United States Environmental Protection Agency Environmental Monitoring Systems Laboratory Research Triangle Park NC 27711 Research and Development EPA/600/S4-87/006 July 1987 &EPA Project Summary Supplement to EPA/600/4-84/041: Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air (Revised 9/86) R. M. Riggin, W. T. Winberry, Jr., and N. V. Tilley This supplement was developed to expand upon the original compendium (4/84), which covered twenty-nine (29) air toxics that could be analyzed by five (5) general methods. The supplement now increases the number of air toxics to thirty-six (36) and the number of pro- cedures to nine (9). The Compendium was developed to complement a previ- ously published document entitled "Technical Assistance Document (TAD) for the Determination of Toxic Organic Compounds in Ambient Air." The com- pendium provides a standardized for- mat for analytical procedures used in determining toxic compounds in ambi- ent air. Further supplements to the Compendium will occur as suitable pro- cedures become available. The current methods may also be modified as ad- vancements are made. The compendium sampling proce- dures range from utilizing liquid im- pingers to cryogenic trapping to adsor- bent technology. Likewise, analytical procedures range from on-line gas chromatography (GC) to high resolu- tion gas chromatography/high resolu- tion mass spectroscopy (HRGC/HRMS) techniques. Consequently, many toxic organic compounds can be sampled and analyzed by several techniques, often with different interferences and detection limitations. This allows the user latitude in selection so as to com- plement his background and laboratory capability. This Project Summary was devel- oped by EPA's Environmental Monitor- ing Systems Laboratory, Research Tri- angle Park, NC, to announce key findings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back). Introduction Toxic air pollutants have been of con- cern for many years, primarily under Section 112 of the Clean Air Act, which establishes procedures for designating National Emission Standards for Haz- ardous Air Pollutants (NESHAP). NESHAPs are intended to provide con- trol of source categories which emit pollutants that "may reasonably be an- ticipated to result in an increase in mor- tality or an increase in serious irre- versible, or incapacitating reversible, illness." Likewise, public concern for protec- tion from exposure to toxic substances has intensified over the last decade. Ev- idence of the presence of these sub- stances in ambient air across the United States has been increasing for some time. Although many of these sub- stances are presently controlled ------- through occupational, consumer pro- tection, water or waste disposal regula- tions, control of air pollution involving specific toxic substances has been lim- ited. This is due, in part, to a lack of information on ambient air levels and the uncertainty of the sampling and analysis methods for their detection. Over the last several years, State and local air pollution control agencies have increased their efforts to measure the concentrations of toxic pollutants in ambient air. These activities have in- cluded monitoring around abandoned hazardous waste dump sites and solid waste landfills, as well as other point source and urban area monitoring. For the most part, network design, siting and sampling/analysis procedures used were based on professional judgments rather than adherence to any docu- mented, uniform procedures and guide- lines. The absence of standardized pro- cedures raises serious concerns about the adequacy of the data collected for their intended uses. Ensuring data ade- quacy is critical, since major decisions on control actions, health effects, and other significant issues could be based on the interpretation of such data. The objective of this project was to develop a compendium that would pro- vide regional, state and local environ- mental regulatory agencies with specific guidance on sampling and ana- lytical procedures, in a standardized for- mat, for selected toxic organic com- pounds. Structure of the Compendium The current compendium consists of nine (9) procedures covering thirty-six (36) organic toxic compounds. Each procedure is written to be used inde- pendently from the others and is di- vided into twelve (12) sections entitled: • Scope • Applicable Documents • Summary of Method • Significance • Definitions • Interferences • Apparatus • Reagents/Materials • Assembly/Calibration • Sampling • Analysis • Performance Criteria and Quality Assurance The procedures are written in a stand- ardized format used by the American Society for Testing and Materials (ASTM). Each procedure has been iden- tified with a revision number and dated to allow future modifications. Addi- tional procedures, which may be compound-specific or of multiple ana- lyte design, will be placed in the com- pendium as they become available. Nearly all the procedures have some flexibility. Consequently, users are re- sponsible for preparing certain stand- ard operating procedures (SOPs) to be employed in their particular laboratory. Each procedure indicates those opera- tions for which SOPs are required. Table 1 lists the procedures contained in the compendium and Table 2 pre- sents a partial listing of toxic organic compounds which can be determined using those procedures. Many of the procedures may be used to determine other toxic organics not indicated in Table 2. The user must be cautioned to evaluate the applicability of the metho for that specific organic toxicant in at vance. Table 1. List of the Procedures Presently in the Compendium Description Procedure Number Types of Compounds Determined TO-1 TO-2 TO-3 TO-4 TO-5 TO-6 TO-7 TO-8 TO-9 Tenax GC Adsorption and GC/MS Analysis Carbon Molecular Sieve Adsorption and GC/MS Cryogenic Trapping and GC/FID or ECD Analysis High Volume PUF Sam- pling and GC/ECD Analysis Dinitrophenylhydrazine Liquid Impinger Sampling and HPLC/UV Analysis High Performance Liquid Chromatography (HPLC) Thermosorb/N Adsorption Sodium Hydroxide Liquid Impinger Sampling with High Performance Liquid Chromatography (HPLC) Analysis High Volume Polyurethane Foam Sampling with High Resolution Gas Chroma- tography/High Resolution Mass Spectrometry (HRGC/ HRMS) Analysis Volatile, nonpolar, organics (e.g., aromatic hydrocarbons, chlorinated hydrocarbons) having boiling points in the range of 80° to 200°C. Highly volatile, nonpolar or- ganics (e.g., vinyl chloride, vinylidene chloride, benzene, toluene) having boiling point in the range of - 15° to + 120°C. Volatile, nonpolar organics having boiling points in the range of - 10° to +200°C. Organochlorine pesticides an PCBs. Aldehydes and Ketones Phosgene N-Nitrosodimethylamine Cresols/Phenols Dioxins ------- Table 2. Applicability of Specific Procedure to Selective Toxic Organics Applicable Compound Procedure Acetaldehyde TO-5 Acrolein TO-5 Acrylonitrile TO-2, TO-3 Allyl Chloride TO-2, TO-3 Benzaldehyde TO-5 Benzene TO-7, TO-2, TO-3 Benzyl Chloride TO-7, TO-3 Carbon Tetrachloride TO-2, TO-3 Chlorobenzene TO-1, TO-3 Chloroform TO-2, TO-3 Chloroprene TO-7, TO-3 <2-Chloro-1, 3-Butadiene) Cresol TO-8 4,4'-DDE TO-4 4,4'-DDT TO-4 1,4-Dichlorobenzene TO-1, TO-3 Dioxin TO-9 Ethylene dichloride TO-2, TO-3 (1,2-Dichloroethane) Formaldehyde TO-5 Methyl Chloroform TO-2, TO-3 (1,1, 1-Trichloroethane) Methylene Chloride TO-2, TO-3 Nitrobenzene TO-1, TO-3 N-Nitrosodimethylamine TO-7 Perchloroethylene TO-7, TO-3 (Tetrachloroethylene) Phenol TO-8 Phosgene TO-6 Polychlorinated Biphenyls TO-4 (PCBs) Propanol TO-5 Toluene TO-7, TO-2, TO-3 Trichloroethylene TO-7, TO-2, TO-3 Vinyl Chloride TO-2, TO-3 Vinylidine Chloride TO-3, TO-3 (1,1-dichloroethene) o,m,p-Xylene TO-7, TO-3 ------- R. M. Riggin was formally with Battelle-Columbus Laboratories, Columbus. OH 43201-2693; William T. Winberry,.Jr., and Nor ma Til ley are with Engineering Science. Gary. NC27511. L. J. Purdue and H. G. Richter are the EPA Project Officers (see below). The complete report and the most recent supplement are entitled: "Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air," (Order No. PB 87-168 688/AS; Cost: $ 18.95) "Supplement to EPA/600/4-84/041: Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air," (Order No PB 87-168 696/AS; Cost: $18.95) The above reports will be available only from: (cost subject to change) National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officers can be contacted at: Environmental Monitoring Systems "Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 U.S. OFFICIAL MAI United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 — A? '" -: | AUG-3'87 X A J . 1 f\ y ... , Vh^> y/ ]iX PENALTY 1 li. 1 'RIVATE i / JSE. S300' ~ / • * i ~ f f 1 METEiJi 6iiOIU9 I .S.P3STAGE 0 2 2: — Official Business Penalty for Private Use $300 EPA/600/S4-87/006 I,II,,II,,,,I!,,limit,,,!,,I,i ------- |