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 ------- 2-ACETYLAMINOFLUORENE (CAS Number 53-96-3) 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 "Hazardous Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Hazardous Compounds," Appendix B. A-307 ------- ACETYL BROMIDE (CAS Number 506-96-7) ROj 2270 kg SAFETY INFORMATION: Reacts violently with water. ""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 Reacts with water. Water Samples Field Method Reacts with water. See "Halides, Cyanides, and Other Compounds," Appendix B, Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Reacts with water. Water Samples Laboratory Method Reacts with water. See "Acid Anions," Appendix B. A-308 ------- ACETYL CHLORIDE (CAS Number 75-36-5) R£: 2270 kg SAFETY INFORMATION: Flash point 40°F . Reacts violently with water. 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 Reacts with water. Water Samples Field Method Reacts with water. See "Halides, Cyanides, and Other Compounds," Appendix B, Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Reacts with water. Water Samples Laboratory Method Reacts with water, See "Acid Anions," Appendix B, A-309 ------- l-ACETYL-2-THIOUREA (CAS Number 591-08-2) 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 See "Thioureas and Other Compounds," Appendix B, Water Samples Laboratory Method A-310 ------- ACROLEIN (CAS Number 107-02-8) RQ: 0.454 kg SAFETY INFORMATION; Exhibits toxicity (inhalation). Exhibits chronic toxicity. Flashpoint -15°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 acrolein 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 acrolein gas detector tube (Bendix/Gastec® 93, or equivalent). A positive result is indicated by a color change in the tube from yellow to red, as acrolein reacts with hydroxylamine phosphate, releasing phosphorus acid that discolors the indicator. INTERFERENCES: Acetaldehyde, acetone, and methyl ethyl ketone will also cause positive results. Sulfur dioxide will cause the acrolein determination to be high. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 15 to 100 milligrams per cubic meter. REFERENCE: Bendix Corp., Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix Corp.: Largo, Florida, p. 66. COST INFORMATION; The cost per sample for analysis by this method is approximately $13-20 (test). See also: "Aldehydes," Appendix B. See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method A-311 ------- Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Acrolein in air samples may be measured spectrophotometrically. A known volume of air is drawn through two impingers in series containing 4-hexylresor- cinol in an ethyl alcohol-trichloroacetic acid solvent medium and mercuric chloride. The acrolein reacts with the reagents to form a blue-colored product that is measured at 605 nm. A variation of this method is to place a 1-percent sodium bisulfite solution in the impingers, and treat the sample with the rea- gent solutions after collection. INTERFERENCES: Dienes interfere slightly. The colored complex begins to fade 2 hours after completion of sampling. QUALITY CONTROL: A method blank should be prepared and its value used in calculating results. EPA/TECHNICAL STATUS: This method is classified as tentative by the National Institute of Occupational Safety and Health (NIOSH). A concentration of 23 micrograms per cubic meter can be determined, using a 50-liter air sample. Precision and accuracy information is not furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, Method P&CAM 118; 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 211; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $20-25 (list), plus sampling costs. Air Samples Laboratory Method 2 A-312 ------- METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of acrolein in air samples. The absorbance at 10430 nm (959 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 23 milligrams per cubic meter. 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. Air Samples Laboratory Method 3 METHOD SUMMARY: Analysis for acrolein in air can be performed by colorimetric analysis. Acrolein-contaminated air is scrubbed through 5 milliliters of water, 0.5 milliliters of Schiff's reagent is added, and the sample is compared colori- metrically to a set of standard acrolein or formaldehyde solutions. The method is sensitive to levels above 0.5 micrograms of acrolein or formaldehyde per sample volume. A-313 ------- INTERFERENCES: No interferences have been reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: No precision or accuracy information is supplied. REFERENCES: Senderikhina, D. P. Gig. Sanit., 12_ (3), 1947, pp. 17-19. Chem. Abstr., 1949, 43:1289h. COST INFORMATION: The cost per sample for analysis by this method is approximately $18-20 (list). See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," 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 "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-314 ------- ACRYLAMIDE (CAS Number 79-06-1) ROj 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 "Non-Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. A-315 ------- ACRYLIC ACID (CAS Number 79-10-7) Rpj 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 METHOD SUMMARY: Acrylic acid in air samples can be measured by gas chromatography with flame ionization detection (GC/FID). The analyte is collected on silica gel treated with p-methoxyphenol, desorbed with acetone, and determined by GC/FID. INTERFERENCES: No interferences are reported. Propionic acid, acetic acid, ethyl acrylate, and butyl acrylate do not interfere. The treatment of the silica gel prevents polymerization of the acrylic acid. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. The limit of detection is approximately 1.5 milligrams of acrylic acid per cubic meter of air. A-316 ------- REFERENCE: Vincent, W. J.; Guient, V., Jr. "Acrylic Acid - The Development of an Air Sampling and Analytical Methodology for Determining Occupational Exposure," Am. Ind. Hyg. Assoc. J., 43, 1982, pp. 499-504. 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 "Acid Anions," Appendix B. See "Carboxylic Acids," Appendix B. A-317 ------- ACRYLONITRILE (CAS Number 107-13-1) RQ: 45.4 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. Flash point 32°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 acrylonitrile 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 an acrylonitrile gas detector tube (Draeger® 67 28591, or equivalent). A positive result is indicated by a color change in the tube from greenish-yellow to red, as acrylonitrile reacts with chromate ion, mercury(II)- chloride, and methyl red. INTERFERENCES: No interferences are reported. SENSITIVITY; This method is sensitive to concentration levels of approximately 2 to 40 milligrams per cubic meter. QUALITY CONTROL: No quality control procedures are given. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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: National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is approprimately $13-18 (list). A-318 ------- See also: "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 to analyze air samples for acrylonitrile. The analysis is performed by passage of a known volume of air through a charcoal or Carbosieve B-containing sampling device, followed by desorption of the analyte with methanol 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 each 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: The method using charcoal as a sorbent is approved by the National Insti- tute for Occupational Safety and Health (NIOSH), and validated over the range of 17 to 70 milligrams per liter using a 20-liter sample. The Carbosieve B sorbent method is classified, as proposed by NIOSH, for use over the range of 40 to 1100 milligrams per cubic meter with a 20-liter sample of air. The method is capable of measurement of much lower levels if the desorption effi- ciency is adequate. 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 202, Publication No. 77-157-A, U.S. DREW: Cincinnati, 1977. A-319 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S156; Publication No. 77-157-C, U.S. DREW: Cincinnati, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Anaytical Methods for Set K, Method S156; PB-254 227 (NTIS), U.S. DHEW: Washington, April 1976. 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 acrylonitrile in air samples. The absorbance at 10490 nm (953 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 23 milligrams per cubic meter. 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. A-320 ------- See also; "Fumigants," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," 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 "Nitriles," Appendix B. See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-321 ------- RQ: 2270 kg SAFETY INFORMATION: ADIPIC ACID (CAS Number 124-04-9) 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 "Organic Acids: Adipic and Fumaric Acids," Appendix B, Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Acid Anions," Appendix B. A-322 ------- ALDICARB (CAS Number 116-06-3) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Sample Field Method See "Aldehydes," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Chlorinated Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-323 ------- ALDRIN (CAS Number 309-00-2) ROj 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 determination of aldrin in air samples. A known volume of air is drawn through a glass fiber filter connected in series to a midget bubbler containing isooctane, followed by desorption with isooctane. The resulting solution is analyzed by gas chromatography with electrolytic conductivity detection (GC/HECD). INTERFERENCES: No specific interferences are given. QUALITY CONTROL: A method blank should be processed with each 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 0.15 to 0.50 milligrams per cubic meter in a 165-liter sample. Precision and accuracy information is furnished. A-324 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set S, Method S275; PB-263 871 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S275; Publication No. 77-157-C, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $90 (list), plus sampling costs. See also: "Chlorinated Pesticides," Appendix B. See also: "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Chlorinated Hydrocarbons," 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. See "Pesticides," Appendix B. A-325 ------- ALLYL ALCOHOL (CAS Number 107-18-6) RC;: 45.4 kg SAFETY INFORMATION: Exhibits chronic toxicity. Flashpoint 70°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 METHOD SUMMARY: Gas chromatography may be used for the determination of allyl alcohol 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 5 percent isopropanol in 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 each 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 has been validated over the range of 2 to 8 milligrams per cubic meter, using a 10-liter sample. The method is capable of measurement A-326 ------- 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 Manual of Analytical Methods. 2nd ed., Vol. 2, Method S52; Publication No. 78-157, U.S. DREW: Cincinnati, 1977- U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set E, Method S52; PB-246 148 (NTIS), U.S. DHEW: Washington, October 1975. 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. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. A-327 ------- ALLYL CHLORIDE (CAS Number 107-05-1) ROj 2270 kg SAFETY INFORMATION: Flashpoint -25°F. 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, Benzyl Chloride, Allyl Chloride, and 1,1-Dichloroethy- lene," 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 determination of allyl chloride in air samples. The analysis is performed by passage of 100 liters of air through a charcoal-tube sampling device, followed by desorption of the analyte with benzene 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 each 10 samples. The desorption effi- ciency and the results of the method-blank analysis should be used in the calcu- lation of the results. A-328 ------- EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 1.8 to 7.2 milligrams per cubic meter, using a 100-liter sample of air. The method is capable of measure- ment 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 I, Method S116; PB-265 028 (NTIS), U.S. DHEW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S116; 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 allyl chloride in air samples. The absorbance at 13220 nm (756 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 15 milligrams per cubic meter. No precision or accuracy information is furnished. A-329 ------- 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 "Volatile Organic Compounds," Appendix B, A-330 ------- 5-(AMINOMETHYL)-3-ISOXAZOLOL (CAS Number 2763-96-4) 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-331 ------- ROj 454 kg SAFETY INFORMATION: 4-AMINOPYRIDINE (CAS Number 504-24-5) 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-332 ------- AMITROLE (CAS Number 61-82-5) RQj 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 "Base/Neutral Extractable Organic Compounds," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B, A-333 ------- AMMONIUM ACETATE (CAS Number 631-61-8) RQ: 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Ammonia," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Ammonia," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Acid Anions," Appendix B. See "Ammonia," Appendix B. A-334 ------- AMMONIUM BENZOATE (CAS Number 1863-63-4) ROj 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Ammonia," Appendix B. See "Volatile Species," Appendix B, Air Samples Laboratory Method See "Ammonia," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Acid Anions," Appendix B. See "Ammonia," Appendix B. A-335 ------- AMMONIUM CARBAMATE (CAS Number 1111-78-0) RQ: 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Ammonia," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Ammonia," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Ammonia," Appendix B. A-336 ------- AMMONIUM CITRATE, DIBASIC (CAS Number 3012-65-5) R£: 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Ammonia," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Ammonia," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Acid Anions," Appendix B. See "Ammonia," Appendix B. A-337 ------- AMMONIUM OXALATE (CAS Numbers 6009-70-7, 5972-73-6, 14258-49-2) RQ: 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Ammonia," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Ammonia," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Acid Anions," Appendix B. See "Amines and Other Nitrogen Compounds," Appendix B. See "Ammonia," Appendix B. A-338 ------- AMMONIUM PICRATE (CAS Number 131-74-8) 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 See "Ammonia," Appendix B. See "Phenolic Compounds," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Ammonia," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Ammonia," Appendix B. A-339 ------- AMMONIUM TARTRATE (CAS Numbers 14307-43-8, 3164-29-2) RQ: 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method See "Ammonia," Appendix B. See "Volatile Species," Appendix B. Air Samples Laboratory Method See "Ammonia," Appendix B. Soil/Sediment Samples Laboratory Method See "Ammonia," Appendix B. Water Samples Laboratory Method See "Acid Anions," Appendix B. See "Ammonia," Appendix B. A-340 ------- AMYL ACETATE (CAS Number 628-63-7) RQj 2270 kg SAFETY INFORMATION: Flash point 60°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Acetate Esters," 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 determination of amyl acetate 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 each 10 samples. The desorption effi- ciency and the results of the method-blank analyses 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 208 to 871 milligrams per liter using an 11-liter sample. The method is capable of measurement of much A-341 ------- lower levels if the desorptlon 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 S51; Publication No. 77-157-B, 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 n-amyl acetate in air samples. The absorbance at 8050 nm (1242 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 which absorb infrared radiation at the wavelength of interest will interfere. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. The sensitivity of the method, using a 10-meter pathlength cell, is 6 milligrams per cubic meter. 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-342 ------- 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 Organic Compounds," Appendix B. A-343 ------- iso-AMYL ACETATE (CAS Number 123-92-2) 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 "Acetates," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-344 ------- se£-AMYL ACETATE (CAS Number 626-38-0) RQ: 2270 kg SAFETY INFORMATION; Flash point 89°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 "Acetates," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-345 ------- tert-AMYL ACETATE (CAS Number 625-16-1) 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 Water Samples Laboratory Method A-346 ------- ANILINE (CAS Number 62-53-3) 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 METHOD SUMMARY: Analysis for aniline in air may be performed by the use of a detector tube. A 0.5 - to 2.5-liter air sample is collected and analyzed with a hand- operated bellows pump and an aniline gas detector tube (Draeger® CH 20401, or equivalent). A positive result is indicated by a color change in the tube from white to red, as the aniline reacts with furfurol and acid. INTERFERENCES: The presence of ammonia levels greater than 50 grams per cubic meter will affect the aniline indication. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 5 to 80 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, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-18 (list). See also: "Aromatic Primary Amines," Appendix B. See also: "Organic Vapors," Appendix B. A-347 ------- Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatic Amines," Appendix B. See "Aromatic Primary Amines," Appendix B. Air Samples Laboratory Method METHOD SUMMARY; Analysis for aniline in air is performed by passage of a known volume of air through a silica-gel sampling device, followed by desorption of the analyte with 95-percent ethanol 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: Method S310 is approved by the National Institute for Occupational Safety and Health (NIOSH), and has been validated over the range of 9 to 38 milligrams per cubic meter in a 20-liter sample of air. Method P&CAM 168 is an operational NIOSH method for use over the range of 0.01 to 14 milligrams per sample. The method is capable of measurement of much lower levels if the desorption effi- ciency is adequate. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set K, Method S310; PB-254 227 (NTIS), U.S. DHEW: Washington, April 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, Method P&CAM 168; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S310; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. A-348 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also; "Aromatic Amines," Appendix B. See also: "Aromatic Primary Amines," Appendix B. See also: "Halogenated, Aromatic, and Other Compounds," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Amines and Other Nitrogen Compounds," Appendix B. See "Aromatic Amines," Appendix B. See "Basic Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. A-349 ------- ANTHRACENE (CAS Number 120-12-7) 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 "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. See "Trace Organic Contaminants," Appendix B. A-350 ------- AURAMINE (CAS Number 492-80-8) RQ: 0.454 kg SAFETY INFORMATION; Potentially carcinogenic. 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-351 ------- AZASERINE (CAS Number 115-02-6) Rg; 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 See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method A-352 ------- AZIRIDINE (CAS Number 151-56-4) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). Potentially carcinogenic. Extremely reactive. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Hydrazines and Other Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Note: NIOSH Method P&CAM 300 (collection in Folin's reagent in a bubbler, extraction with chloroform, and analysis by HPLC) is applicable. (Reference supplied by reviewer). Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-353 ------- BENZ[c]ACRIDINE (CAS Number 225-51-4) IRQ: 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: Thin-layer chromatography and spectrophotometry are used to determine the concentration of benz[c]acridine in air samples. Airborne particulate matter may be collected on a glass fiber filter using a high-volume sampler. The sample is extracted with cyclohexane, dissolved in dichloromethane, and separ- ated from any other organic compounds that may be present by thin-layer chromatography. The benz[c]acridine is eluted with diethyl ether and deter- mined spectrofluorometrically in trifluoroacetic acid. 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 furnished. A-354 ------- REFERENCE: Stanley, T. W.; Morgan, M. J.; Grisby, E. M. "Application of a Rapid Thin-Layer Chromatographic Procedure to the Determination of Benzo(a)pyrene, Benz(c)- acridines, and 7H-Benz(de)anthracen-7-one in Airborne Particulates from Many American Cities," Environ. Sci. Technol.. 2^(9), 1968, pp. 699-702. COST INFORMATION: Cost information has not been obtained. See also: "Polycyclic Aromatic Hydrocarbons," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-355 ------- BENZAL CHLORIDE (CAS Number 98-87-3) ROj 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 "Benzal Chloride, Benzotrichloride, and Benzyl Chloride," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-356 ------- BENZENE (CAS Number 71-43-2) ROj 45.4 kg SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic. Flashpoint 84"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 benzene in air may be performed by use of a detector tube. A 0.2 - to 4-liter air sample is collected and analyzed with a hand-operated bellows pump and a benzene gas detector tube (Draeger® 67 28561, or equivalent). A positive result is indicated by a color change in the tube from white to light brown, as the benzene reacts with formaldehyde and sulfuric acid. INTERFERENCES: Many other aromatic compounds will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels between 1 and 30 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, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is aproximately $13-18 (list). See also: "Organic Vapors," Appendix B. A-357 ------- See also: "Volatile Organic Compounds," 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 benzene 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. An aliquot of the resulting solution is injected into a gas chromatograph equipped with a flame ionization detector (GC/FID). INTERFERENCES: High humidity severely decreases the capacity of the sampling apparatus. QUALITY CONTROL: 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 analyses 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 50 to 210 milligrams per cubic meter in a 2-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set U. Method S311; PB-262 405 (NTIS), U.S. DHEW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S311; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. A-358 ------- 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 benzene in air samples. The absorbance at 9620 nm (1039 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 64 milligrams per cubic meter. 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. See also: "Hydrocarbon Odorants," Appendix B. See also: "Particulate Aromatic Hydrocarbons," Appendix B. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. A-359 ------- 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 "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-360 ------- BENZENESULFONYL CHLORIDE (CAS Number 98-09-9) ROj 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-361 ------- BENZIDINE (CAS Number 92-87-5) 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 Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Benzidine in air samples may be determined by high-performance liquid chromatography (HPLC). A known volume of air is drawn through a high- efficiency glass-fiber filter and a bed of silica gel to collect the analyte. The benzidine is desorbed from the filter and sorbent with a solution of triethylamine in methyl alcohol, and the resulting solution is analyzed by HPLC with a UV detector- INTERFERENCES: Aniline interferes. 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. A-362 ------- 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 130 micrograms per cubic meter in a 50-liter air sample. 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 243; Publication No. 77-157-A, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. See also: "Benzidine and Congeners," Appendix B. See also: "Hazardous Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Amines," Appendix B. See "Acid and Base/Neutral Extractable Organics," Appendix B. Water Samples Laboratory Method METHOD SUMMARY: Analysis of water for benzidine and its salts can be performed by spectrophotometry. A water sample is extracted at basic pH with ethyl acetate, the ethyl acetate extract is extracted with hydrochloric acid, and chloramine- T is added to the acidic solution to oxidize benzidine. The resulting yellow product is extracted with ethyl acetate and the intensity of the yellow color is compared with standards. The full absorption spectrum can aid in the confirmation of the identification. INTERFERENCES: Dichlorobenzidine, £-tolidine, dianisidine, and other compounds with a structure similar to benzidine can interfere. QUALITY CONTROL: Duplicate and spiked samples should be processed. Quality control charts should be used. A method blank should be processed with each set of samples. A-363 ------- EPA/TECHNICAL STATUS: This method is approved for use under the Clean Water Act. Precision and accuracy information is furnished. The method detection limit is 0.2 micrograms per liter for a 1-liter sample. REFERENCE; U.S. Environmental Protection Agency, Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater, "Method for Benzidine and its Salts in Wastewaters," U.S. EPA: Cincinnati, 1978, pp. 1-6. COST INFORMATION: Cost per sample for analysis by this method is approximately $65-90 (list), plus sampling costs. See also: "Amines and Other Nitrogen Compounds," Appendix B. See also: "Aromatic Amines," Appendix B. See also: "Base/Neutral Extractable Organic Compounds," Appendix B. See also: "Benzidine and Congeners," Appendix B. See also: "Hazardous Compounds," Appendix B. A-364 ------- BENZO[a]ANTHRACENE (CAS Number 56-55-3) R£: 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 "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-365 ------- BENZO[b]FLUORANTHENE (CAS Number 205-99-2) Rg: 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 "Particulate Aromatic Hyrocarbons," 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-366 ------- BENZO[k]FLUORANTHENE (CAS Number 207-08-9) ROj 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 "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-367 ------- BENZOIC ACID (CAS Number 65-85-0) RQ: 2270 kg SAFETY INFORMATION: 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 Water Samples Laboratory Method METHOD SUMMARY: Benzoic acid in an aqueous solution can be determined by titration. A water-alcohol mixture is titrated to the bromcresol purple endpoint with standard guanidine carbonate solution. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS; This method is not EPA approved. Precision and accuracy information is furnished. The method is sensitive to concentration levels of benzole acid in water over the range of 0.061 to 0.610 milligrams + 0.005 milligrams. ~ A-368 ------- REFERENCE: Saxena, A. K. "Microdetermination of Benzole and Salicylic Acids with Guanidine Carbonate as a Titrant," Microchem. J., 17(2), 1972, pp. 61-62, COST INFORMATION; Cost per sample for analysis by this method is approximately $10-15 (list), plus sampling costs. See also: "Organic Acids," Appendix B. See also: "Trace Organic Contaminants," Appendix B. See also; "Weak Acids," Appendix B. A-369 ------- BENZONITRILE (CAS Number 100-47-0) R£: 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 See "Nitroaromatic Compounds and Benzonitrile," Appendix B, Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitriles," Appendix B. See "Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B, See "Volatile Organic Compounds," Appendix B, A-370 ------- BENZO[ghi]PERYLENE (CAS Number 191-24-2) R£: 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 "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 "Polycylic Aromatic Hydrocarbons," Appendix B. A-371 ------- BENZO[a]PYRENE (CAS Number 50-32-8) 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 1 METHOD SUMMARY: Benzo[a]pyrene (BaP) in air samples may be measured by fluorometry. The analyte, together with other aromatic hydrocarbons, is collected on a membrane filter and extracted with benzene. The BaP in the extract is separated from the other components by thin-layer chromatography (TLC). The portion of the TLC sheet containing the BaP is extracted with solvent, and the solvent is removed by evaporation. The residue is dissolved in sulfuric acid, and the amount of BaP is measured using a spectrophotofluorometer. INTERFERENCES: The method is highly seletive for BaP, but is sensitive to variations in technique. QUALITY CONTROL: A filter blank should be processed with each group of samples and its value used in the calculation of the results. EPA/TECHNICAL STATUS: This method is classified as operational by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.02 to 0.8 A-372 ------- micrograms per cubic meter with a 0.5 liter air sample. Precision and accuracy information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 186; Publication No. 77-15-7-A, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost information has not been obtained. Air Samples Laboratory Method 2 METHOD SUMMARY: Particulate benzo[a]pyrene in air samples may be measured by high- performance liquid chromatography (HPLC). The particulates are collected on glass fiber and silver membrane filters and extracted ultrasonically into acetonitrile. The extract is filtered, then injected into an HPLC with spectro- photofluorometric detection. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: A blank should be processed with the samples. EPA/TECHNICAL STATUS: This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 6 to 240 nanograms per sample. The limit of detection is 10 picograms per injection. 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 251; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $155 (list), plus sampling costs. A-373 ------- Air Samples Laboratory Method 3 METHOD SUMMARY: Benzo[a]pyrene (BaP) in air samples can be measured by high-performance liquid chromatography (HPLC). The sample is collected using a high-volume sampler, then is Soxhlet-extracted with cyclohexane. The solvent is evaporated in a flash evaporator, and the residue is dissolved in methanol. The solution is analyzed by HPLC with fluorescence detection. INTERFERENCES: No interferences are reported. QUALITY CONTROL: Every tenth sample should be analyzed with a spiked duplicate. A blank, two standards, and another blank should be analyzed with every fifth sample. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is given. The detection limit is 0.01 nanograms of BaP per cubic meter of air. REFERENCES: Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric Pollu- tants, 2nd ed., Method 21516; Alberta Environmental Centre, Vegreville, Alberta, Canada, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $180 (list), plus sampling costs. See also: "Particulate Aromatic Hydrocarbons," Appendix B. See also: "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-374 ------- p-BENZOQUINONE (CAS Number 106-51-4) R£: 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method METHOD SUMMARY: Detection of p-benzoquinone in aqueous solution has been performed by reverse-pulse amperometry. The technique is a variant of normal pulse voltam- metry and shows an increase of approximately 50 percent in sensitivity over conventional d.c. amperometric detection. The method is proposed as suitable for use with liquid chromatography. INTERFERENCES: Dissolved oxygen does not interfere. QUALITY CONTROL: No quality control procedures are given. A-375 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. No precision or accuracy information is furnished. REFERENCE: Wang, J.; Dewald, H. D. "Flow Injection Analysis of Oxidizable Species with Reverse-Pulse Amperometric Detection," Talanta, 29, 1982, pp. 901-904. COST INFORMATION: No cost information has been obtained. A-376 ------- BENZOTRICHLORIDE (CAS Number 98-07-7) 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 See "Benzal Chloride, Benzotrichloride, and Benzyl Chloride," Appendix B. Soil/Sediment Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. A-377 ------- BENZOYL CHLORIDE (CAS Number 98-88-4) R_Q; 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 "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Reacts with water. Water Samples Field Method Reacts with water. See "Halides, Cyanides, and Other Compounds," Appendix B, Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Reacts with water. Water Samples Laboratory Method Reacts with water. A-378 ------- BENZYL CHLORIDE (CAS Number 100-44-7) RQ: 45.4 kg SAFETY INFORMATION: Potentially carcinogenic. Can undergo condensation stabilizer required. 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, Benzyl Chloride, Allyl Chloride, and 1,1-Dichloro- ethylene," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used for the analysis of benzyl chloride 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 calcu- lation of the results. A-379 ------- EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 2 to 8 milligrams per cubic meter in a 10-liter sample of air. 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 H, Method S115; PB-265 027 (NTIS), U.S. DHEW: Washington, January 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S115; 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: "Benzal Chloride, Benzotrichloride, and Benzyl Chloride," Appendix B. Soil/Sediment Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Non-Volatile Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. See "Volatile Organic Compounds," Appendix B. A-380 ------- a-BHC (CAS Number 319-84-6) 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 See "Chlorinated Pesticides," Appendix B. See "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-381 ------- B-BHC (CAS Number 319-85-7) R£: 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 See "Chlorinated Pesticides," Appendix B. See "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Chlorinate Hydrocarbons," 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. See "Pesticides," Appendix B. A-382 ------- 6-BHC (CAS Number 319-86-8) RQj 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 See "Chlorinated Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Chlorinated Pesticides," 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 Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. See "Pesticides," Appendix B. A-383 ------- BIS(2-CHLOROETHOXY)METHANE (CAS Number 111-91-1) 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 See "B-Chloroethers," Appendix B. See "Fumiga'nts," 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-384 ------- BIS(2-CHLOROETHYL)ETHER (CAS Number 111-44-4) RQj 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 1 METHOD SUMMARY: Analysis for bis(2-chloroethyl)ether in air 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 has been validated over the range of 45 to 180 milli- grams per cubic meter in a 15-liter sample. The method is capable of measure- ment of much lower levels if the desorption efficiency is adequate. Precision and accuracy information is furnished. A-385 ------- REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed.. Vol. 3, Method S357; Publication No. 77-157-C, U.S. DREW, 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 bis(2-chloroethyl)ether in air samples. The absorbance at 8780 nm (1139 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 30 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 anlysis by this method is approximately $75-85 (list), plus sampling costs. A-386 ------- See also: "B-Chloroethers," Appendix B. See also: "Fumigants," 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. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Chlorinated and Other Organic Contaminants," Appendix B. See "Halogenated and Aromatic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-387 ------- BIS(2-CHLOROISOPROPYL)ETHER (CAS Number 108-60-1) 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 See "3-Chloroethers," Appendix B. See "Hazardous Organic Emissions," 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-388 ------- BIS(CHLOROMETHYL)ETHER (CAS Number 542-88-1) RQ: 0.454 kg SAFETY INFORMATION; Exhibits toxicity (inhalation). 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 METHOD SUMMARY: Analysis for bis(chloromethyl)ether [bis-CME] in air can be performed by gas chroraatography/mass spectrometry (GC/MS). A known volume of air is drawn through a Chromosorb 101 sampling tube to trap bis-CME, and the tube is heated and backflushed into a temperature-programmed GC/MS instrument. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: Standards should be analyzed after every three samples. EPA/TECHNICAL STATUS: This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 2.4 to 47 micrograms per cubic meter of air in a 5-liter sample. Precision and accuracy information for standards is furnished. A-389 ------- REFERENCES: American Society for Testing and Materials, ASTM Standards on Chromatography, D3476-79; ASTM: Philadelphia, 1981, pp. 435-439. American Society for Testing and Materials, 1983 Annual Book of ASTM Standards. Vo. 11.03, D3476-79; ASTM: Philadelphia, 1983. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 213; Publication No. 77-157-A, U.S. DREW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $250-325 (list), plus sampling costs. See also: "Halogenated and Aromatic Compounds," Appendix B. Air Samples Laboratory Method 2 METHOD SUMMARY: Bis(chloromethyl)ether in air samples can be measured by gas chromato- graphy. A known volume of air is passed through two impingers in series, containing a methanolic solution of the sodium salt of 2,4,6-trichlorophenol. The analyte reacts with the derivatizing reagent to produce stable derivatives. The solution is extracted with hexane and an aliquot of the extract is analyzed by gas chromatography with electron capture detection (GC/ECD). INTERFERENCES: Interferences can be expected from highly halogenated organic compounds or compounds that may produce the same derivatives. If impurities are present in the 2,4,6-trichlorophenol, they may interfere. 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 2.4 to 35 micrograms per cubic meter of air with a 10-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 220; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. A-390 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $90-115 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-391 ------- BIS(2-ETHYLHEXYL)PHTHALATE (CAS Number 117-81-7) ROj 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 bis(Z-ethylhexyl)- phthalate in air samples. The analysis is performed by passage of a known volume of air through a cellulose membrane filter, 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: No specific interferences are reported. QUALITY CONTROL: Desorption efficiency must be determined over the range of interest, and 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 validated over the range of 2.03 to 10.9 milligrams per cubic meter of air for a 32-liter sample. Precision and accuracy information is furnished. A-392 ------- REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set D, Method S40; PB-245 935 (NTIS), U.S. DREW: Washington, October 1975. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Phthalate Esters," Appendix B. Water Samples Laboratory Method See "Phthalate Esters," Appendix B. See "Trace Organic Contaminants," Appendix B. A-393 ------- R(£: 454 kg SAFETY INFORMATION: BROMOACETONE (CAS Number 598-31-2) 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 of air for bromoacetone can be performed by passage of air through an alcoholic potassium hydroxide solution, reaction with sodium nitro- prusside, and measurement of the intensity of the resulting red color. The color intensity is increased by the presence of acetic acid. INTERFERENCES: No interferences are reported, although bromomethyl ethyl ketone will react under the same conditions to give an orange color. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: No sensitivity information is given. REFERENCES: Cox, H. E. "Tests Available for the Identification of Small Quantities of the War Gases," Analyst, 64_, 1939, pp. 807-813. Chem. Abstr., 1940, 34:54li. COST INFORMATION: Cost per sample for analysis by the method is approximately $15-22 (list) Soil/Sediment Samples Field Method Water Samples Field Method A-394 ------- Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-395 ------- BROMOFORM (CAS Number 75-25-2) RQ: 45.4 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 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 determination of bromoform in air samples. The analysis is performed by passage of 10 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 calcu- lation of the results. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and has been validated over the range of 3 to 10 milligrams per cubic meter, using a 10-liter sample. The method is capable of measurement A-396 ------- 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 H, Method S114; PB-265 027 (NTIS), U.S. DREW: Washington, January 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S114; 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: "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 "Chlorinated Ethers and Other 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 Organic Compounds," Appendix B. A-397 ------- 4-BROMOPHENYL PHENYL ETHER (CAS Number 101-55-3) 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 "Acid and Base/Neutral Extractable Organics," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. A-398 ------- BRUCINE (CAS Number 357-57-3) R£: 4.54 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 Water Samples Laboratory Method A-399 ------- BUTYL ACETATE (CAS Number 123-86-4) RQ: 2270 kg SAFETY INFORMATION: Flash point 72°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Acetates," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Acetates," Appendix B. See "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-400 ------- i^o-BUTYL ACETATE (CAS Number 110-19-0) RQ: 2270 kg SAFETY INFORMATION: Flash point 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 "Acetates," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Acetates," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-401 ------- -BUTYL ACETATE (CAS Number 105-46-4) ROj 2270 kg SAFETY INFORMATION: Flash point 88°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: Infrared absorption spectrometry can be used to determine the concentra- tion of sec-butyl acetate in air samples. The absorbance at 8050 run (1242 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-402 ------- 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. 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: "Acetates," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-403 ------- tert-BUTYL ACETATE (CAS Number 540-88-5) RQ: 2270 kg SAFETY INFORMATION: Flash Point 88°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 "Acetates," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-404 ------- i£o-BUTYL ALCOHOL (CAS Number 78-83-1) RQ: 2270 kg SAFETY INFORMATION: Flash point 82°F- CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "n-Butyl Alcohol and iso-Butyl Alcohol," 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 iso-butyl alcohol 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). INTERFERENCE: 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/TECHNCAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 180 to 620 milligrams per 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. A-405 ------- REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S64; Publication No. 77-157-B, U.S. DREW: Cincinnati, April 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. A-406 ------- n-BUTYL ALCOHOL (CAS Number 71-36-3) RQ: 2270 kg SAFETY INFORMATION; Flash point 84°F- CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "n-Butyl Alcohol and iso-Butyl Alcohol," 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 n-butyl alcohol in air samples. The analysis is performed by passage of 10 liters of air through a charcoal-tube sampling device, followed by desorption of the analyte with 1 percent isopropanol in carbon disulfide and analysis of the resulting solution by gas chromatography with flame ionization detection (GC/FID). INTERFERENCE: 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 170 to 610 milligrams per cubic meter, using a 10-liter sample of air. The method is capable of measure- A-407 ------- ment 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 S66; PB-246 148 (NTIS), U.S. DREW: Washington, October 1975. U.S. Deparment of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S66; 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: "Volatile Organic Solvents," Appendix B. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of n-butyl alcohol in air samples. The absorbance at 9350 nm (1069 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 which absorb infrared radiation at the wavelength of interest will interfere. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. The sensitivity of the method, using a 10-meter pathlength cell, is 31 milligrams per cubic meter. No precision or accuracy information is furnished. A-408 ------- 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 Solvents," Appendix B. Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-409 ------- BUTYLAMINE (CAS Number 109-73-9) RQ: 2270 kg SAFETY INFORMATION: Flash point 10°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," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of butylamine in air samples. The absorbance at 12850 nm (778 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. A-410 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. The sensitivity of the method, using a 10-meter pathlength cell, is 31 milligrams per cubic meter. 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. Air Samples Laboratory Method 2 METHOD SUMMARY: Butylamine in air samples can be measured by gas chromatography. A known volume of air is drawn through sulfuric acid-treated silica gel. The butyl- amine is desorbed from the silica gel with 50 percent methanol and analyzed by gas chromatograpy with flame ionization detection (GC/FID). INTERFERENCES: Any compound that has the same retention time as butylamine is an inter- ference. 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 has been validated over the range of 8.1 to 35.5 milligrams per cubic meter. The method is capable of measurement of much lower levels if the desorption efficiency is adequate. Precision and accuracy infor- mation is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4. Method S138; Publication No. 78-175, U.S. DHEW: Cincinnati, August 1978. A-411 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. See also: "Aliphatic Amines," Appendix B. See also: "Low Molecular Weight Aliphatic Amines," Appendix B. Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Aliphatic Amines," Appendix B. See "Amines," Appendix B. See "Amines and Other Nitrogen Compounds," Appendix B. A-412 ------- is£-BUTYLAMINE (CAS Number 78-81-9) 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 See "Hazardous Organic Emissions," Appendix B. See "Low Molecular Weight Aliphatic Amines," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aliphatic Amines," Appendix B. See "Amines and Other Nitrogen Compounds," Appendix B. A-413 ------- sec-BUTYLAMINE (CAS Numbers 513-49-5, 13952-84-6) 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 "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Low Molecular Weight Aliphatic Amines," Appendix B, Soil/Sediment Samples Laboratory Method See "Amines and Alcohols," Appendix B. Water Samples Laboratory Method See "Aliphatic Amines," Appendix B. A-414 ------- tert-BUTYLAMINE (CAS Number 75-64-9) 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 See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Low Molecular Weight Aliphatic Amines," Appendix B, Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aliphatic Amines," Appendix B. A-415 ------- BUTYL BENZYL PHTHALATE (CAS Number 85-68-7) 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 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-416 ------- BUTYRIC ACID (CAS Number 107-92-6) RQ: 2270 kg SAFETY INFORMATION: Air Samples Field Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Hazardous Organic Emissions," Appendix B, See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Acids," Appendix B. See "Organic Compounds," Appendix B. See "Volatile Organic Acids," Appendix B. A-417 ------- iso-BUTYRIC ACID (CAS Number 79-31-2) RQ: 2270 kg SAFETY INFORMATION: Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Organic Acids," Appendix B. A-418 ------- CAPTAN (CAS Number 133-06-2) RQ: 4.54 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 Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Captan in soil samples can be measured colorimetrically- The captan is extracted from the soil with dichloromethane. The suspension is filtered and the filter cake is washed. The filtrate and washings are decolorized with 1:1 Norit A® and Florisil® and filtered. Tetraethylene glycol dimethyl ether is added and the solvent is evaporated. The residue is transferred to a beaker and dried, using a water bath. Just as evaporation is completed, the beaker is removed from the bath, a pyridin tetraethylammonium hydroxide reagent is added, and the flask is gently swirled to dissolve the residue. After 3 minutes, the absorbance of the solution is measured at 427 nm on a colorimeter. INTERFERENCES: Phaltan® interferes with this method; other pesticides do not interfere significantly. Captan is quite reactive and loss due to reaction with organic matter in the soil, as well as to hydrolysis, must be considered. QUALITY CONTROL: Quality control procedures are not furnished. A-419 ------- EPA/TECHNICAL STATUS: This method is not EPA approved. Precision and accuracy information is not furnished. REFERENCE: Ospenson, J. N.; Pack, D. E.; Kohn, G. K.; Burchfield, H. P.; Storrs, E. E. In Analytical Methods for Pesticides, Plant Growth Regulators, and Food Additives, G., Zweig, Ed.; Academic Press: New York, 1964, Vol. Ill, pp. 7-25. COST INFORMATION: Cost per sample for analysis by this method is approximately $90-135 (list). Water Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. See "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides," Appendix B. See "Pesticides," Appendix B. A-420 ------- CARBARYL (CAS Number 63-25-2) 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 "Cholinesterase-Inhibiting Compounds," Appendix B. See "Halides, Cyanides, and Other Compounds," Appendix B. See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Colorimetry may be used for the analysis of carbaryl in air. A known volume of air is drawn through a glass fiber filter. The analyte is extracted and hydrolyzed using methanol in potassium hydroxide. An aliquot is reacted with p-nitrobenzenediazonium fluoroborate to form a colored complex. The absorbance is read on a colorimeter at 475 nm. INTERFERENCES: Phenols such as 1-naphthol will interfere. Any compound that absorbs at 475 nm is an interference. QUALITY CONTROL: A method blank is submitted with every 10 samples and is processed along with samples and standards. EPA/TECHNICAL STATUS; This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 1.96 to 13.43 milligrams per cubic meter. Precision and accuracy information is furnished. A-421 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set S, Method S273; PB-263 871 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S273; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. COST INFORMATION; Cost per sample for analysis by this method is approximately $60 (list), plus sample costs. See also: "Carbamate Pesticides," Appendix B. See also: "Chlorinated Pesticides," Appendix B. See also: "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "0-Aryl Carbamate Pesticides," Appendix B. See "Carbamate and Urea Pesticides," Appendix B, See "N-Methylcarbamates," Appendix B. A-422 ------- CARBOFURAN (CAS Number 1563-66-2) 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 See "Carbamate Pesticides," Appendix B. See "Chlorinated Pesticides," Appendix B. See "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Carbamate Pesticides," Appendix B. See "Organophosphorus and Carbamate Insecticides," Appendix B. Water Samples Laboratory Method See "Carbamate and Urea Pesticides," Appendix B. See "N-Methylcarbamates," Appendix B. A-423 ------- CARBON BISULFIDE (CAS Number 75-15-0) RQ: 2270 kg SAFETY INFORMATION: Flash point -22°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 Samples METHOD SUMMARY: Analysis for carbon disulfide may be performed by use of a detector tube. A 1.1-liter air sample is collected and analyzed with a hand-operated bellows pump and a carbon disulfide gas detector tube (Draeger® 67 28351, or equivalent). A positive result is indicated by a color change in the tube from white to brownish-green, caused by reaction of carbon disulfide with iodine pentoxide to form iodine. INTERFERENCES: Benzene, n-octane, hydrogen sulfide, and carbon monoxide will also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 15 to 200 milligrams per cubic meter. REFERENCES: Snyder, R. E.; Schulte, B. E.; Mangoba, L.; McHale, E. T. Available Field Methods for Rapid Screening of Hazardous Waste Materials at Waste Sites; Atlantic Research Corp. for U.S. Army Medical Research and Development Command, Fort Detrick, Maryland, January 1982, p. 50. National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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: National Draeger: Pittsburgh, December 1981. A-424 ------- 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 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 carbon disulfide in air samples. The analysis is performed by passage of 6 liters of air through a charcoal-tube sampling device, followed by desorption of the analyte with benzene and analysis of the resulting solution by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: High humidity decreases severely 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 is validated over the range of 15 to 59 milligrams per cubic meter in a 6-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 R, Method S248: PB-262 403 (NTIS), U.S. DHEW: Washington, December 1976. A-425 ------- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtical Methods. 2nd ed., Vol. 3, Method S248, 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: Carbon disulfide in air samples may be measured by atomic absorption spectroscopy (AA). The analyte is adsorbed from a known volume of air onto activated carbon, then desorbed with iso-amyl acetate containing pyrrolidine. The resulting organic solution is shaken with an acidic solution of cupric sulfate. Pyrrolidine dithiocarbamate, formed from the carbon disulfide and pyrrolidine, chelates the copper, which is measured by AA. The moles of copper found are equal to half the moles of carbon disulfide collected. INTERFERENCES: High humidity decreases the capacity of the sorbent. QUALITY CONTROL: Desorption efficiency must be determined over the range of interest and a method blank should be processed. The desorption efficiency and the results of the method-blank analysis should be used in the calcualtion of the results. 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 5 to 100 milligrams per cubic meter of air, using 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. 1, Method P&CAM 179; 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), plus sampling costs. A-426 ------- Air Samples Laboratory Method 3 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of carbon disulfide in air samples. The absorbance at 4570 nm (2188 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 64 milligrams per cubic meter. 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. Soil/Sediment Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-427 ------- Water Samples Laboratory Method See "Non-Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-428 ------- CARBON TETRACHLORIDE (CAS Number 56-23-5) RQ: 2270 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 "Carbon Tetrachloride and Trichloromonofluoromethane," Appendix B. See "Organic Vapors," 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 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of carbon tetrachloride 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 chromatog- raphy 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 is validated over the range of 65 to 299 milligrams per A-429 ------- cubic meter in a 17-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 S314; PB-263 959 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtical Methods, 2nd ed., Vol. 3, Method S314, 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 carbon tetrachloride in air samples. The absorbance at 12600 nm (794 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 3.5 milligrams per cubic meter. No precision or accuracy information is furnished. A-430 ------- 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: "Halogenated Vapors," Appendix B. 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 "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Compounds," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B. See "Volatile Organic Compounds," Appendix B. A-431 ------- CARBONYL FLUORIDE (CAS Number 353-50-4) 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-432 ------- RQ: 0.454 kg SAFETY INFORMATION: CHLORAL (CAS Number 75-87-6) 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 "Aldehydes," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Aliphatic Aldehydes," Appendix B. Soil/Sediment Samples Laboratory Method See "Aliphatic Aldehydes," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B, Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B, A-433 ------- CHLORAMBUCIL (CAS Number 305-03-3) 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-434 ------- CHLORDANE (CAS Number 57-74-9) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Air Samples Field Method Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Note; NIOSH Method 278 (filter/solvent collection, extraction with toluene, analysis by GC/ECO) is applicable. (Reference furnished by reviewer) See also: "Base/Neutral Extractable Organic Compounds," Appendix B. See also: "Chlorinated Pesticides," 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 "Chlorinated Pesticides," Appendix B. See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Organochlorine Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. A-435 ------- CHLORNAPHAZINE (CAS Number 494-03-1) 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-436 ------- CHLOROACETALDEHYDE (CAS Number 107-20-0) 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. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Note: NIOSH Method Sll (silica gel collection, desorption with 1/1 methanol/ water, analysis by GC/ECP) is applicable. (Reference furnished by reviewer). See also:"Aliphatic Aldehydes," 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-437 ------- £-CHLOROANILINE (CAS Number 106-47-8) 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 "Amines and Other Nitrogen Compounds," Appendix B. See "Basic Organic Compounds," Appendix B. A-438 ------- CHLOROBENZENE (CAS Number 108-90-7) RQ: 45.4 kg SAFETY INFORMATION: Flash point 84°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Chlorobenzene and Dichlorobenzenes," Appendix B. See "Volatile Organic Compounds," 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 chlorobenzene 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 each 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 is validated over the range of 183 to 736 milligrams A-439 ------- per cubic meter in 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 I, Method S133: PB-265 028 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtical Methods, 2nd ed., Vol. 2, Method S133, Publication No. 77-157-B, U.S. DHEW: Cincinnati, April 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 chlorobenzene in air samples. The absorbance at 9160 nm (1092 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 46 milligrams per cubic meter. No precision or accuracy information is furnished. A-440 ------- 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. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Halogenated 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 "Halogenated Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. See "Volatile Organic Compounds," Appendix B. A-441 ------- £-CHLORO-m-CRESOL (CAS Number 59-50-7) 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 See "Phenolic Compounds," Appendix B. 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 "Phenolics," Appendix B. See "Phenols," Appendix B. A-442 ------- CHLORODIBROMOMETHANE (CAS Number 124-48-1) RQ: 45.4 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 Soil/Sediment Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Chlorinated and Other Organic Contaminants, Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Halogenated Compounds," Appendix B. See "Low-Molecular Weight Halogenated Hydrocarbons," Appendix B, See "Volatile Organic Compounds," Appendix B. A-443 ------- CHLOROETHANE (CAS Number 75-00-3) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Flash point -58°F. 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 Organic Compounds," Appendix B. A-444 ------- 2-CHLOROETHYL VINYL ETHER (CAS Number 110-75-8) RQ: 454 kg SAFETY INFORMATION: Flash point 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 See " -Chloroethers," 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-445 ------- CHLOROFORM (CAS Number 67-66-3) RQ: 2270 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 METHOD SUMMARY: The concentration of chloroform in air may be determined by using a gas detector tube. A 0.5-liter air sample is collected and analyzed with a portable pump and a chloroform gas detector tube (Bendix/Gastec® 137, or equivalent). A positive result is indicated by a color change from white to orange in the tube. INTERFERENCES: Other halogenated hydrocarbons and inorganic halogens may also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 50 to 500 milligrams per cubic meter. REFERENCE: Bendix Corp., Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix Corp.: Largo, Florida. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method A-446 ------- Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of chloroform 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 calcu- lation of the results. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and is validated over the range of 99.8 to 416 milligrams per cubic meter in a 17-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 S351; PB-263 959 (NTIS), U.S. DHEW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analtical Methods, 2nd ed., Vol. 3, Method S351, 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 chloroform in air samples. The absorbance at 12950 nm (772 cm" ) is measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or A-447 ------- 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. 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. 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 Compounds," Appendix B. A-448 ------- 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-449 ------- CHLOROMETHYL METHYL ETHER (CAS Number 107-30-2) 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 METHOD SUMMARY: Chloromethyl methyl ether in air samples may be measured by gas chromatog- raphy. A known volume of air is passed through two impingers containing a methanolic solution of the sodium salt of 2,4,6-trichlorophenol. The analyte reacts with the derivatizing reagent to produce a stable derivative. The sample is heated, diluted with water, and extracted with hexane. An aliquot of the hexane extract is analyzed by gas chromatography with electron capture detection (GC/ECD). INTERFERENCES: Highly halogenated organic compounds or compounds that produce the same derivatives may interfere. High-quality 2,4,6-trichlorophenol must be used to minimize the error due to impurities. 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 2.4 to 35 micrograms per cubic meter for a 10-liter sample. Precision and limited accuracy information is furnished. A-450 ------- REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 220, Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $100-150 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. A-451 ------- 2-CHLORONAPHTHALENE (CAS Number 91-58-7) 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 See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. A-452 ------- 2-CHLOROPHENOL (CAS Number 95-57-8) 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 See "Phenolic Compounds," Appendix B. 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 "Chlorinated Ethers and Other Compounds," Appendix B. See "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. See "Trace Organic Compounds," Appendix B. A-453 ------- 4-CHLOROPHENYL PHENYL ETHER (CAS Number 7005-72-3) 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 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-454 ------- l-(o-CHLOROPHENYL) THIOUREA (CAS Number 5344-82-1) 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-455 ------- 3-CHLOROPROPIONITRILE (CAS Number 542-76-7) 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 Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-456 ------- 4-CHLORO-o-TOLUIDINE HYDROCHLORIDE (CAS Number 3165-93-3) 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 Water Samples Laboratory Method A-457 ------- CHLORPYRIFOS (CAS Number 2921-88-2) 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 See "Organophosphorus Pesticides," Appendix B. Air Samples Laboratory Method See "Organophosphorus Compounds," Appendix B. See "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-458 ------- CHRYSENE (CAS Number 218-01-9) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (dermal). 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 "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-459 ------- COUMAPHOS (CAS Number 56-72-4) 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 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 "Organophosphorus Pesticides," Appendix B. A-460 ------- CREOSOTE (CAS Number 8001-58-9) 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. See* "Acenaphthene," Appendix A. See "Acridine," Appendix A. See "Anthracene," Appendix A. See "Benzofj,k]fluorene," Appendix A. See "Chrysene," Appendix A. See "Fluorene," Appendix A. See "Naphthalene," Appendix A. See "Phenanthrene," Appendix A. See "Pyrene," Appendix A. See "Polycyclic Aromatic Hydrocarbons," Appendix B. *Individual compounds are those listed as present in amounts greater than 1 percent in "Background Document, Resource Conservation and Recovery Act, Subtitle C - Identification and Listing of Hazardous Waste," U.S. Environmental Protection Agency, Office of Solid Waste, November 14, 1980. A-461 ------- CRESOLS (CAS Number 1319-77-3) 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 "Phenols: Cresols," Appendix B. See "Phenols," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenols: Cresols," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Compounds," Appendix B. See "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. A-462 ------- RQ: 454 kg SAFETY INFORMATION: m-CRESOL (CAS Number 108-39-4) 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 "Phenols: Cresols," Appendix B. See "Phenols," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B, Air Samples Laboratory Method See "Phenols: Cresols," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Compounds," Appendix B. See "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. A-463 ------- o-CRESOL (CAS Number 95-48-7) 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 METHOD SUMMARY: o-Cresol in air samples can be measured by UV spectrophotometry. The air sample is collected in a gas washing bottle containing highly purified ethanol. The sample absorbance is read on a spectrophotometer at a wavelength of 272 nm. (This method is described by Carney, G. E.; Sanford, W.K. Anal. Chem. 25, 1953, p. 1417, and is summarized in the reference given below.) INTERFERENCES: Any material absorbing at a wavelength of 272 nm will interfere. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for £-cresol concentrations in the range of approximately 1 to 20 milligrams per cubic meter. REFERENCE: Quantitative Analysis of Gaseous Pollutants, W. E., Ruch, Ed.; Ann Arbor- Humphrey Science: Ann Arbor, 1970; p. 75. COST INFORMATION: Cost per sample for analysis by this method is approximately $15-22 (list), plus sampling costs. See also: "Phenols: Cresols," Appendix B. See also; "Phenols," Appendix B. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method A-464 ------- Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenols: Cresols," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Mehthod See "Organic Compounds," Appendix B. See "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. See "Trace Organic Contaminants," Appendix B. A-465 ------- RQ: 454 kg SAFETY INFORMATION: p-CRESOL (CAS Number 106-44-5) 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 "Phenols: Cresols," Appendix B. See "Phenols," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenols: Cresols," Appendix B. See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Compounds," Appendix B. See "Phenolic Compounds," Appendix B. A-466 ------- CROTONALDEHYDE (CAS Numbers 123-73-9, 4170-30-3) RQ: 45.4 kg SAFETY INFORMATION: Flash point 55°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 Note: NIOSH Method P & CAM 285 (bubbler collection, derivatization with hydroxylamine, analysis by polarography) is applicable. (Reference supplied by reviewers). See also;"Aliphatic Aldehydes," Appendix B. Soil/Sediment Samples Laboratory Method See "Thiourea and Other Compounds," Appendix B. Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-467 ------- CUMENE (CAS Number 98-82-8) RQ: 2270 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 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 METHOD SUMMARY: Analysis for cumene in air 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 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 has been validated for the range of 120 to 480 milli- grams per cubic meter, using a 10-liter sample. The method is capable of A-468 ------- 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 S23; PB-245 852 (NTIS), U.S. DREW: Washington, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S23; 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. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Trace Organic Contaminants," Appendix B A-469 ------- CYCLOHEXANE (CAS Number 110-82-7) RQ: 454 kg SAFETY INFORMATION: Flash point -4°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 cyclohexane in air may be determined by using a gas detector tube. A 0.2-liter sample is collected and analyzed with a portable pump and a hexane gas detector tube (Bendix/ Gastec® 102H, or equivalent). A positive result is indicated by a color change from orange to dark green in the tube, from reduction of Cr(VI) to Cr(III). INTERFERENCES: Hexane, propane, acetylene, benzene, toluene, xylene, and other organic vapors may also cause brown or green color changes. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 500 to 1000 milligrams per cubic meter. REFERENCE: Bendix Corp., Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix Corp.: Largo, Florida. 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 A-470 ------- Water Samples Field Method See "Halides, Cyanides, 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 cyclohexane in air samples. The analysis is performed by passage a known volume of air through a charcoal-tube trap, followed by desorption of 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: The desorption efficiency must be determined over the range of use, and a method blank should be processed with every 10 samples. The desorption effi- ciency and the method-blank results should be used in the calculation of the results. EPA/TECHNICAL STATUS: This method is a approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 510 to 2,010 milli- grams per cubic meter, using a 25-liter sample. The method is capable of measuring 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 S28; PB-245 852 (NTIS), U.S. DHEW: Washington, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S28; 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. A-471 ------- Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of cyclohexane in air samples. The absorbance at 11600 nm (862 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 130 milligrams per cubic meter. 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. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. A-472 ------- CYCLOHEXANONE (CAS Number 108-94-1) 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 See "Cyclohexanone and Furfural," 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 METHOD SUMMARY: Gas chromatography may be used for the analysis of cyclohexanone 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 calcu- lation of the results. A-473 ------- EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 98 to 392 milligrams per cubic meter, using a 40-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 S19; PB-245 850 (NTIS). U.S. DHEW: Washington, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S19; 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. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-474 ------- CYCLOPHOSPHAMIDE (CAS Number 50-18-0) 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-475 ------- 2,4-D ACID (CAS Number 94-75-7) 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 See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: 2,4-D in air samples can be measured by high-performance liquid chromato- graphy (HPLC). The sample is collected on a glass-fiber filter. Methanol is used as the eluent, 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 for Occupational Safety and Health (NIOSH) for use over the range of 5.1 to 20.3 milligrams of 2,4-D per cubic meter of air. Precision and accuracy information is furnished. REFERENCES: 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; Publication No. 80-133, U.S. DHHS, 1980. A-476 ------- Note; NIOSH Method S279 describes the above method in greater detail. (Refer- ence supplied by reviewer). 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 Phenols," Appendix B. See "Chlorinated Phenoxy Acid Herbicides," Appendix B. A-477 ------- DAUNOMYCIN (CAS Number 20830-81-3) 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-478 ------- DDD (CAS Number 72-54-8) 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 "Particulate Aromatic Hydrocarbons," Appendix B. See "Pesticide Residues," 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 "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-479 ------- DDE (CAS Number 72-55-9) 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 See "Chlorinated Pesticides," Appendix B. See "Particulate Aromatic Hydrocarbons," Appendix B. See "Pesticide Residues," 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 "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-480 ------- DDT (CAS Number 50-29-3) 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 METHOD SUMMARY: Gas chromatography may be used for the analysis of DDT in air samples. The analysis is performed by passage of a known volume of air through a glass fiber filter, followed by desorption of the analyte with isooctane and analysis of the resulting solution by gas chromatography with electrolytic conductivity detection. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL; 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 validated over the range of 0.49 to 2.60 milligrams per cubic meter in a 90-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-481 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set S, Method S274; PB-263 871 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S274; Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus satnping costs. See also: "Chlorinated Pesticides," Appendix B. See also: "Particulate Aromatic Hydrocarbons," Appendix B. See also: "Pesticide Residues," 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 "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-482 ------- 2,4-D ESTERS (CAS Numbers 94-11-1, 94-79-1, 94-80-4, 1320-18-9. 1928-38-7, 1928-61-6, 1929-73-3, 2971-38-2, 25168-26-7, 53467-11-1) 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 "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-483 ------- DIALLATE (CAS Number 2303-16-4) 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 METHOD SUMMARY: Diallate in water samples can be measured by gas chromatography with electron capture detection (GC/ECD). A 1-liter sample is acidified to below pH 1 and extracted with dichloromethane. A cleanup is performed that involves base partitioning and treatment on a deactivated Florisil column, then on an activated one. The eluent is analyzed by GC/ECD. INTERFERENCES: All likely interferences are separated by the cleanup procedure. A-484 ------- QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS; This method is not EPA-approved. Precision and accuracy information is furnished. The detection limit for the conditions and samples used is 0.1 micrograms per liter- REFERENCE: Lee, H. B.; Chau, A. S. Y. "Determination of Trifluralin, Diallate, Triallate, Atraine, Barban, Dichlofop-Methyl, and Benzoylprop-Ethyl in Natural Waters at Parts per Trillion Levels," J. Assoc. Off. Anal. Chem. , 66^(3), 1983, pp. 651-658, COST INFORMATION; Cost per sample for analysis by this method is approximately $170-205 (list), plus sampling costs. A-485 ------- DIAZINON (CAS Number 333-41-5) 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 METHOD SUMMARY: Diazinon in soil samples can be measured by spectrophotometry. Diazinon is extracted with petroleum ether and washed with 2-percent sodium hydroxide. A hydrobromic acid extraction follows. The diazinon-containing acid fraction is decomposed and the evolving hydrogen sulfide gas is carried into a solution of zinc acetate. Zinc sulfide precipitates. After cooling in an ice bath, a solution of ferric chloride and dimethyl-p-phenylenediamine reagent is added to the sulfide mixture. The color intensity of the resulting sulfide solution is read on a portable spectrophotometer at 665-670 run. INTERFERENCES: Oxidants in the hydrobromic acid can suppress generation of hydrogen sulfide. Too much hydrogen sulfide can prevent the color reaction. QUALITY CONTROL: No quality control procedure are given. SENSITIVITY: This method is not EPA-approved. Some precision and accuracy information is furnished. REFERENCE: Margot, A.; Stammbach, K. In Analytical Methods for Pesticides, Plant Growth Regulators, and Food Additives Vol. II, G., Zweig, Ed.; Academic Press: New York, 1964, pp. 109-124. COST INFORMATION: Cost per sample for analysis by this method is approximately $45-75 (list). A-486 ------- 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 "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 Compounds," Appendix B. See "Organophosphorus Pesticides," Appendix B. A-487 ------- DIBENZ[a,h]ANTHRACENE (CAS Number 53-70-3) 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 "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-488 ------- DIBENZ[a,i]PYRENE (CAS Number 189-55-9) RQ: 0.45A 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 "Polycyclic Aromatic Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Polycyclic Aromatic Hydrocarbons," Appendix B, A-489 ------- l,2-DIBROMO-3-CHLOROPROPANE (CAS Number 96-12-8) 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 "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 1 METHOD SUMMARY: 1,2-Dibromo-3-chloropropane (DBCP) in water samples can be determined by gas chromatography with electron-capture dection (GC/ECD). The sample is mixed with ethyl acetate and refluxed 15 minutes or until the ethyl acetate distills over into a trap. The distillate is centrifuged and dried before being analyzed by GC/ECD. The presence of DBCP can be confirmed by gas chromato- graphic/mass spectrometric analysis (GC/MS). INTERFERENCES: No interferences are reported. A-490 ------- QUALITY CONTROL: Samples must be frozen after extraction if the analysis is not to be per- formed immediately. EPA/TECHNICAL STATUS: This method is not EPA-approved. Accuracy information is furnished. The limit of detection is 8 nanograms per liter of sample. REFERENCE: Carter, G. E., Jr.; Riley, M. B. "1,2-Dibromo-3-chloropropane Residues in Water in South Carolina, 1979-80," Pestic. Monit. J., lj>(3), 1981, pp. 139-142. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-100 (list). Water Samples Laboratory Method 2 METHOD SUMMARY: 1,2-Dibromo-3-chloropropane in water samples can be measured by gas chromatography with electron capture detection (GC/ECD). A purge-and-trap apparatus with a 100-milliliter water-jacketed purging flask and an ice jacket around the upper part of the trap is used to collect the analyte from the water, The analyte is desorbed with a hot-air gun as the heat source, and is injected directly into the GC column. For higher levels of analyte, gas chromatography/ mass spectrometry (GC/MS) may be used for the analysis. INTERFERENCES: No interferences are reported. QUALITY CONTROL: A blank and a calibration standard are analyzed with every set of samples. Duplicate and spiked samples are also analyzed. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is not furnished. The limit of detection for the GC/ECD analysis is 10 nanograms per liter; for GC/MS, it is 0.2 micrograms per liter. REFERENCE: Krasner, S. W.; Hwang, C. J.; Cohen, R. S.; McGuire, M. J. "Development of a Volatile Organic Analysis Technique for the Orange-Los Angeles County Reuse A-491 ------- Study" In Chemistry in Water Reuse. Vol. II, Ch. 2; W. J. Cooper, Ed.; Ann Arbor Science: Ann Arbor, 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $90-100 (list), plus sampling costs. A-492 ------- DI-n-BUTYL PHTHALATE (CAS Number 84-74-2) 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 METHOD SUMMARY: Gas chromatography may be used for the analysis of di-n-butyl phthalate in air samples. The analysis is performed by cellulose membrane filtration of a known volume of air, followed by extraction of the filter with carbon disulfide and analysis of the extract by gas chromatography with flame ionization detec- tion (GC/FID). INTERFERENCES: No interferences are reported. QUALITY CONTROL: The analytical method recovery should be determined over the range of interest, and a method blank should be processed with each set of 10 or fewer samples. The method recovery and method blank results 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 1.8 to 9.8 milligrams per cubic meter, in a 30-liter sample. Precision and accuracy information is furnished. A-493 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set D, Method S33; PB-245 935 (NTIS), U.S. DREW: Washington, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S33; 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. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phthalate Esters," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Phthalate Esters," Appendix B. A-494 ------- DICAMBA (CAS Number 1918-00-9) 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 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-495 ------- DICHLOBENIL (CAS Number 1194-65-6) 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 See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Analysis for dichlobenil in soil/sediment samples can be performed by gas chromatography. Samples that have been air-dried at room temperature and stored at -5°C are ultrasonically extracted into 60 milliliters of acetonitrile/ water (9/1). This solution is extracted with hexane. The hexane solution is dried and analyzed by gas chromatography with electron capture detection (GC/ECD), using external standards. 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 furnished. A-496 ------- REFERENCE; Smith, A. E. "A Multi-residue Extraction Procedure for the Gas Chromatographic Determination of the Herbicides Dichlobenil, Dinitramine, Triallate and Tri- fluralin in Soils," J. Chromatogr., 97_, 1974, pp. 103-106. COST INFORMATION: Cost per sample for analysis is approximately $110-160 (list). Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B. A-497 ------- DICHLONE (CAS Number 117-80-6) 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Non-Volatile Organic Compounds," Appendix B, A-498 ------- DICHLOROBENZENE (MIXED) (CAS Number 25321-22-6) 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 See "Chlorobenzene and Dichlorobenzenes," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Volatile Organic Compounds," 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-499 ------- 1,2-DICHLOROBENZENE (CAS Number 95-50-1) 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 "Chlorobenzene and Dichlorobenzenes," 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 determination of 1,2-dichloro- benzene in air. A known volume of air is passed through a charcoal tube, the 1,2-dichlorobenzene is 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: The desorption efficiency must be determined over the range of interest and used to correct for adsorption losses. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and is validated over the range of 150 to 629 milligrams per cubic meter in 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. A-500 ------- REFERENCES; U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set J, Method S135; PB-263 959 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S135; Publication No. 77-157-C, 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 1,2-dichlorobenzene in air samples. The absorbance at 13370 nm (747 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 30 milligrams per cubic meter. 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-501 ------- 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: "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 "Acid and Base/Neutral Extractable Organics," Appendix B. See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. A-502 ------- 1,3-DICHLOROBENZENE (CAS Number 541-73-1) 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 "Chlorobenzene and Dichlorobenzenes," Appendix B. See "Volatile Organic Compounds," Appendix B. 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 1,3-dichlorobenzene in air samples. The absorbance at 12750 nm (784 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. A-503 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. The sensitivity of the method, using a 10-meter pathlength cell, is 30 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: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Aromatic Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Aromatic Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. A-504 ------- 1,4-DICHLOROBENZENE (CAS Number 106-46-7) 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 See "Chlorobenzene and Dichlorobenzenes," 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 1,4-dichlorobenzene 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 chromat- ography with flame ionization detection (GC/FID). INTERFERENCES: High humidity severely decreases the capacity of the sampling apparatus. QUALITY CONTROL: The desorption efficiency must be determined over the range of interest, and 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 is validated over the range of 183 to 777 milligrams per cubic meter in 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. A-505 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T, Method S281; PB-262 404 (NTIS), U.S. DREW: Cincinnati, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S281; 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 1,4-dichlorobenzene in air samples. The absorbance at 9100 nm (1099 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 12 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. A-506 ------- 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. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Aromatic Volatile Organic Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Organic Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. Water Samples Laboratory Method See "Aromatic Volatile Organic Compounds," Appendix B. See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated and Other Organic Contaminants," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Halogenated Organic Compounds," Appendix B. See "Halogenated Volatile Organic Compounds," Appendix B. See "Trace Organic Contaminants," Appendix B. A-507 ------- 3,3'-DICHLOROBENZIDINE (CAS Number 91-94-1) 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 "Aromatic Primary Amines," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: 3,3'-Dichlorobenzidine in air samples may be measured by high-performance liquid chromatography (HPLC). A known volume of air is drawn through a high- efficiency glass-fiber filter and a bed of silica gel to trap the analyte. The 3,3'-dichlorobenzidine is desorbed from the filter and silica gel with a solution of triethylamine in methanol. An aliquot of the extract is injected into an HPLC with a UV detector. INTERFERENCES: 4,4'-Methylenebis(2-chloroaniline) interferes due to the closeness of its retention time to that of the analyte. 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. A-508 ------- 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 140 micrograms per cubic meter in a 50-liter air sample. Precision information is given. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 246; Publication No. 77-157-A, U.S. DREW: Cincinnati, 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. See also: "Benzidine and Congeners," Appendix B. See also: "Hazardous Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Aromatic Amines," Appendix B. Water Samples Laboratory Method See "Aromatic Amines," Appendix B. See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Hazardous Compounds," Appendix B. A-509 ------- DICHLOROBROMOMETHANE (CAS Number 75-27-4) 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 "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. A-510 ------- 1.4-DICHLORO-2-BUTENE (CAS Number 764-41-0) RQ: 0.454 kg SAFETY INFORMATION: Flash point 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-511 ------- DICHLORODIFLUOROMETHANE (CAS Number 75-71-8) 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 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of dichlorodifluoromethane in air samples. The analysis is performed by passage of a known volume of air through two charcoal-tubes in series, followed by desorption of the analyte with methylene chloride 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 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 is validated over the range of 2950 to 10500 milligrams per cubic meter in 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. A-512 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods Set-1, Method Sill; PB-271 712 (NTIS), U.S. DHEW: Washington, 1977- U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method Sill; Publication No. 77-157-B, U.S. DHEW: Cincinnati, April 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 dichlorodifluoromethane in air samples. The absorbance at 10850 nm (922 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. A-513 ------- COST INFORMATION; Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Gaseous Contaminants," 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-514 ------- 1,1-DICHLOROETHANE (CAS Number 75-34-3) RQ: 454 kg SAFETY INFORMATION; Flash point 22°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 1,1-dichloroethane 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 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 210 to 840 milligrams per cubic meter, for a 10-liter sample. The method is capable of measurement of A-515 ------- 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 Methods for Set I, Method S123; PB-265 028 (NTIS), U.S. DREW: Washington, December 1976. 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-dichloroethane in air samples. The absorbance at 9420 nm (1061 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 20 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. A-516 ------- 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," Appoendix 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-517 ------- 1,2-DICHLOROETHANE (CAS Number 107-06-2) RQ: 2270 kg SAFETY INFORMATION: Flash point 56°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 1,2-dichloroethane 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 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 195 to 819 milligrams per cubic meter, using a 3-liter sample. The method is capable of measurement of A-518 ------- 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 S122; PB-263 959 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S122; Publication No. 77-157-B, U.S. DHEW: Cincinnati, April 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 1,2-dichloroethane in air samples. The absorbance at 8180 nm (1222 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 8 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. A-519 ------- 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. 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 Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-520 ------- 1,1-DICHLOROETHYLENE (CAS Number 75-35-4) RQ: 2270 kg SAFETY INFORMATION: Flashpoint 36°F. 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 1,1-Dichloro- ethylene, " Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: 1,1-Dichloroethylene in air samples may be measured by gas chromatog- raphy. A known volume of air is drawn through a charcoal tube. The analyte is desorbed with carbon disulfide, and an aliquot of the resulting solution is analyzed by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES; Any substance that has the same retention time as 1,1-dichloroethylene is an interferent and requires a change in separation conditions. QUALITY CONTROL; One method blank should be processed for every 10 samples. 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 12 milligrams per cubic meter for a 7-liter sample. The limit of detection is 7 micrograms per sample, and A-521 ------- could be lower if the desorption efficiency is adequate. Precision information is furnished. REFERENCE; U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, Method P&CAM 266; Publication No. 78-157, U.S. DREW: Cincinnati, August 1978. 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-dichloroethylene in air samples. The absorbance at 12600 nm (794 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 20 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. A-522 ------- 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 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-523 ------- 1,2-trans-DICHLOROETHYLENE (CAS Number 156-60-5) RQ: 454 kg SAFETY INFORMATION; Flashpoint 36° 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 1,2-trans-dichloroethylene in air may be determined by using a gas detector tube. A 0.1-liter sample is collected and analyzed with a portable pump and a trichloroethylene gas detector tube (Bendix/Gastec® 132H, or equivalent). A positive result is indicated by a color change from yellow to purple in the tube, as it reacts with nascent oxygen to liberate hydrogen chloride, discoloring Hammett indicator. INTERFERENCES: Hydrogen chloride, perchloroethylene, trichloroethylene, 1,2-cis-dichloro- ethylene, and other chlorinated hydrocarbons may also give positive results. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 40 to 2000 milligrams per cubic meter- REFERENCE: Bendix Corp., Bendix Gastec Precision Gas Detector System Manual (Blue Book), Bendix: Largo, Florida. 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-524 ------- Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of 1,2-trans-dichloro- ethylene in air samples. The analysis may be performed by passage of 3 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 calcu- lation of the results. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and has been validated over the range of 475 to 1900 milligrams per cubic meter, using a 3-liter sample of air. 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 H, Method S110; PB-265 027 (NTIS), U.S. DHEW: Washington, January 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S110; Publication No. 77-175-B, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list) (1983) plus sampling costs. Air Samples Laboratory Method 2 A-525 ------- METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of 1,2-trans-dichloroethylene in air samples. The absorbance at 12050 nm (830 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 t\he 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 8 milligrams per cubic meter or 2 parts per million. No percision or accuracy information is furnished. REFERENCE: American Public Health Asociation, "Infrared Absorption Spectroscopy" In Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 79-8A. 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. 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-526 ------- 2,4-DICHLOROPHENOL (CAS Number 120-83-2) 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 "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 "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. A-527 ------- 2,6-DICHLOROPHENOL (CAS Number 87-65-0) 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 "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Phenols," Appendix B. Water Samples Laboratory Method See "Phenolic Compounds," Appendix B. See "Phenolics," Appendix B. See "Phenols," Appendix B. A-528 ------- RQ: 454 kg SAFETY INFORMATION: DICHLOROPROPANE (CAS Number 26638-19-7) Flash point 60° 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 "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 "Halogenated Volatile Organic Compounds," Appendix B, See "Volatile Organic Compounds," Appendix B. A-529 ------- 1,2-DICHLOROPROPANE (CAS Number 78-87-5) RQ: 454 kg SAFETY INFORMATION; Flash point 60°F. 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 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of 1,2-dichloropropane 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 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 135 to 665 milligrams per A-530 ------- cubic meter for a 10-liter sample. Precision and accuracy information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set G, Method S95; PB-265 026 (NTIS), U.S. DREW: Washington, December 1976. 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: 1,2-Dichloropropane in air samples can be measured by gas chromatography- A known volume of air is drawn through a tube containing petroleum-based charcoal. The analyte is desorbed with 15 percent (v/v) acetone in cyclohexane, and an aliquot is injected into a gas chromatograph equipped with a Hall electrolytic condutivity detector (GC/HECD). INTERFERENCES: To separate isomers and other compounds likely to be sampled along with 1,2-dichloropropane, different operating conditions may be required. QUALITY CONTROL: One method blank is processed for every 10 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 0.124 to 128 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 P&CAM 321; Publication No. 80-125, U.S. DHHS: Cincinnati, August 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. A-531 ------- See also: "Fumigants," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. Air Samples Laboratory Method 3 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of 1,2-dichloropropane in air samples. The absorbance at 9800 nm (1020 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. INTERFERNCES: 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 46 milligrams per cubic meter or 15 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 See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-532 ------- Water Samples Laboratory Method See "Halogenated Volatile Organic Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B, See "Volatile Organic Compounds," Appendix B. A-533 ------- DICHLOROPROPANE-DICHLOROPROPENE MIXTURE (CAS Number 8003-19-8) RQ: 45.4 kg SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. See methods for Dichloropropane and for Dichloropropene (Appendix A). A-534 ------- DICHLOROPROPENE (CAS Number 26952-23-8) 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 "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-535 ------- 1,3-DICHLOROPROPENE (CAS Numbers 542-75-6, 10061-01-5, 10061-02-6) RQ: 45.4 kg SAFETY INFORMATION: Flash point 95°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 "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-536 ------- 2,2-DICHLOROPROPIONIC ACID (CAS Number 75-99-0) 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 METHOD SUMMARY: Determination of 2,2-dichloropropionic acid in soil/sediment samples can be performed by gas chromatography. A 10-gram sample is extracted with 50 milliliters of 0.1-molar sodium hydroxide, and the extract is filtered, concen- trated, and esterified by dissolution in n-butanol, addition of sulfuric acid, and heating. After cooling, water is added and the resulting solution is extracted with 2,2,4-trimethylpentane. The organic extract is analyzed by gas chromatography with electron capture detection (GC/ECD). INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. A-537 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. The method is applicable to levels of 2,2-dichloropropionic acid above 50 micrograms per kilogram. Precision and accuracy information is furnished. REFERENCE: Cotterill, E. G."Determination of Residues of Dalapon in Soil by Gas Chromatog- raphy of the 1-Butyl Ester," J Chromatogr., 106(2), 1975, pp. 409-411. COST INFORMATION: Cost per sample for analysis by this method is approximately $155-220 (list). Water Samples Laboratory Method A-538 ------- DICHLORVOS (CAS Number 62-73-7) 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 METHOD SUMMARY: Analysis for dichlorvos 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 phosphoric acid ester gas detector tube (Draeger® 67 28461, or equiva- lent). A positive result is indicated by the absence of a color change in the tube from grayish-white to blue. The test is based on suppression of cholines- terase activity by dichlorvos. INTERFERENCES: Other phosphoric acid esters will also give positive results. QUALITY CONTROL: A blank test should be carried out in parallel with each sample. SENSITIVITY: The detector tube will indicate if more than 0.2 milligrams per cubic meter of dichlorvos is present. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). Soil/Sediment Samples Field Method A-539 ------- Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. Air Samples Laboratory Method Note; N10SH Method P & CAM 295 (adsorption on XAD-2 resin, desorption with toluene, analysis by GC/FPD) is applicable. (Reference furnished by reviewer). See also:"Organophosphorus Compounds," Appendix B. See also:"Organophosphorus Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus and Carbamate Insecticides," Appendix B. 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-540 ------- DIELDRIN (CAS Number 60-57-1) 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 METHOD SUMMARY: Gas chromatography may be used for the analysis of air samples for dieldrin. The analysis is performed by passage of a known volume of air through a glass fiber filter followed by extraction of the analyte with iso- octane. An aliquot of the resulting solution is injected into a gas chromato- graph with electrolytic conductivity detection. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: Method blanks and standards are 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 0.12 to 0.59 milligrams per cubic meter in a 170-liter sample. Precision and accuracy information is furnished. A-541 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T. Method S283; PB-262 404 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S283; 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: "Chlorinated Pesticides," Appendix B. See also: "Pesticide Residues," 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 "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-542 ------- 1,2:3,4-DIEPOXYBUTANE (CAS Number 1464-53-5) 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 "Hazardous Organic Emissions," Appendix B, Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-543 ------- DIETHYLAMINE (CAS Number 109-89-7) RQ: 454 kg SAFETY INFORMATION; Flash point -9°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 "Amines: Triethylamine and Other Amines," 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 diethylamine in air samples. The analysis may be performed by passage of a known volume of air through a silica gel tube sampling device, followed by desorption of the analyte with 0.2-N sulfuric acid in 10-percent 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: 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 has been validated over the range of 38 to 165 milli- A-544 ------- grams per cubic meter, in a 50-liter sample. The method is capable of measure- ment 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 S139; PB-263 959 (NTIS), U.S. DREW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Anaytical Methods, 2nd ed., Vol. 3, Method S139; Publication No. 7-175-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 diethylamine in air samples. The absorbance at 8700 nm (1149 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 31 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-545 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. See also: "Aliphatic Amines," Appendix B. See also: "Low Molecular Weight Aliphatic Amines," 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-546 ------- N,N'-DIETHYLHYDRAZINE (CAS Number 1615-80-1) 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-547 ------- 0,0-DIETHYL-S-METHYL DITHIOPHOSPHATE (CAS Number 3288-58-2) 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 "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-548 ------- DIETHYL-£-NITROPHENYL PHOSPHATE (CAS Number 311-45-5) 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 METHOD SUMMARY: Diethyl-p-nitrophenyl phosphate can be detected in water samples by use of a strip test. The paper strip is impregnated with a cholinesterase-buffer solution. The paper is wetted with the analyte-containing sample and then with an Ellman's reagent-butyryl-thiocholine mixture. After 5 minutes, the test strip is compared to a blank strip that has been treated the same way except that the water sample applied did not contain diethyl-jp-nitrophenyl phosphate or any other cholinesterase inhibitor- If the blank strip is a more intense yellow than the test strip, the test is positive. INTERFERENCES: Any cholinesterase-inhibiting organophosphorus or carbamate compound would be expected to react positively to this test. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: The method is suitable for concentrations of diethyl-p-nitrophenyl phos- phate above approximately 2 micrograms per liter. REFERENCE: Breuer, H. "Sensitive and Rapid Detection of Paraoxon by Thin-Layer Chromato- graphy and Strips Using Enzyme Inhibition and Ellman's Method," J. Chromatogr., 243, 1982, pp. 183-187. A-549 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $6-11 (list). Air Samples Laboratory Method See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Pesticides," Appendix B. See "Phosphorus," Appendix B. A-550 ------- DIETHYL PHTHALATE (CAS Number 84-66-2) RQ: 454 kg SAFETY INFORMATION: Potentially chronically toxic. Flash point: 325°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: Phthalate esters in particulate air samples can be measured by gas chromatography/mass spectrometry (GC/MS). The particulate sample is collected on a glass fiber filter in a high-volume sampling unit. The sample is extracted with benzene and by further separations, the acidic and basic frac- tions are removed. The neutral fraction is analyzed by GC/MS. Phthalate esters can be specifically and sensitively determined from the mass chromato- gram. INTERFERENCES: Some phthalate esters may be lost to the acidic fraction during extraction. There is a complete absence of interferences with respect to quantitative determination from the mass chromatogram. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is not furnished. A-551 ------- REFERENCE: Cautreels, W.; Van Cauwenberghe, K. "Determination of Organic Compounds in Airborne Particulate Matter by Gas Chromatography-Mass Spectrometry," Atmos. Environ., 10, 1976, pp. 447-457. COST INFORMATION; Cost per sample or analysis by this method is approximately $355-400 (list), plus sampling costs. See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phthalate Esters," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Phthalate Esters," Appendix B. See "Trace Organic Contaminants," Appendix B. A-552 ------- 0,0-DIETHYL-O-PYRAZINYL PHOSPHOROTHIOATE (CAS Number 297-97-2) RQ: 45.4 kg SAFETY INFORMATION: Exhibits toxlclty. 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 0 ,0-diethyl-0_-pyrazinyl phosphorothioate can be per- formed spectrometrically. For sampling the gaseous phase, bubblers containing aqueous sodium hydroxide and isopropanol are used. After sampling, more isopropanol is added and solution is allowed to stand 17 to 21 hours at 40°C. For sampling particulates, the air is drawn through a glass-fiber filter, which is then broken up in the aqueous sodium hydroxide/isopropanol solution and allowed to hydrolyze. The solutions are cooled to about 15°C, centrifuged or filtered, and heated with acetic acid, bromine water, a phenol- bromide solution, and finally with a p-phenylenediamine hydrochloride solution. The solution is allowed to stand 30 minutes at 40°C, and then its absorbance is read at 465 nm. INTERFERENCES; No significant interferences are reported. QUALITY CONTROL: Factors for collection efficiency when sampling with a bubbler, and for recovery efficiency when sampling with a glass-fiber filter should be included in the calculation of the results. SENSITIVITY: This method is suitable for the determination of the analyte at concentra- tions of about 0.1 milligrams per cubic meter of air. REFERENCE: Lloyd, G. A.; Bell, G. J. "Mobile Laboratory Methods for the Determination of Pesticides in Air, Part II, Thionazin," Analyst, 9±, 1966, pp. 808-809. COST INFORMATION: Cost per sample for analysis by this method is approximately $35-65 (list), plus sampling costs. A-553 ------- Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B, A-554 ------- DIETHYLSTILBESTROL (CAS Number 56-53-1) 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 See "Hazardous Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method See "Hazardous Compounds," Appendix B. A-555 ------- DIHYDROSAFROLE (CAS Number 94-58-6) 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-556 ------- DIISOPROPYL FLUOROPHOSPHATE (CAS Number 55-91-4) 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 See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-557 ------- DIMETHOATE (CAS Number 60-51-5) 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 See "Phosphorodithioates," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 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-558 ------- 3,3'-DIMETHOXYBENZIDINE (CAS Number 119-90-4) 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 See "Aromatic Primary Amines," Appendix B. See "Benzidine and Congeners," Appendix B. See "Hazardous Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Aromatic Amines," Appendix B. Water Samples Laboratory Method See "Aromatic Amines," Appendix B. See "Benzidine and Congeners," Appendix B. See "Hazardous Compounds," Appendix B. A-559 ------- DIMETHYLAMINE (CAS Number 124-40-3) RQ: 454 kg SAFETY INFORMATION; Potentially chronically toxic. 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. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used in the analysis for diethylamine in air samples. The analysis may be performed by passage of a known volume of air through a silica gel-tube sampling device, followed by desorption of the analyte with 0.2-N sulfuric acid in 10-percent 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: 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 has been validated over the range of 7 to 30 milli- grams per cubic meter, using a 48-liter sample. The method is capable of A-560 ------- 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 S142; PB-263 959 (NTIS), U.S. DHEW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Anaytical Methods, 2nd ed., Vol. 3, Method S142; Publication No. 77-175-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: "Aliphatic Amines," Appendix B. See also: "Hazardous Organic Emissions," Appendix B. See also: "Low Molecular Weight Aliphatic Amines," Appendix B. See also: "Methylamines," 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-561 ------- DIMETHYLAMINOAZOBENZENE (CAS Number 60-11-7) 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 METHOD SUMMARY: Spectrophotometry may be used to analyze air samples for dimethylaminoazo- benzene. Samples are collected by glass-fiber filtration of air, then reacted with a p-nitrosophenol/sulfuric acid solution to produce a blue color- The intensity of the blue color is proportional to the concentration of dimethyl- aminoazobenzene in the sample and is determined by Spectrophotometry at a wave- length of 604 or 672 nm. INTERFERENCES: No interferences are reported. QUALITY CONTROL: A blank should be analyzed with each sample. SENSITIVITY: This method may be used to analyze samples containing 10 to 300 micrograms of dimethylaminoazobenzene. REFERENCE: Sawicki, E.; Hauser, T. R.; Stanley, T. W.; Elbert, W.; Fox, F. T. "Spot Test Detection and Spectrophotometric Characterization and Determination of Carbazoles, Azo Dyes, Stilbenes, and Schiff Bases," Anal Chem. 33_(11), 1961, pp. 1574-1579. COST INFORMATION: The cost per sample for analysis by this method is approximately $12-20 (list), plus sampling costs. Soil/Sediment Samples Field Method Water Samples Field Method A-562 ------- Air Samples Laboratory Method METHOD SUMMARY: Dimethylaminoazobenzene in air samples can be measured by gas chromato- graphy. A known volume of air is drawn through a two-stage sampler consisting of a high-efficiency glass-fiber filter and a bed of Gas-Chrom P to collect the analyte aerosol and/or vapor- The dimethylaminoazobenzene is desorbed with 2- propanol, and an aliquot of the solution is injected into a gas chromatograph with a flame ionization detector (GC/FID). INTERFERENCES: 4-Aminoazobenzene interferes since it has the same retention time as the analyte. 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/TECHICAL STATUS: This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 4 to 2000 micrograms per cubic meter, with a 50-liter sample. Precision information is furnished. The detection limit is 1.0 microgram per cubic meter. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, Method P&CAM 284; Publication No. 78-175, U.S. DHEW: Cincinnati, August 1978. COST INFORMATION: Cost per sample for analyses by this method is approximately $70-90 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-563 ------- 7,12-DIMETHYLBENZ[a]ANTHRACENE (CAS Number 57-97-6) 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-564 ------- 3,3'-DIMETHYLBENZIDINE (CAS Number 119-93-7) 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 "Benzidine and Congeners," Appendix B. See "Hazardous Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Benzidine and Congeners," Appendix B. See "Hazardous Compounds," Appendix B. A-565 ------- a,a-DIMETHYLBENZYLHYDROPEROXIDE (CAS Number 80-15-9) 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-566 ------- DIMETHYLCARBAMOYL CHLORIDE (CAS Number 79-44-7) 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 METHOD SUMMARY; Dimethylcarbamoyl chloride in air samples can be measured by gas chromato- graphy with Hall electrolytic conductivity detection (GC/HECD). The analyte is adsorbed on Tenax® GC and thermally desorbed into the GC/HECD instrument, with the detector operating in the chlorine mode. INTERFERENCES: To avoid decomposition of the analyte, an all-glass system must be used. No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Accuracy information is furnished. The detection limit is approximately 0.2 micrograms per cubic meter. REFERENCE: Matienzo, L. V.; Hensler, C. J. "Determination of N,N-Dimethylcarbamoyl Chloride (DMCC) in Air," Am. Ind. Hyg. Assoc. J. 43(11), 1982, pp.838-844. A-567 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $100 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-568 ------- 1,1-DIMETHYLHYDRAZINE (CAS Number 57-14-7) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Flash point 5°F. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method See "Hydrazines and Other Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Hydrazines," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Analysis for 1,1-dimethylhydrazine in air is performed by collection of analyte from a known volume of air with a midget bubbler charged with dilute hydrochloric acid, followed by addition of phosphomolybdic acid to form a bluish-green colored complex and colorimetric analysis of the resulting solu- tion at 730 nm. INTERFERENCES: Reducing agents, such as tin(II), iron(II), zinc, sulfur dioxide, and hydrogen sulfide, interfere. Other hydrazine derivatives may interfere, as may oxidizing agents. QUALITY CONTROL: A method blank should be processed with each set of 10 samples, and the results used 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 0.5 to 2.2 milligrams per A-569 ------- cubic meter in a 20-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set K, Method S143; PB-254 227 (NTIS), U.S. DREW: Washington, April 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S143: Publication No. 77-157-C, U.S. DHEW: Cincinnati, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $20-25 (list), plus sampling costs. See also: "Halogenated, Aromatic and Other Compounds," Appendix B. See also: "Hydrazines," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-570 ------- 1,2-DIMETHYLHYDRAZINE (CAS Number 540-73-8) 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 "Hydrazines and Other Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Hydrazines," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-571 ------- 0,0 -DIMETHYLPHENETHYLAMINE (CAS Number 122-09-8) 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 Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-572 ------- 2,4-DIMETHYLPHENOL (CAS Number 105-67-9) 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 "Phenolic Compounds," Appendix B. 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 "Base/Neutral Extractable Organic Compounds," Appendix B. See "Non-Volatile Organic Compounds," Appendix B. See "Organic Compounds," Appendix B. See "Phenols," Appendix B. A-57 3 ------- DIMETHYL PHTHALATE (CAS Number 131-11-3) 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 "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phthalate Esters," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Phthalate Esters," Appendix B. See "Trace Organic Contaminants," Appendix B. A-574 ------- DIMETHYL SULFATE (CAS Number 77-78-1) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (inhalation). 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; Analysis for dimethyl sulfate may be performed by use of a detector tube. A 0.2- to 2.2-liter air sample is collected and analyzed with a hand- operated bellows pump and a dimethyl sulfate gas detector tube (Draeger® 67 18701 or equivalent). A positive result is indicated by a color change from white to blue in the tube. INTERFERENCES: Other organic alkylating agents may also cause discolorations. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 1 to 25 milligrams per liter. REFERENCES: National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations and Technical Gas Analysis with Draeger® Tubes", 4th ed.; National Draeger: Pittsburgh, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-575 ------- Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method See "Sulfates (Particulate)," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-576 ------- DINITROBENZENE, MIXED (CAS Number 25154-54-5) RQ: 45.4 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 "Dinitrobenzenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Nitroaromatics and Cyclic Ketones," Appendix B. Water Samples Laboratory Method See "Nitroaromatics," Appendix B. See "Nitroaromatics and Cyclic Ketones," Appendix B, A-577 ------- m-DINITROBENZENE (CAS Number 99-65-0) 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 "Dinitrobenzenes," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitroaromatics," Appendix B. A-578 ------- o-DINITROBENZENE (CAS Number 528-29-0) 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 "Dinitrobenzenes," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitroaromatics," Appendix B. See "Non-Volatile Organic Compounds," Appendix B. A-579 ------- £-DINITROBENZENE (CAS Number 100-25-4) 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 "Dinitrobenzenes," Appendix B. See "Nitroaromatic Compounds and Benzonitrile," Appendix B, Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Nitroaromatics," Appendix B. See "Non-Volatile Organic Compounds," Appendix B, A-580 ------- 4,6-DINITRO-o-CRESOL AND SALTS (CAS Number 534-52-1) RQ: 4.54 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 "Phenolic Compounds," Appendix B. Air Samples Laboratory Method Note: NIOSH Method S166 (filter and bubbler collection, ethylene glycol extraction, analysis by HPLC) is applicable. (Reference supplied by reviewer). 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 "Phenols," Appendix B. A-581 ------- 4,6-DINITRO-£-CYCLOHEXYLPHENOL (CAS Number 131-89-5) 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 "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Phenols," Appendix B. Water Samples Laboratory Method See "Phenols," Appendix B. A-582 ------- DINITROPHENOL (CAS Number 25550-58-7) RQ: 45.4 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 See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method See "Phenols," Appendix B, Water Samples Laboratory Method See "Phenols," Appendix B. A-583 ------- 2,4-DINITROPHENOL (CAS Number 51-28-5) 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 See "Phenolic Compounds," Appendix B. 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 "Phenols," Appendix B. A-584 ------- 2,5-DINITROPHENOL (CAS Number 329-71-5) 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 See "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Phenolics," Appendix B. A-585 ------- 2,6-DINITROPHENOL (CAS Number 573-56-8) 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 "Phenolic Compounds," Appendix B. Air Samples Laboratory Method See "Phenolics," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Phenolics," Appendix B. A-586 ------- DINITROTOLUENE (CAS Number 25321-14-6) RQ: 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 METHOD SUMMARY: Dinitrotoluene in air samples can be measured by high-performance liquid chromatography (HPLC). A known volume of air is drawn through a mixed cellulose ester membrane filter connected in series to a midget bubbler containing 10 milliliters of ethylene gylcol. After collection of the sample, the filter is placed in the bubbler flask and 5 milliliters of methanol are added. The resulting solution is analyzed by HPLC with UV detection. INTERFERENCES: Any compound that has the same retention time as dinitrotoluene is an interferent. QUALITY CONTROL: Since no internal standard is used in this method, a standard solution must be analyzed at the same time as the sample. A correction for the blank must be made, as well as a correction for analytical method recovery, for each sample. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH). and validated over the range of 0.90 to 5.0 milligrams per A-587 ------- cubic meter, using a 90-liter sample. Precision and accuracy information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, Method S215; Publication No. 78-175, U.S. DREW: Cincinnati, August 1978. COST INFORMATION: Cost per sample for analysis by this method is approximately $110 (list), plus sampling costs. See also: "Dinitrotoluenes," Appendix B. Soil/Sediment Samples Laboratory Method See "Nitroaromatics and Cyclic Ketones," Appendix B. Water Samples Laboratory Method See "Explosives," Appendix B. See "Nitroaromatics," Appendix B. A-588 ------- 2,4-DINITROTOLUENE (CAS Number 121-14-2) RQ: 45.4 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 "Dinitrotoluenes," 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 "Explosives," Appendix B. See "Nitroaromatics," Appendix B. A-589 ------- 2,6-DINITROTOLUENE (CAS Number 606-20-2) RQ: 454 kg SAFETY INFORMATION: Exhibits chronic toxicity. 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 "Dinitrotoluenes," 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 "Nitroaromatics," Appendix B. A-590 ------- DINOSEB (CAS Number 88-85-7) 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 "Phenolic Compounds," Appendix B. 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-591 ------- Di-n-OCTYL PHTHALATE (CAS Number 117-84-0) 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 "Acid and Base/Neutral Extractable Organics," Appendix B. See "Phthalate Esters," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B, See "Phthalate Esters," Appendix B. A-592 ------- 1,4-DIOXANE (CAS Number 123-91-1) RQ: 0.454 kg SAFETY INFORMATION: Flash point 54°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: Field detection of dioxane can be accomplished by passage of air through a potassium dichromate solution at a rate of 10 to 15 liters per hour until a color change occurs. This method is highly non-specific, as it will respond to any substance present that can be oxidized by the dichromate solution. This method is described by Chemdanova, L. S. "Determination of Small Quantities of Dioxane in the Atmosphere of Industrial Establishments," Gig. Sanit., 13(11), 1948, p. 81, and is summarized in the references given below. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: No sensitivity information is furnished. REFERENCES: Chem. Abstr., 1949, 43:8976f. Chemical Detection of Gaseous Pollutants; W. E., Ruch, Ed.; Ann Arbor Science: Ann Arbor, 1967. COST INFORMATION: Cost per sample for analysis by this method is essentially totally due to sampling costs. See also: "Ethylene Oxide, 1,4-Dioxane, and Propylene Oxide," Appendix B. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method A-593 ------- Air Samples Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used in the analysis for 1,4-dioxane in air samples. The analysis is performed by passage of 10 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 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 155 to 650 milligrams per cubic meter in 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 G, Method S360; PB-265 026 (NTIS), U.S. DHEW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S360; 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 1,4-dioxane in air samples. The absorbance at 8800 nm (1136 cm"1) is measured, using a 10-meter pathlength cell. Air can be sampled in a Saran or A-594 ------- 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 59 milligrams per cubic meter or 20 parts per million. No precision or accuracy information is furnished. REFERENCES; 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: "Volatile Alcohols and Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-595 ------- 1,2-DIPHENYLHYDRAZINE (CAS Number 122-66-7) 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 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-596 ------- DIPROPYLAMINE (CAS Number 142-84-7) RQ: 2270 kg SAFETY INFORMATION: Flash point 63°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 "Primary and Secondary Amines," Appendix B. Water Samples Laboratory Method See "Amines," Appendix B. See "Primary and Secondary Amines," Appendix B. A-597 ------- DIQUAT (CAS Numbers 85-00-7, 2764-72-9) 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 Soil/Sediment Samples Field Method Water Samples Field Method See "Halides, Cyanides, and Other Compounds," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Gas chromatography may be used to analyze soil/sediment samples for diquat. A 20-gram sample is air-dried, pulverized, and refluxed with concentrated sul- furic acid for 5 hours. The extract is hydrogenated, using a platinum dioxide catalyst, extracted with methylene chloride, concentrated, and extracted into hexane. The hexane extract is then concentrated and analyzed by gas chromato- graphy with either flame ionization detection (GC/FID) or alkali flame ioniza- tion detection (GC/AFID). INTERFERENCES: No interferences are reported. QUALITY CONTROL: Samples should be analyzed in duplicate, and hydrogenated standards should also be analyzed. A-598 ------- EPA/TECHNICAL STATUS; This method is not EPA-approved. This method is sensitive to diquat con- centration levels as low as approximately 0.01 parts per million. Precision and accuracy information is furnished. REFERENCE; Khan, S. U. "Determination of Diquat and Paraquat Residues in Soil by Gas Chromatography," J. Agric. Food Chem., 22/5), 1974, pp. 863-867. COST INFORMATION: Cost per sample for analysis by the GC/FID method is approximately $160- 290 (list). Water Samples Laboratory Method METHOD SUMMARY: Diquat can be measured in water samples by pyrolysis followed by gas Chromatography. Silica tubes must be used to contain the samples for pyrolysis, and glass Chromatography columns are required. INTERFERENCES: The herbicide may adsorb onto the glass surfaces of the vessels used. QUALITY CONTROL; Sampling should be carried out in the vessels subsequently used for the analytical determination. Samples should be treated identically to standard solutions used for calibration purposes. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. REFERENCE: Cannard, A.J.; Griddle, W. J. "A Rapid Method for the Simultaneous Determination of Paraquat and Diquat in Pond and River Waters by Pyrolysis and Gas Chromatography," Analyst, 100, 1975, pp. 848-853. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-100 (list). A-599 ------- DISULFOTON (CAS Number 298-04-4) RQ: 0.454 kg SAFETY INFORMATION; Exhibits toxicity (oral, dermal). 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 See "Phosphorodithioates," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Cholinesterase-Inhibiting Compounds," Appendix B. 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 "Non-Volatile Organic Compounds," Appendix B. See "Organochlorine and Organophsophorus Pesticides," Appendix B. See "Organophosphorus Pesticides," Appendix B. A-600 ------- 2,4-DITHIOBIURET (CAS Number 541-53-7) 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 Water Samples Laboratory Method A-601 ------- DIURON (CAS Number 330-54-1) 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 METHOD SUMMARY: Diuron and other phenylamide pesticides in water samples can be measured colorimetrically. The sample is hydrolyzed by sulfuric acid to produce corre- sponding anilines, which are extracted with chloroform, diazotized, and reacted with naphthol to produce azo dyes. Absorbance is measured at wavelengths of maximum absorption and compared with standards. (This method is described by El-Dib, M; Aly, 0. J. Assoc. Off. Anal. Chem., 55 (6), 1972, pp. 1276-1279, and summarized in the reference given below.) INTERFERENCES: Phenylamides may be analyzed in the presence of anilines. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for phenylamide concentrations above 0.02 milligrams per liter. REFERENCE: Simons, J. Bibliography on Hazardous Materials Analysis Methods, EPA 600/2- 81-0-94; U. S. Environmental Protection Agency: Cincinnati, June 1981, p. 4. A-60 2 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $45-75 (list). Air Samples Laboratory Method See "Diuron and Pyrethrins," Appendix B. Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Diuron in soil samples can be measured by gas chromatography with flame ionization detection (GC/FID). The sample is refluxed in 20-percent sodium hydroxide and then distilled. The distillate is acidified, washed with hexane or methylene chloride, made slightly alkaline, and extracted with hexane or methylene chloride. The sample is concentrated and analyzed by GC. INTERFERENCES: Neburon produces the same 3,4-dichloroaniline peak that identifies diuron. Incomplete separation of unknown materials may limit sensitivity. QUALITY CONTROL: Calibration factors are determined daily by analyzing a standard solution in hexane. EPA/TECHNICAL STATUS: This method is not EPA-approved. No precision or accuracy information is furnished. REFERENCE: Lowen, W. R.; Bleidner, W. E.; Kirkland, J. J.: Pease, H. L. In Analytical Methods for Pesticides, Plant Growth Regulators, and Food Additives; Zweig, G., Ed.; Academic Press: New York, 1964, Vol. IV, pp. 157-170^. COST INFORMATION: Cost per sample for analysis by this method is approximately $120-200 (list). Water Samples Laboratory Method A-603 ------- METHOD SUMMARY: Determination of diuron in water samples can be performed by thin-layer chromatography. A 1-liter sample is extracted with dichloromethane and the extract is dried, concentrated, cleaned up by a Florisil® column, and analyzed by thin-layer chromatography with visualization through formation of diazonium salts and reaction with naphthol. Semi-quantitative measurement is made by visual comparison of color intensity with that of standards. INTERFERENCES: Aromatic amines can interfere and may be eliminated by the use of a different solvent system. QUALITY CONTROL; Duplicate, spiked, and performance evaluation samples should be analyzed regularly, and quality control charts should be used as a check on the analyti- cal system. EPA/TECHNICAL STATUS: This method is EPA-approved for National Pollutant Discharge Elimination System (NPDES) analyses. Precision and accuracy information is not furnished. REFERENCE: U.S. Environmental Protection Agency, Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol, and Pesticides in Water and Wastewater Interim Report, U.S. EPA: Washington, September 1978, pp. 104-113. COST INFORMATION: Cost information has not been obtained. See also: "Carbamate and Urea Pesticides," Appendix B. See also: "Thioic Acid Ester Pesticides," Appendix B. A-604 ------- DODECYLBENZENESULFONIC ACID (CAS Number 27176-87-0) 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-605 ------- ENDOSULFAN (CAS Numbers 115-29-7) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (oral). 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 "Polychlorinated Biphenyls and Chlorinated Pesticides," Appendix B. Air Samples Laboratory Method See "Chlorinated Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," 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 Pesticides," Appendix B. See "Organochlorine Pesticides and PCB's," Appendix B. A-606 ------- a-ENDOSULFAN (CAS Number 959-98-8) RQ: 0.454 kg SAFETY INFORMATION; Exhibits toxicity (oral). 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 "Polychlorinated Biphenyls and Chlorinated Pesticides," Appendix B. Air Samples Laboratory Method See "Chlorinated Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method 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 and PCB's," Appendix B. See "Pesticides," Appendix B. A-607 ------- &-ENDOSULFAN (CAS Number 33213-65-9) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity (oral). 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 "Polychlorinated Biphenyls and Chlorinated Pesticides," Appendix B. Air Samples Laboratory Method See "Chlorinated Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method 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 and PCB's," Appendix B. See "Pesticides," Appendix B. A-608 ------- ENDOSULFAN SULFATE (CAS Number 1031-07-8) 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 See "Polychlorinated Biphenyls and Chlorinated Pesticides," Appendix B. Air Samples Laboratory Method 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 Pesticides and PCB's," Appendix B. A-609 ------- ENDOTHALL (CAS Number 145-73-3) 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 METHOD SUMMARY: Endothall in soil/sediment samples can be measured by gas chromatography with nitrogen-specific detection. The sample is suction-filtered to remove excess water, extracted with acetic anhydride, then suction-filtered again. The filtrate is concentrated, water is added, and the solution is extracted, first with carbon disulfide, then with chloroform. Acetic acid is added to the aqueous phase, followed by a concentration step. The endothall is converted to its N-chloroethylimide by reaction with 2-chloroethylamine hydrochloride. The imide derivative is extracted into chloroform, which is evaporated almost to dryness. The residue is dissolved in methanol and the solution is analyzed by GC. INTERFERENCES: No interferences are reported. QUALITY CONTROL: Samples are run in duplicate. A-610 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. REFERENCE; Sikka, H. C.; Rice, C. P- "Persistence of Endothall in Aquatic Environment as Determined by Gas-Liquid Chromatography," J. Agric. Food Chem.. 21(5), 1973 pp. 842-846. — COST INFORMATION: Cost per sample for analysis by this method is approximately $265-310 (list), plus sampling costs. Water Samples Laboratory Method METHOD SUMMARY: Endothall in water samples can be measured by gas chromatography with nitrogen-specific detection. The sample is acidified and concentrated, then the endothall is converted to its N-chloroethylimide by reaction with 2-chloro- ethylamine hydrochloride. The imide derivative is extracted into chloroform, which is evaporated almost to dryness. The residue is dissolved in methanol and the solution is analyzed by GC. INTERFERENCES: No interferences are reported. QUALITY CONTROL: Samples are run in duplicate. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. The limit of detection is 10 micrograms per liter of water. REFERENCE: Sikka, H. C.; Rice, C. P- "Persistence of Endothall in Aquatic Environment as Determined by Gas-Liquid Chromatography," J. Agric. Food Chem., 2_1(5), 1973, pp. 842-846. COST INFORMATION: Cost per sample for analysis by this method is approximately $200-245 (list), plus sampling costs. A-611 ------- ENDRIN (CAS Number 72-20-8) RQ: 0.454 kg SAFETY INFORMATION: Exhibits toxicity. 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 "Polychlorinated Biphenyls and Chlorinated Pesticides," Appendix B. Air Samples Laboratory Method METHOD SUMMARY: Endrin in air samples can be measured by gas chromatography- A known volume of air is drawn through a 37-millimeter mixed cellulose ester filter (MCEF) followed by a tube containing Chromosorb® 102 to trap the endrin. The analyte is desorbed from the filter and sorbent with toluene and an aliquot of the extract is injected into a gas chromatograph equipped with an electron capture detector (GC/ECD). 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 0.06 to 0.31 milligrams per cubic meter in a 120-liter sample. Precision and accuracy information is furnished. A-612 ------- REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol. 6, Method S284; Publication No. 80-125, U.S. DHHS: Cincinnati, August 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-100 (list), plus sampling costs. See also: "Chlorinated Pesticides," Appendix B. See also: "Pesticide Residues," 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 "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-613 ------- ENDRIN ALDEHYDE (CAS Number 7421-93-4) 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 See "Chlorinated Pesticides," 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 Pesticides and PCB's," Appendix B. A-614 ------- EPICHLOROHYDRIN (CAS Number 106-89-8) RQ: 454 kg SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic. Flash point 91°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 epichlorohydrin in air 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 an epichlorohydrin gas detector tube (Draeger® 67 28111, or equivalent). A positive result is indicated by a color change in the tube from pale gray to pale yellowish-orange, as the analyte reacts with chromate ion and o-tolidine. INTERFERENCES: Other easily-cleaved, 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 20 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, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-615 ------- See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method 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 epichlorohydrin 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 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 12 to A3 milligrams per cubic meter, using a 20-liter sample of air. The method is capable of measure- ment 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 I, Method S118; PB-265 028 (NTIS), U.S. DHEW: Washington, December 1976. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S118; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. A-616 ------- 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 epichlorohydrin in air samples. The absorbance at 13360 nm (748 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 76 milligrams per cubic meter or 20 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. also: "Hazardous Organic Emissions," Appendix B. A-617 ------- Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-618 ------- EPINEPHRINE (CAS Number 51-43-4) 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 Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B, Water Samples Laboratory Method A-619 ------- ETHION (CAS Number 563-12-2) RQ: 4.54 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 Pesticides," Appendix B. Air Samples Laboratory Method See "Pesticide Residues," Appendix B. Soil/Sediment Samples Laboratory Method See "Organochlorine Pesticides and PCB's," Appendix B. 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-620 ------- ETHYL ACETATE (CAS Number 141-78-6) RQ: 2270 kg SAFETY INFORMATION: Flash point 24°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 ethyl acetate in air 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 an ethyl acetate gas detector tube (Draeger® CH 20201, or equivalent). A positive result is indicated by a color change in the tube from orange to brownish-green. The test is based on the reaction of ethyl acetate with chromosulfuric acid. INTERFERENCES: Alcohols, ketones, and other esters of acetic acid will also give positive results. Benzene, toluene, and petroleum hydrocarbons will cause discolora- tions. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 700 to 1100 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, August 1979. National Draeger, Inc., Bulletin No. ND-105: National 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: National Draeger: Pittsburgh, December 1981. A-621 ------- COST INFORMATION: Cost per sample for analyses by this method is approximately $13-20 (list). See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method See "Volatile Species," Appendix B. Air Samples Laboratory Method 1 METHOD SUMMARY: Ethyl acetate in air samples may be measured by gas chromatography. A known volume of air is drawn 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: A method-blank is processed along 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 704 to 2950 milligrams per cubic meter for a 6-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. 2, Method S49; Publication No. 77-157-B, U.S. DHEW: Cincinnati, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set E, Method S49; PB-246 148 (NTIS), U.S. DHEW: Washington, October 1975. A-622 ------- 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 ethyl acetate in air samples. The absorbance at 8020 nm (1247 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. REFERENCES: 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. See also: "Volatile Organic Compounds," Appendix B. See also: "Volatile Organic Solvents," Appendix B. A-623 ------- Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B, See "Volatile Organics," Appendix B. A-624 ------- ETHYL ACRYLATE (CAS Number 140-88-5) RQ: 2270 kg SAFETY INFORMATION: Flash point 50°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 ethyl acrylate in air 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 methyl acrylate gas detector tube (Draeger® 67 28161, or equivalent). A positive result is indicated by a color change in the tube from yellow to blue. The test is based upon the reaction of ethyl acrylate with a palladium molybdate compound to form a blue product. INTERFERENCES; Methyl acrylate, hydrogen sulfide, ethene, and carbon monoxide will also cause discolorations in the tube. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 40 to 180 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, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $13-20 (list). A-625 ------- See also: "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 determination of ethyl acrylate in air samples. A known volume of air is drawn through a charcoal tube, followed by desorption with carbon disulfide and injection of the resulting solution 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 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 210 milligrams per cubic meter in a 10-liter sample. Precision and accuracy information is furnished. REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set D, Method S35; PB-245 935 (NTIS), U.S. DHEW: Washington, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 2, Method S35; 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. A-626 ------- Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of ethyl acrylate in air samples. The absorbance at 8350 nm (1200 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: "Halogenated, Aromatic and Other Compounds," Appendix B. See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-627 ------- ETHYLBENZENE (CAS Number 100-41-4) RQ: 454 kg SAFETY INFORMATION: Flash point 59°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 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 ethylbenzene 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 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 222 to 884 milligrams per A-628 ------- 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 C. Method S29; PB-258 852 (NTIS), U.S. DHEW: Washington, October 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S29; 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 ethylbenzene in air samples. The absorbance at 9700 nm (1031 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 200 milligrams per cubic meter or 50 parts per million. No precision or accuracy information is furnished. A-629 ------- 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. See also: "Hydrocarbon Odorants," Appendix B. See also: "Organic Vapors," 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 "Trace Organic Contaminants," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-630 ------- ETHYL CARBAMATE (CAS Number 51-79-6) RQ: 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-631 ------- ETHYL 4,4'-DICHLOROBENZILATE (CAS Number 510-15-6) 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-632 ------- ETHYLENEBIS(DITHIOCARBAMIC ACID) (CAS Number 111-54-6) 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-633 ------- ETHYLENEDIAMINE (CAS Number 107-15-3) RQ: 2270 kg SAFETY INFORMATION; Flash point 93°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," Appendix B. See "Hydrazine and Other Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Ethylenediamine in air samples can be measured by gas chromatography. A known volume of air is drawn through a tube containing silica gel. Hydrochloric acid is added to stabilize the amines collected. The analyte is desorbed with methanol solution. An aliquot is made basic with sodium hydroxide and treated with benzaldehyde to form the dibenzylidine derivative, then analyzed by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: Large amounts of ammonia or primary amines can interfere, but adding additional benzaldehyde should compensate. 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. A-634 ------- EPA/TECHNICAL STATUS; This method is proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.2 to 7 milligrams per sample. Precision information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, Method P&CAM 276; Publication No. 78-175, U.S. DHEW: Cincinnati, August 1978. COST INFORMATION: Cost per sample for analysis by this method is approximately $90-135 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of ethylenediamine in air samples. The absorbance at 12850 nm (778 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 37 milligrams per cubic meter or 15 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-635 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Primary and Secondary Amines," Appendix B. Water Samples Laboratory Method See "Amines and Other Nitrogen Compounds," Appendix B. See "Primary and Secondary Amines," Appendix B. A-636 ------- ETHYLENEDIAMINE TETRAACETIC ACID (CAS Number 60-00-4) 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 Water Samples Laboratory Method METHOD SUMMARY: High-performance liquid chromatography (HPLC) may be used to analyze water samples for ethylenediamine tetraacetic acid (EDTA). A 5-milliliter sample is filtered, then mixed with an iron reagent to form the iron(III)-EDTA complex. The pH is adjusted to between 3 and 4, and the solution is analyzed by HPLC with UV detection at 258 nm. INTERFERENCES: Large amounts of cobalt present in the sample may form a complex with the EDTA. QUALITY CONTROL: No quality control procedures are given. A-637 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. This method will detect concentrations of approximately 0.2 milligrams or higher of EDTA per liter. No precision and accuracy information is furnished. REFERENCE: Harmsen, J.; Van Den Toorn, A. "Determination of EDTA in Water by High- Performance Liquid Chromatography," J. Chromatogr., 249, 1982, pp. 379-384. COST INFORMATION: Cost per sample for analysis by this method is approximately $120-140 (list). See also: "Organic Acids," Appendix B. A-638 ------- ETHYLENE DIBROMIDE (CAS Number 106-93-4) RQ: 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 "Organic Vapors," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method Air Samples Laboratory Method 1 METHOD SUMMARY: Ethylene dibromide in air samples can be measured by gas chromatography. A known volume of air is passed through a charcoal tube, 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 decreases the capacity of the sampling appartus. 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 proposed by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 110 to 470 milligrams per cubic meter using a 1-liter sample. Precision and accuracy information is furnished. A-639 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods. 2nd ed., Vol. 2, Method S104; Publication No. 77-175-B, U.S. DREW: Cincinnati, April 1978. U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set H, Method S104; PB-265 027 (NTIS), U.S. DHEW: Washington, January 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 ethylene dibromide in air samples. The absorbance at 8380 nm (1193 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 procedues 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 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. A-640 ------- COST INFORMATION; Cost per sample for analysis by this method is approximately $75-85 (list), plus sampling costs. Note: NIOSH Method P&CAM 260 (charcoal adsorption, benzene-methanol desorption, analysis by GC/ECD) is applicable. (Reference provided by reviewer). See also; "Fumigants," 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 METHOD SUMMARY: Ethylene dibromide in water samples can be measured by gas chromatography with electron-capture detection (GC/ECD). The water sample is extracted twice with hexane, filtered if necessary, and the extracts are diluted to 50 milli- liters and stored in a freezer until analysis. An aliquot is then injected into the GC/ECD. The extract can be concentrated to 5 milliliters in a Kuderna- Danish apparatus. INTERFERENCES: No specific interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is not furnished. No method detection limit is provided; analyses reported are in the area of 1 microgram per liter. REFERENCE: Going, J.; Long, S. Sampling and Analysis of Selected Toxic Substances, Task II - Ethylene Dibromide; EPA 560/6-75-001, PB-246 213 (NTIS), U.S. Environ- mental Protection Agency: Washington, September 1975. A-641 ------- COST INFORMATION; Cost per sample for analysis by this method is approximately $130-175 (list), plus sampling costs. See also: "Volatile Organic Compounds," Appendix B. A-642 ------- ETHYLENE OXIDE (CAS Number 75-21-8) RQ: 0.454 kg SAFETY INFORMATION: Potentially carcinogenic. Flash point below 0°F. 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 Laboratory Method 1 METHOD SUMMARY: Gas chromatography may be used for the analysis of ethylene oxide in air samples. The analysis is performed by sampling a known volume of air with a charcoal-tube sampling apparatus, followed by desorption with carbon disulfide and analysis of the resulting solution by gas chromatography with flame ioniza- tion detection (GC/FID). INTERFERENCES: High humidity can severely limit the capacity of the sampling apparatus. QUALITY CONTROL: The desorption efficiency must be determined, and results corrected accord- ingly. A method blank should be processed with each set of 10 or fewer samples. EPA/TECHNICAL STATUS: This method is approved by the National Institute for Occupational Safety and Health (NIOSH), and validated over the range of 41 to 176 milligrams per cubic meter in a 5-liter sample. If the desorption efficiency is adequate, the A-643 ------- method is applicable to lower concentrations of ethylene oxide. Precision and accuracy information is furnished. REFERENCES; U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set T, Method S286; PB-262 404 (NTIS), U.S. DHEW: Washington, December 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 3, Method S286; Publication No. 77-175-C, U.S. DHEW: Cincinnati, April 1978. 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 ethylene oxide in air samples. The absorbance at 11480 nm (871 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 10 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. A-644 ------- 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. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-645 ------- ETHYLENETHIOUREA (CAS Number 96-45-7) 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 METHOD SUMMARY: Semiquantitative field analysis for ethylenethiourea in soil samples can be performed by silica gel thin-layer chromatography (TLC). The sample is washed with a 1/1 dioxane/water solution for one hour, and the wash liquor is filtered and concentrated on a water bath. The sample is frozen until analyzed. Three solvent systems can be used for the chromatography. The spots are visu- alized with an iodine-starch detection reagent. INTERFERENCES: No interferences are reported, but the sample will decompose if not stored properly. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method has a sensitivity of 1 milligram of analyte per kilogram of soil. REFERENCE: Blazquez, C. H. "Residue Determination of Ethylenethiourea (2-Imidazolidi- nethione) from Tomato Foliage, Soil, and Water," J. Agric. Food Chem., 21(3), 1973, pp. 330332. COST INFORMATION: Cost information has not been obtained. A-646 ------- Water Samples Field Method METHOD SUMMARY: Semiquantitative field analysis for ethylenethiourea in water samples can be performed by thin-layer chromatography (TLC). The sample is frozen until analyzed. Three solvent systems can be used for the chromatography. The spots are visualized with an iodine-starch detection reagent. INTERFERENCES: No interferences are reported, but the sample will decompose if not stored properly. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method has a sensitivity of 1 milligram per liter of water sample. No precision or accuracy information is furnished. REFERENCE: Blazquez, C. H. "Residue Determination of Ethylenethiourea (2-Imidazolidi- nethione) from Tomato Foliage, Soil, and Water," J. Agric. Food Chem., 21(3), 1973, pp. 330-332. COST INFORMATION: Cost information has not been obtained. Air Samples Laboratory Method METHOD SUMMARY: Ethylenethiourea in air samples can be measured spectrophotometrically. The analyte is collected on a PVC or cellulose ester membrane, then extracted with distilled water. Pentacyanoamineferrate reagent is added to the extract to form a colored coordination complex. The absorbance of the solution at 590 nm is read on a spectrophotometer. INTERFERENCES: Any compound with an absorbance maximum in the same region as ethylenthiourea will interfere. A-647 ------- QUALITY CONTROL: Two method-blanks should be processed with each set 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 0.03 to 1.5 milligrams per cubic meter for a 100-liter sample. The detection limit is .75 micrograms per cubic meter. Precision information is furnished. REFERENCE: U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, Method P&CAM 281; Publication No. 78-175, U.S. DHEW: Cincinnati, 1978. COST INFORMATION: Cost per sample for analysis by this method is approximately $40-60 (list), plus sampling costs. Soil/Sediment Samples Laboratory Method See "Thioureas and Other Compounds," Appendix B. Water Samples Laboratory Method A-648 ------- ETHYL ETHER (CAS Number 60-29-7) RQ: 45.4 kg SAFETY INFORMATION: Flash point -49°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. See "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 METHOD SUMMARY: Ethyl ether in air samples can be determined by gas chromatography- A known volume of air is drawn through a charcoal tube, followed by desorption of the analyte with ethyl acetate. An aliquot of the resulting extract is injected into a gas chromatograph equipped with a flame ionization detector (GC/FID). INTERFERENCES: High humidity can greatly reduce the capacity of the sampling apparatus. QUALITY CONTROL: A method blank is 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 610 to 2400 milli- grams per cubic meter in a 3-liter sample. Precision and accuracy information is furnished. A-649 ------- REFERENCES: U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for Set F, Method S80; PB-246 149 (NTIS), U.S. DREW: Washington, 1975. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, Method S80; 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: "Hazardous Organic Emissions," Appendix B. See also: "Organic Vapors," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Aliphatic Compounds," Appendix B. See "Volatile Organics," Appendix B. A-6 50 ------- ETHYL METHACRYLATE (CAS Number 97-63-2) RQ: 454 kg SAFETY INFORMATION: Flash point 68°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-651 ------- ETHYL METHANESULFONATE (CAS Number 62-50-0) 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 See "Halogenated, Aromatic, and Other Compounds," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-652 ------- FAMPHUR (CAS Number 52-85-7) 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 Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-653 ------- FLUORANTHENE (CAS Number 206-44-0) 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 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-654 ------- FLUORENE (CAS Number 86-73-7) 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 "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 "Organic Compounds," Appendix B. See "Polycyclic Aromatic Hydrocarbons," Appendix B. See "Trace Organic Contaminants," Appendix B. A-655 ------- FLUOROACETAMIDE (CAS Number 640-19-7) 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 Water Samples Laboratory Method A-656 ------- FLUOROACETIC ACID, SODIUM SALT (CAS Number 62-74-8) 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 Note: NIOSH Method S301 (filter collection, deionized water extraction, analysis by ion chromatorgrahpy with electrolytic conductivity detection) is applicable. (Reference provided by reviewer). Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Acid Anions," Appendix B. A-657 ------- FORMALDEHYDE (CAS Number 50-00-0) RQ: 454 kg SAFETY INFORMATION: Flash point: 122°F. 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 formaldehyde may be performed by use of a detector tube. A 0.1- to 1.6-liter air sample is collected and analyzed with a hand-operated bellows pump and a formaldehyde gas detector tube (Draeger® 67 26760, or equiva- lent). A positive result is indicated by a color change in the tube from white to pink. The test is based on the formation of a pink quinoid compound from the reaction product of formaldehyde and xylene reacting with sulfuric acid. INTERFERENCES: Other aldehydes, styrene, and furfuryl alcohol will also cause discolora- tions. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of approximately 0.5 to 15 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, August 1979. National Draeger, Inc., Bulletin No. ND-105; National 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; National Draeger: Pittsburgh, December 1981. A-658 ------- COST INFORMATION; Cost per sample for analysis by this method is approximately $13-20 (list). Soil/Sediment Samples Field Method Water Samples Field Method METHOD SUMMARY: Potentioraetric analysis may be used for the determination of formaldehyde in water samples. A 10-milliliter sample is mixed with an iodide-iodine solution and potassium hydroxide. The resulting solution is stirred for 10 minutes, then mixed with nitric acid and water, and titrated with silver nitrate. INTERFERENCES: Acetone or acetaldehyde will interfere strongly. High concentrations of formic acid or methanol may interfere slightly. QUALITY CONTROL: A blank must be analyzed. SENSITIVITY: This method is sensitive to concentration levels of formaldehyde as low as approximately 5 milligrams per liter. REFERENCE: Ikeda, S. "Determination of Formaldehyde By Argentometric Potentiometric Titration Using an Iodide-Ion Selective Electrode," Anal. Lett., 7/5), 1974, pp. 343-346. COST INFORMATION: Cost per sample for analysis by this method is approximately $20-30 (list). Air Sample Laboratory Method 1 METHOD SUMMARY: Analysis for formaldehyde in air is performed by passage of a known volume of air through four 1-percent sodium bisulfite-filled impingers, followed by A-659 ------- colorimetric analysis of the resulting solutions. Formaldehyde is released from the sodium bisulfite solution by the addition of sulfuric acid, and color is developed by the addition of chromotropic acid. Five standard solutions, with concentrations from 2.5 to 20 micrograms per milliliter, should be used for calibration. Alternatively, the air is drawn through a series of two impingers filled with distilled water. Formaldehyde reacts with a chromotropic acid-sulfuric acid solution, and the absorbance is read spectrometrically at 580 nm. Another variation is collection of the formaldehyde on alumina, followed immediately by desorption into 99/1 water/methanol. The solution is then analyzed by the chromotropic acid-sulfuric acid method. INTERFERENCES: Methanol and formic acid both interfere with the analysis, but other aldehydes do not. QUALITY CONTROL: No quality control procedures are given for the Environment Canada Method. A method blank and standards are prepared and anlayzed in the NIOSH method. EPA/TECHNICAL STATUS; The Environment Canada (sodium bisulfite collection, chromotropic acid color development) method is not EPA-approved. The method detection limit is 0.1 milligram per liter in the sodium bisulfite solution, and the method is applicable over the concentration range of 0.01 to 0.1 milligrams per cubic meter. Method P&CAM 125 (collection in distilled water) is tentatively approved by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 0.1 to 2.0 milligrams per cubic meter for a 60-liter air sample. Method P&CAM 235 (collection on alumina) is proposed by NIOSH for use over the range of 0.4 to 52 milligrams per cubic meter for a 6-liter air sample. Precision and accuracy information is furnished only for the NIOSH methods • REFERENCES: Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric Pollutants, 2nd ed., Method 12525, Alberta Environmental Centre: Vegreville, Alberta, Canada, 1981. Method 43501-02-74T, Health Laboratory Science, 1975, p. 163. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1, Method P&CAM 125; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical Methods, P&CAM 125; Publication No. 75-11; U.S. DHEW: Cincinnati, 1974. A-660 ------- D.S Apartment of Health, Education and Welfare, NIOSH Manual of Analytical •• 77-137-A. U.S. DHEW: COST INFORMATION: Cost per sample for analysis by this method is approximately $25-35 (list), plus sampling costs. Air Sample Laboratory Method 2 METHOD SUMMARY: Capillary column gas chromatography can be used for the determination of formaldehyde in air samples. A known volume of air is drawn through a sorbent tube containing Chromosorb® 102 coated with N-benzylethanolamine , which con- verts the formaldehyde to 3-benzyloxazolidine. The analyte is desorbed with isooctane and an aliquot is injected into a capillary-column gas chromatograph equipped with a flame ionization detector (GC/FID). INTERFERENCES : No specific interferences are reported. QUALITY CONTROL: Method blanks 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 0.55 to 4.71 milligrams per cubic meter for a 12-liter sample. Precision and accuracy information is furnished. REFERENCE : U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol 7, Method P&CAM 354; Publication No. 82-100, U.S. DHHS : Cincinnati, August 1981. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90 (list), plus sampling costs. Air Samples Laboratory Method 3 A-661 ------- METHOD SUMMARY: Formaldehyde in air samples can be measured by ion chromatography. A known volume of air is drawn through an impregnated characoal tube to trap the formaldehyde. The formaldehyde is desorbed from the charcoal with hydrogen peroxide, and an aliquot of the desorbed sample solution is injected into the ion chromatograph. INTERFERENCES: Particulate formate and formic acid interfere. The particulate formate can be removed by using a prefilter connected in front of the charcoal tube. 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 0.03 to 2 milligrams per cubic meter for a 96-liter air sample. Precision and accuracy information is fur- nished. REFERENCE: U.S. Department of Health and Human Services, NIOSH Manual of Analytical Methods, Vol. 6, Method P&CAM 318; Publication No. 80-125, U.S. DHHS: Cincinnati, August 1980. COST INFORMATION: Cost per sample for analysis by this method is approximately $70 (list), plus sampling costs. Air Samples Laboratory Method 4 METHOD SUMMARY: Formaldehyde in air samples can be measured by drawing a known volume of air through a midget bubbler containing a buffered solution of Girard T reagent, which derivatizes the formaldehyde, and then determining the formaldehyde-Girard T reagent derivative by polarography. INTERFERENCES: Other volatile aldehydes and components of polyvinyl chloride tubing may interfere. A-662 ------- QUALITY CONTROL: One 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 validated over the range of 1.7 to 7.6 milligrams per cubic meter, using an 18-liter sample for a 24-hour weighted average, and over the range of 5.6 to 24.3 milligrams per cubic meter for 30-minute peak samples. 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 S327; Publication No. 78-175, U.S. DHEW: Cincinnati, August 1978. COST INFORMATION: Cost information has not been obtained. Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Analysis of soil/sediment samples for formaldehyde can be performed by gas chromatography. A 10-gram sample is suspended in water, the resulting mixture is steam-distilled, and the distillate is treated with 2,4-dinitrophenyl- hydrazine. The derivative formed is extracted into carbon disulfide at pH 6 to 8, and the resulting solution is concentrated and analyzed by gas chromatography with flame ionization detection (GC/FID). INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved, and is a modification of an unofficial method developed by the U.S. Food and Drug Administration. The detection limit is 20 milligrams per kilogram (wet weight basis). No precision or accuracy information is furnished for analysis of a soil/sediment matrix. A-663 ------- REFERENCES: Nelson, J. J.; Barry, T. L.; Ting, S. "GLC and GC/MS Analysis of Formaldehyde in Olives as its 2,4-Dinitrophenylhydrazone Derivative," Laboratory Information Bulletin, No. 2180, March 31, 1978; U.S. Food and Drug Administration: Washington. Personal communication, E. William Loy, Jr., U.S. Environmental Protection Agency, Region 4, Athens, Georgia, February 1984. COST INFORMATION; Cost per sample for analysis by this method is approximately $130-175 (list). Water Samples Laboratory Method See "Volatile Carbonyl Compounds," Appendix B. A-664 ------- FORMIC ACID (CAS Number 64-18-6) 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 "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 1 METHOD SUMMARY: Analysis for formic acid in air can be performed by passage of 60 liters of air through a Chromosorb® 103 sampling tube, followed by leaching of the analyte from the sampling medium with deionized water and analysis of the resulting solution by ion chromatography. INTERFERENCES: Late-eluting carbonate and bicarbonate peaks from one sample injection can interfere in later ion chromatographic analyses. The chromatographic analysis time can be shortened to approximately 20 minutes per injection by use of a stronger eluting solvent to remove these interferences. QUALITY CONTROL: Collected samples are stable on the sampling cartridge for 7 days. Each lot of sampling material should be tested for interferences. gPA/TECHNICAL STATUS: This method is not EPA-approved and has undergone single-laboratory evalua- tion of precision and accuracy. This method is sensitive to concentration levels of formic acid vapor above 80 micrograms per cubic meter. The collection A-665 ------- efficiency is 100 percent at 85 percent humidity and 22 milligrams formic acid per cubic meter. REFERENCE: Haynes, D. L. In Ion Chromatographic Analysis of Environmental Pollutants, Vol. 2, Mulik J. D.; Sawicki, E., Eds.; Ann Arbor Science: Ann Arbor, 1979, pp. 157-169. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-90 (list), plus sampling costs. Air Samples Laboratory Method 2 METHOD SUMMARY: Gas chromatography may be used for the determination of formic acid in air samples. A known volume of air is passed through a midget impinger containing dilute sodium hydroxide. A derivatizing solution of ethanol and sulfuric acid is added to the absorbing solution. The formic acid is converted to ethyl formate. A partitioning of the volatile ethyl formate takes place between the solution and the headspace gas above it. The headspace gas is analyzed for ethyl formate in a gas chromatograph with dual flame ionization detectors (GC/FID). INTERFERENCES: Low-molecular-weight acids and alcohols in high concentrations may inter- fere in the derivatization step. QUALITY CONTROL: A blank should be processed with the samples and its value used in the cal- culation of the results. EPA/TECHNICAL STATUS: This method is classified as operational by the National Institute for Occupational Safety and Health (NIOSH) for use over the range of 3.8 to 75 milligrams per cubic meter in a 10-liter sample of air. The detection limit is 0.75 milligrams per cubic meter. 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 232; Publication No. 77-157-A, U.S. DHEW: Cincinnati, 1977. A-666 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $80-105 (list), plus sampling costs. Note: NIOSH Method S173 is applicable. (Reference provided by reviewer). Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Acids," Appendix B. A-667 ------- RQ: 2270 kg SAFETY INFORMATION: FUMARIC ACID (CAS Number 110-17-8) 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 "Organic Acids: Adipic and Fumaric Acids," Appendix B. Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Carboxylic Acids," Appendix B. A-668 ------- FURAN (CAS Number 110-00-9) RQ: 45.4 kg SAFETY INFORMATION: Flash point below 32°C. 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 "Gaseous Contaminants," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Organic Compounds," Appendix B. A-669 ------- FURFURAL (CAS Number 98-01-1) 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 See "Aldehydes," Appendix B. See "Cyclohexanone and Furfural," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method Water Samples Field Method METHOD SUMMARY: Furfural in water samples can be measured using a portable fluorometer. Aromatic aldehydes react with 2,2'-dithiobis(l-aminonaphthalene) in the presence of tri-p-butylphosphine, sodium sulfite, and sodium phosphate. For furfural, excitation occurs at 380 nm and emission at 475 nm. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is sensitive to concentration levels of furfural above 10 micrograms per liter. REFERENCE: Ohkura, Y.; Ohtsubo, K.; Zaitsu, K.; Kohashi, K. "Fluorimetric Determination of Aromatic Aldehydes with 2,2'-Dithiobis(l-Aminonaphthalene) " Anal Chim Acta., 99(2), 1978, pp. 317-324. ' 1 A-670 ------- COST INFORMATION: Cost per sample for analysis by this method is approximately $25-40 (list). Air Samples Laboratory Method METHOD SUMMARY: Infrared absorption spectrometry can be used to determine the concentra- tion of furfural in air samples. The absorbance at 13270 nm (754 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(s) 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. Soil/Sediment Samples Laboratory Method A-671 ------- Water Samples Laboratory Method See "Volatile Carbonyl Compounds," Appendix B. See "Volatile Organic Compounds," Appendix B. A-672 ------- GLYCIDYLALDEHYDE (CAS Number 765-34-4) 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 Air Samples Laboratory Method See "Aliphatic Aldehydes," Appendix B. See "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-673 ------- GUTHION® (CAS Number 86-50-0) 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 See "Cholinesterase-Inhibiting Compounds," Appendix B. See "Organophosphorus Pesticides," Appendix B. Air Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. Water Samples Laboratory Method See "Organophosphorus Pesticides," Appendix B. A-674 ------- HEPTACHLOR (CAS Number 76-44-8) 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 Note: NIOSH Method S287 (collection on chromasorb® 102, toluene desorption, analysis by GC/ECD) is applicable. (Reference furnished by reviewer) See also:"Chlorinated Pesticides," 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 "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-675 ------- HEPTACHLOR EPOXIDE (CAS Number 1024-57-3) 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 "Chlorinated Pesticides," Appendix B. See "Pesticide Residues," 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 "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-676 ------- HEXACHLOROBENZENE (CAS Number 118-74-1) 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 Pesticides," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Chlorinated Benzenes," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Organochlorine Pesticides and PCB's," 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 "Organochlorine and Organophosphorus Pesticides," Appendix B A-677 ------- RQ: 0.454 kg SAFETY INFORMATION: HEXACHLOROBUTADIENE (CAS Number 87-68-3) 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 "Halogenated, Aromatic, and Other Compounds," Appendix B. See "Hazardous Organic Emissions," Appendix B. See "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," 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 Ethers and Other Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B, A-678 ------- HEXACHLOROCYCLOPENTADIENE (CAS Number 77-47-4) RQ: 0.454 kg SAFETY INFORMATION: Exhibits chronic toxiclty. 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 to analyze air samples for hexachlorocyclo- pentadiene. A 3-liter air sample is passed through a Porapak T® tube, the analyte is desorbed with hexane, and the resulting solution is analyzed by gas chromatography with electron capture detection (GC/ECD). INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. EPA/TECHNICAL STATUS: This method is not EPA-approved. Precision and accuracy information is furnished. This method has been validated over the range of 13 to 868 micro- grams per cubic meter. A-679 ------- REFERENCE: National Institute for Occupational Safety and Health, Development of Air Sampling and Analytical Methods for Toxic Chlorinated Organic Compounds, Southern Research Insitute for National Institute for Occupational Safety and Health (NIOSH), Contract No. 210-78-0012, 1979. COST INFORMATION: Cost per sample for analysis by this method is approximately $80-100 (list), plus sampling costs. Note; NIOSH Method P&CAM 308 describes the above method. (Reference provided by reviewer). Soil/Sediment Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Chlorinated Hydrocarbons," Appendix B. A-680 ------- HEXACHLOROETHANE (CAS Number 67-72-1) 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 METHOD SUMMARY: Gas chromatography can be used for the analysis of air samples for hexachloroethane. 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 5 to 25 milligrams per cubic meter using a 5-liter sample. The method is capable of measurement of A-681 ------- 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 Methods for Set H, Method S101; PB-265 027 (NTIS), U.S. DHEW: Washington, 1977- See also: "Hazardous Organic Emissions," Appendix B. Soil/Sediment Samples Laboratory Method See "Acid and Base/Neutral Extractable Organics," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. Water Samples Laboratory Method See "Base/Neutral Extractable Organic Compounds," Appendix B. See "Chlorinated Ethers and Other Compounds," Appendix B. See "Chlorinated Hydrocarbons," Appendix B. See "Volatile Chlorinated Aliphatic Hydrocarbons," Appendix B. A-68 2 ------- HEXACHLOROHEXAHYDRO-ENDO-ENDO-DIMETHANONAPHTHALENE (CAS Number 465-73-6) RQ: 0.454 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 "Organochlorine Pesticides and PCB's," Appendix B. Water Samples Laboratory Method See "Organochlorine and Organophosphorus Pesticides," Appendix B. See "Pesticides," Appendix B. A-683 ------- HEXACHLOROPHENE (CAS Number 70-30-4) 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 Soil/Sediment Samples Laboratory Method METHOD SUMMARY: Hexachlorophene in soil/sediment samples can be determined by gas chromatography with electron-capture detection (GC/ECD). The sample is dried and Soxhlet-extracted with ethyl ether. Organisms are removed, then the extract is filtered through anhydrous sodium sulfate and evaporated to near dryness. The residue is resuspended in benzene, the sample is acetylated, and an aliquot is analyzed by GC/ECD. INTERFERENCES: No interferences are reported. QUALITY CONTROL: Extraction efficiencies should be determined, and the values used in the calculation of the results. A-684 ------- EPA/TECHNICAL STATUS: This method is not EPA-approved. No precision or accuracy information or limits of detection are reported. REFERENCE: Sims, J. L.; Pfaender, F. K. "Distribution and Biomagnification 'of Hexachloro- phene in Urban Drainage Areas," Bull. Environ. Contain. Toxicol.. 14(2), 1975, pp. 214-220. COST INFORMATION: Cost per sample for analysis by this method is approximately $160-185 (list), plus sampling costs. Water Samples Laboratory Method See "Chlorinated Phenols," Appendix B. A-685 ------- HEXACHLOROPROPENE (CAS Number 1888-71-7) 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 Air Samples Laboratory Method Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method A-686 ------- HEXAETHYL TETRAPHOSPHATE (CAS Number 757-58-4) 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 See "Phosphorus," Appendix B. Soil/Sediment Samples Laboratory Method See "Phosphorus," Appendix B. Water Samples Laboratory Method See "Phosphorus," Appendix B. A-687 ------- INDENO[l,2,3-cd]PYRENE (CAS Number 193-39-5) 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 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 "Acid and Base/Neutral Extractable Organic," 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-688 ------- ISOPHORONE (CAS Number 78-59-1) 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 METHOD SUMMARY: Isophorone in air samples can be measured spectrometrically. The sample is drawn through 20 milliliters of glacial acetic acid. One milliliter of phosphomolybdic acid reagent is added to 10 milliliters of the acetic acid solution. The sample is heated in a boiling water bath for 45 minutes, cooled, and diluted. The intensity of the resulting molybdenum blue complex is measured on a portable spectrometer at 650 nm and compared to a calibration curve. Elevated concentrations of isophorone will react with the reagent with- out use of the boiling water bath. (This method is described by Kacy, H. W., Jr.; Pope, R. W. Am. Ind. Hyg. Assoc. Quart., 16, 1975, pp. 55-59, 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 supplied. REFERENCE: Chemical Detection of Gaseous Pollutants, Ruch, W. E., Ed.; Ann Arbor Science: Ann Arbor, 1967, p. 121. COST INFORMATION: Cost per sample for analysis by this method is approximately $65-110 (list), plus sampling costs. Soil/Sediment Samples Field Method Water Samples Field Method A-689 ------- Air Samples Laboratory Method METHOD SUMMARY: Analysis for isophorone in air 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 results. 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 67.5 to 283 milli- grams per cubic meter in a 12-liter sample. The method is capable of measure- ment of 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. 3, Method S367; Publication No. 77-157C, U.S. DREW: Washington, 1977. COST INFORMATION: Cost per sample for analysis by this method is approximately $70-90, plus sampling costs. 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 "Chlorinated Ethers and Other Compounds," Appendix B. See "Volatile Alcohols and Other Organic Compounds," Appendix B. A-690 ------- ISOPRENE (CAS Number 78-79-5) RQ: 0.454 kg SAFETY INFORMATION: Flash point -65°F. Potentially chronically toxic. Can undergo auto-polymerization. CAUTION: The user should obtain additional toxicity/hazard information before handling this substance or using this analytical procedure. Air Samples Field Method METHOD SUMMARY: Air samples can be analyzed for isoprene using a gas chroraatograph adapted for mobile field units. A sample trap immersed in nitrogen is preceded by a drying loop, containing anhydrous potassium carbonate. The contents of the trap collected from the are sample are swept into the gas chromatographs dual flame instrument directly, onto a -70° Durapak column, and the temperature program is initiated. INTERFERENCES: No interferences are reported. QUALITY CONTROL: No quality control procedures are given. SENSITIVITY: This method is suitable for isoprene concentrations above approximately 0.5 milligrams per cubic meter. REFERENCE: Westberg, H. H.; Rasmussen, R. A.; Holdren, M. "Gas Chromatographic Analysis of Ambient Air for Light Hydrocarbons Using a Chemically Bonded Stationary Phase," Anal. Chem., 46(12), 1974, pp. 1852-1854. COST INFORMATION: Cost information has not been obtained. See also: "Volatile Organic Compounds," Appendix B. Soil/Sediment Samples Field Method A-691 ------- Water Samples Field Method See "Aromatics and Other Compounds," Appendix B. Air Samples Laboratory Method See "Hydrocarbon Odorants," Appendix B. Soil/Sediment Samples Laboratory Method Water Samples Laboratory Method See "Volatile Organic Compounds," Appendix B. A-692 ------- |