123-63-7) RQ: 454 kg SAFETY INFORMATION: Flash point 96°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B, A-808 ------- PARATHION (CAS Number 56-38-2) RQ: 4.54 kg SAFETY INFORMATION; Exhibits toxicity (oral). Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method' See "Cholinesterase-Inhibiting Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography can be used for the analysis of air samples for parathion. A known volume of air is drawn through an impinger charged with ethylene glycol. The resulting solution is diluted, extracted with hexane, concentrated, and injected into a gas chromatograph with a flame photometric detector (GC/FPD) (Method P&CAM 158). Alternatively, the air is drawn through a glass-fiber filter which is extracted with isooctane, and the resulting solution is analyzed by GC/FPD (Method S295). INTERFERENCES: Phosphorus compounds with retention times close to that of parathion will interfere. Glassware and equipment must be scrupulously cleaned to remove any traces of phosphate detergents. QUALITY CONTROL: A method blank and standards are prepared and injected along with the samples. EPA/TECHNICAL STATUS: Method P&CAM 158 is a National Institute for Occupational Safety and Health (NIOSH) method for use over the range of 5 to 250 micrograms per cubic A-809 ------- meter for a 50-liter sample. Method S295 is approved by NIOSH and validated over the range of 0.07 to 0.26 milligrams per cubic meter for a 115-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T, Method S295; PB-262 404 (NTIS), U.S. DREW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 158; 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 158; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974. COST INFORMATION: Cost per sample for analysis by this method is approximately $130-220 (list), plus sampling costs. See also: "Chlorinated Pesticides," Appendix B. See also: "Organophosphorus Compounds," Appendix B. See also: "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organophosphorus Pesticides," Appendix B. See "Pesticides," Appendix B. A-810 ------- PENTACHLOROBENZENE (CAS Number 608-93-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Chlorinated Benzenes," Appendix B. See "Chlorobenzenes," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Chlorinated and Other Organic Contaminants," Appendix B, A-811 ------- PENTACHLOROETHANE (CAS Number 76-01-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Geminal Trihalogenated Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for penta- chloroethane. A known volume of air is drawn through a tube containing Porapak® R to trap the pentachloroethane vapor present. The analyte is desorbed with hexane and an aliquot of the resulting solution is injected into a gas chromato- graph with an electron capture detector (GC/ECD). INTERFERENCES: Using the described operating conditions, 1,2,2,3-tetrachloropropane cannot be separated from pentachloroethane, and high concentrations of 1,1,2,2-tetra- chloroethane may obscure the analyte peak. QUALITY CONTROL: One method blank should be processed for every 10 samples. EPA/TECHNICAL STATUS: This method has been accepted by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 14 to 5370 micrograms per cubic meter in a 3-liter sample. Precision and accuracy information is furnished. A-812 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods. Vol. 6, Method P&CAM 335; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980. COST INFORMATION; Cost per sample for analysis by this method is approximately $80 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B, A-813 ------- PENTACHLORONITROBENZENE (CAS Number 82-68-8) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. "CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Chlorinated Benzenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Chlorinated Benzenes," Appendix B. Water Samples Laboratory Method See "Organochlorine and Organophsophorus Pesticides," Appendix B. See "Organochlorine Pesticides," Appendix B. A-814 ------- PENTACHLOROPHENOL (CAS Number 87-86-5) RQ: 4.54 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). Exhibits chronic toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Pentachlorophenol in air samples may be measured by high-performance liquid chromatography (HPLC). A known volume of air is drawn through a cellu- lose ester filter and a midget bubbler containing 15 milliliters of ethylene glycol. After collection of the pentachlorophenol, the filter is placed in the bubbler flask. Just before analysis, 10 milliliters of methanol are added to the flask. The resulting solution is analyzed by HPLC with ultraviolet absor- bance (UV) detection. INTERFERENCES: Any compound that has the same retention time as pentachlorophenol is an interferent. QUALITY CONTROL: A blank should be processed with every 10 samples. Corrections for the blank and for recovery should be included in the calculations. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 0.265 to 1.130 milligrams A-815 ------- per cubic meter, using a 180-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 S297; Publication No. 78-175, U.S. DREW: Cincinnati, 1978. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. See also: "Chlorinated Phenols," Appendix B. See also: "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phenols," Appendix A. Water Samples Laboratory Method METHOD SUMMARY: A series of extractions and subsequent analysis by gas chromatography (GC) is used to determine pentachlorophenol in water samples. A 1-liter sample is acidified and the pentachlorophenol extracted into benzene. The pentachloro- phenol is then extracted into potassium carbonate, acetylated by the addition of acetic anhydride, extracted into hexane, and the hexane extract is analyzed by gas chromatography. Samples must be acidified, mixed with cupric sulfate and stored in the dark after collection. Samples must be analyzed within 24 hours of collection. INTERFERENCES: Interfering sulfur compound may be removed by acidification with sulfuric acid and addition of cupric sulfate. QUALITY CONTROL: No quality control procedures are provided. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is provided. A-816 ------- REFERENCE: Environment Canada, "Pentachlorophenol," Analytical Methods Manual; Environment Canada, Inland Waters Directorate, Water Quality Branch: Ottawa, Canada, 1974. COST INFORMATION: Cost per sample for analysis by this method is approximately $110-170 (list). See also: "Acid Extractable Organic Compounds," Appendix B. See also: "Chlorinated Phenols," Appendix B. See also: "Phenolics," Appendix B. See also: "Phenols," Appendix B. A-817 ------- 1,3-PENTADIENE (CAS Number 504-60-9) RQ: 45.4 kg SAFETY INFORMATION; Flash point -20°F. —— CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-818 ------- PHENACETIN (CAS Number 62-44-2) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method No Matrix Given Laboratory Method See "Nitrogenous Drugs," Appendix B. A-819 ------- PHENANTHRENE (CAS Number 85-01-8) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated and Aromatic Compounds," Appendix B. See "Halogenated, Aromatic and Other Compounds," Appendix B. See "Particulate Aromatic Hydrocarbons," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B, See "Polycyclic Aromatic Hydrocarbons," Appendix B. A-820 ------- PHENOL (CAS Number 108-95-2) RQ: 454 kg SAFETY INFORMATION: Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Organic Vapors," Appendix B. See "Phenols," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Analysis of air samples for phenol can be performed by passage of a known volume of air through a bubbler charged with 0.1-N sodium hydroxide, followed by acidification with sulfuric acid and analysis of the resulting solution by gas chromatography with flame-ionization detection (GC/FID). INTERFERENCES: No interferences are reported. QUALITY CONTROL: A method blank should be processed and sample results 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 9.5 to 38 milligrams per cubic meter in a 100-liter sample. Precision and accuracy information is furnished. A-821 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set L, Method S330; PB-250 159 (NTIS), U.S. DREW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtyical Methods, 2nd ed., Vol. 3, Method S330; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977- COST INFORMATION: Cost per sample for analysis by this method is approximately $60-90 (list), plus sampling costs. See also: "Halogenated and Aromatic Compounds," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. See also: "Phenolic Compounds," Appendix B. See also: "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Amines and Alcohols," Appendix B. See "Phenols," Appendix B. Water Samples Laboratory Method See "Acid Extractable Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Organic Acids," Appendix B. See "Organic Compounds," Appendix B. See "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. See "Trace Organic Contaminants," Appendix B. See "Weak Acids," Appendix B. A-822 ------- N-PHENYLTHIOUREA (CAS Number 103-85-5) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity- CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B Water Samples Laboratory Method A-823 ------- PRORATE (CAS Number 298-02-2) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). Potentially chronically " toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Phosphorodithioates," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organophosphorus Pesticides," Appendix B. A-824 ------- PHOSGENE (CAS Number 75-44-5) RQ: 454 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for phosgene may be performed by use of a detector tube. A 0.1- to 3.3-liter air sample is collected and analyzed with a hand-operated bellows pump and a phosgene gas detector tube (Draeger® CH 19401, or equivalent). A positive result is indicated by a color change in the tube from yellow to bluishgreen. The method is based on the reaction of phosgene with dimethyl- aminobenzaldehyde and diethylaniline. INTERFERENCES: Carbonyl bromide and acetyl chloride will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 0.2 to 6 milligrams per cubic meter. REFERENCES; Snyder, R. E. Development of Hazardous Toxic Wastes Analytical Screening Proce- dures, Atlantic Research Corporation for U.S. Army Medical Research and Development Command, July 16, 1982, p. 5. National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. A-825 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). Soil/Sediment Samples Field Method Water Samples Field Method See "Halides, Cyanides, and Other Compounds," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Phosgene in air samples may be determined colorimetrically - The air sample is collected in a midget impinger containing a 4,4'-nitrobenzyl pyridine color reagent, which reacts with traces of phosgene to produce a brillant red color. N-phenylbenzylamine in the reagent stabilizes the color and increases sensitivity. The absorbance of the solution is measured at 475 nm on a photo- meter. INTERFERENCES: Other acid chlorides, alkyl and aryl derivatives that are substituted by active halogen atoms and sulfate esters may produce color, but most of these interferences are removed by use of a prescrubber. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: The method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.026 to 20 milligrams per cubic meter, using a 2.5-liter sample. Precision and accuracy information is not furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 219; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. A-826 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $20-25 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of phosgene in air samples. The absorbance at 11680 nm (856 cm~^) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 4 milligrams per cubic meter or 1 part per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy." In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method A-827 ------- Water Samples Laboratory Method A-828 ------- PHTHALIC ANHYDRIDE (CAS Number 85-44-9) RQ: 2270 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Analysis for phthalic anhydride in air can be performed by cellulose membrane filtration of a known volume of air, followed by hydrolysis, extrac- tion, and analysis of the resulting solution by high-performance liquid chromatography (HPLC) with ultraviolet absorbance (UV) detection. INTERFERENCES: No interferences are reported. QUALITY CONTROL: A method blank should be analyzed with each 10 samples. Percent recovery must be determined, and, if less than 95 percent, results should be corrected accordingly - EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 5.5 to 28 milligrams per cubic meter in a 100-liter sample. Precision and accuracy information is furnished. A-829 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set M, Method S179; PB-265 029 (NTIS), U.S. DREW: Cincinnati, 1976.~ U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 3, Method S179; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $150-195 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Acids," Appendix B. A-830 ------- 2-PICOLINE (CAS Number 109-06-8) RQ: 2270 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Basic Organic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-831 ------- POLYCHLORINATED BIPHENYLS (PCB's) (CAS Numbers 1336-36-3, 12674-11-2, 11104-28-2, 11141-16-5, 53469-21-9, 12672-29-6, 11097-69-1, 11096-82-5) RQ: 4.54 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Polychlorinated Biphenyls and Chlorinated Pesticides," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Polychlorinated biphenyls (PCB's) in air may be measured by gas chromato- graphy. The PCB's are collected on polyurethane foam, using a calibrated sampling device. The polyurethane foam is Soxhlet-extracted, and the extract is cleaned up, concentrated, and analyzed by gas chromatography with electron- capture detection (GC/ECD) or halogen-specific detection (GC/HSD). The PCB's may also be collected on Florisil and desorbed with hexane, followed by GC/ECD analysis. When using the latter procedure, if the composition of the air sample differs significantly from a PCB standard, a prechlorination step must be added before the GC analysis. INTERFERENCES: Chlorinated pesticides such as DDT and DDE may interfere. Cleanup of the extract by deactivated silicic acid column chromatography should be performed before GC/ECD analysis when necessary. QUALITY CONTROL: Desorption efficiency should be determined over the range of interest, and a method blank should be processed with each set of samples. The desorption efficiency and the results of the method-blank analysis should be used in the calculation of the results. A-832 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved, but has undergone EPA technical review. The method employing sample collection on Florisil is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.01 to 10 milligrams per cubic meter in a 48-liter air sample. Precision information is furnished. REFERENCES; U.S. Environmental Protection Agency, Manual of Analytical Methods for the Analysis of Pesticides in Humans and Environmental Samples, Sections 8,9; EPA-600/8-80-038, U.S. EPA: Washington, 1980. Guidelines for Air Monitoring at Hazardous Waste Sites, Appendix B, GCA Corporation for U.S. EPA, Research Triangle Park, NC (Contract 68-02-3168), May 1982. Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol. Ill, Available Laboratory Analytical Methods, "Sampling and Analysis of Air for Polychlorinated Biphenyls," pp. III-213 to III-215; EPA-600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas, 1984. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 244; 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. 1, Method P&CAM 253; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximatley $80-215 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Analysis for Aroclor 1242 (CAS No. 53469-21-9) in air samples can be performed using gas chromatography. A known volume of air is drawn through a glass-fiber filter and a midget bubbler containing isooctane. The filter and isooctane are placed in a scintillation vial, and an aliquot is injected into a gas chromatograph equipped with a Hall electrolytic conductivity detector (GC/HECD). INTERFERENCES: Any other compound with the same retention time as Aroclor 1242 will interfere. A-833 ------- QUALITY CONTROL: One method blank is prepared with every 10 samples taken. Standards and blanks are analyzed along with the samples. EPA/TECHNICAL STATUS; This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated for use over the range of 0.51 to 2.7 milli- grams per cubic meter, using a 270-liter sample. Precision and accuracy information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods, Set-2, Method S120; PB-271 464 (NTIS), U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. See also: "Particulate Aromatic Hydrocarbons (Aroclor 1260)," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. A-834 ------- PRONAMIDE (CAS Number 23950-58-5) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-835 ------- PROPANEDINITRILE (CAS Number 109-77-3) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Substituted Nitriles and Tetranitromethane," Appendix B, A-836 ------- PROPANENITRILE (CAS Number 107-12-0) RQ: 4.54 kg SAFETY INFORMATION: Flash point 36°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Compounds," Appendix B. A-837 ------- 1,3-PROPANE SULTONE (CAS Number 1120-71-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-838 ------- PROPARGITE (CAS Number 2312-35-8) RQ: 4.54 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. A-839 ------- PROPIONIC ACID (CAS Number 79-09-4) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Formic Acid and Propionic Acid," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Organic Acids," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. See "Organic Acids," Appendix B. See "Volatile Organic Acids," Appendix B. A-840 ------- PROPIONIC ANHYDRIDE (CAS Number 123-62-6) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-841 ------- n-PROPYLAMINE (CAS Number 107-10-8) RQ: 2270 kg SAFETY INFORMATION: Flash point -35°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Primary and Secondary Amines," Appendix B. Water Samples Laboratory Method See "Aliphatic Amines," Appendix B. See "Primary and Secondary Amines," Appendix B. A-842 ------- PROPYLENE OXIDE (CAS Number 75-56-9) RQ: 45.4 kg SAFETY INFORMATION: Flash point -35°F. May polymerize and generate heat when in contact with active catalytic surfaces. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Ethylene Oxide, 1,4-Dioxane, and Propylene Oxide," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Lab oratory Method METHOD SUMMARY: Analysis for propylene oxide can be performed by passage of a known volume of air through a charcoal-tube trap, desorption of the analyte with carbon disulfide, and analysis of the resulting solution by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: High humidity impairs the efficiency of the charcoal-tube trap. QUALITY CONTROL: A method blank must be processed with each set of 10 samples, and the desorption efficiency must be determined over the range of interest. The method-blank results and desorption efficiency are 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 validated over the range of 121 to 482 milligrams per cubic meter, using a 5-liter sample. The method is capable of measuring much A-843 ------- smaller amounts if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set F, Method S75; PB-246 149 (NTIS), U.S. DHEW: Cincinnati, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S75; Publication No. 78-175, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of propylene oxide in air samples. The absorbance at 11960 nm (836 cm"-'-) is measured, using a 10-meter pathlength cell. Air can be sampled in a Saran or Mylar® plastic bag; approximatley 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 that 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 pathlength cell, is 23 milligrams per cubic meter or 10 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., Katz, M., Ed.; APHA: Washington, 1977, pp. 79-84. A-844 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Halogenated and Aromatic Compounds," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-84 5 ------- 2-PROPYN-l-OL (CAS Number 107-19-7) RQ: 454 kg SAFETY INFORMATION: Flash point 97°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-846 ------- PYRENE (CAS Number 129-00-0) RQ: 2270 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Particulate Aromatic Hydrocarbons," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. A-847 ------- PYRETHRINS (CAS Numbers 121-29-9, 121-21-1, and 8003-34-7) RQ: 0.454 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Pyrethrins in air samples may be measured using high-performance liquid chromatography (HPLC). A known volume of air is drawn through a glass-fiber filter. The analyte is extracted into acetonitrile and an aliquot of the resulting solution is analyzed by HPLC with ultraviolet absorbance (UV) detec- tion at 225 nm. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: One method blank is processed for every 10 samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH) and validated over the range of 1.413 to 8.47 milligrams per cubic meter in a 120-liter sample. Precision and accuracy information is furnished. A-848 ------- REFERENCE; U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods. Vol. 6, Method S298; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. See also: "Diuron and Pyrethrins," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-849 ------- PYRIDINE (CAS Number 110-86-1) RQ: 0.454 kg SAFETY INFORMATION: Flash point 68°F. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method 1 METHOD SUMMARY: Field analysis of air for pyridine may be performed by use of a detector tube. A 2-liter air sample is collected and analyzed with a hand-operated bellows pump and a pyridine gas detector tube (Draeger® 67 28651, or equivalent) A positive result is indicated by a color change in the tube to brownish-red. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The detector tube will indicate if more than approximately 16 milli- grams per cubic meter of pyridine is present. REFERENCES: National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $15-23 (list). A-850 ------- Air Samples Field Method 2 METHOD SUMMARY: Field analysis of air for pyridine can be performed by using a gas detector tube. A 0.1-liter air sample is collected and analyzed with a portable pump and a pyridine gas detector tube (Bendix/Gastec® 182, or equivalent). A posi- tive result is indicated by a color change in the tube from pink to yellow. INTERFERENCES: Ammonia, alkylamines, and hydrazine will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 5 to 50 milligrams per cubic meter using the sample size given above. REFERENCE: Bendix, Bendix Gastec Precision Gas Detector Systems Manual (Blue Book), Bendix Corp.: Largo, Florida. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method A-851 ------- Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography can be used for the analysis of air samples for pyri- dine. 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 methylene chloride 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 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 (NIOSH), and validated over the range of 7.6 to 30.4 milligrams per cubic meter, using a 100-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set L, Method S161; PB-250 159 (NTIS), U.S. DHEW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S161;l 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. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of pyridine in air samples. The absorbance at 9600 nm (1042 cm"1) is measured, using a 10-meter pathlength cell. Air can be sampled in a Saran or Mylar® plastic bag: approximately 5 liters of the sample are drawn into an A-852 ------- 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 that 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 pathlength cell, is 97 milligrams per cubic meter or 30 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. See also': "Organic Vapors," Appendix B. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Basic Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. A-853 ------- QUINOLINE (CAS Number 91-22-5) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard ~ information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Quinoline in air samples can be determined by gas chromatography with flame ionization detection (GC/FID). The sample is collected in a high-volume sampl- ing device that contains deactivated Florisil® adsorbent and a glass-fiber filter. The Florisil is eluted with ammonia-saturated ethyl ether; the filter is Soxhlet-extracted with ethyl ether. Both the eluent and the extract are con- centrated. An acid extraction is performed, and the organic layer is separated and analyzed by GC/FID. The aqueous layer is base-extracted. The organic layer is separted and analyzed by GC/FID. Confirmation is by gas chromato- graphy/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 information is furnished. A-854 ------- REFERENCE; Adams, J.; Atlas, E. L.; Giam, C. S. "Ultratrace Determination of Vapor-Phase Nitrogen Heterocyclic Bases in Ambient Air," Anal. Chem., 5_4, 1982, pp. 1515- 1518. COST INFORMATION: Cost per sample for analysis by this method is approximately $140 (list), plus sampling costs. Cost of the GC/MS confirmation is approximately $150-200 (list). Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Basic Organic Compounds," Appendix B. See "Non-Volatile Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. A-855 ------- RESERPINE (CAS Number 50-55-5) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard "~ information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B. Water Samples Laboratory Method See "Alkaloids," Appendix B. See "Phenols and Other Compounds," Appendix B. A-856 ------- RESORCINOL (CAS Number 108-46-3) RQ: 2270 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix See "Weak Acids," Appendix B. A-857 ------- SACCHARIN AND SALTS (CAS Number 81-07-2) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method METHOD SUMMARY: Saccharin in water samples can be measured by direct potentiometry using a substituted phenanthroline and saccharin ion-selective electrode. This method is suitable for saccharin concentrations in the range of 2 milligrams to 20 grams per liter. INTERFERENCES: Electrode interferences can occur that will affect results. A-858 ------- be preconditioned: solutions measured should be kept he electrode should be immersed to the same depth in lutions should be stirred vigorously. This method is not EPA-approved. No precision or accuracy information is furnished. REFERENCE: Vesely, J.; Weiss, D.; Stulik, L. Analysis With Ion-Selective Electrodes; Ellis Horwood: Chichester, 1978, pp. 89-105, 205. COST INFORMATION: Cost per sample for analysis by this method is approximately $10-19 (list). A-859 ------- SAFROLE (CAS Number 94-59-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-860 ------- STREPTOZOTOCIN (CAS Number 18883-66-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, Water Samples Laboratory Method See "Phenols and Other Compounds," Appendix B, A-861 ------- STRYCHNINE AND SALTS (CAS Number 57-24-9) RQ: 4.54 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Note: NIOSH Method S302 (filter collection, extraction with the HPLC mobile phase, analysis by HPLC/UV) is applicable. (Reference provided by reviewer.) Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Alkaloids," Appendix B. A-862 ------- STYRENE (CAS Number 100-42-5) RQ: 454 kg SAFETY INFORMATION: Flash point 90°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for styrene in air may be performed by use of a detector tube. A 0.2- to 1.5-liter air sample is collected and analyzed with a hand-operated bellows pump and a monostyrene 10/a gas detector tube (Draeger® 67 23301, or equivalent). A positive result is indicated by a color change from white to pale yellow in the tube, due to a reaction between styrene and sulfuric acid. INTERFERENCES: A few organic compounds that tend to polymerize will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 50 to 900 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger®, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e: National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-863 ------- See also: "Volatile Organic Compounds," Appendix B. See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography can be used for the analysis of styrene in air samples. 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 disulfide 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 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 (NIOSH), and validated over the range of 426 to 1710 milligrams per cubic meter, using a 5-liter sample. The method is capable of measurement of much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set C, Method S30; PB-258 852 (NTIS), U.S. DHEW: Cincinnati, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S30; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. A-864 ------- COST INFORMATION; Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of styrene in air samples. The absorbance at 12900 nm (775 cm~^) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 43 milligrams per cubic meter or 10 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. A-865 ------- Soil/Sediment Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated and Other Contaminants," Appendix B, See "Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-866 ------- 2,4,5-T ACID (CAS Number 93-76-5) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: 2,4,5-T acid in air samples can be measured by high-performance liquid chromatography (HPLC). The sample is collected with a glass-fiber filter. Methanol is used as the eluent, and the resulting solution is analyzed by HPLC with UV detection. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method has been validated by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 4.9 to 21.4 milligrams of 2 4 5-T per cubic meter of air. Precision and accuracy information is furnished. A-867 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Research Report: Develop- ment and Validation of Methods for Sampling and Analysis of Workplace Toxic Substances; Method S303 Publication No. 80-133, U.S. DHHS, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. Water Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. See "Chlorinated Phenols," Appendix B. A-868 ------- 2,4,5-T AMINES (CAS Number 2008-46-0) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. Water Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. A-869 ------- 2,4,5-T ESTERS (CAS Numbers 93-79-8, 2545-59-7, 61792-07-2, 1928-47-8, 25168-15-4) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Herbicides," Appendix B. Soil/Sediment Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. Water Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. A-870 ------- 1,2,4,5-TETRACHLOROBENZENE (CAS Number 95-94-3) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Chlorobenzenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. See "Trace Organic Contaminants," Appendix B. A-871 ------- 2,3,7,8-TETRACHLORODIBENZO-Ł-DIOXIN (CAS Number 1746-01-6) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (oral). Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: 2,3,7,8-Tetrachlorodibenzo-Ł-dioxin (TCDD) in air particulates can be measured by gas chromatography with electron capture detection. Samples of fly ash and particulates are collected on a filter, the filter is Soxhlet-extracted with hot benzene, and the extract is cleaned up by an activated-carbon treat- ment. The activated carbon is dispersed on silica gel and the dispersion is Soxhlet-extracted before being used. An additional cleanup step using alumina is suggested for very low levels of TCDD. INTERFERENCES: The recovery of dioxin can be affected by the amount of carbon used. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Accuracy information is furnished. A-872 ------- REFERENCES: Cutie, S. S. "Recovery Efficiency of 2,3,7, 8-Tetrachlorodibenzo-_p-dioxin from Active Carbon and Other Particulates," Anal. Chim. Acta.. 123, 1981, pp. 25-31. Federal Register, 40(160), August 18, 1977, p. 41777. COST INFORMATION: Cost per sample for analysis by this method is approximately $230 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Analysis of soil/sediment for 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) can be performed by gas chromatography. A 10-gram sample is spiked with isotopically-labeled 2,3,7,8-TCDD, dried, and extracted with a hexane/methanol mixture. The extract is concentrated and analyzed by fused- silica capillary column (FSCC) gas chromatography/mass spectrometry (GC/MS). The method is designed for use with samples of 1 part per billion or more of 2,3,7,8-TCDD and is specific for that isomer. INTERFERENCES: Most samples require cleanup by either silica gel column chromatography or potassium hydroxide extraction. QUALITY CONTROL: Recovery of the spike should be 25 to 125 percent, one method blank should be analyzed with each set of 20 or fewer samples, and 5 percent of the samples should be analyzed in duplicate. At least 5 percent of the samples should be Soxhlet-extracted with toluene to confirm results obtained. It should be demon- strated, by periodically processing laboratory reagent blanks, that solvents, reagents, glassware and other equipment are not contaminated with 2,3,7,8-TCDD. EPA/TECHNICAL STATUS: This method is not EPA-approved, but has been used in the CERCLA program. 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. A-873 ------- U.S. Environmental Protection Agency, Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater, Method 613, Longbottom J. E.; Lichtenburg, J. J., Eds.; EPA-600/4-82-057, U.S. EPA: Cincinnati, July 1982. Plumb, R. H. Characterization of Hazardous Waste Sites; A Methods Manual. Vol. Ill, Available Laboratory Analytical Methods," Methods for the Determina- tion of Dioxin (TCDD)," pp. 111-327 to III-363; 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 $600 and up (list), $275 and up (bid). Water Samples Laboratory Method METHOD SUMMARY: Analysis of water samples for 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) can be performed by gas chromatography. Water samples are screened by extraction of a 1-liter sample at pH 11 and then at pH 2 with methylene chloride, followed by concentration and extract analysis by gas chromatography/mass spectrometry (GC/MS). If screening results are positive, a 1-liter sample is spiked with an isotopically-labeled 2,3,7,8-TCDD internal standard, extracted with methylene chloride, solvent-exchanged into hexane, concentrated, and analyzed by GC/MS in selected ion monitoring mode. INTERFERENCES: Interferences may be overcome by alumina column and silica column cleanup steps. QUALITY CONTROL: At least 10 percent of the samples must be fortified samples, and a laboratory reagent blank must be analyzed with each set of samples. Percent recovery data should be monitored as a check on performance. EPA/TECHNICAL STATUS: This method is approved for National Pollutant Discharge Elimination System (NPDES) and Safe Drinking Water Act (SDWA) analyses. 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. A-874 ------- U.S. Environmental Protection Agency: Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater, Method 613; Longbottom J. E.; Lichtenburg, J- J., Eds.; 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," Methods for the Determina- tion of Dioxin (TCDD)," pp. III-327 to III-363; 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 $500 and up (list), $275 and up (bid). A-875 ------- 1,1,1,2-TETRACHLOROETHANE (CAS Number 630-20-6) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B. See "Volatile Organic Compounds," Appendix B. A-876 ------- 1,1,2,2-TETRACHLOROETHANE (CAS Number 79-34-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Vinyl Chloride and Other Chlorinated Hydrocarbons," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for 1,1,2,2-tetrachloroethane. 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 disulfide 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 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 (NIOSH), and validated over the range of 16 to 70 milligrams per cubic meter, using a 15-liter sample. The method is capable of measurement of A-877 ------- much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set I, Method S124; PB-265 028 (NTIS), U.S. DHEW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S124; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. COST INFORMATION; Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated Ethers and Other Compounds," Appendix B. See "Halogenated Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B. See "Volatile Organic Compounds," Appendix B. A-878 ------- TETRACHLOROETHYLENE (CAS Number 127-18-4) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for tetrachloroethylene is performed by use of a detector tube. A 4-liter air sample is collected and analyzed with a hand-operated bellows pump and a perchloroethylene 5/2 gas detector tube (Draeger® 67 26699, or equivalent). A positive result is indicated by a color change in the tube from pale gray to grayish-blue. The test is based on liberation of chlorine from tetrachloro- ethylene and reaction of that chlorine with N,N'-diphenylbenzidine. INTERFERENCES: Free halogens, hydrogen halides, and easily cleaved halogenated hydrocar- bons will also give positive results. Petroleum vapors will cause the 1,1,2,2- tetrachloroethylene determination to be low. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 35 to 350 milligrams per cubic meter when a 4-liter sample volume is used. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. A-879 ------- COST INFORMATION; Cost per sample for analysis by this method is approximately $13-20 (list). See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method See "Volatile Species," Appendix B. Water Samples Field Method See "Volatile Species," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of tetrachloroethylene in air samples. 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 disulfide and analysis of the resulting solution by gas chromato- graphy 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 every 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 (NIOSH), and validated over the range of 655 to 2749 milligrams per cubic meter, using a 3-liter sample. The method is capable of measurement of much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J, Method S335; PB-263 959 (NTIS), U.S. DHEW: Cincinnati, 1976.~~ A-880 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 3, Method S335; Publication No. 77-157-C, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of tetrachloroethylene in air samples. The absorbance at 10920 nm (916 cm"1) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 95 milligrams per cubic meter or 2 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Fumigants," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. A-881 ------- See also; "Volatile Organic Compounds," Appendix B. See also; "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated and Aromatic Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated Ethers and Other Compounds," Appendix B. See "Halogenated and Aromatic Compounds," Appendix B. See "Halogenated Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Low-Molecular Weight Halogenated Hydrocarbons," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-882 ------- 2,3,4,6-TETRACHLOROPHENOL (CAS Number 58-90-2) RQ: 4.54 kg SAFETY INFORMATION: Exhibits chronic toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Phenols," Appendix B. Water Samples Laboratory Method See "Chlorinated Phenols," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. A-883 ------- TETRAETHYLDITHIOPYROPHOSPHATE (CAS Number 3689-24-5) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-884 ------- TETRAETHYL PYROPHOSPHATE (CAS Number 107-49-3) RQ: 45.4 kg SAFETY INFORMATION; Exhibits toxicity (skin absorption). Potentially chroni- cally toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY; Tetraethyl pyrophosphate in air can be measured by gas chromatography. A known volume of air is drawn through a series of two Chromosorb® 102 tubes. The analyte is desorbed with toluene and analyzed by gas chromatography with flame photometric detection (GC/FPD). INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: A method blank and standard are 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 0.025 to 0.102 milligrams per cubic meter, using a 48-liter sample. Precision and accuracy information is furnished. A-885 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol. 6, Method P&CAM 336; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-120 (list), plus sampling costs. See also: "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-886 ------- TETRAHYDROFURAN (CAS Number 109-99-9) RQ: 454 kg SAFETY INFORMATION; Flash point 6°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Ethyl Ether and Tetrahydrofuran," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Analysis of air for tetrahydrofuran can be performed by passage of a known volume of air through a charcoal-tube sampling device, followed by desorption of the analyte with carbon disulfide 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 10 samples. The desorption efficiency and the results of the method-blank analysis 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 validated over the range of 320 to 1240 milligrams per cubic meter using a 9-liter sample. The method is capable of measurement of much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. A-887 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set F. Method S78; PB-246 149 (NTIS), U.S. DREW: Cincinnati, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S78; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of tetrahydrofuran in air samples. The absorbance at 9220 nm (1084 cm"'-) is measured, using a 10-meter pathlength cell. Air can be sampled in a Saran or Mylar® plastic bag and 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 that 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 pathlength cell, is 29 milligrams per cubic meter or 10 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. A-888 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Organics," Appendix B. A-889 ------- TETRANITROMETHANE (CAS Number 509-14-8) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). Explosive. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Analysis for tetranitromethane in air can be performed by gas chromato- graphy. A known volume of air is passed through ethyl acetate impingers followed by analysis of the resulting solution by gas chromatography with alkali flame ionization detection (GC/AFID). INTERFERENCES: No interferences are reported. QUALITY CONTROL: The analytical method recovery must be determined, and, if it is less than 95 percent, the appropriate correction factor should be used in calcula- tions. A method blank should be processed and the results used in the calcula- tions. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), has been reviewed and evaluated by that agency, and vali- dated over the range of 2.7 to 11.5 milligrams per cubic meter, using a 250- liter sample. Precision and acccuracy information is furnished. A-890 ------- REFERENCE; U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set Q. Method S224; PB-258 435 (NTIS), U.S. DREW: Cincinnati, 1975. COST INFORMATION: Cost per sample for analysis by this method is approximately $120 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Substituted Nitriles and Tetranitromethane," Appendix B. A-891 ------- THIOACETAMIDE (CAS Number 62-55-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Mercapto Compounds," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method A-892 ------- THIOFANOX (CAS Number 39196-18-4) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Gas chromatography can be used to analyze soil/sediment samples for thiofanox. Fifty to 100 grams of air-dried sample are extracted with acetone. The extract is concentrated, oxidized, dried, and cleaned by Florisil® column chromatography. The eluate is then concentrated, dissolved in benzene, and analyzed by gas chromatography with flame photometric detection (GC/FPD). An alternate procedure may be followed in which the sample is extracted with acetone, the resulting solution is then extracted with chloroform, and the Florisil® cleanup step is omitted. This method determines the total concentra- tion of thiofanox and its immediate oxidation and hydrolysis products in soil. INTERFERENCES: Most interferences are removed by Florisil® column cleanup or use of chloroform extraction. QUALITY CONTROL: No quality control procedures are given. A-893 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. Accuracy information is furnished. REFERENCE: Chin, W.; Duane, W. C.; Szalkowski, M. B.; Stallard, D. E. "Gas Chromatographic Determination of Thiofanox Residues in Soil, Plants, and Water," J. Agric. Food Chem., 23(5), 1975, pp. 963-966. COST INFORMATION: Cost per sample for analysis by this method is approximately $150-200 (list). Water Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used to analyze water samples for thiofanox. A water sample is filtered, acidified, and extracted with chloroform. The extract is concentrated, oxidized, and cleaned by Florisil® column chromato- graphy. The eluate is then concentrated, dissolved in benzene, and analyzed by gas chromatography with flame photometric detection (GC/FPD) . The total con- centration of thiofanox and its immediate oxidation and hydrolysis products in water is determined. 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. REFERENCE: Chin, W.; Duane, W. C.; Szalkowski, M. B.; Stallard, D. E. "Gas Chromatographic Determination of Thiofanox Residues in Soil, Plants, and Water " J. Agric. Food Chem., 23(5), 1975, pp. 963-966. COST INFORMATION: Cost per sample for analysis by this method is approximately $150-200 (list). A-894 ------- THIOPHENOL (CAS Number 108-98-5) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Mercaptans," Appendix B. Soil/Sediment Samples Laboratory Method See "Amine and Alcohols," Appendix B. Water Samples Laboratory Method A-895 ------- THIOSEMICARBAZIDE (CAS Number 79-19-6) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Mercapto Compounds," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B, Water Samples Laboratory Method A-896 ------- RQ: 45.5 kg SAFETY INFORMATION: THIOUREA (CAS Number 62-56-6) Is a known carcinogen and skin iritant. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Mercapto Compounds," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B, Water Samples Laboratory Method No Matrix Given Laboratory Method METHOD SUMMARY: Thiourea can be measured by reaction-kinetic spectrophotometry. Thiourea acts as a catalyst for the reaction of indigo carmine with hydrogen peroxide. The speed of the reaction is dependent upon the amount of thiourea present and is measured with a spectrophotometer. Twenty milliliters of unstabilized hydrogen peroxide solution, 36 milligrams per milliliter, at pH 4.0 are mixed with 2 milliliters of a sodium acetate buffer solution and 300 microliters of indigo carmine solution. The spectrophotometer is adjusted to full absorbance, A-897 ------- 0.5 milliliter of sample solution is added, and the decrease in absorbance with time is monitored. This method is sensitive to thiourea concentration levels of approximately 0.8 to 8 grams per liter. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. No precision and accuracy information is provided. REFERENCE: Weisz, H.; Pantel, S.; Marquardt, G. "Catalytic-Kinetic Absorptiostat Technique with the Indigo Carmine-Hydrogen Peroxide Reaction as the Indicator Reaction," Anal. Chim. Acta, 143, 1982, pp. 177-184. COST INFORMATION: No cost information has been obtained. A-898 ------- THIRAM (CAS Number 137-26-8) RQ: 4.54 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Thiram in air samples may be determined spectrophotometrically. A known volume of air is passed through a membrane filter. The collected analyte is extracted from the filter with chloroform. If acrylamide polymers are present, they are removed by precipitation with acetone. Cuprous iodide is added to the chloroform solution to form cupric dimethyldithiocarbamate. The absorbance of the solution is measured at 440 nm with a spectrophotometer. INTERFERENCES: Acrylamide polymers interfere and must be removed. Other dithiocarbamates, metallic chelates, iron and other metal compounds interfere with the analysis. Latex particules may clog the filter and reduce sampling efficiency. QUALITY CONTROL: A blank should be processed and extraction efficiency determined, and the associated values should be used in the calculation of the results. EPA/TECHNICAL STATUS: This method is classifed as operational by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 1 to 5 milli- grams per cubic meter for air, using a 50-liter sample. The method detection A-899 ------- limit is about 0.5 milligrams per cubic meter. Limited 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 228; Publication No. 77-157-A, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. Note: NIOSH Method S256 (filter collection, extraction by acetonitrile, and analysis by HPLC/UV) is also applicable. (Reference provided by reviewer.) Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B. Water Samples Laboratory Method See "Phenols and Other Compounds," Appendix B. A-900 ------- TOLUENE (CAS Number 108-88-3) RQ: 454 kg SAFETY INFORMATION; Flash point 40°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Organic Vapors," Appendix B. See "Toluene and Other Aromatics," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. Soil/Sediment Samples Field Method See "Volatile Species," Appendix B. Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for toluene. A known volume of air is drawn through a charcoal tube, desorbed with carbon disulfide, and the resulting 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 every 10 samples. The desorption effi- ciency and the results of the method-blank analysis should be used in the calculation of the results. A-901 ------- EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH) and validated over the range of 547 to 2182 milligrams per cubic meter in a 2-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. 3, Method S343; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-100 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of toluene in air samples. The absorbance at 13750 nm (727 cm~^) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 19 milligrams per cubic meter or 5 parts per million. No precision or accuracy information is furnished. A-902 ------- REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, Pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also; "Hazardos Organic Emissions," Appendix B. See also: "Hydrocarbon Odorants, Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Nitroaromatics," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-903 ------- TOLUENEDIAMINE (CAS Number 95-80-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. ~CAUTION: The user should obtain additional toxicity/hazara information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Toluenediamine in air samples can be determined by gas chromatography using a thermionic specific detector (GC/TSD). The analyte is collected in a glass impinger filled with 0.05 M sulfuric acid. A ten-fold enrichment is achieved by adding solid sodium hydroxide and toluene to the sample solution and centrifuging. An aliquot of the toluene layer is injected into the GC instrument. This method enables the 2,4- and 2,6-isomers of toluenediamine to be determined separately. INTERFERENCES: Large amounts of N-methylmorpholine can affect the extraction of toluene- diamine. QUALITY CONTROL: Amine standards should be processed the same way as the samples. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. The method detection limit is approximately 3 micrograms of toluenediamine per cubic meter of air. A-904 ------- REFERENCE: Audunsson, G.; Mathiasson, L. "Simultaneous Determination of Amines and Isocyanates in Working Atmospheres by Gas-Liquid Chromatography," J. Chromatogr., 261. 1983, pp. 253-264. COST INFORMATION: Cost per sample for anlaysis by this method is approximately $130 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-905 ------- TOLUENE DIISOCYANATE (CAS Number 584-84-9) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for toluene diisocyanate in air may be performed by use of a detector tube. A 2.5-liter air sample is collected and analyzed with a hand- operated bellows pump and a toluene diisocyanate gas detector tube (Draeger® 67 24501, or equivalent). A positive result is indicated by a color change in the tube from white to orange. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 0.15 to 1.5 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105, National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-906 ------- Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: High-performance liquid chromatography (HPLC) may be used to analyze air samples for toluene diisocyanate. A known volume of air is passed through a tube coated with 9-(N-methylaminomethyl)anthracene. The urea derivative, 2,4-TDIU, formed is desorbed with N,N-dimethylformamide (DMF) and the resulting solution is analyzed by HPLC with ultraviolet absorbance (UV) detection. Alternatively, the sample is collected in a tube containing glass wool coated with N-Ł-nitrobenzyl-N-propylamine, extracted with dichloromethane, and the resulting solution is analyzed by HPLC with UV detection at 254 nm. INTERFERENCES: N-p_-nitrobenzyl-N-propylamine on glass wool is unstable and interferences can result if sampling tabes are exposed to light or stored in the dark at room temperature. Compounds with the same retention time as the analyte can inter- fere. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: The 9-(N-methylaminomethyl)anthracene method is not EPA-approved; it is sensitive to concentrations of approximately 1 milligram per cubic meter, using a 15-liter sample. The N-p-nitrobenzyl-N-propylamine method has been proposed by the National Institute for Occupational Safety and Health for use over the range of 0.017 to 0.58 milligrams per cubic meter. 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 326; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980. A-907 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Toluene diisocyanate in air samples can be measured by colorimetry- A known volume of air is passed through a sampling tube containing an absorbing solution that hydrolyzes the toluene diisocyanate to a toluenediamine deriva- tive. The diamine is diazotized by a sodium nitrite-sodium bromide solution, and the diazo salt is coupled with N-(l-naphthyl)ethylenediamine to form a colored compound. The absorbance of the resulting solution at 550 nm is measured. INTERFERENCES: Any aromatic amine may form a diazo salt and a colored compound, and may be a positive interference. QUALITY CONTROL: A method-blank and standards are prepared and processed with the samples. EPA/TECHNICAL STATUS: i j This is an operational method according to the National Institute for Occupational Safety and Health, for use over the range of 6.5 to 916 micrograms per cubic meter, using a 20-liter sample. No precision or accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. Method P&CAM 141; Publication No. 75-121, U.S. DHHS: Cincinnati, 1974. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 141; Publication No. 77-157-A, U.S. DREW: Cincinnati, 1977. American Society for Testing and Materials, 1983 Annual Book of ASTM Standards, Vol. 11.03, D3422-75T; ASTM: Philadelphia, 1983T~ COST INFORMATION: Cost per sample for analysis by this method is approximately $36 (list), plus sampling costs. A-908 ------- Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-909 ------- o-TOLUIDINE HYDROCHLORIDE (CAS Number 636-21-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatic Amines," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aromatic Amines," Appendix B. A-910 ------- TOXAPHENE (CAS Number 8001-35-2) RQ: 0.454 kg SAFETY INFORMATION; Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method METHOD SUMMARY: Toxaphene in water may be detected by thin-layer chromatography (TLC). An isopropanol-ammonia (95:5) solvent system is used. Visualization is achieved by a spray reagent consisting of silver nitrate in acetone and ammoniacal solution, or diphenylamine in acetone, followed by exposure to UV light. (This method is described by Thielemann, H.; Grahneis, H. Z. Gesamte Hyg. Ihre Grenzgeb, 24(3), 1978, p. 214, and is summarized from German in the reference given below.) INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to amounts of toxaphene over 0.06 micrograms, or concentrations above approximately 1 milligram per liter. REFERENCES: Pesticides Abstracts, 11(9), 78-2243, 1978, p. 561. A-911 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $20-35 (list). Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of toxaphene in air samples. A known volume of air is drawn through a cellulose membrane filter and the filter is extracted with petroleum ether. An aliquot of the extract is injected into a gas chromatograph equipped with an electron capture detector (GC/ECD). INTERFERENCES: Toxaphene is composed of a mixture of compounds that are retained by the chromatograph over a range of time. Any compound showing an electron capture response or the same retention time band will interfere. QUALITY CONTROL: A method blank should be processed along with the samples. EPA/TECHNICAL STATUS: This method has been approved by the National Institute for Occupational Safety and Health (NIOSH) and validated over the range of 0.23 to 1.12 millli- grams per cubic meter, using a 15-liter sample. Precision and accuracy informa- tion is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set F. Method S67; PB-246 149 (NTIS), U.S. DHEW: Cincinnati, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S67; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-90 (list), plus sampling costs. See also: "Chlorinated Pesticides," Appendix B. A-912 ------- Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds, Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. A-913 ------- 2,4,5-TP ACID (CAS Number 93-72-1) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B, Water Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. A-914 ------- 2,4,5-TP ACID ESTERS (CAS Number 32534-95-5) RQ; 45-4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. Water Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. A-915 ------- TRICHLORFON (CAS Number 52-68-6) RQ: 454 kg SAFETY INFORMATION: Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. See "Organophosphorus and Carbamate Insecticides," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Organophosphorus and Carbamate Insecticides," Appendix B, Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. See "Organophosphorus Pesticides," Appendix B. A-916 ------- 1,2,4-TRICHLOROBENZENE (CAS Number 120-82-1) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Chlorobenzenes, Appendix B. See "Halogenated, Aromatic, and Other Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated and Other Organic Contaminants, Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. A-917 ------- 1,1,1-TRICHLOROETHANE (CAS Number 71-55-6) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for 1,1,1-trichloroethane in air may be performed by use of a detector tube. A 1-liter air sample is collected and analyzed with a hand- operated bellows pump and a trichloroethane gas detector tube (Draeger® CH 21101, or equivalent). A positive result is indicated by a color change in the tube from gray to brownish-red. The method is based on liberation of chlorine from trichloroethane by chromate, followed by the reaction of the chlorine with Ł-toluidine. INTERFERENCES: Trichloroethylene and tetrachloroethylene will also give positive results. Aromatic compounds can cause the 1,1,1-trichloroethane determination to be low. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 300 to 3000 milli- grams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e;~~ National Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-918 ------- See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for 1,1,1-trichloroethane. 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 disulfide 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 10 samples. The desorption effi- ciency and the results of the method-blank analysis should be used in the calcu- lation of the results. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 904 to 3790 milligrams per cubic meter, using a 3-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J, Method S328; PB-263 959 (NTIS), U.S. DHEW: Cincinnati, 1976. U.S. Departemtn of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S328; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. A-919 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Appendix B. See also: "Fumigants," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds, See also: "Hazardous Organic Emissions," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated Ethers and Other Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Low-Molecular Weight Halogenated Hydrocarbons," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B. See "Volatile Organic Compounds," Appendix B. A-920 ------- 1,1,2-TRICHLOROETHANE (CAS Number 79-00-5) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for 1,1,2-trichloroethane. 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 disulfide 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: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with every 10 samples. The desorption effi- ciency and the results of the method-blank analysis should be used in the calcu- lation of the results. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 26 to 111 milligrams per cubic meter, using a 10-liter sample. The method is capable of measurement of A-921 ------- much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J, Method S134; PB-263 959 (NTIS). U.S. DREW: Cincinnati, 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S134; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of 1,1,2-trichloroethane in air samples. The absorbance at 10600 nm (943 cm"-'-) is measured, using a 10-meter pathlength cell. Air can be sampled in a Saran or Mylar® plastic bag; approximatley 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 that 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 pathlength cell, is 55 milligrams per cubic meter or 10 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis. 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. A-922 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Organic Vapors," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated Ethers and Other Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-923 ------- TRICHLOROETHYLENE (CAS Number 79-01-6) RQ: 454 kg SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic. Flash point 90°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Analysis for trichloroethylene in air may be performed by use of a detector tube. A 0.3- to 0.5-liter air sample is collected and analyzed with a hand- operated bellows pump and a trichloroethylene 2/a gas detector tube (Draeger® 67 28541, or equivalent). A positive result is indicated by a color change from pale gray to orange in the tube. The method is based on the generation of chlorine from trichloroethylene by chromate, followed by reaction of the chlorine with Ł-toluidine. INTERFERENCES: Free halogens, hydrogen halides, and readily-cleaved halogenated hydrocarbons will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 10 to 1100 milli- grams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; National Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e;" National Draeger: Pittsburgh, 1981. A-924 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). See also: "Organic Vapors," Appendix B. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method See "Volatile Species," Appendix B. Water Samples Field Method See "Volatile Species," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for tri- chloroethylene. 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 disulfide and analysis of the resulting solution by gas chromato- graphy 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 every 10 samples. The desorption effi- ciency and the results of the method-blank analysis should be used in the calcu- lation of the results. EPA/TECHNICAL STATUS; This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 519 to 2176 milligrams per cubic meter, using a 3-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J, Method S336; PB-263 959 (NTIS), U.S. DHEW: Cincinnati, 1976. A-925 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S336; Publication No. 77-157-C, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of trichloroethylene in air samples. The absorbance at 11780 nm (849 cm~l) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 11 milligrams per cubic meter or 2 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Fumigants," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. A-926 ------- See also: "Volaitle Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix A. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated Ethers and Other Compounds," Appendix B. See "Halogenated Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix A. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B, See "Volatile Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-927 ------- TRICHLOROMETHANESULFENYL CHLORIDE (CAS Number 594-42-3) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-928 ------- TRICHLOROMONOFLUOROMETHANE (CAS Number 75-69-4) RQ: 2270 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Carbon Tetrachloride and Trichloromonofluoromethane," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for tri- chloromonofluoromethane. The analysis is performed by passage of 4 liters of air through a charcoal sampling tube, followed by desorption of the analyte with carbon disulfide and analysis of the resulting solution by gas chromato- graphy with flame ionization detection (GC/FID). INTERFERENCES: High humidity can severely decrease the capacity of the sampling appara- tus . QUALITY CONTROL: The efficiency of desorption must be determined and analytical results corrected accordingly. A method blank should be analyzed with each set of 10 or fewer samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health, and has been validated over the range of 2,390 to 10,500 milligrams per cubic meter, using a 4-liter sample. Precision and accuracy information is furnished. A-929 ------- REFERENCE; U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S102; Publication No. 77-157-B, U.S. DHEWl Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Halogenated Vapors," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-930 ------- TRICHLOROPHENOL (CAS Number 25167-82-2) RQ: 4.54 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Chlorinated Phenols," Appendix B. See "Phenolics," Appendix B. A-931 ------- 2,4,5-TRICHLOROPHENOL (CAS Number 95-95-4) RQ: 4.54 kg SAFETY INFORMATION: Potentially carcinogenic CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Chlorinated Phenols," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Phenolics," Appendix B. A-932 ------- 2,4,6-TRICHLOROPHENOL (CAS Number 88-06-2) RQ: 4.54 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Chlorinated Phenols," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phenols," Appendix B. Water Samples Laboratory Method See "Acid Extractable Organic Compounds," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. See "Trace Organic Contaminants," Appendix B. A-933 ------- TRIETHANOLAMINE DODECYLBENZENE SULFONATE (CAS Number 27323-41-7) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Anionic Detergents," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Alkyl Benzene Sulfonates," Appendix B. A-934 ------- TRIETHYLAMINE (CAS Number 121-44-8) RQ: 2270 kg SAFETY INFORMATION: Flash point 20°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Amines: Triethylamine and Other Amines," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Volatile Species," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Triethylamine in air samples can be measured by gas chromatography. A known volume of air is drawn through a midget bubbler containing 0.05-molar sulfuric acid. The resulting solution is made alkaline, and an aliquot is analyzed by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: Any compound with the same retention time as triethylamine under the given operating conditions is an interferent. QUALITY CONTROL: A blank is analyzed with every 10 samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 50 to 193 milligrams per cubic meter, using a 100-liter sample. Precision and accuracy information is furnished. A-935 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set K, Method S152; PB-254 227 (NTIS). U.S. DREW: Cincinnati, 1976.'"~~ U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtyical Methods. 2nd ed., Vol. 3, Method S152; Publication No. 77-157-C, U.S. DHEWl Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Aliphatic Amines," Appendix B. Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Amines," Appendix B. A-936 ------- TRIMETHYLAMINE (CAS Number 75-50-3) RQ: 454 kg SAFETY INFORMATION: Flash point: gas. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: The concentration of trimethylamine in air may be determined by using a gas detector tube. A 0.4-liter air sample is collected and analyzed with a portable pump and an ammonia gas detector tube (Bendix/Gastec® 3M, or equivalent) A positive result is indicated by a color change from purple to dull yellow in the tube, due to the amines reacting with phosphoric acid. INTERFERENCES: Ammonia, amines, and diamines will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 6 to 120 milligrams per cubic meter. REFERENCE: Bendix, Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix Corp.: Largo, Florida, p. 22. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). Soil/Sediment Samples Field Method Water Samples Field Method A-937 ------- Air Samples Laboratory Method METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of trimethylamine in air samples. The absorbance at 12100 nm (826 cm'1) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 12 milligrams per cubic meter or 5 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Low Molecular Weight Aliphatic Amines," Appendix B. See also: "Methylamines," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-938 ------- See "Aliphatic Amines," Appendix B. A-939 ------- ^yjn-TRINITROBENZENE (CAS Number 99-35-4) RQ: 0.454 kg SAFETY INFORMATION: Explosive. Potentially chronically toxic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitroaromatics," Appendix B. A-940 ------- TRIS(2,3-DIBROMOPROPYL) PHOSPHATE (CAS Number 126-72-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-941 ------- TRYPAN BLUE (CAS Number 72-57-1) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method A-942 ------- 2,4,5-T SALTS (CAS Number 13560-99-1) RQ: 45.4 kg SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. Water Samples Laboratory Method See "Chlorinated Phenoxy Acid Herbicides," Appendix B. A-943 ------- URACIL MUSTARD (CAS Number 66-75-1) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity. Potentialy carcinogenic. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-944 ------- VINYL ACETATE (CAS Number 108-05-4) RQ: 227° kg SAFETY INFORMATION: Flash point 18°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: The concentration of vinyl acetate in air may be determined by using a gas detector tube. A 0.4-liter air sample is collected and analyzed with a portable pump and a vinyl acetate detector tube (Bendix/Gastec® 143, or equivalent). A positive result is indicated by a color change from white to dark brown in the tube, due to vinyl acetate reacting with xylene, followed by dehydration of the product by sulfuric acid. INTERFERENCES: Aldehydes, acrolein, styrene, and formaldehyde will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will detect concentrations of approximately 15 to 35 milligrams per cubic meter. REFERENCE: Bendix, Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix Corp.: Largo, Florida, p. 97- COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method A-945 ------- Water Samples Field Method Air Samples Laboratory Method Note: NIOSH Method P&CAM 278 (chromosorb 107 adsorption, desorption, and analy- sis by GC/FID) is applicable. (Reference provided by reviewer). See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-946 ------- VINYL CHLORIDE (CAS Number 75-01-4) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). Flash point: gas. Potentially carcinogenic. Potentially chronically toxic. ^ CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Vinyl Chloride and Other Chlorinated Hydrocarbons," Appendix B. See "Vinyl Chloride, Benzyl Chloride, Allyl Chloride, and Dichloro- ethylene," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Vinyl chloride in air samples can be determined by gas chromatography. A known volume of air is drawn through a charcoal tube. The analyte is desorbed with carbon disulfide and an aliquot 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 is processed along with the sample tubes. 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 0.008 to 5.2 milligrams per cubic meter, using a 5-liter sample. Precision and accuracy information is furnished. A-947 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, Method P&CAM 178; 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 178; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Analysis for vinyl chloride in air can be performed by passage of approxi- mately 70 liters of air through a Spherocarb® cartridge, thermal desorption of the adsorbed vinyl chloride, and analysis of the desorbed vapors by gas chroma- tography with photoionization detection (GC/PID). INTERFERENCES: Certain volatile hydrocarbons may interfere. QUALITY CONTROL: Blanks and standards should be run as part of a quality control program. EPA/TECHNICAL STATUS: This method is approved by the Alberta Environmental Centre, Alberta, Canada. Single-laboratory precision and accuracy information is given. This method is sensitive to concentration levels of vinyl chloride above 3 micrograms per cubic meter. REFERENCES: Alberta Environmental Centre, Methods Manual for Chemical Analysis of Atmospheric Pollutants, 2nd ed., Method 16060; Alberta Environment: Vegreville, Alberta, Canada, 1981. Determination of Vinyl Chloride in the Atmosphere, Ontario Ministry of the Environment: Ontario, 1975. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. A-948 ------- Air Samples Laboratory Method 3 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of vinyl chloride in air samples. The absorbance at 10630 nm (941 cm"1) is measured, using a 10-meter pathlength 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 that 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 pathlength cell, is 25 milligrams per cubic meter or 10 parts per million. No precision or accuracy information is furnished. REFERENCE: American Public Health Association, "Infrared Absorption Spectroscopy," In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-84. COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Gaseous Contaminants," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-949 ------- Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-950 ------- WARFARIN (CAS Number 81-81-2) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Warfarin in air samples can be measured by high-performance liquid chromatography (HPLC). A known volume of air is drawn through a polytetra- fluoroethylene filter, the filter is extracted with methanol, and an aliquot of the resulting solution is analyzed by an HPLC instrument equipped with ultra- violet absorbance (UV) detection. INTERFERENCES: Any compound with the same retention time as warfarin can interfere. QUALITY CONTROL: One method blank is processed for every 10 samples taken. EPA/TECHNICAL STATUS: This method has been proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.054 to 0.244 milligrams per cubic meter, using a 408-liter sample. Precision and accuracy information is furnished. A-951 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol. 6, Method P&CAM 313; Publication No. 80-125, U.S. DHHS: Cincinnati, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Phenols and Other Compounds," Appendix B. Water Samples Laboratory Method See "Phenols and Other Compounds," Appendix B. A-952 ------- XYLENE (CAS Number 1330-20-7) RQ: 454 kg SAFETY INFORMATION: Flash point 81 to 90°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Toluene and Other Aromatics," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Hydrocarbon Odorants," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Volatile Organic Solvents," Appendix B. See "Xylenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-953 ------- m-XYLENE (CAS Number 108-38-3) RQ: 454 kg SAFETY INFORMATION: Flash point 81 to 90°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Toluene and Other Aromatics," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Hydrocarbon Odorants," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Xylenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Organic Compounds," Appendix B. A-954 ------- o-XYLENE (CAS Number 95-47-6) RQ: 454 kg SAFETY INFORMATION: Flash point 81 to 90°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Toluene and Other Aromatics," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B, See "Hydrocarbon Odorants," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Xylenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-955 ------- Ł-XYLENE (CAS Number 106-42-3) RQ: 454 kg o SAFETY INFORMATION: Flash point 81 to 90 F. ~~ CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Toluene and Other Aromatics," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Hydrocarbon Odorants," Appendix B. See "Volatile Organic Compounds," Appendix B. See "Xylenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B, A-956 ------- XYLENOL (CAS Number 1300-71-6) RQ: 454 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-957 ------- APPENDIX B Contents B-i ------- CAUTION The following information is presented in each volume containing the appendices to the report "Annotated Bibliography of Analytical Methods for CERCLA Hazardous Substances." 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. The Method Descriptions presented 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 at the beginning of the Method Descriptions which tells the name for each substance used throughout the report. See the text of the report for a detailed description 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. B-ii ------- CONTENTS - APPENDIX B Part I. Field Methods A. Inorganic Substances Aluminum g-4 Ammonia and Ammonium Compounds B-6 Antimony B-8 Arsenic B-ll Beryllium B-13 Cadmium B-14 Calcium B-17 Chromium B-19 Chromates B-19 Chromic Acid and Strontium Chromate B-20 Chromium B-21 Chromium, Hexavalent B-27 Cobalt B-28 Copper B-30 Cyanides B-37 Fluorides B-42 Fluorides and Other Compounds B-43 Halides , Cyanides, and Other Compounds B-45 Hydrazines B-47 Hydrazines and Other Compounds B-48 Hydroxides B-50 Iron B-53 Iron Compounds (Particulate) B-51 Lead B-55 Lead and Compounds (Particulate) B-61 Mercury B-63 Nickel and Compounds (Particulate) B-65 Nickel Ions B-67 Nitrate Ions B-68 Potassium B-70 Selenium B-71 Silver B-74 Sulfides B-75 Sulfite Ions B-78 Zinc B-81 Zinc and Compounds (Particulate) B-79 Zirconium B-85 B-iii ------- Contents (continued) Part I. Field Methods B. Organic Substances Page Acetates • B-87 Acetic Acid and Acetic Anhydride B-88 Acetone and Methyl Ketones B-89 Aldehydes B-91 Amines B-92 Amines B-92 Aromatic Amines B-93 Aromatic Primary Amines B-94 Triethylamines and Other Amines B-95 Anionic Detergents B-96 Aromatics and Other Compounds B-97 ii-Butyl Alcohol and Isobutyl Alcohol B-99 Carbon Tetrachloride and Trichloromonofluoromethane B-100 Chlorobenzene and Dichlorobenzenes B-101 Cholinesterase-Inhibiting Compounds B-102 Cyclohexanone and Furfural B-104 Ethylene Oxide, 1,4-Dioxane, and Propylene Oxide B-105 Ethyl Ether and Tetrahydrofuran B-106 Geminal Trihalogenated Compounds B-107 Mercapto Compounds B-108 Nitro Compounds B-109 Organic Acids B-110 Adipic and Fumaric Acids B-110 Formic Acid and Propionic Acid B-lll Organic Vapors B-112 Organophosphorus Pesticides B-114 Phenols B-115 Cresols B-115 Phenolic Compounds B-116 Phenols B-118 Phosphorodithioates B-119 Polychlorinated Biphenyls and Chlorinated Pesticides B-121 Toluene and Other Aromatics B-122 Vinyl Chloride and Other Chlorinated Hydrocarbons B-124 Vinyl Chloride, Benzyl Chloride, Allyl Chloride, and 1,1-Dichloro- ethylene B-125 Volatile Organic Compounds B-127 Volatile Species B-129 B-iv ------- Contents (Continued) Part II. Laboratory Methods A. Inorganic Substances Acid Anions B-135 Aluminum B-137 Ammonia B-146 Antimony B-156 Arsenic B-168 Arsines B-188 Beryllium B-190 Cadmium B-199 Calcium B-208 Chlorides B-217 Chromium B-223 Chromic Acid and Chromates B-223 Chromium B-225 Chromium, Hexavalent B-239 Chromium, Trivalent B-245 Cobalt B-246 Copper B-253 Cyanides B-263 Fluorides B-269 Hydrazines B-281 Inorganic Acids B-282 Iodides and Bromides B-283 Iron B-285 Lead B-297 Lead and Cadmium B-312 Mercury B-314 Nickel B-320 Nitrates B-332 Nitrates and Sulfates B-338 Nitrogen Dioxide and Nitric Oxide B-342 Phosphorus B-345 Potassium B-351 Selenium B-359 Silver B-370 Sodium B-376 Strontium B-384 Sulfates (Particulate) B-389 Sulfides B-395 Sulfites B-399 Sulfur Compounds (Particulate) B-401 Thallium B-403 Thiocyanates B-410 Uranium B-411 Vanadium B-413 Zinc B-421 Zirconium B-434 B-v ------- Contents (continued) Part II. Laboratory Methods B. Organic Substances Acetates B-437 Acid and Base/Neutral Extractable Organics B-439 Acid Extractable Organic Compounds B-442 Aliphatic Aldehydes B-444 Aliphatic Amines B-445 Aliphatic Compounds B-447 Alkaloids B-448 Alkyl Benzene Sulfonates B-449 Amines B-453 Amines and Alcohols B-454 Amines and Other Nitrogen Compounds B-455 Aromatic Amines B-456 Aromatic Primary Amines B-460 Aromatic Volatile Organic Compounds B-461 0-Aryl Carbamate Pesticides . . . « B-465 Base/Neutral Extractable Organic Compounds B-466 Basic Organic Compounds B-469 Benzal Chloride, Benzotrichloride, and Benzyl Chloride B-470 Benzidine and Congeners B-471 Carbamate and Urea Pesticides B-473 Carbamate Pesticides B-475 Carboxylic Acids B-477 Chlorinated and Other Organic Contaminants B-478 Chlorinated Benzenes B-479 Chlorinated Ethers and Other Compounds B-481 Chlorinated Hydrocarbons B-483 Chlorinated Phenoxy Acid Herbicides B-487 Chlorinated Pesticides B-497 Chlorinated Phenols B-499 Chlorobenzene B-501 B-Chloroethers B-502 Cresols B-503 Dinitrobenzenes . . . • B-504 Dinitrotoluenes B-505 Diuron and Pyrethrins B-506 Explosives B-507 Fumigants B-508 Gaseous Contaminants B-509 Halogenated, Aromatic, and Other Compounds B-511 Halogenated Compounds B-513 Halogenated Vapors B-514 Halogenated Volatile Organic Compounds B-515 Hazardous Compounds B-521 Hazardous Organic Emissions B-523 B-vi ------- Contents (continued) Part II. Laboratory Methods B. Organic Substances Herbicides B-524 Hydrocarbon Odorants B-526 Low-Molecular-Weight Aliphatic Amines B-527 Low-Molecular-Weight Halogenated Hydrocarbons B-528 Mercaptans B-529 Methylamines B-530 N-Methylcarbamates B-531 Naphthylamines B-532 Nitriles B-533 Nitroaromatic Compounds and Benzonitrile B-534 Nitroaromatics B-535 Nitroaromatics and Cyclic Ketones B-537 Nitrogenous Drugs B-541 Nitrophenols B-542 N-Nitrosamines B-543 Nitroso Compounds B-546 N-Nitroso Compounds B-548 Non-Halogenated Volatile Organic Compounds B-549 Non-Volatile Organic Compounds B-553 Organic Acids B-555 Organic Compounds B-557 Organic Vapors B-559 Organochlorine and Organophosphorus Pesticides B-561 Organochlorine Pesticides B-563 Organochlorine Pesticides and PCB's B-655 Organophosphorus and Carbamate Insecticides B-573 Organophosphorus Compounds B-574 Organophosphorus Pesticides . B-576 Particulate Aromatic Hydrocarbons B-584 Pesticide Residue B-586 Pesticides B-588 Phenolic Compounds B-591 Phenolics B-591 Phenols B-596 Phenols and Other Compounds B-600 Phthalate Esters B-602 Polycyclic Aromatic Hydrocarbons B-606 Primary and Secondary Amines B-631 Substituted Nitriles and Tetranitromethane B-633 Sulfur-Containing Gases B-634 Thioic Acid Ester Pesticides B-635 Thioureas and Other Compounds B-636 Trace Organic Contaminants B-637 Volatile Alcohols and Other Organic Compounds B-639 B-vii ------- Contents (continued) Part II. Laboratory Methods B. Organic Substances Volatile Carbonyl Compounds -, B-641 Volatile Chlorinated Aliphatic Hydrocarbons B-642 Volatile Organic Acids B-643 Volatile Organic Compounds B-644 Volatile Organic Solvents B-655 Volatile Organics B-652 Weak Acids B-658 Xylenes B-659 B-viii ------- Appendix B Multi-Compound Methods Part I. Field Methods A. Inorganic Substances B. Organic Substances Part II. Laboratory Methods A. Inorganic Substances B. Organic Substances B-l ------- Part I. Field Methods B-2 ------- A. Inorganic Substances B-3 ------- ALUMINUM Water Samples Field Method 1 Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Field analysis for aluminum ions from the above compounds in water samples can be performed by spectrophotometric analysis. A 50-milliliter water sample is treated with Eriochrome cyanine R indicator, and the re- sulting red-orange color is measured with a portable spectrophotometer. This method does not identify any specific aluminum-containing compound, but measures the total amount of aluminum in the sample. INTERFERENCES: High alkalinity can interfere, and significant fluoride concentrations cause errors. High levels of iron and chlorine interfere. An ascorbate reagent is added to remove iron interference. QUALITY CONTROL: Accuracy of the analysis can be tested by analysis of an aluminum standard solution. SENSITIVITY: This method is sensitive to concentration levels of aluminum above 50 micrograms per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, Hach Chemical Company: Ames, Iowa, 1975, pp. 2-8, 2-9. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-23 (list). B-4 ------- ALUMINUM Water Samples Field Method 2 Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Field analysis for aluminum ions from the above compounds in water samples can be performed by use of test sticks. A test stick (Quantofix®, or equivalent) is dipped briefly into the sample and the resulting color is compared with a color scale. This method is not used to identify any specific aluminum- containing compound, but to measure the total amount of aluminum in the sample. INTERFERENCES: Beryllium and copper interfere and may be removed by precipitation with potassium iodide and filtration. Citrate, tartrate, permanganate, phosphate, sulfide, sulfite, tetraborate, hydrosulfite, ferricyanide, and metabisulfite ions may cause the aluminum determination to be low. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 0 to 500 milligrams per liter. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers Brochure, 14th ed.; Gallard-Schlesinger Chemical Mfg. Corp. Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-5 ------- AMMONIA and AMMONIUM COMPOUNDS Compound Ammonia Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Ammonium Water Samples Field Method CAS Number Compound Acetate Benzoate Bicarbonate Bifluoride Bisulfite Carbamate Carbonate Chloride Chromate Citrate, Dibasic Dichromate Fluoborate Fluoride Hydroxide Oxalate 7664- 631- 1863' 1066- 1341' 10192' 1111 506' 12125 7788 3012 7789 13826 12125 1336 6009 5972 14258 -41-7 -61-8 -63-4 -33-7 -49-7 -30-0 -78-0 -87-6 -02-9 -98-9 -65-5 -09-5 -83-0 -01-8 -21-6 -70-7 -73-6 -49-2 Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Cupric Sulfate, Ammoniated Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferrous Ammonium Sulfate Nickel Ammonium Sulfate Zinc Ammonium Chloride CAS Number 131-74-8 16919-19-0 7773-06-0 12135-76-1 10196-04-0 14307-43-8 3164-29-2 1762-95-4 7783-18-8 7803-55-6 10380-29-7 1185-57-5 2944-67-4 55488-87-4 10045-89-3 15699-18-0 52628-25-8 14639-97-5 14639-98-6 METHOD SUMMARY: Field analysis for ammonia and the above ammonium compounds in water can be performed by colorimetric analysis for ammonia nitrogen. A 25-milliliter sample is treated with Nessler Reagent, and the intensity of the color is measured with a portable spectrophotometer. This method is not used to identify ammonia or any particular ammonium compound, but to measure the total ammonia content of the sample. INTERFERENCES: Iron and sulfide can interfere by causing turbidity. Hydrazine, glycine, various aliphatic and aromatic amines, organic chloramines, acetone, aldehydes, and alcohols may cause color or turbidity in the prepared samples and require distillation of the sample before analysis. Samples of more than 100 milli- grams per liter total hardness should be treated with Rochelle Salt. Tempera- tures above or below 20°C will cause higher or lower results. QUALITY CONTROL: No quality control procedures are given. B-6 ------- SENSITIVITY; This method is sensitive to concentration levels of 0.1 milligrams ammonia per liter or higher in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-75, 2-76. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-23 (list). B-7 ------- ANTIMONY Air Samples Field Method Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Field analysis for antimony ions from the above particulate compounds in air may be performed by filtration of air using a high-speed sampler and deter- mination of the amount of antimony present on the filter medium by X-ray fluo- rescence spectrometry. This method measures the total antimony concentration in the particulates in air, and does not distinguish between different antimony compounds. The method is non-destructive so that further analyses may be performed on samples after this test. The sample-collection time may be up to 8 hours, but analysis time of the collected samples is approximately 1 minute. INTERFERENCES: Polyvinyl chloride (PVC) filters are unacceptable, and glass-fiber filters are acceptable 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. SENSITIVITY: The method is sensitive to concentration levels greater than 180 micrograms of antimony, with a precision of 11 percent or better, and should be applicable over the range of 0.1 to 1.0 microgram per cubic meter- 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-8 ------- 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-9 ------- ANTIMONY Water Samples Field Method Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Field analysis for antimony ions from the above compounds in water can be performed by measurement using test papers. An antimony test paper strip (Quantofix®, or equivalent) is dipped briefly into the sample and compared visually to a color scale. A positive result is indicated by the appearance of orange-red spots on a yellow background on the test paper strip. Antimony(V) must be reduced to antimony(III) by the addition of magnesium before analysis. This method is not used to identify any particular antimony compound, but can be used to differentiate between the valence states of antimony in the sample. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control information is given. SENSITIVITY: This method is sensitive to concentration levels of 5 milligrams per liter or greater of antimony present in the sample in the absence of interferences. REFERENCES: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.; Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-10 ------- ARSENIC Soil/Sediment Samples Field Method Compound Arsenic Arsenic Acid Arsenic Bisulfide Arsenic Pentoxide Arsenic Trichloride Arsenic Trioxide Arsenic Trisulfide Cacodylic Acid METHOD SUMMARY: CAS Number 7440-38-2 1327-52-2 7778-39-4 1303-32-8 1303-28-2 7784-34-1 1327-53-3 1303-33-9 75-60-5 Compound Calcium Arsenate Calcium Arsenite Cupric Acetoarsenate Lead Arsenate Potassium Arsenate Potassium Arsenite Sodium Arsenate Sodium Arsenite CAS Number 7778- 52740- 12002- 7784- 7645- 10102- 7784- 10124- 7631- 7784- •44-1 •16-6 •03-8 •40-9 •25-2 •48-4 •41-0 •50-2 89-2 46-5 Field analysis for the above arsenic compounds in soil samples may be performed by pulverizing the samples, and determining the amount of arsenic present by X-ray fluorescence spectrometry. This method cannot be used to identify any specific arsenic compounds, but can be used to measure the total arsenic content of the sample. Analysis time of the prepared sample is approxi- mately 4 minutes. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for use over the range of 0 to 1 gram of arsenic per kilogram of soil, with a standard deviation of 5 milligrams per kilogram. REFERENCES: Columbia Scientific Industries Corporation, CSI Model 740 Compact Materials Analyzer, Application Note 83-171; Columbia Scientific Industries: Austin, Texas. Rhodes, J. R. ; Rautala, P. Application of a Microprocessor - Based Portable XRF Analyzer in Minerals Analysis, ARD Internal Report No. 368, Columbia Scientific Industries, Austin, Texas, June 1981. B-ll ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $39 (list), B-12 ------- BERYLLIUM Air Samples Field 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: Field analysis of air samples for beryllium ions from the above compounds can be performed by analysis of particulate matter from 0.5 to 2.0 cubic meters of air by a ring oven method. The filter paper from sampling is treated with ammonium acetate, the resulting beryllium-acetate complex is washed to the heated ring zone with deionized water, and determination of beryllium is made by application of morin reagent. Measurement of the amount of beryllium present is made by visual comparison to standards of the fluorescent intensity of the yellow-green beryllium complex under a UV lamp. This method cannot be used to identify any specific beryllium-containing compound, but can be used to measure the total beryllium content of the sample. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels of beryllium above 0.01 micrograms per cubic meter. REFERENCE: "Determination of Airborne Particulate Beryllium by the Ring Oven Technique," Environmental Pollutants-Selected Analytical Methods (Scope 6); W. Gallay, H. Egan, J. L. Monkman, R. Truhaut, P. W. West, G. Widmark, Eds.; Ann Arbor Science: Ann Arbor, 1975, p. 149. COST INFORMATION: No cost information has been obtained. B-13 ------- CADMIUM Air Samples Field 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: Field 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 can be used to measure total cadmium present in the sample, but not to differentiate between cadmium compounds or cadmium valence states. The method is non-destructive, so that further analyses may be per- formed 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. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels of cadmium above 120 micrograms with a precision of 15 percent at that level. The method is applic- able to 0.01 to 1.0 micrograms of cadmium 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 Iri 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-14 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-15 ------- CADMIUM Water Samples Field 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: Field analysis for cadmium compounds in water can be performed by color!- metric analysis. A 250-milliliter sample is treated with dithizone color reagi and extracted with chloroform, and the chloroform extract is analyzed for the resultant pink cadmium complex with a portable spectrophotometer. INTERFERENCES: Copper and silver concentrations above 2 milligrams per liter and bismuth concentrations over 80 milligrams per liter cause high results. Strong oxi- dants can cause high results, and sample pretreatment is necessary when high levels of oxidizing materials (such as chlorine) or organic matter, are present. Interferences from mercury and higher levels of copper, silver, and bismuth can be eliminated by pretreatment. This method cannot be used to identify any specific cadmium compound, but can be used to measure the total cadmium content of the sample. QUALITY CONTROL: Blanks should be analyzed with each set of samples, and a standard solution may be analyzed as a check on the accuracy of the test. SENSITIVITY: This method is sensitive to concentration levels of cadmium above 15 micr- ograms per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-23, 2-247" COST INFORMATION: The cost per sample for analysis by this method is approximately $22-37 (list). B-16 ------- CALCIUM Air Samples Field Method Compound Calcium Arsenate Calcium Arsenite Calcium Carbide Calcium Chromate Calcium Cyanide Calcium Dodecylbenzene Sulfonate Calcium Hypochlorite CAS Number 7778-44-1 52740-16-6 75-20-7 13765-19-0 592-01-8 26264-06-2 7778-54-3 METHOD SUMMARY: Field analysis for the above calcium compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry. The method is used to measure total calcium present in the sample, but not to differentiate between calcium compounds. 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. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels of calcium above 30 micro- grams of calcium, with a precision of 60 percent at that level, and 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 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-17 ------- 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-18 ------- CHROMATES Water Samples Field Method Compound Ammonium Chrornate Calcium Chromate Lithium Chromate Potassium Chromate Sodium Chromate Strontium Chromate CAS Number 7788-98-9 13765-19-0 14307-35-8 7789-00-6 7775-11-3 7789-06-2 METHOD SUMMARY: Analysis for the above chromates in water can be performed colorimetri- cally. A 25-milliliter sample is adjusted to an alkaline pH, and the intensity of the resulting yellow color is determined with a portable spectrophotometer. The method determines the concentration of total chromate in the sample, but does not identify any specific chromate-containing compounds. INTERFERENCES; Turbid samples may require filtration. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels of chromate ions above approximately 100 milligrams per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-33, 2-34. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-23 (list). B-19 ------- CHROMIC ACID AND STRONTIUM CHROMATE Air Samples Field Method Compound CAS Number Chromic Acid 11115-74-5 Strontium Chromate 7789-06-2 METHOD SUMMARY: Field analysis for chromic acid and strontium chromate in air may be performed by use of a detector tube. A 4-liter sample is collected and analyzed with a hand-operated bellows pump and a chromic acid gas detector tube (Draeger® 67 28681, or equivalent). A positive result is indicated by a violet coloration occurring in the tube from the reaction of the analyte with diphenylcarbazide. This method does not identify any particular compound, but measures the total amount of hexavalent chromium in the sample. INTERFERENCES: Other hexavalent chromium compounds also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY; This method is sensitive to concentration levels of chromic acid of approximately 0.1 to 0.5 milligrams per cubic meter. Strontium chromate is indicated with one-half the sensitivity of chromic acid. REFERENCES: National Draeger Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger, Inc.: Pittsburgh, December 1981. Edward G. Ligus, National Draeger Inc., Pittsburgh, personal communication, July 12, 1983. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). B-20 ------- CHROMIUM Air Samples Field Method Compound CAS Number Ammonium Chromate Ammonium Bichromate Calcium Chromate Chromic Acetate Chromic Acid Chromic Sulfate Chromium Chromous Chloride Lithium Chromate Potassium Chromate Potassium Bichromate Sodium Chromate Sodium Bichromate Strontium Chromate 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 METHOB SUMMARY: Field analysis for the above chromium compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry . The method measures total chromium present in the sample, and does not differentiate between chromium compounds or chromium 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. SENSITIVITY: The method is sensitive to concentration levels of chromium above 30 micrograms, with a precision of 60 percent at that level, and should be applic- able to levels of chromium above 1.0 microgram of chromium per cubic meter, for a 30-cubic-meter sample size. B-21 ------- 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-22 ------- CHROMIUM Soil/Sediment Samples Field 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 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: Field analysis for the above chromium compounds in soil samples may be performed by pulverizing the sample, then determining the amount of chromium present by X-ray fluorescence spectrometry. This method does not identify any specific chromium compound, but measures the total chromium content of the sample. Analysis time of the prepared sample is approximately 4 minutes. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for use over the range of 0 to 1000 milligrams of chromium per kilogram and has a standard deviation of approximately 25 milli- grams . REFERENCES: Columbia Scientific Industries Corporation, CSI Model 740 Compact Materials Analyzer, Application Note 83-171; Columbia Scientific Industries: Austin, Texas. B-23 ------- Rhodes, J. R.; Rautala, P. Applications of a Microprocessor - Based Portable XRF Analyzer in Minerals Analysis, ARD Internal Report No. 368; Columbia Scientific Industries, Austin, Texas, June 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $39 (list). B-24 ------- CHROMIUM Water Samples Field Method 1 Compound CAS Number Ammonium Chromate 7788-98-9 Chromic Acetate 1066-30-4 Chromic Acid 11115-74-5 Chromic Sulfate 10101-53-8 Chromium 7440-47-3 Chromous Chloride 10049-05-5 Potassium Chromate 7789-00-6 Sodium Chromate 7775-11-3 Strontium Chromate 7789-06-2 METHOD SUMMARY: Field analysis for the above chromium compounds in water samples can be performed by use of test sticks for the determination of chromium(III) and chromium(VI) ions. A test stick (Quantofix®, or equivalent) is dipped briefly into the sample and is compared with a color scale. This method does not identify any particular chromium-containing compound, but measures the total chromium content of the sample. INTERFERENCES: Ferric, cupric, and molybdate ion interferences may be eliminated by the addition of a small amount of oxalic acid. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: Chromium(VI) is indicated with approximately half the sensitivity of chromium(III). This method will semiquantitatively determine chroraium(VI) concentrations above approximately 5 milligrams per liter. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers Brochure, 14th ed.; Gallard-Schlesinger Chemical Mfg. Corp.; Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-25 ------- CHROMIUM Compound Ammonium Chromate Ammonium Bichromate Calcium Chromate Chromic Acetate Chromic Acid Chromic Sulfate Chromium Water Samples Field Method 2 CAS Number 7788-98-9 7789-09-5 13765-19-0 1066-30-4 11115-74-5 10101-53-8 7440-47-3 Compound CAS Number 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: Field analysis for the above chromium compounds in water samples can be performed by colorimetry. A 25-milliliter sample is treated with alkaline hypobromite to transform all chromium present to hexavalent chromium, 1,5- diphenylcarbohydrazide is added, and the intensity of the resultant purple color is determined with a portable spectrophotometer. The method does not identify any specific chromium-containing compound, but measures the total dissolved chromium content of the sample. INTERFERENCES: Interferences from turbidity can be overcome by centrifugation or filtra- tion. Large amounts of organic materials in the sample may inhibit the total oxidation of the sample. QUALITY CONTROL: A chromium standard solution should be prepared fresh daily for use as a check on method accuracy. SENSITIVITY: This method is sensitive to concentration levels of chromium above approx- imately 90 micrograms per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa1975, pp. 2-36, 2-37. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-25 (list). B-26 ------- CHROMIUM, HEXAVALENT Water Samples Field Method Compound Ammonium Chromate Ammonium Bichromate Calcium Chromate Chromic Acid Lithium Chromate METHOD SUMMARY: CAS Number 7788-98-9 7789-09-5 13765-19-0 11115-74-5 14307-35-8 Compound Potassium Chromate Potassium Bichromate Sodium Chromate Sodium Bichromate Strontium Chromate CAS Number 7789-00-6 7778-50-9 7775-11-3 10588-01-9 7789-06-2 Field analysis for the above hexavalent chromium compounds in water samples can be performed by colorimetric analysis for chromium(VI) ions. 1,5-Biphenyl- carbohydrazide is added to a 25-milliliter sample and the intensity of the resultant purple color is measured with a portable spectrophotometer. This method does not identify specific hexavalent chromium-containing compounds present, but measures the total hexavalent chromium content of the sample. INTERFERENCES: Mercury ions and levels of iron above 1 milligram per liter can interfere. Turbidity may require centrifugation or filtration of the sample. Interference from vanadium can be overcome by allowing 10 minutes before reading. QUALITY CONTROL: A hexavalent chromium standard solution can be analyzed to check the accuracy of the test. SENSITIVITY: The method is sensitive to concentration levels of hexavalent chromium above approximately 200 micrograms per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-35, 2-36. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-23 (list). B-27 ------- COBALT Soil/Sediment Samples Field Method Compound CAS Number Cobaltous Bromide 7788-43-7 Cobaltous Formate 544-18-3 Cobaltous Sulfamate 14017-41-5 METHOD SUMMARY: Field analysis for the above cobalt compounds in soil samples may be performed by pulverizing the sample and then determining the amount of cobalt present by X-ray fluorescence spectrometry. This method does not identify any specific cobalt compound, but measures the total cobalt content of the sample. Analysis time of the prepared sample is approximately 2 minutes. INTERFERENCES: No interferences are reported. QUALITY CONTROL; No quality control procedures are given. SENSITIVITY: This method is suitable for use over the range of 0 to 2 grams of cobalt per kilogram, with results plus or minus 20 milligrams per kilogram. REFERENCES: Columbia Scientific Industries Corporation, CSI Model 740 Compact Materials Analyzer, Application Note 83-171; Columbia Scientific Industries: Austin, Texas. Rhodes, J. R.; Rautala, P- Application of a Microprocessor - Based Portable XRF Analyzer in Minerals Analysis ARD Internal Report No. 368: Columbia Scientific Industries, Austin, Texas, June 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $39 (list). B-28 ------- COBALT Water Samples Field Method Compound CAS Number Cobaltous Bromide 7789-43-7 Cobaltous Formate 544-18-3 Cobaltous Sulfamate 14017-41-5 METHOD SUMMARY: Field analysis of water samples for the above cobalt compounds can be performed by use of test paper for cobalt(II) ions. A cobalt test-paper strip (Gallard-Schlesinger®, or equivalent) is dipped briefly into the sample and compared to a color scale. A positive result is indicated by blue spots on a white background on the test paper. This method does not identify specific cobalt(II) compounds, but indicates the total cobalt(II) present in the sample. INTERFERENCES: Iron and copper may interfere. QUALITY CONTROL; No quality control information is given. The test will qualitatively determine if a concentration of 25 milligrams per liter or greater of cobalt (II) is present in the sample in the absence of interferences. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers Brochure, 14th ed.; Gallard-Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION; The cost per sample for analysis by this method is approximately $3-5 (list). B-29 ------- COPPER Air Samples Field Method Compound CAS Number Copper Copper Cyanides Cupric Acetate Cupric Acetoarsenate Cupric Chloride Cupric Nitrate Cupric Oxalate Cupric Sulfate Cupric Sulfate, Ammoniated Cupric Tartrate 7440- 544- 142- 12002- 7447- 3251- 5893- 7758- 10380- 815- •50-8 92-3 •71-2 03-8 39-4 23-8 •66-3 98-7 •29-7 82-7 METHOD SUMMARY: Field analysis for the above copper compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry. The method measures total copper present in the sample, and does not differentiate between copper compounds or copper valence states. 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 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. SENSITIVITY: The method is sensitive to concentration levels of copper above 35 micro- grams, with a precision of 60 percent at that level, and should be applicable to levels of copper above 10 micrograms 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 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-30 ------- 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-31 ------- COPPER Soil/Sediment Samples Field Method Compound CAS Number Copper 7440-50-8 Copper Cyanides 544-92-3 Cupric Acetate 142-71-2 Cuprlc 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: Field analysis for the above copper compounds in soil samples may be performed by pulverizing the sample, then determining the amount of copper present by X-ray fluorescence spectrometry. This method does not identify any specific copper compound, but measures the total copper content of the sample. Analysis time of the prepared sample is approximately 4 minutes. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for use over the range of 0 to 1 grams of copper per kilogram of soil, with a standard deviation of 1.5 percent. REFERENCES: Columbia Scientific Industries Corporation, CSI Model 740 Compact Materials Analyzer, Application Note 83-171; Columbia Scientific Industries: Austin, Texas. Rhodes, J. R.; Rautala, P- Application of a Microprocessor-Based Portable XRF Analyzer in Minerals Analysis ARD Internal Report No. 368; Columbia Scientific Industries: Austin, Texas, June 1981. B-32 ------- COST INFORMATION; Cost oer sample for analysis by this method is approximately $39 (list) B-33 ------- COPPER Water Samples Field 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: Field analysis for the above copper compounds in water samples can be performed by spectrophotometric analysis for copper. Bicinchoninate color reagent is added to a 25-milliliter sample, and the intensity of the color of the purple complex formed is measured with a portable spectrophotometer. The method does not identify specific copper compounds, but measures the total copper content of the sample. INTERFERENCES: Interferences from turbidity can be removed by filtration or centrifuga- tion. Interferences from silver can be eliminated by addition of potassium chloride. Cyanide interference can be removed by additon of formaldehyde to the sample. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels above approximately 0.5 milligrams of copper per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis. 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-38, 2-39. B-34 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $25-40 t) • (list). B-35 ------- COPPER Water Samples Field 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: Field analysis of water samples for the above copper compounds can be performed by the use of test sticks for copper ions. A test stick (Quantofix®, or equivalent) is dipped briefly into the sample at pH 3 to 7, and is compared with a color scale. A positive test for copper compounds is indicated by a color change to red-violet. This method does not identify particular copper compounds and cannot distinguish between cupric and cuprous ions. INTERFERENCES; No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method will semi-quantitatively determine concentrations of approxi- mately 10 to 1000 milligrams per liter. REFERENCE; Gallard-Schlesinger, pH Indicator Papers and Test Papers Brochure, 14th ed.; Gallard-Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-36 ------- CYANIDES Air Samples Field Method Compound CAS Number Potassium Cyanide 151-50-8 Sodium Cyanide 143-33-9 METHOD SUMMARY: Field analysis of air for potassium cyanide, sodium cyanide can be per- formed by use of a detector tube. A 1-liter sample is collected and analyzed with a hand-operated bellows pump and a cyanide gas detector tube (Draeger® 67 28791, or equivalent). A positive result is indicated by a color change from orange-yellow to reddish in the tube as the cyanide reacts with sulfuric acid to form hydrogen cyanide, which in turn reacts with mercury chloride, indicated by methyl red. This method does not distinguish between different cyanide salts. INTERFERENCES; Free hydrogen cyanide is indicated immediately and discolors the entire tube. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentrations levels of cyanide of approxi- mately 2 to 15 milligrams per cubic meter. REFERENCES: National Draeger Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information Leaflet 4340.3e; National Draeger, Inc.: Pittsburgh, December 1981. Edward G. Ligus, National Draeger Inc., Pittsburgh, personal communication, June 29, 1983. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). B-37 ------- CYANIDES Soil/Sediment Samples Field Method Compound CAS Number Barium Cyanide 542-62-1 Calcium Cyanide 592-01-8 Copper Cyanides 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: A multi-step spot test can be used for the detection of the above cyanides in soil/sediment samples. A 1-gram sample is mixed with a magnesium chloride solution and methyl violet indicator in a small test tube. A second test tube, containing sodium hydroxide and a cadmium nitrate solution, is connected to the first. The first tube is heated, aluminum-treated hydrochloric acid is added, and nitrogen is bubbled through the two tubes. The contents of the second tube are centrifuged and hydrochloric acid and a buffer are added to the centri- fugate. Three drops of the resultant solution are mixed with a chloramine-T solution and pyridine-barbituric acid. If cyanide is present, a pink to violet color will appear. This method does not identify particular cyanide salts, but measures the cyanide content of the sample. INTERFERENCES: This test does not detect cyanide complexed with platinum, gold, or cobalt. Thiocyanate also responds to the test. QUALITY CONTROL: Magnesium chloride should be analyzed as a blank solution. The perfor- mance of the test should be checked daily with a 1-milliliter standard solution of cyanide (approximately 100 milligrams per liter). B-38 ------- SENSITIVITY; This method is sensitive to concentration levels of cyanide of 0.01 milli- grams or greater. REFERENCE: U.S. Environmental Protection Agency, Chemical Analytical Services for Low and Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid (Solicitation Number WS 82-A072), U.S. EPA: Washington, March 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $20-35 (list). B-39 ------- CYANIDES Water Samples Field Method Compound CAS Number Barium Cyanide 542-62-1 Calcium Cyanide 592-01-8 Copper Cyanides 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 7143-33-9 Zinc Cyanide 557-21-1 METHOD SUMMARY: Screening for the above cyanides in water may be performed by use of a colorimetric spot test. Three drops of sample are mixed with phosphate buffer until the pH is approximately 8. Chloramine-T solution and pyridine-barbituric acid are added, and a pink to red color appears if the concentration of cyanide is 0.06 milligrams per liter or greater. This method does not identify particular cyanide salts, but measures the total cyanide amenable to chlorina- tion in the sample. INTERFERENCES: This method should not be used if the sample is turbid or highly colored. Aldehydes, and thiocyanate can interfere. It may be necessary to add additional chloramine-T solution if a high reducing chemical content is found in the sample. QUALITY CONTROL: The performance of the test should be checked daily by analyzing a standard. SENSITIVITY: The method is sensitive to concentration levels of cyanide greater than 0.05 milligrams per liter. B-40 ------- 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, April 23, 1982. American Society for Testing and Materials, 1983 Annual Book of ASTM Standards, Vol. 11.02, D2036-82, Annex; ASTM: Philadelphia, 1983, p. 126. COST INFORMATION: The cost per sample for analysis by this method is approximately $10-18 (list). B-41 ------- FLUORIDES Air Samples Field Method Compound CAS Number Ammonium Bifluoride 1341-49-7 Ammonium Fluoride 12125-01-8 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 Zirconium Potassium 16923-95-8 Fluoride METHOD SUMMARY: Field analysis of air for the above fluorides can be accomplished by drawing air through wet filter paper impregnated with zirconium azoarsenate. The presence of fluoride ions is indicated by a change from light brown to a pink color, and the depth of the pink color is proportional to the amount of fluoride drawn through the paper. This method is non-specific and responds to all inorganic fluorides. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is semi-quantitative, and concentration levels of 6 to 10 milligrams per cubic meter are indicated with an uncertainty of approximately 1 milligram per cubic meter. REFERENCE: Harrold, G. C.; Hurlburt, R. V. "Device and Technique for Rapid Determination of Effluent Fluorides," Anal. Chem. . 21., 1949, pp. 1504-1506. COST INFORMATION: The cost per sample for analysis by this method is due entirely to sampling costs. B-42 ------- FLUORIDES AND OTHER COMPOUNDS Water Samples Field Method Compound Aluminum Sulfate Ammonium Bifluoride Ammonium Fluoride Ammonium Silicofluoride Antimony Trifluoride Beryllium Fluoride Chlorosulfonic Acid Ferric Fluoride Hydrochloric Acid Hydrogen Fluoride Lead Fluoride Nitrogen Dioxide Phosphorus Pentasulfide Sodium Bifluoride Sodium Fluoride Zinc Fluoride Zirconium Potassium Fluoride CAS Number 10043- 1341- 12125- 16919- 7783- 7787- 7790- 7783- 7647- 7664- 7783- 10102- 1314- 1333- 7681- 7783- 16923- •01-3 49-7 01-8 •19-0 •56-4 49-7 94-5 50-8 •01-0 39-3 •46-2 44-0 80-3 83-1 •49-4 49-5 •95-8 METHOD SUMMARY: Fluorides and certain other compounds may be detected in water samples by colorimetry. A 25-milliliter sample is treated with SPADNS color reagent and analyzed spectrophotometrically. Because the fluoride dissociates a portion of the colored lake into a colorless complex, the color becomes progressively lighter as the fluoride concentration increases. The resulting solution is compared to a distilled water blank using a spectrophotometer. INTERFERENCES: Color may be completely bleached at very high concentrations of fluorides or by positive interferents. Alkalinity, aluminum, chloride, ferric iron, phosphate, and sulfate interfere, and may be eliminated by distillation from an acidified solution before testing. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels above approximately 10 milligrams per liter. B-43 ------- REFERENCES: U.S. Environmental Protection Agency, Development of a Kit for Detecting Hazardous Material Spills in Waterways, Appendix B; EPA-600/2-78-055. uVs. EPA: Cincinnati, March 1978. Hach Chemical Company, Hach Wastewater Analysis Handbook; Hach Chemical Company: Ames, Iowa, 1978. American Public Health Association, Standard Methods for the Examination of Water and Wastewater, 15th ed.. Method 413C; APHA: Washington, 1981, pp. 337-339. COST INFORMATION: The cost per sample for analysis by this method is approximately $12-20 (list). B-44 ------- HALIDES, CYANIDES, AND OTHER COMPOUNDS Water Samples Field Method CAS Number Compound CAS Number Acetone Cyanohydrin 75-86-5 Acetyl Bromide 506-96-7 Acetyl Chloride 75-36-5 Ammonium Chloride 12125-02-9 Ammonium Sulfide 12135-76-1 Antimony Pentachloride 7647-18-9 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Arsenic Trichloride 7784-34-1 Barium Cyanide 542-62-1 Benzoyl Chloride 98-88-4 Beryllium Chloride 7787-47-5 Cadmium Bromide 7789-42-6 Cadmium Chloride 10108-64-2 Calcium Cyanide 592-01-8 Calcium Hypochlorite 7778-54-3 Carbaryl 63-25-2 Chlorine 7782-50-5 Chlorosulfonic Acid 7790-94-5 Cobaltous Bromide 7789-43-7 Cupric Chloride 7447-39-4 Cyclohexane 110-82-7 Diquat 85-00-7 2764-72-9 METHOD SUMMARY: Halide, cyanide, and certain other ions from the above compounds in water samples may be detected by spectrophotometry. A filtered 25-milliliter sample is mixed with a ferric ion solution and mercuric thiocyanate. The light orange to reddish-brown color change in the resultant solution is indicative of a positive result and is measured spectrophotometrically• This method is not specific for any individual compound or ion, but will respond to any ions resulting from the above compounds, as well as others. INTERFERENCES: No interferences are reported. QUALITY CONTROL: A 25-milliliter distilled water blank is treated identically and is used to compare samples by aid of a spectrophotometer. Compound Ferric Chloride Ferrous Chloride Hydrogen Cyanide Lead Chloride Lead Iodide Mercuric Cyanide Nickel Chloride Phosgene Phosphorus Oxychloride Phosphorus Pentasulfide Phosphorus Trichloride Potassium Cyanide Sodium Cyanide Sodium Hydrosulfide Sodium Hypochlorite Zinc Ammonium Chloride Zinc Bromide Zinc Chloride Zinc Cyanide 7705- 7758- 74- 7758- 10101- 592- 7718- 37211- 75- 10025- 1314- 7719- 151- 143- 16721- 7681- 10022- 52628- 14639- 14639- 7699- 7646- 557- •08-0 •94-3 •90-8 •95-4 •63-0 •04-1 •54-9 05-5 •44-5 87-3 •80-3 •12-2 •50-8 33-9 •80-5 52-9 •70-5 •25-8 •97-5 •98-6 •45-8 •85-7 •21-1 B-45 ------- SENSITIVITY: This method is sensitive to concentration levels greater than approximately 10 milligrams per liter. REFERENCE; U.S. Environmental Protection Agency, Development of a Kit for Detecting Hazardous Material Spills in Waterways, Appendix B; EPA-600/2-78-055, U.S. EPA: Cincinnati, March 1978. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-25 (list). B-46 ------- HYDRAZINES Water Samples Field Method Compound CAS Number 1,1-Dimethylhydrazine 57-14-7 1,2-Dimethylhydrazine 540-73-8 Hydrazine 302-01-2 METHOD SUMMARY; Field analysis for the above hydrazines in water can be performed by colorimetry. A 25-milliliter sample is treated with a color reagent containing p_-dimethylaminobenzaldehyde, and the intensity of the yellow color is measured with a portable spectrophotometer. This method does not identify any particular compound, but responds to all of the above substances. INTERFERENCES: High levels of color and/or turbidity interfere, and require comparison with a blank, prepared by oxidizing the hydrazine in a portion of the water sample. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels of hydrazine above approxi- mately 10 micrograms per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-52, 2-53. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-23 (list). B-47 ------- HYDRAZINES AND OTHER COMPOUNDS Air Samples Field Method Compound CAS Number Ammonia 7664-41-7 Aziridine 151-56-4 1,1-Dimethylhydrazine 57-14-7 1,2-Dimethylhydrazine 540-73-8 Ethylenediamine 107-15-3 Hydrazine 302-01-2 METHOD SUMMARY: Field analysis for the above hydrazines and other compounds in air may be performed by use of a detector tube. A minimum of 1-liter of air is collected and analyzed with a hand-operated bellows pump and a hydrazine gas detector tube (Draeger® CH 31801, or equivalent). A positive result is indicated by a color change in the tube from yellow to blue as the analyte reacts with acid to form the hydrazinium salt, indicated by bromophenol blue. Ethylenediamine is indicated with about one-half the sensitivity of 1,1-dimethylhydrazine, ammonia, and aziridine. This method does not identify any specific compound, but responds to all of the above substances. INTERFERENCES: Other amines will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The lower detection limit of the tube varies from approximately 0.2 to 4 milligrams per cubic meter, depending on sample size and analyte. REFERENCES: National Draeger® Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.: National Draeger, Inc.: Pittsburgh, 1979. National Draeger® Inc., Bulletin No. ND-105, National Draeger, Inc.: Pittsburgh, 1982. National Draeger® Inc., Measurements with Draeger® Tubes in the Threshold Limij Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; National Draeger, Inc.: Pittsburgh, December 1981. B-48 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-49 ------- HYDROXIDES Air Samples Field Method Compound CAS Number Ammonium Hydroxide 1336-21-6 Potassium Hydroxide 1310-58-3 Sodium Hydroxide 1310-73-2 METHOD SUMMARY: Field analysis for the above compounds in air can be performed by bubbling air through water and acid-titration of the resulting solution using methyl red indicator. This method is non-specific, giving the total amount of alkaline substance in the air volume sampled, and cannot differentiate between different alkalis. (This method is described by Luzina, G. S. Zavodskaya Lab., 16, 1950, p. 1402, and is summarized in the reference given below.) INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: No sensitivity data are supplied. REFERENCE: Chemical Abstracts; 45, 10135, 1951. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list), plus sampling costs. B-50 ------- IRON COMPOUNDS (PARTICULATE) Air Samples Field 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: Field analysis for the above iron compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry. The method measures the total iron present in the sample, and does not differentiate between chemical compounds or iron valence states. The method is non-destructive, so that further analyses may be performed on samples after this procedure. 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. SENSITIVITY; The method is sensitive to amounts of iron above 15 micrograms with a precision of 60 percent at that level. The method should be applicable to 0.01 to 1.0 microgram of iron per cubic meter, depending on sample size. B-51 ------- 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), plus sampling costs. B-52 ------- IRON Water Samples Field 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; Field analysis for the above iron compounds can be performed by analysis for ferrous ions in water, using test sticks. A test stick (Quantofix®, or equivalent) is dipped briefly into the sample and the resulting color is visually compared with a color scale. The presence of ferrous ions is indi- cated by a red color with use of Quantofix® - Iron (0-1000 ppm) papers or a blue color with use of Quantefix® - Iron (0-100 ppm) papers. Ferric ions may be reduced by ascorbic acid to ferrous ions and measured. This method does not identify any specific iron compounds. INTERFERENCES: A small amount of cadmium powder should be added when the sample contains a high concentration of heavy metals. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method will semi-quantitatively determine concentrations of iron above 5 milligrams per liter. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.; Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. B-53 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-54 ------- LEAD Soil/Sediment Samples Field Method Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Sulfide 1314-87-0 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Field analysis for the above lead compounds in soil samples may be per- formed by pulverizing the sample, then determining the amount of lead present by X-ray fluorescence spectrometry. This method does not identify any specific lead compound, but measures the total lead content of the sample. Analysis time of the prepared sample is approximately 4 minutes. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY; This method is suitable for use over the range of 0.01 to 1.0 gram of lead per kilogram of soil, with a standard deviation of 17 milligrams per kilogram. B-55 ------- REFERENCES; Columbia Scientific Industries Corporation, CSI Model 740 Compact Materials Analyzer, Application Note 83-171; Columbia Scientific Industries: Austin, Texas. Rhodes, J. R.; Rautala, P- Application of a Microprocessor-Based Portable XRF Analyzer in Minerals Analysis ARD Internal Report No. 368; Columbia Scientific Industries, Austin, Texas, June 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $39 (list) B-56 ------- LEAD Water Samples Field Method 1 Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Field analysis of water samples for the above lead compounds can be per- formed by qualitative determination of lead(II) ions with lead test papers. A lead test paper strip (Gallard-Schlesinger Plumbtesmo Papers, or equivalent) is moistened with distilled water, dipped briefly into the sample solution, and compared visually with a color scale. A positive result is indicated by a color change from yellow to a pink-to-purple-red color within 15 minutes. Larger lead(II) concentrations will produce a faster color change. This method does not identify any specific lead(II) compound, but measures the total amount of lead(II) ions present in the sample. INTERFERENCES; Tellurium, silver, cadmium, barium, and strontium may interfere. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The test will qualitatively determine if a concentration of 25 milligrams per liter or greater of lead(II) ions is present in the sample in the absence of interferences. This method will not detect lead(IV) ions and does not B-57 ------- differentiate between different lead compounds, but responds to any lead(II) ions present in the sample. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.; Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-58 ------- LEAD Water Samples Field Method 2 Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Field analysis for lead from the above compounds in water samples can be performed by extraction and colorimetry. A 250-milliliter sample is treated with buffer and dithizone and extracted with chloroform. The resulting extract is colorimetrically compared to a blank chloroform solution. This method does not identify any particular lead compound, but responds to all of the lead present in the sample. INTERFERENCES: Turbid samples may require filtration. Bismuth, copper, mercury, silver, and tin can interfere, and such interferences can be eliminated by preliminary extractions. Interferences from cadmium, nickel, zinc, and cobalt are removed with potassium cyanide. Strong oxidants must not be present in the sample. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to concentration levels of lead greater than approximately 25 micrograms per liter. B-59 ------- REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Co.: Ames, Iowa, 1975, pp. 2-63~ 2-64. COST INFORMATION; The cost per sample for analysis by this method is approximately $22- 38 (list). B-60 ------- LEAD AND COMPOUNDS (PARTICULATE) Air Samples Field Method Compound Lead Lead Acetate Lead Arsenate Lead Chloride Lead Fluoborate Lead Fluoride Lead Iodide Lead Nitrate Lead Phosphate Lead Stearate Lead Subacetate Lead Sulfate Lead Sulfide Lead Thiocyanate CAS Number 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: Field analysis for the above lead compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry- The method measures the total lead content of the sample, and does not differentiate between chemical compounds or lead valence states. The method is non-destructive, so that further analyses may be performed on samples after this procedure. 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. B-61 ------- SENSITIVITY: The method is sensitive to amounts of lead above 6 micrograms, with a precision of 60 percent at that level, and should be applicable to 1 microgram of lead 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 La 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-62 ------- MERCURY Water Samples Field Method Compound Mercuric Cyanide Mercuric Nitrate Mercuric Sulfate Mercuric Thiocyanate Mercurous Nitrate Mercury Mercury Fulminate CAS Number 592-04-1 10045-94-0 7783-35-9 592-85-8 10415-75-5 7782-86-7 7439-97-6 628-86-4 METHOD SUMMARY: Field analysis for mercury and the above mercury compounds in water samples can be performed by colorimetry. A dithizone color reagent is added to a 250- milliliter sample and the intensity of the color from the excess dithizone is measured with a portable spectrophotometer at 610 nm. This method does not identify any specific mercury-containing compound, but measures the total mercury content of the sample. INTERFERENCES: The presence of organic matter and chlorine in the samples interferes, and the interference can be overcome by use of a permanganate oxidation pretreatment step. Interferences from turbidity can be overcome by glass- fiber filtration. The dithizone indicator is decomposed by heat, light, and/or high humidity. Bismuth, cadmium, copper, ferric iron, lead, and zinc do not interfere at levels below 5 milligrams per liter. QUALITY CONTROL: A mercury standard should be analyzed to check the accuracy of the test. SENSITIVITY: The method is sensitive to levels of mercury over 5 micrograms per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-68, 2-69, 2-70. B-63 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $12- 20 (list). B-64 ------- NICKEL AND COMPOUNDS (PARTICULATE) Air Samples Field Method Compound Nickel Nickel Ammonium Sulfate Nickel Chloride Nickel Cyanide Nickel Hydroxide Nickel Nitrate Nickel Sulfate CAS Number 7440-02-0 15699-18-0 7718-54-9 37211-05-5 557-19-7 12054-48-7 14216-75-2 7786-81-4 METHOD SUMMARY: Field analysis for the above nickel compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry. The method measures the total nickel content of the sample, and does not differentiate between chemical compounds or nickel valence states. The method is non-destructive, so that further analyses may be performed on samples after this procedure. 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. SENSITIVITY; The method is sensitive to amounts of nickel above 40 micrograms with a precision of 60 percent at that level. The method should be applicable to levels over 1.0 microgram of chromium 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 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-65 ------- 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-66 ------- NICKEL IONS Water Samples Field Method Compound CAS Number Nickel Ammonium Sulfate 15699-18-0 Nickel Chloride 7718-54-9 37211-05-5 Nickel Cyanide 557-19-7 Nickel Hydroxide 12054-48-7 Nickel Nitrate 14216-75-2 Nickel Sulfate 7786-81-4 METHOD SUMMARY: Field analysis for the above nickel compounds in water samples can be performed using test sticks for the determination of nickel(II) ions. A test stick (Quantofix®, or equivalent) is dipped briefly into the sample at pH 2 to 7, and is compared visually to a color scale. This method does not identify any particular compound, but measures the total nickel content of the sample. INTERFERENCES: Large quantities of cupric, mercurous, and other ions may interfere. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY; This method will semi-quantitatively determine concentrations of approx- imately 10 to 100 milligrams per liter. REFERENCE; Gallard-Schlesinger, pH Indicator Papers and Test Papers Brochure, 14th ed.; Gallard-Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION; The cost per sample for analysis by this method is approximately $3-5 (list). B-67 ------- NITRATE IONS Water Samples Field Method Compound CAS Number Beryllium Nitrate 13597-99-4 7787-55-5 Cupric Nitrate 3251-23-8 Ferric Nitrate 10421-48-4 Lead Nitrate 10099-74-8 Mercuric Nitrate 10045-94-0 Nickel Nitrate 14216-75-2 Nitric Acid 7697-37-2 Silver Nitrate 7761-88-8 Sodium Nitrate 7632-00-0 Thallium(I) Nitrate 10102-45-1 Uranyl Nitrate 10102-06-4 36478-76-9 Zinc Nitrate 7779-88-6 Zirconium Nitrate 13746-89-8 METHOD SUMMARY: Field analysis for the above nitrate compounds in water samples can be performed by reduction of the nitrate ions in a 25-milliliter sample to nitrite ions, followed by spectrophotometric analysis for nitrite. A cadmium reducing reagent is added to the sample, producing an amber color when nitrate is present, and the intensity of the color is measured with a portable spectrophotometer at 500 nm. This method does not identify any specific nitrate-containing compound, but measures the total nitrate content of the sample. INTERFERENCES: Nitrite ion interferences can be compensated for by treatment with bromine water and phenol. Strong oxidizing and reducing agents will interfere, and ferric ion causes high results. Large amounts of chloride ion cause low re- sults . QUALITY CONTROL: Analyst technique must be checked by analysis of a procedural blank. SENSITIVITY: The method is sensitive to levels of nitrate ions above approximately 10 milligrams per liter in the absence of interferences. B-68 ------- REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis. 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-77, 2-78. COST INFORMATION; The cost per sample for analysis by this method is approximately $12- 20 (list). B-69 ------- POTASSIUM Water Samples Field Method Compound Antimony Potassium Tartrate Potassium Arsenate Potassium Arsenite Potassium Chromate Potassium Cyanide Potassium Bichromate Potassium Hydroxide Potassium Permanganate Potassium Silver Cyanide Zirconium Potassium Fluoride CAS Number 28300 7784 10124 7789 151 7778 1310 7722 506 16923 -74-5 -41-0 -50-2 -00-6 -50-8 -50-9 -58-3 -64-7 -61-6 -95-8 METHOD SUMMARY: Field analysis of water samples for the above potassium compounds can be performed by use of potassium test papers. A potassium test paper strip is dipped briefly into the sample and inspected visually. A positive result is indicated by orange spots on a bright yellow background on the test paper. INTERFERENCES: Cesium, rubidium, and titanium ions may interfere. This method does not identify any specific potassium compound, but indicates the total potassium content of the sample. QUALITY CONTROL: No quality control information is given. SENSITIVITY: The test will qualitatively determine if a concentration of 250 milligrams per liter or greater of potassium ions is present in the sample in the absence of interferences. This test is not specific for any potassium compound and will respond to potassium ions from any source, including background sources. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.; Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-70 ------- SELENIUM Air Samples Field Method Compound CAS Number Selenious Acid 7783-00-8 Selenium 7782-49-2 Selenium Dioxide 7446-08-4 Selenium Disulfide 7488-56-4 Selenourea 630-10-4 Sodium Selenite 10102-18-8 7782-82-3 Thallium(I) Selenide 12309-52-0 METHOD SUMMARY: Field analysis for the above selenium compounds in air may be performed by filtration of air and analysis of the filter medium by X-ray fluorescence spectrometry. The method measures the total selenium content of the sample and does not differentiate between chemical compounds or selenium valence states. The method is non-destructive, so that further analyses may be performed on samples after this procedure. 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. SENSITIVITY; The method is sensitive to amounts of selenium above 30 micrograms with a precision of 60 percent at that level, and is applicable above 1.0 microgram of selenium 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 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-71 ------- 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: The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-72 ------- SELENIUM Water Samples Field Method Compound CAS Number Selenious Acid 7783-00-8 Selenium 7782-49-2 Selenium Dioxide 7446-08-4 Selenium Disulfide 7488-56-4 Sodium Selenite 10102-18-8 7782-82-3 Thallium(I) Selenide 12309-52-0 METHOD SUMMARY: Field analysis for selenium compounds in water samples can be performed by colorimetric analysis for selenium. A 100-milliliter sample is treated with 3,3'-diaminobenzidine, and the intensity of the yellow color of the selenium complex formed is measured after extraction into toluene. A blank consisting of distilled water is analyzed in parallel with each sample. This method does not identify any specific selenium compound, but measures the total selenium content of the sample. INTERFERENCES; Strong oxidizing agents can cause low results. No positive interferences are reported. QUALITY CONTROL; A blank should be analyzed with each sample. SENSITIVITY: The method is sensitive to concentration levels greater than approximately 0.5 milligrams of selenium per liter. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-106, 2-107. COST INFORMATION: The cost per sample for analysis by this method is approximately $22- 37 (list). B-73 ------- SILVER Water Samples Field Method Compound CAS Number Potassium Silver Cyanide 506-61-6 Silver Cyanide 506-64-9 Silver Nitrate 7761-88-8 METHOD SUMMARY: Silver test papers may be used for the qualitative colorimetric determination of silver ions from the above compounds in water samples. A silver test paper strip is dipped briefly into the sample and inspected visually. A positive result is indicated by purple-red spots on a salmon- red background on the test paper. This method is not specific for any silver compound, but determines the total amount of silver ions present in the sample. INTERFERENCES: Mercury(II) ions, copper(II) ions, gold, platinum, and palladium may interfere. QUALITY CONTROL: No quality control information is given. SENSITIVITY: The test will qualitatively determine if a concentration of 20 milligrams per liter or greater of silver ions is present in the sample in the absence of interferences. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.; Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-74 ------- SULFIDES Soil/Sediment Samples Field 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: Field analysis for sulfide ions from the above compounds in soil/sediment samples can be performed using lead acetate test papers. A 1-gram sample is mixed with a magnesium chloride/hydrochloric acid solution and methyl violet indicator in a small test tube. A lead acetate strip moistened with acetate buffer is suspended above the sample. A cadmium nitrate solution and sodium hydroxide are placed in a second test tube which is attached to the first. The first test tube is heated, nitrogen is bubbled through the two tubes, and aluminum-treated hydrochloric acid is added to the first test tube. Darkening of the lead acetate strip within 3 minutes indicates the presence of 0.01 milli- grams per gram or greater of sulfide. A higher sulfide concentration is indi- cated by yellow coloration in the second test tube. This method measures the total sulfide present in the sample, but does not identify any specific sulfide- containing compound. INTERFERENCES: This test does not detect copper sulfides. Thiocyanates respond to the test. QUALITY CONTROL; Magnesium chloride should be analyzed as a blank solution. The test performance should be checked daily with 1 milliliter of a standard solution of sulfide (approximately 100 milligrams per liter). SENSITIVITY: The method is sensitive to concentrations of 0.01 milligrams of sulfide per gram and higher. B-75 ------- REFERENCE: 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. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-23 (list). B-76 ------- SULFIDES Water Samples Field Method Compound CAS Number Ammonium Sulfide 12135-76-1 Arsenic Disulfide 1303-32-8 Arsenic Trisulfide 1303-33-9 Hydrogen Sulfide 7783-06-4 Phosphorus Pentasulfide 1314-80-3 Selenium Disulfide 7488-56-4 Sodium Hydrosulfide 16721-80-5 Strontium Sulfide 1314-96-1 METHOD SUMMARY: Field analysis for the above sulfides in water samples may be performed by use of test papers. One drop of sample is placed on a strip of lead acetate test paper which has been moistened with acetic acid. The test paper will darken if a sulfide concentration of 4 milligrams per liter or greater is present. This method measures the total amount of sulfide in the sample, and does not identify specific sulfide-containing compounds. INTERFERENCES: This method should not be used on turbid or highly colored samples. QUALITY CONTROL: A 100-milligram-per-liter sulfide standard must be used daily to ensure correct test performance. SENSITIVITY: The method will detect concentrations of sulfide greater than 4 milligrams per liter. REFERENCE: 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. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-77 ------- SULFITE IONS Water Samples Field Method Compound Ammonium Bisulfite Ammonium Sulfite Zinc Hydrosulfite CAS Number 10192-30-0 10196-04-0 7779-86-4 METHOD SUMMARY: Test sticks may be used for the determination of sulfite ions from the above compounds in water samples. A test stick (Quantofix®. or equivalent) is dipped briefly into the sample at pH 6 to 9, and its color compared with a color scale. This method does not identify specific sulfite salts, but measures the total sulfite ion content of the sample. INTERFERENCES: Sulfate and sulfide ions will interfere, but sulfide interference may be eliminated by precipitation with an excess of nickel(II) ion and filtration. Large amounts of reducing agents in the sample will cause the sulfite determin- ation to be low. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method will determine semi-quantitatively concentration levels of approximately 10 to 100 milligrams of sulfite ion per liter. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.: Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-78 ------- ZINC AND COMPOUNDS (PARTICULATE) Air Samples Field Method Compound CAS Number Zinc Zinc Acetate Zinc Ammonium Chloride Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc Zinc Borate Bromide Carbonate Chloride Cyanide Fluoride Formate Hydrosulfite Nitrate Phenolsulfonate Phosphide Silicofluoride Sulfate 7440- 557- 52628- 14639- 14639- 1332- 7699- 3486- 7646- 557- 7783- 557- 7779- 7779- 127- 1314- 16871- 7733- •66-6 •34-6 •25-8 97-5 •98-6 07-6 45-8 35-9 85-7 21-1 •49-5 41-5 86-4 88-6 82-2 84-7 •71-9 02-0 METHOD SUMMARY: Field analysis for the above zinc compounds in air may be performed by filtration of air and analysis of the filter medium for zinc by X-ray fluores- cence spectrometry. The method measures the total zinc present in the sample, and does not differentiate between chemical compounds. The method is non- destructive, so that further analyses may be performed on samples after this procedure. 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. SENSITIVITY: The method is sensitive to amounts of zinc above 30 micrograms. with a precision of 60 percent at that level, and should be applicable to 0.01 to 1.0 micrograms of zinc per cubic meter, depending on sample size. B-79 ------- 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 The cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-80 ------- ZINC Soil/Sediment Samples Field Method Compound CAS Number Zinc 7440-66-6 Zinc Acetate 557-34-6 Zinc Ammonium Chloride 52628-25-8 14639-97-5 14639-98-6 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: Field analysis for the above zinc compounds in soil samples may be per- formed by pulverizing the sample, then determining the amount of zinc present by X-ray fluorescence spectrometry- This method does not identify any specific zinc compound, but measures the total zinc content of the sample. Analysis time of the prepared sample is approximately 4 minutes. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for use over the range of 0.01 to 1.0 gram of zinc per kilogram of soil, with a standard deviation of 15 milligrams per kilogram. B-81 ------- REFERENCES: Columbia Scientific Industries Corporation, CSI Model 740 Compact Materials Analyzer, Application Note 83-171; Columbia Scientific Industries: Austin, Texas. Rhodes, J. R.; Rautala, P- Application of a Microprocessor - Based Portable XRF Analyzer in Minerals Analysis ARD Internal Report No. 368; Columbia Scientific Industries, Austin, Texas, June 1981. COST INFORMATION; Cost per sample for analysis by this method is approximately $39 (list). B-82 ------- Compound Zinc Zinc Acetate Zinc Ammonium Chloride Zinc Borate Zinc Bromide Zinc Carbonate Zinc Chloride METHOD SUMMARY: ZINC Water Samples Field Method CAS Number 7440-66-6 557-34-6 52628-25-8 14639-97-5 14639-98-6 1332-07-6 7699-45-8 3486-35-9 7646-85-7 Compound Zinc Cyanide Zinc Fluoride Zinc Formate Zinc Hydrosulfite Zinc Nitrate Zinc Phenolsulfonate Zinc Phosphide Zinc Silicofluoride Zinc Sulfate CAS Number 557-21-1 7783-49-5 557-41-5 7779-86-4 7779-88-6 127-82-2 1314-84-7 16871-71-9 7733-02-0 Analysis for the above zinc compounds in water samples can be performed by colorimetry. The zinc in a 50-milliliter sample is complexed by cyanide, freed with cyclohexanone, and complexed with 2-carboxy-2'-hydroxy-5'-sulfoformazyl benzene indicator (Zincon®). The intensity of the resulting orange to red- orange color is measured with a portable spectrophotometer. This method does not identify any specific zinc-containing compound present, but measures the total zinc content of the sample. INTERFERENCES: A brown or blue color indicates a concentration of zinc which is too high for the method, or the presence of an interfering metal. Sample dilution should be used until an orange to reddish-orange color is obtained. Cadmium, aluminum, manganese, iron, nickel, and copper ions interfere. QUALITY CONTROL: A reagent blank should be analyzed and the results subtracted from the sample results. Standards should be analyzed as a check on accuracy. SENSITIVITY: The method measures zinc concentrations above approximately 1 milligram per liter in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach Chemical Company: Ames, Iowa, 1975, pp. 2-126, 2-127. B-83 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $23-38 (list). B-84 ------- ZIRCONIUM Water Samples Field 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: Zirconium test papers may be used for the qualitative colorimetric deter- mination of zirconium(IV) ions from the above compounds in water samples. A zirconium test paper strip is dipped briefly into the sample and inspected visually. A positive result is indicated by purple-red spots on a yellow background on the test paper. This method is not specific for any one zirconium compound, but responds to all zirconium(IV) ions present in the sample. INTERFERENCES: Hydrogen fluoride may interfere and aluminum will also give positive results. QUALITY CONTROL: No quality control information is given. SENSITIVITY: The test will qualitatively determine if a concentration of 20 milligrams per liter or greater of zirconium(IV) ions is present in the sample in the absence of interferences. REFERENCE: Gallard-Schlesinger, pH Indicator Papers and Test Papers, 14th ed.; Gallard- Schlesinger Chemical Mfg. Corp.: Carle Place, New York, 1982. COST INFORMATION: The cost per sample for analysis by this method is approximately $3-5 (list). B-85 ------- B. Organic Substances B-86 ------- ACETATES Air Samples Field Method Compound CAS Number Amyl Acetate 628-63-7 Butyl Acetate 123-86-4 iso-Butyl Acetate 110-19-0 METHOD SUMMARY: Analysis for amyl acetate, butyl acetate, and iso-butyl acetate in air may be performed by use of a gas detector tube. A 200-milliliter sample is collected and analyzed with a portable pump and a butyl acetate gas detector tube (Bendix/Gastec®, or equivalent). A positive result is indicated by a color change from orange to brownish-green in the tube. This method is based on the reduction of dichromate to form chromic sulfate. INTERFERENCES: Propane, acetylene, and organic vapors other than halogenated hydrocarbons may also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 200 to 30,000 milli- grams per cubic meter of iso-butyl acetate and butyl acetate, and concentrations of approximately 500 to 40,000 milligrams per cubic meter of amyl acetate. REFERENCE: Bendix Environmental and Process Instruments Division, Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-87 ------- ACETIC ACID AND ACETIC ANHYDRIDE Air Samples Field Method Compound CAS Number Acetic Acid 64-19-7 Acetic Anhydride 108-24-7 METHOD SUMMARY: Analysis for acetic acid and acetic anhydride in air may be performed by use of a detector tube. A 300-milliliter sample is collected and analyzed with a hand-operated bellows pump and an acetic acid detector tube (Draeger® 67 22101, or equivalent). A positive result is indicated by a color change in the tube from bluish-violet to yellow as the analyte activates an acid indicator. This method does not identify any specific compound, but measures the content of the above compounds and other acids in the sample. INTERFERENCES: Other acids may also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: Acetic anhydride is indicated with one-fourth the sensitivity of acetic acid. The lower detection limit of the tube varies from approximately 10 to 200 milligrams per cubic meter for acetic acid. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, 1979. National Draeger®, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger: Pittsburgh, 1981. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-88 ------- ACETONE AND METHYL KETONES Air Samples Field Method Compound CAS Number Acetone 67-64-1 Methyl Ethyl Ketone 78-93-3 Methyl Isobutyl Ketone 108-10-1 METHOD SUMMARY: Analysis for acetone and the above methyl ketones in air may be performed by use of a detector tube. A 1-liter sample is collected and analyzed with a handoperated bellows pump and an acetone gas detector tube (Draeger® CH 22901, or equivalent). A positive result is indicated by a color change in the tube from pale yellow to yellow. This method is based on the reaction of the analyte with 2,4-dinitrophenylhydrazine to form a yellow hydrazone. It does not identify any specific compounds, but measures the total content of the above compounds in the sample. INTERFERENCES: The methyl isobutyl ketone determination may be up to 20 percent low. Alcohols and esters will not change the tube color, but may cause positive errors in the determination of acetone. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The lower detection limit of the tube varies from approximately 250 to 29,000 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, 1979. National Draeger®, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range. Draeger® Gas Analysis Product Information, Leaflet 4340.3e: Draeger: Pittsburgh, 1981. B-89 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-90 ------- ALDEHYDES Air Samples Field Method Compound CAS Number Acetaldehyde 75-07-0 Acrolein 107-02-8 Aldicarb 116-06-3 Chloral 75-87-6 Chloroacetaldehyde 107-20-0 Furfural 98-01-1 Paraformaldehyde 30525-89-4 METHOD SUMMARY: Field analysis for the above aldehydes in air can be performed by visual color detection in a sampling tube. Aldehydes are adsorbed from an air stream onto purified silica gel, a color reagent consisting of p-phenylenediamine and hydrogen peroxide (1:2) is added to the tube, and the length of the pale purple- brown to deep purple-brown or black band formed indicates the amount of aldehyde absorbed. The method is nonspecific, giving a positive result for all aldehydes, and does not differentiate between aldehydes. INTERFERENCES: Nitriles, oximes, aldehyde ammonia, and aldehyde bisulfite compounds interfere; ketones do not. Pure gum-rubber tubing should be used for connec- tions to avoid contamination from aldehyde-containing plastics. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: As little as 0.5 micrograms aldehyde per cubic meter of air can be detected by the method. PFERENCES ; Hughes, E. E.; Lias, S. G. "Detection and Estimation of Low Concentrations of Aldehyde in Air," Anal. Chem., 32, 1960, pp. 707-708. Industrial Hygiene Digest, 24_, 1960, p. 596. COST INFORMATION: The cost per sample for analysis by this method is approximately $5-10 (list), plus sampling costs. B-91 ------- AMINES Air Samples Field Method Compound CAS Number Butylamine 109-73-9 Ethylenediamine 107-15-3 1,2-Propylenimine 75-55-8 METHOD SUMMARY: Analysis for the above amines in air may be performed by use of a gas detector tube. A 200-milliliter sample is collected and analyzed with a port- able pump and an amine gas detector tube (Bendix/Gastec® 180, or equivalent). A positive test is indicated by a color change from pink to yellow in the tube. This method does not differentiate between different amines or identify any particular amine compound. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 2 to 6 milligrams per cubic meter. REFERENCE: Bendix Environmental and Process Instruments Division, Bendix Gastec Precision Gas Detector System Manual, (Blue Book), Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-92 ------- AROMATIC AMINES Water Samples Field Method 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: Field analysis for aromatic amines in water samples can be performed by diazotization and spectrophotometry. A 35-milliliter sample is treated with hydrochloric acid and sodium nitrite. A color reagent, either l-amino-8- naphthol-3,6-disulfonic acid (H-acid) or N-(l-naphthyl)ethylendiamine (N-na), is added to produce a cherry-red or purplish-red color, respectively. After 90 minutes, the intensity of the color is measured spectrophotometrically. This method does not differentiate between different amines or identify any specific amine compounds. INTERFERENCES: No specific interferences are reported. This method is not applicable to secondary or tertiary aromatic amines. All glassware, including absorption cells, should be cleaned frequently with hydrochloric acid. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: 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: The cost per sample for analysis by this method is approximately $33-55 (list). B-93 ------- AROMATIC PRIMARY AMINES Air Samples Field Method Compound CAS Number Aniline 62-53-3 3,3'-Dichlorobenzidine 91-94-1 3,3'-Dimethoxybenzidine 119-90-4 4,4'-Methylenebis(2- 101-14-4 chloroaniline) Ł-Nitroaniline 100-01-6 METHOD SUMMARY: The above aromatic primary amines in air samples can be measured colorimet- rically. A 1-liter air sample is drawn through a filter paper impregnated with a reagent containing 4-(dimethylamino)cinnamaldehyde (DAC). The amine reacts with the DAC to form a yellow stain. The intensity of the color is compared visually with standards to determine the concentration of the amine. It is expected that other aromatic primary amines can be measured by this method unless steric hindrances inhibit the color-forming reaction. This method does not identify a specific aromatic primary amine, but measures the total concen- tration of aromatic primary amines. INTERFERENCES: Alkaline or acidic compounds in the air sample can affect the color-forming reaction. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for amine concentrations in the range of 10 to 100 micrograms per cubic meter for a sample size of 1 liter. The limit of detec- tion may be expanded by increasing the volume of air sampled up to 10 liters and applying a factor. REFERENCE: Meddle, D. W.; Smith, A. F. "Field Method for the Determination of Aromatic Primary Amines in Air," Analyst, 106, 1981, pp. 1088-1095. COST INFORMATION: The cost per sample for analysis by this method is $3-5 (list), plus sampling costs. B-94 ------- AMINES: TRIETHYLAMINE AND OTHER AMINES Air Samples Field Method Compound CAS Number Diethylamine 109-89-7 Dimethylamine 124-40-3 Monoethylamine 75-04-7 Monomethylamine 74-89-5 Triethylamine 121-44-8 METHOD SUMMARY: Analysis for the above amines in air may be performed by use of a detector tube. A 500-milliliter sample is collected and analyzed with a hand-operated bellows pump and a triethylamine gas detector tube (Draeger® 67 18401, or equivalent). A positive result is indicated by a color change in the tube from yellowish-gray to blue as the amine reacts with acid, indicated by bromothymol blue. This method does not identify any particular amine compound, but responds to all the above amines. INTERFERENCES: Ammonia, hydrazine, and some organic amines also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The lower detection limit of the tube varies from approximately 20 to 250 milligrams per cubic meter- REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger: Pittsburgh; December 1981. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-95 ------- ANIONIC DETERGENTS Water Samples Field Method 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: Field analysis for the above anionic detergents can be performed by colorimetry. A 300-milliliter water sample is extracted with benzene in the presence of a crystal violet color reagent. The intensity of the violet color in the benzene extract is measured spectrophotometrically. This method does not measure any specific compound, but indicates the total amount of anionic detergents in the samples. INTERFERENCES: Perchlorate and periodate ions interfere, and high chloride concentrations, as found in seawater, will cause low results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method can measure from approximately 100 to 300 micrograms of deter- gent per liter, in the absence of interferences. REFERENCE: Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and Wastewater Analysis, 2nd ed.; Hach: Ames, Iowa, 1978, pp. 2-44, 2-45. COST INFORMATION: The cost per sample for analysis by this method is approximately $15-25 (list). B-96 ------- AROMATICS AND OTHER COMPOUNDS Water Samples Field Method Compound Benzene Benzyl Chloride Carbon Disulfide Chlorobenzene 2,4-D Acid Dichlobenil Ethylbenzene Isoprene Malathion Methylmercaptan Naphthalene Nitrobenzene Phosphorus Pentasulfide Quinoline Styrene Sulfur Monochloride 2,4,5-T Acid Toluene Xylene CAS Number 71- 100- 75- 108- 94- 1194- 100- 78- 121- 74- 91- 98- 1314- 91- 100- 12771- 93- 108- 1330- •43-2 •44-7 •15-0 90-7 •75-7 65-6 •41-4 79-5 •75-5 93-1 •20-3 95-3 80-3 22-5 42-5 08-3 •76-5 88-3 20-7 METHOD SUMMARY: The aromatics and other compounds listed above may be detected in water by using a benzene air analyzer tube (Bendix-Gastec® 121L, or equivalent) attached to an effervescent jar assembly. An 80-milliliter sample is placed in a jar connected to a benzene air analyzer tube. An effervescent tablet (Alka-Seltzer®, or equivalent) is added to the sample, and when the effervescence has ceased, a positive result is indicated by a discoloration of the white silica gel in the analyzer tube. This method does not identify any particular compound, but responds to all of the substances listed above. INTERFERENCES: The test is non-specific, as aromatics not listed above and a few other compounds will also yield positive results. QUALITY CONTROL: This method is sensitive to concentration levels greater than approximately 1 milligram per liter when an 80-milliliter sample size is used. SENSITIVITY: The test is qualitative, but the length of discoloration in the tube may be taken as relative indication of the compound concentration. B-97 ------- REFERENCE: U.S. Environmental Protection Agency, Development of a Kit for Detecting Hazardous Material Spills in Waterways, Appendix B; EPA-600/2-78-055, U.S. EPA: Cincinnati, March 1978. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-98 ------- n-BUTYL ALCOHOL AND ISOBUTYL ALCOHOL Air Samples Field Method Compound CAS Number n-Butyl Alcohol 71-36-3 Isobutyl Alcohol 78-83-1 METHOD SUMMARY: Analysis for n-butyl alcohol and isobutyl alcohol in air may be performed by use of a gas detector tube. A 0.4-liter sample is collected and analyzed with a portable pump and an ethyl alcohol detector tube (Bendix/Gastec® No. 112, or equivalent). A positive result is indicated by a color change from rose to pale blue. The change is based on the reduction of dichromate ion to chromic ion. This method does not identify any specific compound, but responds to many alcohols when they are present in the sample. INTERFERENCES: Other alcohols will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure n-butyl alcohol concentrations of approximately 300 to 4,500 milligrams per cubic meter and isobutyl alcohol concentrations of approximately 300 to 2,000 milligrams per cubic meter. REFERENCE; Bendix Corporation, Bendix/Gastec Precision Gas Detector System Manual (Blue Book); Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-99 ------- CARBON TETRACHLORIDE AND TRICHLOROMONOFLUOROMETHANE Air Samples Field Method Compound CAS Number Carbon Tetrachloride 56-23-5 Trichloromonofluoromethane 75-69-4 METHOD SUMMARY: Field analysis for carbon tetrachloride and trichloromonofluoromethane in air can be performed by use of a detector tube. A 0.5-liter sample is collected and analyzed with a hand-operated bellows pump and a carbon tetrachloride gas detector tube (Draeger® CH 27401, or equivalent). A positive result is indicated by a color change in the tube from yellow to bluish-green. The change is due to the reaction of the analyte with fuming sulfuric acid to produce phosgene, which in turn reacts with diraethylaminobenzaldehyde and dimethyl aniline. This method does not identify any specific compound, but measures the total content of the above compounds in the sample. INTERFERENCES: Phosgene interferes strongly. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 30 to 300 milligrams per cubic meter. REFERENCE; U.S. Environmental Protection Agency, Development of a Kit for Detecting Hazardous Material Spills in Waterways, Appendix B; EPA-600/2-78-055. U.S. EPA: Cincinnati, March 1978. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-100 ------- CHLOROBENZENE AND DICHLOROBENZENES Air Samples Field Method Compound CAS Number Chlorobenzene 108-90-7 1,2-Dichlorobenzene 95-50-1 1,3-Dichlorobenzene 541-73-1 1,4-Dichlorobenzene 106-46-7 METHOD SUMMARY; Field analysis for chlorobenzene and dichlorobenzenes in air can be per- formed by use of a gas detector tube. A 0.1- to 0.2-liter sample is collected and analyzed with a portable pump and a benzene gas detector tube (Bendix/ Gastec® 121, or equivalent). A positive result is indicated by a color change from white to brownish-green in the tube. This method does not identify any particular compound, as several compounds give positive results. INTERFERENCES: Toluene, xylene, styrene, alcohol, ketones, esters, vinyl chloride, hexane, ethylene, and acetylene will also cause positive results and/or errors. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 300 to 4000 milli- grams per cubic meter. REFERENCE: Bendix Corporation, Bendix/Gastec Precision Gas Detector System Manual (Blue Book); Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-101 ------- CHOLINESTERASE-INHIBITING COMPOUNDS Water Samples Field Method Compound CAS Number Carbaryl 63-25-2 Chlorosulfonic Acid 7790-94-5 Coumaphos 56-72-4 Diazinon 333-41-5 Dichlorvos 62-73-7 Disulfoton 298-04-4 Ethion 563-12-2 Guthion 86-50-0 Malathion 121-75-5 Methyl Parathion 298-00-0 Mevinphos 7786-34-7 Naled 300-76-5 Parathion 56-38-2 Tetraethyl Pyrophosphate 107-49-3 Trichlorfon 52-68-6 METHOD SUMMARY: A colorimetric method may be used to detect compounds that inhibit activ- ity of the enzyme cholinesterase. The square end of a horse serum choline- sterase enzyme ticket (Army, or equivalent) is placed in a 20-milliliter sample. One drop of tris buffer is added to the sample and a few drops are added to the round end of the ticket. After 5 minutes, the ticket is removed from solution and a few drops of substrate are added to each end. The round (control) end of the ticket should turn blue within a few minutes. Any signi- ficant color difference in the square end of the ticket indicates a positive result and the probable presence of an anticholinesterase compound. This method does not identify any specific compound, since any cholinesterase inhibitor will give a positive result. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels greater than approximately 3 milligrams per liter of the compounds listed above in the absence of inter- ferences . B-102 ------- REFERENCES: U.S. Environmental Protection Agency, Development of a Kit for Detecting Hazardous Material Spills in Waterways; Appendix B, EPA-600/2-78-055, U.S. EPA: Cincinnati, March 1978. U.S. Environmental Protection Agency, Operator's Manual for Hazardous Materials Detector Kit, Appendix B, ibid. COST INFORMATION: The cost per sample for analysis by this method is approximately $10-18 (list). B-103 ------- CYCLOHEXANONE AND FURFURAL Air Samples Field Method Compound CAS Number Cyclohexanone 108-94-1 Furfural 98-01-1 METHOD SUMMARY: Field analysis for cyclohexanone and furfural in air can be performed by use of a gas detector tube. A 0.4-liter sample is collected and analyzed with a portable pump and a cyclohexanone gas detector tube (Bendix/Gastec® 154, or equivalent). A positive result is indicated by a color change from pale yellow to yellow in the tube. This method is based on the reaction with 2,4-dinitro- phenylhydrazine to form a 2,4-dinitrophenylhydrazone. This method does not identify any particular compound, as many ketones give positive results. INTERFERENCES: Other ketones will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure concentrations of approximately 10 to 125 milligrams per cubic meter. REFERENCE: Bendix Corporation, Bendix Gastec Precision Gas Detector System Manual (Blue Book); Bendix Corp.: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-104 ------- ETHYLENE OXIDE, 1,4-DIOXANE, AND PROPYLENE OXIDE Air Samples Field Method Compound CAS Number 1,4-Dioxane 123-91-1 Ethylene Oxide 75-21-8 Propylene Oxide 75-56-9 METHOD SUMMARY: Field analysis for ethylene oxide, 1,4-dioxane, and propylene oxide in air can be performed by use of a gas detector tube. A 0.1-liter sample is collected and analyzed with a portable pump and an ethylene oxide gas detector tube (Bendix/Gastec® 163, or equivalent). A positive result is indicated by a color change from orange to green in the tube. This method does not identify any particular compound. INTERFERENCES: Other organic vapors may also cause positive results. QUALITY CONTROL; No quality control procedures are given. SENSITIVITY: The method will measure ethylene oxide concentrations of approximately 2 to 50 grams per cubic meter, 1,4-dioxane concentrations of approximately 20 to 200 grams per cubic meter, and propylene oxide concentrations of 7 to 85 grams per cubic meter. REFERENCE: Bendix Corporation, Bendix/Gastec Precision Gas Detector System Manual (Blue Book); Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-105 ------- ETHYL ETHER AND TETRAHYDROFURAN Air Samples Field Method Compound CAS Number Ethyl Ether 60-29-7 Tetrahydrofuran 109-99-9 METHOD SUMMARY: Field analysis for ethyl ether and tetrahydrofuran in air can be performed by use of a gas detector tube. A 0.1- to 0.5-liter sample is collected and analyzed with a portable pump and an ethyl ether gas detector tube (Bendix/ Gastec® 161, or equivalent). A positive result is indicated by a color change from orange to blackish-green in the tube. The method is based on the reduction of dichromate ions to chromic ions, and does not identify any particular compound, but will give a positive response to many organic compounds. INTERFERENCES: Propane, acetylene, and other organic vapors may also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure tetrahydrofuran concentrations of approximately 300 to 7500 milligrams per cubic meter, and ethyl ether concentrations of approxi- mately 12 to 300 grams per cubic meter. REFERENCE: Bendix Corporation, Bendix/Gastec Precision Gas Detector System Manual (Blue Book); Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-106 ------- GEMINAL TRIHALOGENATED COMPOUNDS Air Samples Field Method Compound CAS Number Bromoform 75-25-2 Pentachloroethane 76-01-7 METHOD SUMMARY: Field analysis of air for the above compounds with three halogens bonded to one carbon can be performed by colorimetry. The air sample is collected in a bubbler containing 95-percent ethyl alcohol. The sample is transferred to a volumetric flask and diluted to volume. Pyridine, sodium hydroxide, and an aliquot of the sample are placed in a test tube and heated in a water bath for 1 minute. The color in the pyridine layer is matched to standards in a color comparator. Permanent color standards are prepared from basic fuchsin in acidified ethyl alcohol. This method does not identify any specific geminal trihalide, but measures the total content of such compounds in the sample. (This method is described in Jacobs, M. B. The Analytical Chemistry of Indus- trial Poisons, Hazards and Solvents, 2nd ed.; Interscience: New York, 1949, p. 565, and is summarized in the reference given below.) INTERFERENCES: No interferences are reported. QUALITY CONTROL; No quality control procedures are given. SENSITIVITY: This method is suitable for the analysis of concentrations from approxi- mately 10 to 15,000 milligrams per cubic meter. REFERENCE: Quantitive Analysis of Gaseous Pollutants; W. E., Ruch, Ed.; Ann Arbor-Humphrey Science: Ann Arbor, 1970, pp. 44, 184. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-23 (list), plus sampling costs. B-107 ------- MERCAPTO COMPOUNDS Water Samples Field Method Compound CAS Number Thioacetamide 62-55-5 Thiosemicarbazide 79-19-6 Thiourea 62-56-6 METHOD SUMMARY: The above mercapto compounds may be detected in water samples by reaction with alkaline sodium nitrosylpentacyanoferrate (NP) and visual color comparison. Several grains of Amberlite® IRA-68 resin are placed on a white spot plate, 1 drop of NP reagent and 1 drop of sodium hydroxide are added, and the solution is allowed to react for 2 minutes to adsorb the basic NP on the resin. One drop of 30-percent acetic acid and 1 drop of sample solution are added, and the resulting color(s) are compared to a reagent blank. Thioacetamide (ThA) gives a reddish-violet color, thiosemicarbazide (ThS) bluish-violet, and thiourea (ThU) bluish-green. This method does not identify any particular mercapto compound. INTERFERENCES: The correct order of steps must be followed, and maximum sensitivity occurs at a final pH of 4.5. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to 1 nanogram ThA, and to 0.4 nanograms ThS and ThU. REFERENCE: Grdinic, V.; JakSevac-Miksa, M. "Selective Detection of Mercapto Compounds with Ion Exchange Resin as a Reagent," Acta Pharm. Jugosl.. 32, 1982, pp. 197-200. COST INFORMATION: The cost per sample for analysis by this method is approximately $10-18 (list). B-108 ------- NITRO COMPOUNDS No Matrix Given Field Method Compound CAS Number Nitrobenzene 98-95-3 Nitrotoluene 1321-12-6 METHOD SUMMARY: The presence of the above nitro compounds may be detected by colorimetry. A 0.1-milliliter to 0.2-milliliter sample is mixed with alcohol, ammonium chlo- ride, and zinc dust and then heated for 2 to 4 minutes. The solution is centri- fuged and the residue washed with ether and treated with chloroform, hydrochloric acid, and ammonium metavanadate. In the presence of a nitro compound, the chloroform layer will turn purple or blue violet. This test does not differ- entiate between various nitro compounds. INTERFERENCES: Other nitro compounds will also give a positive result. Phenols, salicylic acid, and hydroxylamines will interfere in the detection. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is not quantitative, but will detect concentrations of approximately 250 to 500 milligrams per liter. REFERENCE: Sahu, B.; Tandon, U. "A Selective and Sensitive Method for Detection of Nitro Compounds," J. Indian Chem. Soc., LVIII, 1981, pp. 519-520. COST INFORMATION: The cost per sample for analysis by this method is approximately $22-38 (list). B-109 ------- ORGANIC ACIDS: ADIPIC and FUMARIC ACIDS Water Samples Field Method Compound CAS Number Adipic Acid 124-04-9 Fumaric Acid 110-17-8 METHOD SUMMARY: Titration may be used to analyze water samples for fumaric and adipic acids. The sample is centrifuged and 10- to 15-milliliters of the supernatant are mixed with thymol blue indicator and concentrated sulfuric acid. The acids in the sample are then adsorbed on a column of silicic acid, eluted with n- butanol in chloroform, and titrated with sodium hydroxide. This method is not specific for adipic and fumaric acids, but measures the total concentration of short-chain (C^ to Cg). organic acids, alkyl sulfates, and alkyl-aryl sulfo- nates in the sample. INTERFERENCES: Carbon dioxide will interfere if it is not removed from the sample before titration. QUALITY CONTROL; A blank of distilled water should also be adsorbed on another silicic acid column, eluted, and titrated. SENSITIVITY: The sensitivity of the method is not given. The method may require modification for samples containing organic acid concentrations above 5,000 milligrams per liter. REFERENCE: American Public Health Association, Standard Methods for the Determination of Water and Wastewater. 15th ed.; APHA: Washington, 1980, pp. 467-471. COST INFORMATION: The cost per sample for analysis by this method is approximately $30-50 (list). B-110 ------- ORGANIC ACIDS: FORMIC ACID AND PROPIONIC ACID Air Samples Field Method Compound CAS Number Formic Acid 64-18-6 Propionic Acid 79-09-4 METHOD SUMMARY: Field analysis for formic acid and propionic acid in air may be performed by use of a detector tube. A 2-liter sample is collected and analyzed with a hand-operated bellows pump and a formic acid gas detector tube (Draeger® 67 22701, or equivalent). A positive result is indicated by a color change in the tube from bluish-violet to yellow as the analyte reacts with an acid indicator. This method does not identify any particular compound, but measures the total concentration of several acids in the sample. INTERFERENCES: Other acids will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The lower detection limit of the tube varies from approximately 2 to 30 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, 1979. National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger: Pittsburgh, 1981. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-lll ------- ORGANIC VAPORS Air Samples Field Method Compound Acetone Acetonitrile Acrolein Allyl Alcohol Ammonia Aniline Benzene Carbon Bisulfide Carbon Tetrachloride Chloroform Crotonaldehyde Cyclohexane Cyclohexanone 1,2-Dibromo-3-chloro- propane 1,1-Dichloroethane 1,2-Dichloroethane METHOD SUMMARY: CAS Number 67- 75- 107- 107- 7664- 62- 71- 75- 56- 67- 123- 4170- 110- 108- 96- 64-1 05-8 02-8 •18-6 •41-7 53-3 •43-2 •15-0 •23-5 •66-3 •73-9 •30-3 •82-7 •94-1 •12-8 75-34-3 107-06-2 Compound CAS Number Diethylamine 109-89-7 Ethylene Dibromide 106-93-4 Hydrogen Sulfide 7783-06-4 Methanol 67-56-1 Methyl Ethyl Ketone 78-93-3 Methyl Isobutyl Ketone 108-10-1 Methyl Isocyanate 624-83-9 Methylmercaptan 74-93-1 Nitrobenzene 98-95-3 Nitrogen Dioxide 10102-44-0 Phenol 108-95-2 Phosphine 7803-51-2 Pyridine 110-86-1 Styrene 100-42-5 Tetraethyl Lead 78-00-2 Toluene 108-88-3 Trichloroethylene 79-01-6 Field analysis for the above compounds in air can be performed by gas chromatography. The gas chromatographic analysis is either by direct injection or by heating and back-flushing the contents of a Tenax® sampling cartridge into a portable gas chromatograph with a flame ionization detector and a photo- ionization detector (GC/FID-PID). The ratio of the responses to the two detec- tors aids in identification of peaks in the chromatogram. Direct injection via a gas sampling valve or gas-tight syringe is applicable to headspace analysis. This method has been demonstrated to be field-applicable by the National Insti- tute for Occupational Safety and Health (NIOSH). INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: No sensitivity data are supplied. B-112 ------- REFERENCE: Driscoll J. N.; Hewitt, G. F. "A Rapid Screening Method for On Site Identifi- cation of Hazardous Waste," In Proc. of 2nd Oil and Hazardous Mat.rl.l Spills Conference and Exhibition; Hazardous Materials Control Research Institute- Silver Spring, Maryland, 1980. COST INFORMATION: No cost information has been obtained. B-113 ------- ORGANOPHOSPHORUS PESTICIDES Water Samples Field Method Compound CAS Number Chlorpyrifos 2921-88-2 Ethion 563-12-2 Guthion 86-50-0 Malathion 121-75-5 METHOD SUMMARY: Field analysis of water samples for several organophosphorus pesticides, including those listed above, can be accomplished by thin-layer chromatography. Water samples are extracted with an organic solvent and the extract is chromato- graphed on silica gel N plates. Positive confirmation is accomplished by spraying with a quenched solution of palladiura(II)-calcein or palladium(II)- calcein blue, followed by fluorescence detection. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to amounts above approximately 10 to 50 nanograms. REFERENCE: Bidleman, T. F.; Nowlan, B.; Frei, R. W. "Metallofluorescent Indicators as Spray Reagents for the In Situ Determination of Organophosphorus Pesticides on Thin-Layer Chromatograms," Anal. Chim. Acta, 60, 1972, pp. 13-23. COST INFORMATION: No cost information has been obtained. B-114 ------- PHENOLS: CRESOLS Air Samples Field Method Compound CAS Number Cresol 1319-77-3 m-Cresol 108-39-4 o-Cresol 95-48-7 p-Cresol 106-44-5 METHOD SUMMARY: Field analysis for cresols in air can be performed by titration. The sample is collected in a fritted bubbler or gas-washing bottle containing a 1.0- normal sodium hydroxide solution. The resulting solution is transferred to a flask, neutralized, and diluted. Potassium bromide and hydrochloric acid solu- tions are added, and the sample is placed in a water bath at 25°C for 1 hour. Potassium bromate is added and the heating is continued another hour. Potas- sium iodide is added, and after 30 minutes the liberated iodine in the sample is titrated with a standard sodium thiosulfate solution. This method does not identify a specific cresol, but measures the total cresol content of the sample. (This method is described in Jacobs, M. B. The Analytical Chemistry of Industrial Poisons, Hazards and Solvents, 2nd ed.; Interscience Publishers: New York, 1949, p. 698, and is summarized in the reference given below.) INTERFERENCES: Aromatic amines will interfere with the analysis. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The cresol sample must be greater than 10 milligrams in the volume of air sampled. REFERENCE: Quantitative Analysis of Gaseous Pollutants, W. E. Ruch, Ed.; Ann Arbor- Humphrey Science: Ann Arbor, 1970, pp. 74-75. COST INFORMATION: The cost per sample for analysis by this method is approximately $30-50 (list), plus sampling costs. B-115 ------- PHENOLIC COMPOUNDS Water Samples Field Method Compound Dinitrophenol 2,4-Dinitrophenol 2,5-Dinitrophenol 2,6-Dinitrophenol Dinoseb Pentachlorophenol Phenol Resorcinol Trichlorophenol 2,4,5-Trichlorophenol 2 ,4,6-Trichlorophenol Xylenol Zinc Phenolsulfonate 25550- 51- 329- 573- 88- 87- 108- 108- 25167- 95- 88- 1300- 127- •58-7 •28-5 •71-5 56-8 •85-7 86-5 95-2 46-3 82-2 95-4 06-2 71-6 82-2 Compound CAS Number Compound CAS Number Ammonium Picrate 131-74-8 Carbaryl 63-25-2 Ł-Chloro-m-cresol 59-50-7 2-Chlorophenol 95-57-8 Cresols 1319-77-3 m-Cresol 108-39-4 o-Cresol 95-48-7 Ł-Cresol 106-44-5 2,4-Dichlorophenol 120-83-2 2,6-Dichlorophenol 87-65-0 2,4-Dimethylphenol 105-67-9 4,6-Dinitro-o-cresol 534-52-1 and salts 4,6-Dinitro-o- 131-89-5 cyclohexylphenol METHOD SUMMARY: Field analysis for the above phenolic compounds in air may be performed by colorimetry. A 25-milliliter sample is treated with color reagents and 1 milliliter of chloroform. An orange-to-brown or rose-to-purple color in the resulting chloroform layer indicates the presence of phenolic compounds. The absence of phenolic compounds is indicated by a deep yellow color, or by com- parison with a blank of distilled water that has similarly been treated with color reagents and chloroform. The method is non-specific and will give posi- tive results for many phenolic compounds. INTERFERENCES: No interferences are reported. QUALITY CONTROL: A blank of distilled water should be processed for comparison with samples. SENSITIVITY: The method is sensitive to concentrations of phenolic compounds over approximately 1 milligram per liter- B-116 ------- REFERENCE: U.S. Environmental Protection Agency, Development of a Kit for Detecting Hazardous Material Spills in Waterways. Append^ R- BPA-ftnn/o-TB-n^ A EPA: Cincinnati, March 1978. ' COST INFORMATION: (list). The cost per sample for analysis by this method is approximately $10-18 •\. B-117 ------- PHENOLS Air Samples Field Method Compound CAS Number Cresol 1319-77-3 m-Cresol 108-39-4 o-Cresol 95-48-7 p-Cresol 106-44-5 Phenol 108-95-2 METHOD SUMMARY: Field qualitative analysis for cresols and phenol in air may be performed by use of a gas detector tube. A 1-liter sample is collected and analyzed with a hand-operated bellows pump and a phenol gas detector tube (Draeger® CH 31501, or equivalent). A positive result is indicated by a color change in the tube from pale gray to bluish-violet as the analyte reacts with 2,6-dibromo- quinonechlorimide to produce indophenol blue dye. This method does not identify any specific compound, but measures the total content of aromatic compounds with OH groups in the ring. INTERFERENCES: Other aromatic compounds and quinones may also discolor the tube. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This test will qualitatively determine whether 5 parts per million or greater of phenol or cresols are present. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, 1979. National Draeger, Inc., Measurement with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger: Pittsburgh, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $-13-20 (list). B-118 ------- PHOSPHORODITHIOATES Air Samples Field Method Compound Dimethoate Disulfoton Phorate CAS Number 60-51-5 298-04-4 298-02-2 METHOD SUMMARY: Field analysis for phosphorodithioates in air samples can be performed spectrophotometrically. For analytes in the gaseous phase, the sample is collected in bubblers containing a trapping reagent consisting of an aqueous solution of sodium hydroxide and sodium cyanide, diluted one to one with isopro- panol. After sampling, more isopropanol is added and the solution is allowed to stand 24 hours at about 15°C to convert the phosphorodithionates to thiols. For particulates, the sample is drawn through a glass-fiber filter, which is placed in the trapping solution and dispersed. A 24-hour period at 15°C allows the extraction and hydrolysis to be completed, after which the mixture is filtered. The hydrolyzed solutions are treated with sulfuric acid, sodium nitrite, ammonium sulfamate, and finally with a chromogenic reagent containing sulfanilamide, N-1-naphthylethylenedi- amine, and mercuric acetate. After the solution has stood for 2 hours, its absorbance is read at 540 nm on a portable spectrophotometer. This procedure is not specific for any particular phosphorodithioate compound, but measures the total phosphorodithioate present in the sample. INTERFERENCES: No interferences are reported. QUALITY CONTROL: When using bubblers for sample collection, collection efficiency should be determined and the value used in calculation of results. When using filters, a recovery factor should be included in the calculations. SENSITIVITY; This method is suitable for determinations to less than 0.1 milligrams of phosphorodithioate per cubic meter of air. REFERENCE; Lloyd, G. A.; Bell, G. J. "Mobile Laboratory Methods for the Determination of Pesticides in Air. Part I. Phosphorothiolothionates," Analyst, 91., 1966, pp. 806-808. B-119 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $30-55 (list), plus sampling costs. B-120 ------- POLYCHLORINATED BIPHENYLS AND CHLORINATED PESTICIDES Water Samples Field Method Compound CAS Number o-Endosulfan 959-98-8 B-Endosulfan 33213-65-9 Endosulfan 115-29-7 Endosulfan Sulfate 1031-07-8 Endrin 72-20-8 Polychlorinated Biphenyls 1336-36-3 12674-11-2 11104-28-2 11141-16-5 53469-21-9 12672-29-6 11097-69-1 11096-82-5 METHOD SUMMARY: Field analysis of water samples for the above PCB's and chlorinated pesti- cides can be performed by thin-layer chromatography . The sample is extracted with n-heptane and chromatographed on Silufol foil with n-heptane as a solvent or on FND foil with methanol : chloroform (90:10) as a solvent. Positive confir- mation is accomplished by spraying with sodium hydroxide, then thymol reagent, and heating for 20 minutes. (This method is given by Thielemann, H. Z. Chem. , 1978, pp. 147-148 and is summarized in the reference given below). INTERFERENCES : No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is sensitive to amounts of analyte above 6 micrograms REFERENCE : Chem. Abstr.. 1978, 89 (3): 18216X,. COST INFORMATION: No cost information has been obtained. B-121 ------- TOLUENE AND OTHER AROMATICS Air Samples Field Method Compound CAS Number Cumene 98-82-8 Ethylbenzene 100-41-4 Toluene 108-88-3 Xylene 1330-20-7 m-Xylene 108-38-3 o-Xylene 95-47-6 Ł-Xylene 106-42-3 METHOD SUMMARY: Analysis for toluene and other aromatic compounds listed above may be performed by use of a detector tube. A 1-liter sample is collected and analyzed with a hand-operated bellows pump and a toluene gas detector tube (Draeger® CH 27801, or equivalent). Positive results are indicated by a color change in the tube from pale gray to brownish-violet. This method is based on a reaction with selenium dioxide and sulfuric acid to form the colored product. The method does not identify any particular compound. INTERFERENCES: Benzene may cause yellowish-brown discolorations, which will not affect the determination of toluene, xylenes, cumene, or ethylbenzene. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The lower detection limit of the tube is approximately 500 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, 1979. National Draeger®, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger: Pittsburgh, 1981. B-122 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-123 ------- VINYL CHLORIDE AND OTHER CHLORINATED HYDROCARBONS Air Samples Field Method Compound CAS Number 1,1-Dichloroethylene 75-35-4 1,2-Dichloropropane 78-87-5 1,1,2,2-Tetrachloroethane 79-34-5 Vinyl Chloride 75-01-4 METHOD SUMMARY: Field analysis for vinyl chloride, 1,1-dichloroethylene , 1,2-dichloropro- pane, and 1,1,2,2-tetrachloroethane may be performed by use of a gas detector tube. A 0.2-liter to 0.4-liter sample is collected with a portable pump and analyzed with a vinyl chloride gas detector tube (Bendix/Gastec® 131 La, or equivalent). A positive result is indicated by a color change from yellow to reddish-brown in the tube. INTERFERENCES; High concentrations of chlorine, hydrogen chloride, trichloroethylene, and perchloroethylene may also give positive results. Benzene, toluene, xylene, and ethylene can interfere. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The tube will measure vinyl chloride concentrations of approximately 0.5 to 3 milligrams per cubic meter, 1,1-dichloroethylene concentrations of approximately 1 to 25 milligrams per cubic meter, 1,1,2,2-tetrachloroethane concentrations of approximately 20 to 500 milligrams per cubic meter, and 1,2-dichloropropane concentrations of approximately 150 to 3,000 milligrams per cubic meter. REFERENCE: Bendix Corporation, Bendix/Gastec® Precision Gas Detector System Manual (Blue Book); Bendix: Largo, Florida, 1983. COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-124 ------- VINYL CHLORIDE, BENZYL CHLORIDE, ALLYL CHLORIDE, AND 1,1-DICHLOROETHYLENE Air Samples Field Method Compound CAS Number Allyl Chloride 107-05-1 Benzyl Chloride 100-44-7 1,1-Dichloroethylene 75-35-4 Vinyl Chloride 75-01-4 METHOD SUMMARY: Field analysis for vinyl chloride, benzyl chloride, allyl chloride, and 1,1-dichloroethylene in air may be performed by use of a detector tube. A 0.5- liter to 2-liter sample is collected and analyzed with a hand-operated bellows pump and a vinyl chloride gas detector tube (Draeger® 67 28031, or equivalent). A positive result is indicated by a color change in the tube from white to weak yellowish-orange. This method is based on liberation of chlorine followed by reaction with o_-tolidine, and does not identify any specific compound. INTERFERENCES: Tetrachloroethylene and trichloroethylene will also give positive results and organic solvent vapors may cause the determinations to be low. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: 1,1-Dichloroethylene is indicated with about twice the sensitivity of benzyl chloride and vinyl chloride. Allyl chloride is indicated with about half the sensitivity of vinyl chloride. The lower detection limit of the tube varies from approximately 2 to 5 milligrams per cubic meter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh, August 1979. National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1, 1982. National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit Value Range. Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger: Pittsburgh, December 1981. E. G. Ligus, National Draeger, Inc., Pittsburgh, personal communication, 1983. B-125 ------- COST INFORMATION: The cost per sample for analysis by this method is approximately $13-20 (list). B-126 ------- VOLATILE ORGANIC COMPOUNDS . Air Samples Field Method Compound Acetic Acid Acetic Anydride Acetone Acetone Cyanohydrin Acetonitrile Acetophenone Acetyl Chloride Acrylic Acid Acrylonitrile Allyl Alcohol Benzene Benzonitrile Benzoyl Chloride Benzyl Chloride Butyl Acetate n-Butyl Alcohol Butylamine sec-Butylamine tert-Butylamine Butyric Acid Carbon Bisulfide Carbon Tetrachloride Chloroacetaldehyde Chlorobenzene Chloroethane Chloroform 2-Chlorophenol Ł-Cresol Crotonaldehyde Cumene Cyclohexane Cyclohexanone 1,2-Dichlorobenzene 1,3-Dichlorobenzene 1,1-Dichloroethane 1,2-Dichloroethane 1,1-Dichloroethylene 1,2-trans-Dichloro- ethylene 1,2-Dichloropropane CAS Number 64- 108- 67- 75- 75- 98- 75- 79- 107- 107- 71- 100- 98- 100- 123- 71- 109- 513- 13952- 75- 107- 75- 56- 107- 108- 75- 67- 95- 95- 123- 4170- 98- 110- 108- 95- 541- 75- 107- 75- 156- 19-7 24-7 64-1 86-5 05-8 86-2 36-5 •10-7 •13-1 •18-6 •43-2 •47-0 •88-4 •44-7 •86-4 •36-3 •73-9 •49-5 •84-6 •64-9 •92-6 •15-0 •23-5 •20-0 •90-7 •00-3 •66-3 •57-8 •48-7 •73-9 -30-3 •82-8 •82-7 •94-1 •50-1 •73-1 •34-3 •06-2 •35-4 •60-5 78-87-5 Compound Dichloropropene 1,1-Dimethylhydrazine 1,4-Dioxane Epichlorohydrin Ethyl Acetate Ethyl Acrylate Ethylbenzene Ethylenediaraine Ethylene Oxide Ethyl Ether Formic Acid Furfural Isoprene Methanol Methyl Chloride Methyl Ethyl Ketone Methyl Isobutyl Ketone Methyl Methacrylate Nitrobenzene Phenol 2-Picoline Propionic Acid Propylene Oxide Pyridine Styrene 1,1,1,2-Tetrachloro- ethane 1,1,2,2-Tetrachloro- ethane Tetrachloroethylene Toluene 1,2,4-Trichlorobenzene 1,1,1-Trichloroethane 1,1,2-Trichloroethane Trichloroethylene Triethylamine Vinyl Acetate Vinyl Chloride m-Xylene o-Xylene p-Xylene CAS Number 26952- 57- 123- 106- 141- 140- 100- 107- 75- 60- 64- 98- 78- 67- 74- 78- 108- 23-8 14-7 •91-1 89-8 78-6 88-5 41-4 15-3 21-8 29-7 •18-6 01-1 79-5 56-1 •87-3 93-3 •10-1 80-62-6 98-95-3 108-95-2 109-06-8 79-09-4 75-56-9 110-86-1 100-42-5 630-20-6 79-34-5 127-18-4 108-88-3 120-82-1 71-55-6 79-00-5 79-01-6 121-44-8 108-05-4 75-01-4 108-38-3 95-47-6 106-42-3 B-127 ------- METHOD SUMMARY: Field analysis for the above organic compounds in air samples can be per- formed semi-quantitatively using a volatile organic chemical (VOC) analyzer. The VOC analyzer may be a portable flame ionization detector (FID) or a com- bustible gas detector. A response factor is used to correct the observed concentration to obtain the actual concentration. This method does not identify the specific organic compound(s) present, but measures the total organic content of the sample. A gas chromatograph option is available for the FID analyzer that will provide some specificity. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is suitable for concentrations of volatile organic compounds in the range of approximately 1 to 150 grams per cubic meter. The maximum concentrations do not apply if the air becomes saturated with the volatile organic compounds. REFERENCE: Harris, G.; Tichenor, B. In Energy and Environmental Chemistry. Vol. I, Ch. 16, L. Keith, Ed.; Ann Arbor Science: Ann Arbor, 1982. COST INFORMATION: The cost of analysis by this method is approximately $15-25 (list). B-128 ------- VOLATILE SPECIES Soil/Sediment Samples Field Method Compound CAS Number Acetone 67-64-1 Benzene 71-43-2 Chlorobenzene 108-90-7 Ethyl Ether 60-29-7 Methylene Chloride 75-09-2 Tetrachloroethylene 127-18-4 Toluene 108-88-3 Trichloroethylene 79-01-6 METHOD SUMMARY: Field analysis for the above volatile species in soil/sediment samples can be performed using a detector tube (Draeger®, or equivalent). About 50 grams of sample are mixed with distilled water, and the paste is placed in a 250- milliliter gas scrubbing bottle with frit inset. The appropriate detector tube is connected to the scrubbing bottle and to a gas detector pump. Air is drawn through the sample, volatilizing some of the analyte. A color change to brownish-green in the tube indicates a positive result. A screening type of detector tube (Draeger Polytest, or equivalent) can sometimes be used when the contaminant is unknown. INTERFERENCES: If several contaminants are present in a sample, the detection limits may change. Reactions such as hydrolysis may also occur. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY; The approximate detection limit for acetone, benzene, ethyl ether, and toluene is 50 milligrams per kilogram of sample; for chlorobenzene, 10 milli- grams per kilogram; for methylene chloride, 200 milligrams per kilogram: for tetrachloroethylene and trichloroethylene, 20 milligrams per kilogram. REFERENCE: Mussman, B. "Analyses for Environmental Protection," Draeger Rev., 51, 1983, pp. 17-19. B-129 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $20-30 (list). B-130 ------- VOLATILE SPECIES Water Samples Field Method Compound Acetaldehyde Acetone Ammonia Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Bifluoride Ammonium Bisulfite Ammonium Carbamate Ammonium Carbonate Ammonium Chloride Ammonium Chromate Ammonium Citrate, Dibasic Ammonium Bichromate Ammonium Fluoborate Ammonium Fluoride Ammonium Hydroxide Ammonium Oxalate Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate CAS Number 75- 67- 7664- 631- 1863- 1066- 1341- 10192- 1111- 506- 12125- 7788- 3012- 7789- 13826- 12125- 1336- 6009- 5972- 14258- 131- 16919- 7773- 12135- 10196- 14307- 3164- •07-0 64-1 •41-7 61-8 •63-4 •33-7 •49-7 •30-0 •78-0 •87-6 •02-9 •98-9 •65-5 •09-5 •83-0 •01-8 •21-6 •70-7 73-6 •49-2 •74-8 •19-0 •06-0 •76-1 •04-0 •43-8 •29-2 Compound Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Benzene Carbon Bisulfide Carbon Tetrachloride Chlorobenzene Cupric Sulfate, Ammoniated Cyclohexane Ethyl Acetate Ethylbenzene Ethyl Ether Epichlorohydrin Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferrous Ammonium Sulfate Methylene Chloride Methylmercaptan Nickel Ammonium Sulfate Tetrachloroethylene Thiophenol Toluene Trichloroethylene Triethylamine Zinc Ammonium Chloride CAS Number 1762- 7783- 7803- 71- 75- 56- 108- 10380- 110- 141- 100- 60- 106- 1185- 2944- 55488- 10045- 75- 74- 15699- 127- 108- 108- 79- 121- 52628- 14639- 14639- •95-4 •18-8 •55-6 •43-2 •15-0 •23-5 •90-7 •29-7 •82-7 78-6 •41-4 •20-7 89-8 57-5 •67-4 87-4 89-3 09-2 93-1 18-0 •18-4 98-5 •88-3 01-6 •44-8 •25-8 •97-5 98-6 METHOD SUMMARY: Analysis for the above volatile species in water samples can be performed using a detector tube (Draeger, or equivalent). About 100 milliliters of sample are placed in a 250-milliliter gas scrubbing bottle with frit inset. The appropriate detector tube is connected to the scrubbing bottle and to a gas detector pump. Air is drawn through the sample, volatilizing some of the analyte. A color change in the tube indicates a positive result. A screening type of detector tube, such as the Draeger Polytest, can sometimes be used when the contaminant is unknown. Analysis for ammonium and mercapto compounds are not specific for any particular ammonium or mercapto compound, but indicate the total ammonium content or the total mercapto content of the sample. B-131 ------- INTERFERENCES: If several contaminants are present in a sample, the detection limits may change. Reactions such as hydrolysis may also occur. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The approximate detection limit for acetaldehyde is 10 milligram per liter of sample; for acetone, benzene, chlorobenzene, ethyl ether, ethylbenzene, and methylene chloride, 1 milligram per liter; for acrylonitrile, 2 milligrams per liter; for ammonium in ammonium compounds, carbon disulfide, and toluene, 0.5 milligram per liter; for carbon tetrachloride, epichlorohydrin, tetra- chloroethylene, and trichloroethylene, 0.1 milligram per liter; for cyclohexane, 5 milligrams per liter; for ethyl acetate, 50 milligrams per liter; for mer- captan in mercapto compounds, 0.2 milligram per liter; for triethylamine, 30 milligrams per liter. REFERENCE: Mussman, B. "Analyses for Environmental Protection," Draeger Rev.. 51, 1983, pp. 17-19. COST INFORMATION: Cost per sample for analysis by this method is approximately $17-27 (list). B-132 ------- Part II. Laboratory Methods A. Inorganic Substances B. Organic Substances B-133 ------- A. Inorganic Substances B-134 ------- ACID ANIONS Water Samples Laboratory Method Compound Acetic Acid Acetyl Bromide Acetyl Chloride Acrylic Acid Adipic Acid Aluminum Sulfate Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Carbonate Ammonium Citrate, Dibasic Ammonium Fluoride Ammonium Oxalate Ammonium Sulfamate Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Antimony Potassium Tartrate Antimony Trifluoride Barium Cyanide Beryllium Fluoride METHOD SUMMARY: CAS Number Compound CAS Number 64-19-7 Beryllium Nitrate 506-96-7 75-36-5 Cadmium Acetate 79-10-7 Calcium Cyanide 124-04-9 Chromic Acetate 10043-01-3 Chromic Sulfate 631-61-8 Cobaltous Formate 1863-63-4 Cupric Acetate 1066-33-7 Cupric Oxalate 506-87-6 Cupric Tartrate 3012-65-5 Ferric Ammonium Citrate 12125-01-8 Ferric Ammonium Oxalate 6009-70-7 5972-73-6 Ferric Fluoride 14258-49-2 Fluoroacetic Acid, 7773-06-0 Sodium Salt 10196-04-0 Lead Acetate 301-04-2 14307-43-8 Mercuric Thiocyanate 592-85-8 3164-29-2 Sodium Bisulfite 7631-90-5 1762-95-4 Sodium Fluoride 7681-49-4 7783-18-8 Thallium (I) Acetate 563-68-8 28300-74-5 Zinc Acetate 557-34-6 Zinc Fluoride 7783-49-5 7783-56-4 Zinc Formate 557-41-5 542-62-1 Zirconium Potassium 16923-95-8 7787-49-7 Fluoride 13597- 7787- 543- 592- 1066- 10101- 544- 142- 5893- 815- 1185- 55488- 2944- 7783- 62- 99-4 55-5 •90-8 01-8 •30-4 53-8 •18-3 71-2 66-3 82-7 57-5 87-4 •67-4 50-8 74-8 Analysis for the anions from strong and weak acids in water samples can be performed by ion chromatographic analysis with resistivity detection. Use of 0.0025 N phosphoric acid as an eluent allows simultaneous analysis for cyanide, bicarbonate, sulfate, fluoride, and nitrate ions. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. B-135 ------- EPA/TECHNICAL STATUS: This method has been evaluated on standard solutions and is not EPA- approved and has not undergone rigorous evaluation. No precision and accuracy information is furnished. The method can detect levels above approximately 1 milligram per liter. REFERENCES: U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-11, "Anions by Ion Chromatography;" HASL-300, Environmental Measurements Laboratory, U.S. DOE: New York, 1983. Pinschmidt, R. K. "Ion Chromatographic Analysis of Weak Acid Ions Using Resistivity Detection," In Ion Chromatographic Analysis of Environmental Pollutants, Vol. 2, J. D. Mulick; E. G. Sawicki, Eds.; Ann Arbor Science: Ann Arbor, 1979, p. 41. COST INFORMATION: Cost per sample for analysis by this method is approximately $70 (list). B-136 ------- ALUMINUM Air Samples Laboratory Method 1 Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Determination of aluminum ions from the above compounds in air may be performed by atomic absorption (AA) spectrometric analysis for aluminum. Samples are collected by cellulose-membrane filtration. The filter medium is digested with nitric acid, diluted, and analyzed by AA. This method does not differentiate between specific aluminum-containing compounds, but measures the total aluminum content of the sample. INTERFERENCES: Cesium should be added to samples and standards to control ionization interferences. Lanthanum should be added to standards and samples as a releasing agent. Sulfate, vanadium, iron, hydrochloric acid, and sulfuric acid may interfere. The methods of standard additions and/or background monitoring may be needed to correct for interferences. Some aluminum compounds may not be dissolved by this procedure. 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 not EPA-approved. Precision information is furnished. The detection limit of this method is 20 micrograms of aluminum per liter. 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. U.S. Department of Energy and 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-137 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $10-20 (list), plus sampling costs. B-138 ------- ALUMINUM Air Samples Laboratory Method 2 Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Analysis for aluminum ions from the above compounds in air may be per- formed by inductively coupled plasma atomic emission spectroscopic (ICP) analysis for aluminum. A known volume of air is drawn through a mixed cellu- lose 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 aluminum-containing compounds, but measures the total aluminum 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 of aluminum per cubic meter for a 500-liter sample. Precision and accuracy infor- mation is furnished. REFERENCE: U.S. Department of Health Education and Welfare, NIOSH Manual of Analytical Methods, Vol. 7, Method P&CAM 351; Publication No. 82-100, U.S. DREW: Cincinnati, August 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $10 (list), plus sampling costs. B-139 ------- ALUMINUM Soil/Sediment Samples Laboratory Method Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Analysis for aluminum ions from the above compounds in soil/sediment samples can be performed by atomic spectrometric analysis for aluminum. A 2-gram sample is digested with nitric acid and hydrogen peroxide and analyzed by inductively coupled plasma (ICP) or by flame or furnace atomic absorption (AA) spectrometry. Analysis for aluminum 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 the aluminum-containing compounds present, but measure the total aluminum content of the sample. INTERFERENCES: For flame AA, potassium should be added to the sample and standards to prevent the partial oxidation of aluminum in the flame. For furnace AA, chloride ion and the use of nitrogen as a purge gas may suppress the signal. 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 analyses for the Clean Water Act and for the Resource Conservation and Recovery Act. Precision and accuracy information is furnished for the flame A and ICP methods. 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 202.1, 202.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. B-140 ------- U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, SW-846, 2nd ed., Methods 6010, 3010, 3020; U.S. EPA: Washington, 1984. Federal Register, 44_(233), December 3, 1979, pp. 69559-69564. Fassel, 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. , ^8_ (3), 1976, pp. 516-519. COST INFORMATION: Cost per sample for analysis by flame AA is approximately $20-30 (list); by furnace AA, approximately $28-60 (list); by ICP, approximately $20 (list). B-141 ------- ALUMINUM Water Samples Laboratory Method 1 Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Water samples may be analyzed for aluminum ions from the above compounds by atomic spectrometric analysis for aluminum. A 100-milliliter sample is digested with nitric acid and hydrogen peroxide and the resulting solution is analyzed for aluminum by either inductively coupled plasma (ICP) or flame atomic absorption (AA) spectrometry. Alternatively, the digested sample can be extracted with a solution of 8-hydroxyquinoline in methyl isobutyl ketone and the extract analyzed by flame AA. These methods do not identify the aluminum- containing compounds present, but measure the total aluminum content of the sample. INTERFERENCES; For direct AA, potassium should be added to the sample and standards to prevent the partial oxidation of aluminum in the flame. Iron concentrations above 10 milligrams per liter can interfere. 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 analyses for the Clean Water Act and the Resource Conservation and Recovery Act (RCRA). The direct AA method is suitable for concentrations from 0.1 to 5 milligrams per liter, while the extraction/AA procedure is applicable over the range of 10 to 300 micrograms per liter. 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 202.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. B-142 ------- U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Wastes, SW-846, 2nd ed., Methods 3010, 3020, 6010; U.S. EPA: Washington, 1984. 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. 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., Method 306A; APHA: Washington, 1980. Fassel, 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., ^8 (3), 1976, pp. 516-519. U.S. Department of Energy and 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 the analysis by AA is approximately $10-20 (list); by ICP it is approximately $10 (list). B-143 ------- ALUMINUM Water Samples Laboratory Method 2 Compound CAS Number Aluminum Phosphide 20859-73-8 Aluminum Sulfate 10043-01-3 METHOD SUMMARY: Water samples may be analyzed for aluminum ions from the above compounds by spectrometric or fluorimetric analysis for aluminum. For fluorimetry, the fluorescence intensity of an aluminum-morin complex formed at pH 3 is measured and quantified by use of a calibration curve. Spectrophotometric analysis is performed either by reaction of aluminum with ferron and measurement of the ultraviolet absorbance of the resulting complex at 370 nm, or by complexation of aluminum in the sample with sodium fluoride, removal of interfering cations with cation exchange resin and 8-quinolinol-chloroform extraction, pH adjust- ment to form the aluminum-8-quinolinol complex, and measurement of the result- ing ultraviolet absorbance at 380 nm. These methods do not identify any specific aluminum-containing compound, but measure the total aluminum content of the sample. INTERFERENCES; The fluorimetric and direct Spectrophotometric methods are suitable for use for relatively high-purity water samples, as heavy-metal ion concentrations above approximately 20 micrograms per liter interfere. In the direct Spectro- photometric method, iron interferences can be minimized by the addition of orthophenanthroline. The complexation/extraction/spectrophotometric method suffers interferences from manganous, cupric, and ferric ion concentrations above 0.01, 0.11, and 0.1 milligrams per liter, respectively, and from phos- phate, polyphosphate, fluoride and magnesium ion concentrations above 0.5 milligrams per liter. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: These methods are not EPA-approved. The fluorimetric method is applicable to aluminum concentrations below 5 micrograms per liter, while the chelation/ extraction/spectrophotoraetric method is applicable over the range of 0 to 0.5 milligrams per liter, based on a 100-milllliter sample. Precision and accuracy information is furnished. B-144 ------- REFERENCE: American Society for Testing and Materials, 1983 Annual Book of ASTM Standards, Volume 11.01, Methods D857A, D857B, D857C; ASTM: Philadelphia, 1983. COST INFORMATION: Cost per sample for analysis by these methods range from $20-85 (list). B-145 ------- AMMONIA Air Samples Laboratory Method Compound CAS Number Ammonia Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Bifluoride Ammonium Bisulfite Ammonium Carbamate Ammonium Carbonate Ammonium Chloride Ammonium Chr ornate Ammonium Citrate, Dibasic Ammonium Dichr ornate Ammonium Fluoborate Ammonium Fluoride Ammonium Hydroxide Ammonium Oxalate 7664-41-7 631-61-8 1863-63-4 1066-33-7 1341-49-7 10192-30-0 1111-78-0 506-87-6 12125-02-9 7788-98-9 3012-65-5 7789-09-5 13826-83-0 12125-01-8 1336-21-6 6009-70-7 5972-73-6 14258-49-2 Compound Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Cupric Sulfate, Ammoniated Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferrous Ammonium Sulfate Nickel Ammonium Sulfate Zinc Ammonium Chloride CAS Number 131- 16919- 7773- 12135- 10196- 14307- 3164- 1762- 7783- 7803- 10380- 1185- 2944- 55488- 10045- 15699- 52628- 14639- 14639- -74-8 •19-0 -06-0 •76-1 •04-0 •43-8 •29-2 •95-4 •18-8 55-6 •29-7 57-5 •67-4 87-4 •89-3 •18-0 •25-8 97-5 •98-6 METHOD SUMMARY: Ammonia and the above ammonium compounds in air samples may be measured spectrophotometrically. The sample is collected in impingers containing dilute sulfuric acid. The resulting solution is reacted with alkaline phenol and hypochlorite to form indophenol, a blue compound. The intensity of the blue color is measured at 630 nm. Sodium nitroprusside is added to increase the sensitivity. This method does not differentiate between various ammonia- containing compounds, but responds to any ammonium ions or ammonia in the sample. INTERFERENCES: Color and turbidity may interfere with this method. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. No precision and accuracy information is furnished. The detection limit for the indophenol method is 0. 1 milligrams ammoniacal nitrogen per liter of test solution (Alberta Environment). B-146 ------- REFERENCES: Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual. Vol. HI, Available Laboratory Analytical Methods," Methods for the Determination of Ammonia," pp. IV-156 to IV-181; EPA-600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas, 1984. Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric Pollutants, Method 11010; Alberta Environmental Centre: Alberta, Canada, 1981. COST INFORMATION; Cost per sample for analysis by this method is approximately $15-30 (list), plus sampling costs. B-147 ------- AMMONIA Soil/Sediment Samples Laboratory Method Compound CAS Number Ammonia Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Bifluoride Ammonium Bisulfite Ammonium Carbamate Ammonium Carbonate Ammonium Chloride Ammonium Chromate Ammonium Citrate, Dibasic Ammonium Dichromate Ammonium Fluoborate Ammonium Fluoride Ammonium Hydroxide Ammonium Oxalate 7664-41-7 631-61-8 1863-63-4 1066-33-7 1341-49-7 10192-30-0 1111-78-0 506-87-6 12125-02-9 7788-98-9 3012-65-5 7789-09-5 13826-83-0 12125-01-8 1336-21-6 6009-70-7 5972-73-6 14258-49-2 Compound Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Cupric Sulfate, Ammoniated Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferrous Ammonium Sulfate Nickel Ammonium Sulfate Zinc Ammonium Chloride CAS Number 131- 16919- 7773- 12135- 10196- 14307- 3164- 1762- 7783- 7803- 10380- 1185- 2944- 55488- 10045- 15699- 52628- 14639- 14639- -74-8 -19-0 -06-0 -76-1 -04-0 •43-8 •29-2 •95-4 •18-8 •55-6 •29-7 •57-5 •67-4 •87-4 89-3 •18-0 •25-8 •97-5 98-6 METHOD SUMMARY: Analysis for ammonia and the above ammonium compounds in soil/sediment samples can be performed by potentiometric or colorimetric analysis for ammonia. For potentiometry, a sample is extracted with NaCl/HCl, and the resulting solu- tion is made basic by the addition of sodium hydroxide and analyzed potentiom- etrically using an ion-selective ammonia electrode and a pH meter. Samples must be preserved by acidification and refrigeration at 4°C. For colorimetry, a representative sample is extracted with aqueous potassium chloride, and the ammonia in the extract is determined by reaction with phenol and alkaline sodium hypochlorite to form a blue-colored indophenol derivative, followed by measurement of the intensity of the resulting color. This method does not differentiate between compounds, but responds to any ammonium ions or ammonia in the sample. INTERFERENCES: Volatile amines and mercury may interfere. QUALITY CONTROL: No quality control procedures are given. B-148 ------- EPA/TECHNICAL STATUS: This method is in use in the CERCLA program and is approved for the National Pollutant Discharge Elimination System (NPDES). The colorimetric method is applicable over the range 12 to 720 milligrams ammonia per kilogram of sample (Alberta Environmment). 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, April 23, 1982. U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and Wastes, Method 350.3; EPA-600/4-79-020, U.S. EPA, March 1979. Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determination of Ammonia," pp. IV-156 to IV-181; EPA-600/S4-84-038, U.S. Environmental Protec- tion Agency: Las Vegas, 1984. Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water and Wastes, "Nitrogen, Ammonia, Exchangeable;" Publication No. AECV81-M1, Alberta Environmental Centre: Vegreville, Alberta, Canada, 1981. Plumb, R. H. Procedures for Handling and Chemical Analysis of Sediment and Water Samples, pp. 3-154 to 3-158; Environmental Laboratory U.S. Army Engineer Waterways Experiment Station; Vicksburg, Mississippi, 1981. COST INFORMATION: Cost per sample for analysis by the potentiometric method is approxmately $10-19 (list); by the colorimetric method it is approximately $25-50 (list). B-149 ------- AMMONIA Water Samples Laboratory Methodl Compound CAS Number Ammonia Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Bifluoride Ammonium Bisulfite Ammonium Carbamate Ammonium Carbonate Ammonium Chloride Ammonium Chromate Ammonium Citrate, Dibasic Ammonium Dichromate Ammonium Fluoborate Ammonium Fluoride Ammonium Hydroxide Ammonium Oxalate 7664-41-7 631-61-8 1863-63-4 1066-33-7 1341-49-7 10192-30-0 1111-78-0 506-87-6 12125-02-9 7788-98-9 3012-65-5 7789-09-5 13826-83-0 12125-01-8 1336-21-6 6009-70-7 5972-73-6 14258-49-2 Compound Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Cupric Sulfate, Ammoniated Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferrous Ammonium Sulfate Nickel Ammonium Sulfate Zinc Ammonium Chloride CAS Number 131- 16919- 7773- 12135- 10196- 14307- 3164- 1762- 7783- 7803- 10380- 1185- 2944- 55488- 10045- 15699- 52628- 14639- 14639- -74-8 •19-0 •06-0 •76-1 •04-0 •43-8 •29-2 95-4 •18-8 55-6 •29-7 57-5 •67-4 87-4 •89-3 •18-0 25-8 97-5 98-6 METHOD SUMMARY: Analysis for ammonia and the above ammonium compounds in water samples can be performed by potentiometric analysis for ammonia. A 100-milliliter sample is made basic by the addition of sodium hydroxide and analyzed potentiometri- cally using an ion-selective ammonia electrode and a pH meter. Samples must be preserved by acidification and refrigeration at 4°C. This method does not differentiate between compounds, but responds to any ammonium ions or ammonia in the sample. INTERFERENCES: Volatile amines, mercury, and silver may interfere. QUALITY CONTROL: No quality control information is given. EPA/TECHNICAL STATUS: This method is in use in the CERCLA program and is approved for the National Pollutant Discharge Elimination System (NPDES). Precision and accuracy information is furnished. B-150 ------- 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 350.3; 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., Method 417E; APHA: Washington, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $10-20 (list). B-151 ------- AMMONIA Water Samples Laboratory Method 2 Compound CAS Number Ammonia Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Bifluoride Ammonium Bisulfite Ammonium Carbamate Ammonium Carbonate Ammonium Chloride Ammonium Chromate Ammonium Citrate, Dibasic Ammonium Bichromate Ammonium Fluoborate Ammonium Fluoride Ammonium Hydroxide Ammonium Oxalate 7664-41-7 631-61-8 1863-63-4 1066-33-7 1341-49-7 10192-30-0 1111-78-0 506-87-6 12125-02-9 7788-98-9 3012-65-5 7789-09-5 13826-83-0 12125-01-8 1336-21-6 6009-70-7 5972-73-6 14258-49-2 Compound Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Cupric Sulfate, Ammoniated Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferric Ammonium Sulfate Nickel Ammonium Sulfate Zinc Ammonium Chloride CAS Number 131- 16919- 7773- 12135- 10196- 14307- 3164- 1762- 7783- 7803- 10380- 1185- •74-8 •19-0 •06-0 76-1 •04-0 43-8 •29-2 95-4 18-8 55-6 •29-7 57-5 2944-67-4 55488-87-4 10045-89-3 15699-18-0 52628-25-8 14639-97-5 14639-98-6 METHOD SUMMARY: Analysis of water samples for ammonia and the above ammonium compounds can be performed by distillation, followed by titrimetry, potentiometry, or colori- metry. A 400-milliliter sample, buffered with alkali, is distilled into boric acid and the resulting solution is analyzed colorimetrically by reaction with Nessler's reagent, titrimetrically with sulfuric acid, or potentiometrically with an ammonia electrode. Ammonia concentrations above 1 milligram per liter should be determined titrimetrically. Samples must be preserved by acidifica- tion and storage at 4°C. These methods are not compound-specific, but will determine the ammonia-nitrogen present in the sample. INTERFERENCES: Volatile alkaline compounds such as ketones, aldehydes, and alcohols may cause an off-color during the reaction with Nessler's reagent and require removal before distillation when using the colorimetric method. Cyanate will hydrolyze to some extent even at the pH of 9.5 at which distillation is carried out. Volatile amines can be a positive interference, and silver ions and mercury ions can interfere by complexing ammonia. For all methods, residual chlorine must be removed by the addition of sodium thiosulfate before distilla- tion. This method is not specific for any ammonia compound, but responds to any ammonium ions or ammonia in the sample. B-152 ------- QUALITY CONTROL: Both distilled and undistilled standards should be analyzed. EPA/TECHNICAL STATUS: These methods are in use in the CERCLA program and are approved for the National Pollutant Discharge Elimination System (NPDES). 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 350.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol. Ill, Available Laboratory Analytical Methods: "Methods for the Determina- tion of Ammonia," pp. IV-156 to IV-181; 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., Method 417E; APHA: Washington, 1980. COST INFORMATION: Cost per sample for analysis by these methods is approximately $28-38 (list). B-153 ------- AMMONIA Water Samples Laboratory Method 3 (Automated) Compound CAS Number Ammonia Ammonium Acetate Ammonium Benzoate Ammonium Bicarbonate Ammonium Bif luoride Ammonium Bisulfite Ammonium Carbatnate Ammonium Carbonate Ammonium Chloride Ammonium Chromate Ammonium Citrate, Dibasic Ammonium Bichromate Ammonium Fluoborate Ammonium Fluoride Ammonium Hydroxide Ammonium Oxalate 7664-41-7 631-61-8 1863-63-4 1066-33-7 1341-49-7 10192-30-0 1111-78-0 506-87-6 12125-02-9 7788-98-9 3012-65-5 7789-09-5 13826-83-0 12125-01-8 1336-21-6 6009-70-7 5972-73-6 14258-49-2 Compound Ammonium Picrate Ammonium Silicofluoride Ammonium Sulfamate Ammonium Sulfide Ammonium Sulfite Ammonium Tartrate Ammonium Thiocyanate Ammonium Thiosulfate Ammonium Vanadate Cupric Sulfate, Ammoniated Ferric Ammonium Citrate Ferric Ammonium Oxalate Ferric Ammonium Sulfate Nickel Ammonium Sulfate Zinc Ammonium Chloride CAS Number 131- 16919- 7773- 12135- 10196- 14307- 3164- 1762- 7783- 7803- 10380- 1185- 2944- 55488- 10045- 15699- 52628- 14639- 14639- •74-8 •19-0 •06-0 •76-1 •04-0 •43-8 •29-2 •95-4 •18-8 55-6 •29-7 57-5 •67-4 87-4 89-3 18-0 •25-8 97-5 98-6 METHOD SUMMARY: Analysis for ammonia and the above ammonium compounds in water can be performed by automated colorimetric analysis for ammonia nitrogen. An auto- mated analytical system is used to colorimetrically analyze the samples. A 400-milliliter sample is made basic with sodium hydroxide, distilled into boric acid, reacted to form indophenol blue, and the resulting solution is analyzed colorimetrically. Samples must be preserved by acidification and refrigeration at 4°C. This method is not compound-specific, but measures the total ammonia nitrogen present in a sample. INTERFERENCES: Interferences from high concentrations of calcium and magnesium ions may be prevented by the addition of a 5-percent EDTA solution. Sample turbidity and color may interfere. QUALITY CONTROL: The pH of the samples and standards should be the same. should be prepared fresh daily. Standard solutions B-154 ------- EPA/TECHNICAL STATUS: This method is in use in the CERCLA program and is approved for the National Pollutant Discharge Elimination Service (NPDES). 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 350.1; 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 Determination of Ammonia," pp. IV-156 to IV-181; EPA-600/S4-84-038, U.S. Environmental Protec- tion Agency: Las Vegas, 1984. Alberta Environmental Centre, Methods Manual for Chemical Analysis of Water and Wastes, "Nitrogen, Ammonia Dissolved;" Publication NO. AECV81-M1, Alberta Environmental Centre, Vegreville, Alberta, Canada, 1981. COST INFORMATION: Cost information has not been obtained. B-155 ------- ANTIMONY Air Samples Laboratory Method 1 Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Analysis for antimony and the above antimony compounds in air can be performed by membrane filtration of a known volume of air, followed by acid digestion of the sampling medium and flame or furnace atomic absorption (AA) analysis of the resulting solution for antimony. These methods are not appli- cable to antimony compounds which exist as vapors and do not differentiate between different antimony compounds, but measure the total antimony in the sample. INTERFERENCES: Tartaric acid is added to the digested sample to prevent formation of antimony hypochlorite, and use of an alternative wavelength may be required when lead or copper is present in the sample. Standard addition methods are desirable when furnace AA is used. QUALITY CONTROL: A method blank should be processed with each set of 10 or fewer samples. Analytical recovery should be determined and if less than 95 percent, results should be corrected accordingly. Duplicate analyses should agree within 5 percent. EPA/TECHNICAL STATUS: The flame AA method is approved by the National Institute for Occupational Safety and Health (NIOSH) and has been validated over the range of 0.25 to 1.1 milligrams of antimony per cubic meter for a 360-liter sample. Another flame AA method is classified as operational by NIOSH over the range of 0.42 to 1.65 milligrams per cubic meter in a 240-liter sample. The furnace AA method has been proposed by NIOSH for use over the range of 0.5 to 1.0 milligrams per cubic meter in a 50-liter sample. Precision and accuracy information is furnished. B-156 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods, Set 1, Method S2; PB-271 712 (NTIS), U.S. DREW: Cincinnati, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, Vol. 4, Method P&CAM, 261; Publication Number 78-175, U.S. DHEW: Cincinnati, 1978. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S2; Publication Number 77-157-B, 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 Number 77-157-A, U.sT DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by the flame AA method is approximately $10-20 (list); by furnace AA, it is approximately $18-50 (list). B-157 ------- ANTIMONY Air Samples Laboratory Method 2 Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Analysis for antimony and the above antimony compounds in air may be per- formed by filtration of air using a high-speed sampler, followed by X-ray fluorescence spectrometric analysis for the antimony present on the filter medium. This method measures total antimony concentration in the air particu- lates, and does not distinguish between different antimony compounds. The method is non-destructive so that further analyses may be performed on samples after this test. The sample-collection time may be up to 8 hours, but analysis time of the collection sample is only approximately 1 minute. INTERFERENCES: Polyvinyl chloride (PVC) filters are unacceptable for sampling, and glass-fiber filters are acceptable 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 concentration levels greater than 60 micrograms of antimony and should be applicable to 0.05 to 5 micrograms per cubic meter. Precision and accuracy 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-158 ------- 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-159 ------- ANTIMONY Air Samples Laboratory Method 3 Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: The above particulate antimony compounds in air samples may be measured electrochemically. A known volume of air is passed through a membrane filter and the filter and particulates are wet-ashed with a mixture of nitric, per- chloric, and sulfuric acids. The resulting Sb(V) is reduced to Sb(III) with a solution of hydrochloric acid and hydrazine dihydrochloride. The reduced sample is analyzed by anionic stripping voltammetry with a composite mercury- graphite electrode. This method does not identify any specific antimony- containing compound, but measures the total antimony content of the sample. INTERFERENCES: Copper may interfere, but its effects can be minimized; bismuth may also interfere. QUALITY CONTROL: Blanks should be processed with the samples, and values obtained should be used in calculation of results. EPA/TECHNICAL STATUS: This method is described as proposed by the National Institute of Occupa- tional Safety and Health (NIOSH) for use over the range of 0.15 to 5 micrograms per cubic meter of air, using a 100-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. 1, Method P&CAM 189; Publication Number 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost information has not been obtained. B-160 ------- ANTIMONY Air Samples Laboratory Method 4 Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Antimony and the above antimony compounds can be measured in air colori- metrically. A known volume of air is passed through a membrane filter, the filter is wetashed with nitric/sulfuric acid, and the antimony present is oxidized to Sb(V) with perchloric acid. The resulting solution is then reacted with Rhodamine B to form a pink-colored complex and the absorbance is measured at 565 nm. The amount of antimony present is determined by reference to a calibration curve. This method does not identify any particular antimony- containing compound, but measures the total antimony content of the sample. INTERFERENCES: Interference by iron can be minimized by addition of phosphoric acid or extraction with isopropyl ether. The analysis will fail if any nitric acid remains in the digest. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. The range of the method for a 20-liter sample is 10 to 50 micrograms per cubic meter. REFERENCES: Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol. Ill, Available Laboratory Analytical Method^, "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. American Public Health Association, Methods of Air Sampling and Analysis, 2nd ed., Method 802; APHA: Washington, 1977. B-161 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $25-35 (list), plus sampling costs. B-162 ------- ANTIMONY Soil/Sediment Samples Laboratory Method Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Analysis for the above antimony compounds in soil/sediment samples can be performed by atomic spectrometric analysis for antimony. A 2-gram sample is digested with nitric acid and hydrogen peroxide and analyzed by atomic absorp- tion (AA) spectrometry. Furnace AA is used for low concentrations, while flame AA is used for higher concentration samples. This method does not identify specific antimony compounds, but measures the total antimony content of the sample. INTERFERENCES: The presence of lead in the sample may cause a spectral interference at the 217-nm resonance line. If this occurs, the 231-nm line should be used. QUALITY CONTROL: The acid concentration in the sample and standards should be matched. 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. Precision and accuracy information is provided. 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 204.1, 204.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. B-163 ------- U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 6010; 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. American Public Health Association, Standard Methods for the Examination of Water and Wastewater, 15th ed., Method 303A; APHA: Washington, 1980. 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 $24 (list), and $38 (list) by furnace AA. B-164 ------- ANTIMONY Water Samples Laboratory Method 1 Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Analysis for antimony ions from the above compounds in water may be performed by spectrometric analysis for antimony. A 100-milliliter sample is digested with nitric acid and hydrogen peroxide and analyzed by inductively coupled plasma (ICP) or by flame or furnace atomic absorption (AA) spectrometry. This method does not identify the antimony-containing compounds in the sample, but measures the total antimony present. 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. 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. Precision and accuracy information is furnished for the flame AA and ICP methods. For flame AA, the detection limit is 0.07 milligrams of antimony per liter, and the sensitivity is 0.5 milligrams per liter (Standard Methods). Instrumental detection limit for ICP is 32 micrograms per liter (EPA-600/4-82-055). 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 204.1, 204.2, EPA-600/4-79-020), U.S. EPA: Cincinnati, 1979. B-165 ------- U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, 2nd end., Methods 3010, 3020, 6010, 7040, 7041; SW-846, U.S. EPA: Washington, 1982. Federal Register, ^4_(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. 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. American Public Health Association, Standard Methods for the Examination of Water and Wastewater, 15th ed., Method 303A; APHA: Washington, 1980. Fassel, V. A.; Peterson, C. A.; Abercrombie, F. N.; Rniseley, 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 furnace AA, $18-50 (list); and by ICP, $10-20 (list). B-166 ------- ANTIMONY Water Samples Laboratory Method 2 Compound CAS Number Antimony 7440-36-0 Antimony Pentachloride 7647-18-9 Antimony Potassium Tartrate 28300-74-5 Antimony Tribromide 7789-61-9 Antimony Trichloride 10025-91-9 Antimony Trifluoride 7783-56-4 Antimony Trioxide 1309-64-4 METHOD SUMMARY: Analysis of water samples for antimony ions from the above compounds can be performed by atomic spectrometry. A sample of 100 milliliters or less is digested with sulfuric and nitric acids and heat, and the inorganic antimony in the resulting solution is reacted with potassium iodide and stannous chloride and then with sodium borohydride to form stibine. The stibine is purged from solution with nitrogen into a hydrogen-flame-atomization atomic absorption spectrometer and the absorbance at 217.6 nanometers is measured. This method does not identify any particular antimony-containing compound, but measures the total antimony content of the sample. INTERFERENCES: Selenium and arsenic do not interfere. 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 15 micrograms antimony per liter. Precision and accuracy information is furnished. REFERENCE: American Society for Testing and Materials, 1983 Annual Book of ASTM Standards, Vol. 11.01, Method D3697-78; ASTM: Philadelphia, 1983. COST INFORMATION: Cost information has not been obtained. B-167 ------- ARSENIC Air Samples Laboratory Method 1 Compound Arsenic Arsenic Acid Arsenic Bisulfide Arsenic Pentoxide Arsenic Trichloride Arsenic Trioxide Arsenic Trisulfide Cacodylic Acid CAS Number 7440-38-2 1327-52-2 7778-39-4 1303-32-8 1303-28-2 7784-34-1 1327-53-3 1303-33-9 75-60-5 Compound Calcium Arsenate Calcium Arsenite Cupric Acetoarsenite Lead Arsenate Potassium Arsenate Potassium Arsenite Sodium Arsenate Sodium Arsenite CAS Number 7778- 52740- 12002- 7784- 7645- 10102- 7784- 10124- 7631- 7784- •44-1 •16-6 •03-8 •40-9 •25-2 •48-4 •41-0 50-2 •89-2 46-5 METHOD SUMMARY: The above particulate arsenic compounds in air samples may be measured by atomic absorption spectrometry (AA). The sample is collected by filtration of a known volume of air and the filter is acid-digested. The resulting solution is analyzed by flame, furnace, or hydride-generation AA. This method is not specific for any given arsenic compound, but measures total arsenic. INTERFERENCES: High concentrations of heavy metals can interfere, so fortified samples should be analyzed to establish adequate recovery. QUALITY CONTROL: Fortified samples and a blank should be processed and these values used in calculation of results. EPA/TECHNICAL STATUS: The furnace AA method is approved by the National Institute for Occupa- tional Safety and Health (NIOSH) and validated over the range of 0.2 to 0.9 milligrams arsenic per cubic meter, using an 85-liter air sample. The hydride- generation AA method is classified as operational by NIOSH over the range of 2 to 60 micrograras per cubic meter, using a 30-liter air sample, and is utilized by Alberta Environment for concentrations above the detection limit of 0.2 nanograms per cubic meter. The flame AA method is classified as operational by NIOSH over the range of 0.4 to 2.1 milligrams per cubic meter, using a 240- liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set N, Method S309; PB-258-433 (NTIS), U.S. DHEW: Cincinnati, 1976. B-168 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S309; Publication No. 77-157C, U.S. DREW: Cincinnati, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, P&CAM 139; 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 139, Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. Alberta Environment, Methods Manual for Chemical Analyses of Atmospheric Pollutants, 2nd ed., Method 21010; Alberta Environmental Centre: Vegreville, Alberta, Canada, 1981. 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: Washington, 1977. COST INFORMATION: Cost per sample for analysis by flame AA is approximately $10-20 (list), plus sampling costs; by furnace or hydride-generation AA, it is approximately $18-50 (list), plus sampling costs. B-169 ------- ARSENIC Air Samples Laboratory Method 2 Compound CAS Number Compound CAS Number Arsenic 7440-38-2 Calcium Arsenate 7778-44-1 Arsenic Acid 1327-52-2 Calcium Arsenite 52740-16-6 7778-39-4 Cupric Acetoarsenate 12002-03-8 Arsenic Bisulfide 1303-32-8 Lead Arsenate 7784-40-9 Arsenic Pentoxide 1303-28-2 7645-25-2 Arsenic Trichloride 7784-34-1 10102-48-4 Arsenic Trioxide 1327-53-3 Potassium Arsenate 7784-41-0 Arsenic Trisulfide 1303-33-9 Potassium Arsenite 10124-50-2 Cacodylic Acid 75-60-5 Sodium Arsenate 7631-89-2 Sodium Arsenite 7784-46-5 METHOD SUMMARY: Analysis for the above arsenic-containing compounds in air may be per- formed by inductively coupled plasma (ICP) spectrometry analysis for arsenic. 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 by inductively coupled argon plasma spectrometry, and monitoring of the emission spectrum. This method does not identify any specific arsenic-containing com- pound, but measures the total arsenic 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 arsenic per cubic meter, using a 500-liter sample. Limited precision and accuracy is furnished. REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Volume 7, P&CAM 351; Publication No. 82-100, U.S. DHHS: Cincinnati, August 1981. B-170 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $10 (list), plus sampling costs. B-171 ------- ARSENIC Air 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 Disulfide 1303-32-8 Lead Arsenate 7784-40-9 Arsenic Pentoxide 1303-28-2 7645-25-2 Arsenic Trichloride 7784-34-1 10102-48-4 Arsenic Trioxide 1327-53-3 Potassium Arsenate 7784-41-0 Arsenic Trisulfide 1303-33-9 Potassium Arsenite 10124-50-2 Cacodylic Acid 75-60-5 Sodium Arsenate 7631-89-2 Calcium Arsenate 7778-44-1 Sodium Arsenite 7784-46-5 METHOD SUMMARY: The above particulate arsenic 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 or dry ashed in a low-temperature asher. The nitric acid is removed from the wet-ashed sample, or the dry-ashed sample is dissolved in sulfuric acid. The resulting As(V) is reduced to As(III) with an acidic solution of potassium iodide and sodium formate. The reduced sample is neutralized. The As(III) in the sample promotes the osmium [Os(VIIl)] catalysis of the oxidation of iodide to iodine by bromate. The rate of iodine production is proportional to the concentration of As(III); it is determined after a 4-minute reaction time by measurement of the absorbance at 580 nanometers on a recording spectrophotometer, using starch as an indicator. This method does not identify any specific arsenic compound. If the determination of total arsenic is desired, the reduction of As(V) to As(III) is necessary prior to the catalytic reaction. If the determination of As(III) only is desired, it can be readily separated from As(V) by solvent extraction. INTERFERENCES: Cu(II), Fe(II), and Fe(III) ions may interfere, but their effects can be' removed by a masking agent. Sulfite ions interfere in the catalytic reaction, but the ashing step should oxidize them to sulfates. As(V) interferes with the determination and must be removed or reduced. QUALITY CONTROL: A filter blank should be processed with samples. Filter standards should also be processed to determine recovery. The value of the blank and the recovery should be used in calculation of results. B-172 ------- EPA/TECHNICAL STATUS: This method is classified as proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.1 to 1 milligram per cubic meter of air in a 25-liter sample. Limited 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 180; Publication No. 77-157-A, U.S. DREW: Cincinnati, 1977- COST INFORMATION: Cost information has not been obtained. B-173 ------- ARSENIC Air Samples Laboratory Method 4 Compound Arsenic Arsenic Acid Arsenic Bisulfide Arsenic Pentoxide Arsenic Trichloride Arsenic Trioxide Arsenic Trisulfide Cacodylic Acid Calcium Arsenate METHOD SUMMARY: 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 The above arsenic compounds in air samples may be measured spectrophoto- metrically. A known volume of air is passed through a filter to collect the arsenic. The sample is ashed, treated with ammonium oxalate, transferred to an arsine generator, and converted to the trivalent form with potassium iodide and stannous chloride. Arsine is generated by the addition of metallic zinc, passed through an I^S scrubber, and then absorbed by a solution of pyridine- silver diethyldithiocarbamate to form a soluble red complex. The absorbance is read on a spectrophotometer at 560 nanometers. This method is not specific for any arsenic-containing compound, but results represent total arsenic in the sample. INTERFERENCES: No interferences are reported. QUALITY CONTROL: A method blank and standards are prepared and analyzed with the samples. EPA/TECHNICAL STATUS: This method is recommended by the National Institute of Occupational Safety and Health (NIOSH) for use over the range of 0.01 to 0.8 milligrams per cubic meter for a 30-liter air sample. Limited precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. Method P&CAM 140; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974. B-174 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 140; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. American Public Health Association, Methods of Air Sampling and Analysis, 2nd ed., Method 803; APHA: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $30 (list), plus sampling costs. B-175 ------- ARSENIC Air Samples Laboratory Method 5 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: The above particulate arsenic compounds in air samples may be measured electrochemically. A known volume of air is passed through a membrane filter, the filter and particulates are wet-ashed with a mixture of nitric, perchloric, and sulfuric acids, and the resulting As(V) is reduced to As(III) with an acidic solution of sodium bisulfite and ferrous perchlorate. An acid solution of hydrazine dihydrochloride is added to prevent air oxidation of Fe(II) ions. The reduced sample is analyzed by anodic stripping voltammetry with a composite gold-graphite electrode. INTERFERENCES: High levels of bismuth and antimony may interfere. Copper and arsenic are not completely resolved at high levels of both metals. QUALITY CONTROL: Blanks should be processed with the samples, and values obtained should be used in calculation of results. EPA/TECHNICAL STATUS: This method is classified as proposed by the National Institute of Occupational Safety and Health (NIOSH) for use over the range of 0.5 to 5 micrograms per cubic meter of air, using a 100-liter sample. Limited 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 188; Publication No. 75-157-A, U.S. DHEW: Cincinnati, 1977. B-176 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. The method should be applicable to 0.01 to 1.0 micrograms of lead per cubic meter, depending on sample size. Precision information is furnished. 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-301 ------- LEAD Air Samples Laboratory Method 3 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: Analysis of air for the above particulate lead compounds can be performed by proton-induced X-ray emission (PIXE) analysis for lead. Analyte is collected on polystyrene thin foil and on the filter then analyzed by PIXE. The method result indicates the total lead and lead compounds present as nanograms lead per cubic meter of air and does not identify specific lead compounds. 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-302 ------- REFERENCE: Johanssen, T. B; Van Grieken, R. E.; Nelson, J. W.; Winchester, J. W. "Elemental Trace Analysis of Small Samples by Proton Induced X-ray Emission" Anal. Chem., _47_, 1975, pp. 855-860. COST INFORMATION: Cost information has not been obtained. ------- LEAD Air Samples Laboratory Method 4 Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Sulfide 1314-87-0 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Analysis for the above lead-containing compounds in air may be performed by inductively coupled plasma atomic spectroscopic (ICP) analysis for lead. 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. The method does not identify any specific lead-containing compound, but measures the total lead 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 lead per cubic meter for a 500-liter sample. Limited precision and accuracy information is furnished. B-304 ------- 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 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-305 ------- LEAD Soil/Sediment Samples Laboratory Method Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Sulfide 1314-87-0 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Analysis of soil/sediment samples for the above lead compounds can be performed by atomic spectrometric analysis for lead. A 2-gram sample is digested with nitric acid and hydrogen peroxide and analyzed by atomic spec- trometry. Furnace atomic absorption spectrometry (AA) is used to measure low concentrations of lead, while inductively coupled plasma (ICP) and flame AA are used for higher concentrations. Analysis for lead in oily samples may be performed by ICP after dilution of the sample with methyl isobutyl ketone (MIBK) or xylene, using standards miscible with these solvents. These methods measure the total particulate lead content of the sample, and do not identify any specific lead-containing compounds. INTERFERENCES: All glassware must be cleaned immediately prior to its use. Lanthanum nitrate is added to suppress sulfate interference in samples and standards. 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. B-306 ------- EPA/TECHNICAL STATUS: These methods are in use in the CERCLA program and are approved for analysis for the Resource Conservation and Recovery Act (RCRA) and for the Clean Water Act. Precision and accuracy information is furnished (APHA). The optimum concentration range for analysis by flame AA is 1 to 20 milligrams per kilogram, by furnace AA 5 to 100 micrograms per kilogram, and the sensitivity by flame AA is 0.5 milligrams per kilogram. 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 239.1, 239.2; EPA-600/4-79-020, U.S. EPA: Washington, March 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, 3040, 3050, 6010, 7420, 7421; 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. 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 furnace AA, approximately $28-50 (list); by ICP, approximately $20 (list). B-307 ------- LEAD Water Samples Laboratory Method 1 Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Sulfide 1314-87-0 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Analysis of water samples for the above lead compounds can be performed by atomic spectrometric analysis for lead. A 100-milliliter sample is digested with nitric acid and hydrogen peroxide and analyzed by atomic spectrometry. Furnace atomic absorption (AA) spectrometry is used for lower levels of lead, while inductively coupled plasma (ICP) spectrometry is used for higher-concen- tration samples. Alternatively, the lead may be chelated with pyrrolidine- dithiocarbamic acid and extracted with chloroform, the chloroform evaporated, and the residue dissolved in acid and analyzed for lead by AA. This method measures the total lead content of the sample, but does not identify specific lead compounds. INTERFERENCES: Lanthanum nitrate may be added to suppress sulfate interferences. High levels of calcium can cause a positive interference in direct AA analysis. 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. At least 10 percent of the samples should be duplicates and/or standards. B-308 ------- EPA/TECHNICAL STATUS: The direct AA and TCP 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. The direct AA method is applicable in the range from 1.0 to 10 milligrams per liter of lead, while the chelation-extraction AA procedure is applicable from 0.1 to 1 milligrams lead 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. U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and Wastes, Methods 239.1, 239.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. 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, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, Methods 3010, 3020, 6010, 7420, 7421; 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 Method^, "Methods for the Determina- tion of Trace Metals Using Inductively Coupled Plasma Atomic Emission Spectro- scopy," pp. IV-99 to IV-124; EPA-600/S4-84-033, 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 D3559(A), D3559(B); 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-309 ------- LEAD Water Samples Laboratory Method 2 Compound CAS Number Lead 7439-92-1 Lead Acetate 301-04-2 Lead Arsenate 7784-40-9 7645-25-2 10102-48-4 Lead Chloride 7758-95-4 Lead Fluoborate 13814-96-5 Lead Fluoride 7783-46-2 Lead Iodide 10101-63-0 Lead Nitrate 10099-74-8 Lead Phosphate 7446-27-7 Lead Stearate 7428-48-0 1072-35-1 56189-09-4 Lead Subacetate 1335-32-6 Lead Sulfate 15739-80-7 7446-14-2 Lead Sulfide 1314-87-0 Lead Thiocyanate 592-87-0 METHOD SUMMARY: Analysis of water samples for the above lead compounds can be performed electrochemically. A sample is digested with nitric acid in a polarographic cell, a buffer and hydroxylamine are added, the sample is deaerated, and the lead is deposited into a hanging mercury drop electrode at -0.80 volts. The lead is then stripped back into solution, using the differential pulse scanning mode, and current flow is measured. INTERFERENCES: Interference from ferric iron is avoided by the addition of hydroxylamine. The presence of a stripping peak within 100 millivolts of the lead peak will interfere. QUALITY CONTROL: No quality control procedures are furnished. EPA/TECHNICAL STATUS: This method is not EPA-approved. The method is applicable up to a concen- tration of 100 micrograms of lead per liter, and the lower limit of detection for lead is 1 microgram per liter. Precision and accuracy information is furnished. B-310 ------- REFERENCE: American Society for Testing and Materials, 1983 Annual ASTM Book of Standards, Vol. 11.01, Method D3559(C); ASTM: Philadelphia, 1983. COST INFORMATION: Cost information has not been obtained. B-311 ------- LEAD AND CADMIUM Air Samples Laboratory Method Compound CAS Number Compound CAS Number Cadmium 7440-43-9 Lead Iodide 10101-63-0 Cadmium Acetate 543-90-8 Lead Nitrate 10099-74-8 Cadmium Bromide 7789-42-6 Lead Phosphate 7446-27-7 Cadmium Chloride 10108-64-2 Lead Stearate 7428-48-0 Lead 7439-92-1 1072-35-1 Lead Acetate 301-04-2 56189-09-4 Lead Arsenate 7784-40-9 Lead Subacetate 1335-32-6 7645-25-2 Lead Sulfate 15739-80-7 10102-48-4 7446-14-2 Lead Chloride 7758-95-4 Lead Sulfide 1314-87-0 Lead Fluoborate 13814-96-5 Lead Thiocyanate 592-87-0 Lead Fluoride 7783-46-2 METHOD SUMMARY: The above particulate lead and cadmium compounds in air samples may be measured electrochemically. The sample is collected from a known volume of air on a membrane filter. The filter and particulates are wet-ashed with a mixture of nitric, perchloric, and sulfuric acids. The residue is dissolved in an acetate buffer solution which is analyzed by anodic stripping voltammetry with a composite mercury-graphite electrode. This method does not identify any specific lead or cadmium compounds present, but measures the total lead content and the total cadmium content of the sample. INTERFERENCES: Thallium present in the sample at a concentration similar to that of lead or cadmium may interfere. QUALITY CONTROL: Blanks should be processed with the samples, and values obtained should be used in the calculation of the results. EPA/TECHNICAL STATUS: This method is classified as proposed by the National Institute of Occupational Safety and Health (NIOSH) for use over the range of 0.16 to 10 micrograms of lead or 0.08 to 10 micrograms of cadmium per cubic meter of air using a 100-liter sample. Precision and accuracy information is furnished. B-312 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 191; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. American Society for Testing and Materials, 1983 ASTM Annual Book of Standards, Vol. 11.03, D3413-75T; ASTM: Philadelphia, 1983. U.S. Department of Energy Environmental Measurements Laboratory, EML Procedures Manual, H. L. Volchok and G. de Planque, Eds., Method E-00-08, "Trace Metals by Anodic Stripping;" HASL-300, Environmental Measurements Laboratory, U.S. DOE: New York, 1983. COST INFORMATION: Cost information has not been obtained. B-313 ------- MERCURY Air Samples Laboratory Method Compound CAS Number Mercuric Cyanide 592-04-1 Mercuric Nitrate 10045-94-0 Mercuric Sulfate 7783-35-9 Mercuric Thiocyanate 592-85-8 Mercurous Nitrate 10415-75-5 7782-86-7 Mercury 7439-97-6 Mercury Fulminate 628-86-4 Phenylmercuric Acetate 62-38-4 METHOD SUMMARY: The above particulate mercury, organic mercury vapors, and metallic mercury vapor in air may be measured by flameless atomic absorption spectro- scopy. The particulate mercury is collected on a membrane prefilter ahead of a 2-stage solid-phase sampling tube. The organic mercury vapor is collected in the first section of the tube while the metallic mercury vapor is amalgamated in the second section. The membrane filter undergoes acid digestion and the analyte is transferred onto a tube containing a silver-coated substrate. The mercury is thermally desorbed from the silver into a flameless atomic absorp- tion spectrophotometer (AA). The 2-section tube is separated and each section is analyzed by thermal desorption through the absorption cell of the flameless AA. This method measures mercury and does not differentiate between mercury- containing compounds. INTERFERENCES: High humidity may interfere if water has condensed in the sampling tube. QUALITY CONTROL: A method blank and standards are 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 0.001 to 2.5 micrograms. Precision and accuracy informtion is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, Method P&CAM 175; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974. B-314 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 175; 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, "Methods for the Determina- tion of Mercury," pp. IV-51 to IV-69; 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-315 ------- MERCURY Soil/Sediment Samples Laboratory Method Compound CAS Number Mercuric Cyanide 592-04-1 Mercuric Nitrate 10045-94-0 Mercuric Sulfate 7783-35-9 Mercuric Thiocyanate 592-85-8 Mercurous Nitrate 10415-75-5 7782-86-7 Mercury 7439-97-6 Mercury Fulminate 628-86-4 Phenylmercuric Acetate 62-38-4 METHOD SUMMARY: Analysis of soil/sediment samples for the above mercury compounds can be performed by cold-vapor atomic absorption spectrometric analysis for mercury. Triplicate 0.2-gram samples are digested with acidic potassium permanganate, reduced, and purged into the absorption cell of a flameless atomic absorption spectrometer. This method does not identify the specific mercury-containing compounds present, but measures the total mercury content of the sample. INTERFERENCES: Care must be taken to avoid extraneous contamination of the sample. High concentrations of sulfides and copper may interfere. Samples containing volatile organic materials or high levels of chloride may require background correction. QUALITY CONTROL: Fresh standards should be prepared daily- All samples should be analyzed in triplicate. EPA/TECHNICAL STATUS: This method is in use in the CERCLA program and is approved for 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. U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and Wastes, Method 245.5; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. B-316 ------- U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, 2nd ed., Method 7471; 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 Mercury," pp. IV-51 to IV-69; EPA-600/S4-84-038, U.S. Environmental Protection Agency: Las Vegas, 1984. COST INFORMATION: Cost per sample for analysis by cold-vapor AA is approximately $28-60 (list), $26 (1983 bid). B-317 ------- MERCURY Water Samples Laboratory Method Compound CAS Number Mercuric Cyanide 592-04-1 Mercuric Nitrate 10045-94-0 Mercuric Sulfate 7783-35-9 Mercuric Thiocyanate 592-85-8 Mercurous Nitrate 10415-75-5 7782-86-7 Mercury 7439-97-6 Mercury Fulminate 628-86-4 Phenylmercuric Acetate 62-38-4 METHOD SUMMARY: Analysis for the above mercury compounds in water samples may be performed by atomic absorption spectrometric analysis for mercury. A 100-milliliter sample is analyzed by manual or automated flameless atomic absorption spectrom- etry (AA)- The sample is digested with potassium permanganate and potassium persulfate, reduced with tin(II) ions and purged into an absorption cell. The sample should be preserved by acidification with nitric acid at the time of collection. This method does not identify the specific mercury-containing compounds present, but measures the total mercury content of the sample. INTERFERENCES: A high chloride concentration and/or certain volatile organics in the sample may require background correction. Copper may interfere. QUALITY CONTROL: Fresh standards should be prepared daily- EPA/TECHNICAL STATUS: These methods are in use in the CERCLA program and are approved for use in the Resource Conservation and Recovery Act (RCRA) and Clean Water Act. This method is applicable to the determination of total mercury in water in the range from 2 to 10 micrograms mercury per liter. 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-318 ------- U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and Wastes. Methods 245.1, 245.2; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. Plumb, R. H. Characterization of Hazardous Waste Sites: A Methods Manual, Vol. Ill, Available Laboratory Analytical Methods, "Methods for the Determina- tion of Mercury," pp. IV-51 to IV-69; 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., Method 304; APHA: Washington, 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $18-50 (list), $18 (1983 bid). B-319 ------- NICKEL Air Samples Laboratory Method 1 Compound CAS Number Nickel 7440-02-0 Nickel Ammonium Sulfate 15699-18-0 Nickel Chloride 7718-54-9 37211-05-5 Nickel Cyanide 557-19-7 Nickel Hydroxide 12054-48-7 Nickel Nitrate 14216-75-2 Nickel Sulfate 7786-81-4 METHOD SUMMARY: Analysis for the above nickel compounds in air may be performed by filtra- tion of air and analysis of the filter medium for nickel 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 only approximately 1 minute. The method measures total nickel present in the sample and does not differentiate between chemical compounds or nickel 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 microgram of nickel per cubic meter, depending on sample size. The method is sensitive to amounts of nickel above 40 micrograms, with a precision of 60 percent at that level. 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. B-320 ------- 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 approximately $30 (list), $20 (bid), plus sampling costs. B-321 ------- NICKEL Air Samples Laboratory Method 2 Compound Nickel Nickel Ammonium Sulfate Nickel Chloride Nickel Cyanide Nickel Hydroxide Nickel Nitrate Nickel Sulfate CAS Number 7440-02-0 15699-18-0 7718-54-9 37211-05-5 557-19-7 12054-48-7 14216-75-2 7786-81-4 METHOD SUMMARY: Analysis for nickel and the above soluble nickel compounds in air can be performed by cellulose-membrane or glass-fiber filtration of a known volume of air, followed by acid digestion of the filter and the deposited particles, and analysis of the resulting solution by flame atomic absorption spectrometry (AA). This method measures the total nickel content of the sample and does not identify specific nickel compounds. This method is applicable only to nickel and compounds soluble in perchloric/nitric acid. INTERFERENCES: No specific interferences are reported. 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: Method S206 is approved by the National Institute for Occupational Safety and Health (NIOSH), and has been validated over the range of 0.45 to 2.1 milli- grams per cubic meter for an 85-liter sample size. Measurement of lower concen- trations can be made by use of smaller solution volumes, longer sampling times, or scale expansion. An operational method from NIOSH, P&CAM 173, is for use over the range of 21 to 210 micrograms per cubic meter in a 240-liter sample. Alberta Environment has determined the limit of detection to be 0.001 micro- grams per cubic meter. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set N, Method S206; PB-258 433 (NTIS), U.S. DHEW: Cincinnati, September 1976. B-322 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 3, Method S206; 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.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. 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 X-ray Fluorescence;" HASL-300, Environmental Measurements Laboratory, U.S. DOE: New York, 1983. Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric Pollutants, Methods 23535, 23544; Alberta Environmental Centre: Vegreville, Alberta, Canada, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $20 (list), plus sampling costs. B-323 ------- NICKEL Air Samples Laboratory Method 3 Compound Nickel Nickel Ammonium Sulfate Nickel Chloride Nickel Cyanide Nickel Hydroxide Nickel Nitrate Nickel Sulfate CAS Number 7440-02-0 15699-18-0 7718-54-9 37211-05-5 557-19-7 12054-48-7 14216-75-2 7786-81-4 METHOD SUMMARY: The above inorganic nickel, nickel metal, and nickel compounds can be measured in air by atomic absorption spectrophotometry. A known volume of air is drawn through a hydrofluoric acid/nitric acid mixture, the solution is taken to dryness, and diluted with a known volume of hydrochloric acid. The result- ing solution is analyzed by graphite furnace atomic absorption spectrometry (AA). This method is not specific for any nickel compound, but measures the total nickel content of the sample. INTERFERENCES: Iron is a positive interference when present in high concentrations. Silica, antimony, and beryllium can interfere. Background absorption may be overcome by the use of a deuterium-arc background corrector. QUALITY CONTROL: Blanks and standards are analyzed with the samples. EPA/TECHNICAL STATUS: This method has been accepted by the National Institute for Occupational Safety and Health (NIOSH) and evaluated over the range of 0.6 to 30.7 micrograms per cubic meter, using a 400-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 298; Publication No. 82-100, U.S. DHHS: Cincinnati, August 1981. B-324 ------- 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 X-ray Fluorescence;" HASL-300, Environmental Measurements Laboratory, U.S. DOE: New York, 1983. American Public Health Association, Methods of Air Sampling and Analysis, 2nd ed., Method 320; APHA: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $18-50 (1983 list), plus sampling costs. B-325 ------- NICKEL Air Samples Laboratory Method 4 Compound Nickel Nickel Ammonium Sulfate Nickel Chloride Nickel Cyanide Nickel Hydroxide Nickel Nitrate Nickel Sulfate CAS Number 7440-02-0 15699-18-0 7718-54-9 37211-05-5 557-19-7 12054-48-7 14216-75-2 7786-81-4 METHOD SUMMARY: Analysis for the above nickel compounds in air may be performed by inductively coupled plasma atomic spectroscopic (ICP) analysis for nickel. 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 inductively coupled argon plasma atomic spectroscopy- The method does not identify any specific nickel-containing compound, but measures the total nickel 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 nickel per cubic meter for a 500-liter sample. Limited precision and accuracy infor- mation 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-326 ------- 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-327 ------- NICKEL Soil/Sediment Samples Laboratory Method Compound CAS Number Nickel 7440-02-0 Nickel Ammonium Sulfate 15699-18-0 Nickel Chloride 7718-54-9 37211-05-5 Nickel Cyanide 557-19-7 Nickel Hydroxide 12054-48-7 Nickel Nitrate 14216-75-2 Nickel Sulfate 7786-81-4 Nickel Tetracarbonyl 13463-39-3 METHOD SUMMARY: Analysis of soil/sediment samples for the above nickel compounds can be performed by atomic spectrometric analysis for nickel. A 2-gram sample is digested with nitric acid and hydrogen peroxide and analyzed by flame atomic absorption (AA) or inductively coupled plasma (ICP) spectrometry. Lower levels of nickel should be analyzed by ICP- Analysis for nickel in oily samples may be performed by ICP after dilution of the sample with methyl isobutyl ketone (MIBK) or xylene, using standards miscible with these solvents. These methods do not identify any specific nickel-containing compounds, but measure the total nickel 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 use in 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 249.1, EPA-600/4-79-020, U.S. EPA: Washington, 1979. B-328 ------- Federal Register. 44(233), December 3, 1979, pp. 69559-69564. U.S. Environmental Proection Agency, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, 2nd ed., Methods 3010, 3020, 3040, 3050, 6010, 7520, 7521; 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 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. 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. 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. B-329 ------- NICKEL Water Samples Laboratory Method Compound CAS Number Nickel 7440-02-0 Nickel Ammonium Sulfate 15699-18-0 Nickel Chloride 7718-54-9 37211-05-5 Nickel Cyanide 557-19-7 Nickel Hydroxide 12054-48-7 Nickel Nitrate 14216-75-2 Nickel Sulfate 7786-81-4 Nickel Tetracarbonyl 13463-39-3 METHOD SUMMARY: Analysis of water samples for the above nickel compounds can be performed by atomic spectrometric analysis for nickel. A 100-milliliter sample is digested with nitric acid and hydrogen peroxide and analyzed by flame-atomiza- tion atomic absorption (AA) or inductively coupled plasma atomic spectrometry (ICP). Alternatively, the sample can be extracted at pH 2 to 4 with ammonium pyrrolidinedithiocarbamate and methyl isobutyl ketone and the extract analyzed by flame AA spectrometry. Lower levels of nickel should be analyzed by ICP or extraction/AA spectrometry. The methods measure the total nickel content of the sample and do not identify specific nickel 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- 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 Clean Water Act analyses. The detection limit for direct flame AA spectrometry is 0.02 milligrams per liter, the sensitivity 0.15 milligrams per liter, and the optimum concentration range 0.3 to 10 milligrams per liter (APHA). The chelation-extraction AA procedure is applicable in the range from 0.01 to 1 milligram nickel per liter (ASTM). The estimated instrumental detection limit for analysis by ICP is 15 micrograms/liter. Precision and accuracy information is furnished. B-330 ------- 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 249.1; 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. U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, 2nd ed. , Methods 3010, 3020, 3040, 3050, 6010, 7520, 7521; 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 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. 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/S8-84-038, 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 D1886(C), D1866(D); 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. COST INFORMATION: Cost per sample for analysis by flame AA is approximately $10-20 (list): by ICP; it is approximately $10 (list). B-331 ------- NITRATES Air Samples Laboratory Method 1 Compound Beryllium Nitrate Cupric Nitrate Ferric Nitrate Lead Nitrate Mercuric Nitrate Mercurous Nitrate METHOD SUMMARY: CAS Number 7787-55-5 13597-99-4 3251-23-8 10421-48-4 10099-74-8 10045-94-0 10415-75-5 7782-86-7 Compound Nickel Nitrate Silver Nitrate Thallium(I) Nitrate Uranyl Nitrate Zinc Nitrate Zirconium Nitrate CAS Number 14216-75-2 7761-88-8 10102-45-1 10102-06-4 36478-76-9 7779-88-6 13746-89-9 Analysis for the above particulate nitrate compounds in air can be per- formed by high-volume filtration followed by dissolution of the analyte in water and colorimetric analysis for nitrate ions. Following high-volume sampling, the analyte is eluted from the filter paper by water washes, the resulting solution is treated with chromotropic acid, and the absorbance of the resulting yellow solution is compared to that of standards. This method does not identify any specific nitrate-containing compound, but measures the total nitrate concentration in the sample. INTERFERENCES: Interferences due to nitrites, oxidizing agents, chloride, and iron(III) are not of importance in this method. 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: "Spectrophotometric Determination of Nitrate in Air," In Environmental Pollutants - Selected Analytical Methods, (SCOPE 6); W. Gallay; H. Egan, J. L. Monkman; R. Truhaut, P- W. West, G. Widmark, Eds.; Ann Arbor Science: Ann Arbor, Michigan, 1975, p. 236. COST INFORMATION: Cost per sample for analysis by this method is approximately $30-40 (list), plus sampling costs. B-332 ------- NITRATES Air Samples Laboratory Method 2 Compound Beryllium Nitrate Cupric Nitrate Ferric Nitrate Lead Nitrate Mercuric Nitrate Mercurous Nitrate METHOD SUMMARY: CAS Number 7787-55-5 13597-99-4 3251-23-8 10421-48-4 10099-74-8 10045-94-0 10415-75-5 7782-86-7 Compound Nickel Nitrate Nitric Acid Silver Nitrate Thallium(I) Nitrate Uranyl Nitrate Zinc Nitrate Zirconium Nitrate CAS Number 14216-75-2 7697-37-2 7761-88-8 10102-45-1 10102-06-4 36478-76-9 7779-88-6 13746-89-9 The above particulate nitrate compounds in air can be measured using an ion-specific electrode. The particulates are collected with a high-volume sampler, extracted with hot water, and the nitrate content of the resulting solution is determined by a nitrate-specific electrode and an expanded-scale pH/mv meter- This method does not identify the specific nitrate-containing compounds present, but measures the total nitrate content of the sample. INTERFERENCES: A buffer is added to prevent interferences from anions such as carbonate, bicarbonate, and nitrite. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. The detection limit is 0.01 micrograms nitrate per cubic meter of air. No precision or accuracy information is furnished. REFERENCE: Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric Pollutants, Method 24040; Alberta Environmental Centre: Vegreville, Alberta, Canada. COST INFORMATION: Cost per sample for analysis by this method is approximately $20-29 (list), plus sampling costs. B-333 ------- NITRATES Soil/Sediment Samples Laboratory Method Compound Beryllium Nitrate Cupric Nitrate Ferric Nitrate Lead Nitrate Mercuric Nitrate Mercurous Nitrate CAS Number 7787-55-5 13597-99-4 3251-23-8 10421-48-4 10099-74-8 10045-94-0 10415-75-5 7782-86-7 Compound Nickel Nitrate Nitric Acid Silver Nitrate Thallium(I) Nitrate Uranyl Nitrate Zinc Nitrate Zirconium Nitrate CAS Number 14216-75-2 7697-37-2 7761-88-8 10102-45-1 10102-06-4 36478-76-9 7779-88-6 13746-89-9 METHOD SUMMARY: Analysis of soil/sediment samples for the above nitrates can be performed by spectrophotometry. A representative portion of a dried and ground sample is extracted with neutral aqueous potassium chloride. The nitrates in the extract are reduced to nitrites by passage through a copperized cadmium column. The resulting solution is then reacted with acidic sulfanilamide to form a diazo compound that is coupled with N-1-naphthylethylenediamine dihydrochloride. The intensity of the resulting red color is measured spectrophotometrically at 550 nanometers. Subtraction of contributions from nitrite ions can be accomplished by analysis of an unreduced sample. This method does not identify any specific nitrate salt, but measures the total extractable nitrate content of the sample. INTERFERENCES: Color and turbidity may interfere. QUALITY CONTROL: The reduction column must be tested and show sufficient efficiency. Fortified samples should be processed with all samples. EPA/TECHNICAL STATUS: This method is not EPA-approved. The method is useful over the range of 40 to 2400 milligrams nitrate per kilogram. Precision and accuracy information is furnished. REFERENCE: Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water and Wastes, "Nitrogen, Nitrate and Nitrite;" Publication No. AECM1-81, Alberta Environmental Centre: Vegreville, Alberta, Canada, 1981. B-334 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $65 (list) B-335 ------- NITRATES Water Samples Laboratory Method Compound Beryllium Nitrate Cupric Nitrate Ferric Nitrate Lead Nitrate Mercuric Nitrate Mercurous Nitrate CAS Number 7787-55-5 13597-99-4 3251-23-8 10421-48-4 10099-74-8 10045-94-0 10415-75-5 7782-86-7 Compound Nickel Nitrate Silver Nitrate Thallium(I) Nitrate Uranyl Nitrate Zinc Nitrate Zirconium Nitrate CAS Number 14216-75-2 7761-88-8 10102-45-1 10102-06-4 36478-76-9 7779-88-6 13746-89-9 METHOD SUMMARY: Analysis for the above nitrate-containing compounds in water samples can be performed by colorimetric analysis for nitrate ions. Samples and standards are acidified and treated with a brucine-sulfanilic acid color reagent at 100°C for 25 minutes. The absorbance of the resulting solution at 410 run is measured. This method does not identify any specific nitrate-containing compounds, but measures the total nitrate concentration in the sample. INTERFERENCES: Color from dissolved organic matter must be compensated for by processing samples without the color reagent. Strong oxidizing and reducing agents inter- fere. Residual chlorine may be removed by addition of sodium arsenite. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is approved for the EPA National Pollutant Discharge Elimina- tion System (NPDES). Precision and accuracy information is furnished. The method is applicable to concentrations from 1 to 50 milligrams of nitrate ion per liter. REFERENCES: U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water and Wastes, Method 352.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979. American Society for Testing and Materials, 1983 Annual Book of ASTM Standards, Vol. 11.01, Method D992-71; ASTM: Philadelphia, 1983. B-336 ------- Alberta Environmental Centre, Methods Manual for the Chemical Analysis of Water and Wastes, "Nitrogen;" Publication No. AECML-81, Alberta Environmental Centre: Vegreville, Alberta, Canada, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $20-35 (list). B-337 ------- Compound Aluminum Sulfate Beryllium Nitrate Chromic Sulfate Cupric Nitrate Cupric Sulfate Cupric Sulfate, Ammoniated Ferric Nitrate Ferric Sulfate Ferrous Ammonium Sulfate Ferrous Sulfate Lead Nitrate Lead Sulfate NITRATES AND SULFATES Air Samples Laboratory Method CAS Number 10043-01-3 13597-99-4 7787-55-5 10101-53-8 3251-23-8 7758-98-7 10380-29-7 10421-48-4 10028-22-5 10045-89-3 7720-78-7 7782-63-0 10099-74-8 15739-80-7 7446-14-2 Compound CAS Number Mercuric Nitrate 10045-94-0 Mercuric Sulfate 7783-35-9 Mercurous Nitrate 10415-75-5 7782-86-7 Nickel Ammonium Sulfate 15699-18-0 Nickel Nitrate 14216-75-2 Nickel Sulfate 7786-81-4 Silver Nitrate 7761-88-8 Thallium(I) Nitrate 10102-45-1 Thallium(I) Sulfate 7446-18-6 Uranyl Nitrate 10102-06-4 36478-76-9 Vanadyl Sulfate 27774-13-6 Zinc Nitrate 7779-88-6 Zinc Sulfate 7733-02-0 Zirconium Nitrate 13746-89-9 Zirconium Sulfate 14644-61-2 METHOD SUMMARY: Analysis for the above nitrate salts in air samples can be performed colorimetrically. High-volume membrane filtration is followed by perchloric acid-extraction of the ions from the sampling medium and automated analysis of the resulting solution by an automated analysis system (Technicon AutoAnalyzer II®, or equivalent), which utilizes the reduction of nitrate to nitrite, diazotization and azo dye formation, and colorimetric analysis. Sulfate ions are measured by colorimetric analysis of the free ligand displaced from a methylthymol blue-barium complex by sulfate ion. Alternatively, the solution from the perchloric acid extraction can be analyzed by ion chromatography- This method requires approximately 12 minutes per sample and has been demon- strated to be comparable to the usual automated method for standard solutions, but has not been evaluated in other applications. These methods measure the total nitrate and/or sulfate concentration of the sample and do not identify specific nitrate or sulfate compounds. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: No quality control procedures are given. B-338 ------- EPA/TECHNICAL STATUS: The colorimetric method can detect levels of sulfate above 1 milligram per liter and of nitrate above 10 milligrams per liter in the resulting solution. The automated method for analysis of the solution is EPA-approved for Clean Water Act analyses. Limited precision and accuracy information is furnished. REFERENCES; Fung, K. K.; Heisler, S. L.; Price, A.; Nuesca, B. V.; Mueller, P- K. "Compar- ison of Ion Chromatography and Automated Wet Chemical Methods for Analysis of Sulfate and Nitrate in Ambient Particulate Filter Samples." In Ion Chromato- graphic Analysis of Environmental Pollutants, Vol. 2; J. D. Mulik; E. G. Sawicki, Eds.; Ann Arbor Science: Ann Arbor, 1979. pp. 203-209. U.S. Environmental Protection Agency, Improvement and Evaluation of Methods for Sulfate Analysis, Appendix E, "Tentative Method for the Determination of Sulfates in the Atmosphere"; EPA-600/4-79-028, U.S. EPA: Research Triangle Park, 1979. COST INFORMATION; Cost per sample for automated colorimetric analysis is approximately $60, plus sampling costs; by ion chromatography, it is approximately $95-105, plus sampling costs . B-339 ------- NITRATES AND SULFATES Soil/Sediment Samples Laboratory Method Compound CAS Number Compound CAS Number Aluminum Sulfate 10043-01-3 Mercuric Nitrate 10045-94-0 Beryllium Nitrate 13597-99-4 Mercuric Sulfate 7783-35-9 7787-55-5 Mercurous Nitrate 10415-75-5 Chromic Sulfate 10101-53-8 7782-86-7 Cupric Nitrate 3251-23-8 Nickel Ammonium Sulfate 15699-18-0 Cupric Sulfate 7758-98-7 Nickel Nitrate 14216-75-2 Cupric Sulfate, 10380-29-7 Nickel Sulfate 7786-81-4 Ammoniated Silver Nitrate 7761-88-8 Ferric Nitrate 10421-48-4 Thallium(I) Nitrate 10102-45-1 Ferric Sulfate 10028-22-5 Thallium(I) Sulfate 7446-18-6 Ferrous Ammonium 10045-89-3 Uranyl Nitrate 10102-06-4 Sulfate 36478-76-9 Ferrous Sulfate 7720-78-7 Vanadyl Sulfate 27774-13-6 7782-63-0 Zinc Nitrate 7779-88-6 Lead Nitrate 10099-74-8 Zinc Sulfate 7733-02-0 Lead Sulfate 15739-80-7 Zirconium Nitrate 13746-89-9 7446-14-2 Zirconium Sulfate 14644-61-2 METHOD SUMMARY; Simultaneous analysis for the above sulfate and nitrate compounds in soil/sediment samples can be performed by shake-extraction of 10 grams of soil with an aqueous solution, followed by analysis for sulfate ion and nitrate ion by ion chromatography- This method does not identify the specific nitrate or sulfate-containing compounds present, but measures the total nitrate or sulfate content of the sample. INTERFERENCES: No interference in determination of nitrate ion occurs from the presence of chloride ion. Large fluctuations in instrument temperature should be avoided when performing this analysis. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved and has undergone single-laboratory evalua- tion. Precision and accuracy information is furnished. B-340 ------- REFERENCE: Tabatabai, M. A.; Dick, W. A. "Ion Chromatographic Analysis of Sulfate and Nitrate in Soil," jn Ion Chromatographic Analysis of Environmental Pollutants, Vol. 2; J. D. Mulik, E. G. Sawicki, Eds.; Ann Arbor Science: Ann Arbor, 1979, pp. 361-370. COST INFORMATION: Cost per sample for analysis by this method is approximately $95 (list). B-341 ------- NITROGEN DIOXIDE AND NITRIC OXIDE Air Samples Laboratory Method 1 Compound CAS Number Nitric Oxide 10102-43-9 Nitrogen Dioxide 10102-44-0 METHOD SUMMARY: Nitric oxide and nitrogen dioxide in air samples may be determined colori- metrically. The analytes are collected from a known volume of air in a three- section sorbent tube. The nitrogen dioxide is absorbed in the first section which contains a molecular sieve impregnated with triethanolamine. The nitric oxide is converted to nitrogen dioxide by an oxidizer in the second section, and this nitrogen dioxide is absorbed in the third section by another bed of triethanolamine-impregnated molecular sieve. The first and third sections are desorbed with solutions of triethanolamine in water, and the nitrite in these solutions is determined spectrophotometrically at 540 nm after the Griess- Saltzman reaction. The nitrite found in the first section is reported as nitrogen dioxide and that from the third section as nitric oxide. INTERFERENCES: Inorganic nitrites cause positive interference. QUALITY CONTROL: Desorption efficiency must be determined over the range of interest, and a method blank should be processed with each set of samples. The desorption efficiency and the results of the method-blank analysis should be used in the calculation of the results. EPA/TECNICAL STATUS: This method is classifed as operational by the National Institute for Occupational Safety and Health (NIOSH), for use over the range of 1 to 37 milligrams of nitric oxide or 1.5 to 56 milligrams of nitrogen dioxide per cubic meter in a one-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 231; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $30-40 (list) for each analyte, plus sampling costs. B-342 ------- |