United States Environmental Protection Agency National Exposure Research Laboratory Research Triangle Park, NC 27711 Research and Development EPA/600/SR-97/014 March 1997 Project Summary Investigation of Selected Detectors for Application on Hydrocarbons Continuous Emissions Monitoring Systems Dave-Paul Dayton, Joan T. Bursey, and Stephanie B. Philipp The development of a prototype emis- sions monitoring instrument to provide continuous or semi-continuous quanti- tative measurement of total gaseous nonmethane organic carbon (TGNMOC) emissions from stationary sources will provide better characterization and con- trol of compounds listed in Title III of the Clean Air Act Amendments of 1990. To meet this goal a search was initi- ated to identify detection systems for TGNMOC that are both simple to use and accurate for a wide range of or- ganic compounds. The measurement of oxygenated compounds is of par- ticular interest since many emission sources emit a considerable volume of these compounds. Detection systems were identified by searching detector manufacturers' lit- erature and talking with manufactur- ers' technical personnel. Several de- tector systems are marketed as capable of measuring TGNMOC. In this report, data are presented on the laboratory evaluation of a Catalyzed Flame loniza- tion Detector, a Thermionic lonization Detector, an Oxygen-Flame lonization Detector, and an Elemental Analyzer for TGNMOC measurement. Fourier Transform Infrared Spectroscopy was also evaluated as a candidate detector. The primary performance requirement was that the detectors produce equal response for all organic compounds in a mixture, including oxygenated com- pounds, based on the number of car- bon atoms in the compound. None of the detection systems evaluated met the primary performance goal of uni- formly measuring organic carbon re- gardless of the chemical structure. Some detectors were successful for many classes of organic compounds, but oxygenated compounds presented a challenge that none of the detection systems could master. This Project Summary was developed by EPA's National Exposure Research Laboratory, Research Triangle Park, NC, to announce key findings of the re- search project that is fully documented in a separate report of the same title (see Project Report ordering informa- tion at back). Introduction The objective of this project was to iden- tify an appropriate detection system for incorporation into a prototype total gas- eous nonmethane organic carbon (TGNMOC) emissions monitoring instru- ment. The accurate measurement of TGNMOC is critical to total VOC mea- surement required at many industrial pro- cesses. The measurement of oxygenated compounds is of particular interest since many emission sources emit a consider- able volume of these compounds. The primary performance requirement was that the detectors produce equal response for all organic compounds in a mixture, in- cluding oxygenated compounds, based on the number of carbon atoms in the com- pound. Although the flame ionization detector (FID) has been used as a universal detec- tor for complex mixtures of organic com- pounds, compounds containing heteroat- oms have been shown to yield lower re- sponse than straight chain aliphatic hy- drocarbons1, producing an underestimate 1 Skoog, D. A. Principles of Instrumental Analysis. Third Edition, Saunders College Publishing, New York, 1985. p. 767. ------- of organic carbon. The following manufac- turers of instruments indicated in their lit- erature that they should be successful in determining TGNMOC including oxygen- ated organic compounds. These instru- ments were evaluated in this study. The Catalytic Flame lonization Detector (CFID) manufactured by DETector Engi- neering and Technology, Inc, (Walnut Creek, CA) is marketed as a detection system that provides enhanced responses for organic compounds containing heteroa- toms. The Thermionic Flame lonization Detector (TID), also manufactured by DETector Engineering and Technology, is marketed as an oxygen-selective detector when operated in a nitrogen (N2) environ- ment. The Oxygen-Flame lonization De- tector (O-FID) manufactured by Fisons In- struments (Danvers, MA) is marketed as the recommended detection system of the European Economic Community and the U.S. Environmental Protection Agency for analysis of oxygenated compounds in gasoline. The Elemental Analyzer (EA) also manu- factured by Fisons, is marketed as a de- tection system for simultaneous carbon, H2, N2, and O2 determinations from solid, liquid, or gas samples. High detection lim- its and detection of methane and carbon dioxide interfere with the application of this detection system to TGNMOC mea- surement. A Fourier Transform Infrared (FTIR) op- tical detection system was investigated. The FTIR technique allows the collection of the entire IR spectrum from about 4000 to 200 wave numbers within a few sec- onds. The molecular signature is obtained over a broad spectral range; accurate iden- tification of the species can be made from this signature. The advantage of taking the entire IR spectrum is that if interfering species are present they will almost cer- tainly not be present at all of the same frequencies, and judicious selection of analysis regions will produce interference- free detection. Laboratory Procedures The FID, CFID and TID were evaluated with liquid standards containing the oxy- genated and non-oxygenated compounds. The compounds were acetaldehyde, methanol, acetone, 2-butanone, benzene, butyl cellosolve®, benzaldehyde, hexane, heptane, iso-octane, nonane, methylene chloride, and triethylamine. The FTIR spec- trometer was evaluated using a synthetic mixture of standards prepared in SUMMA® canisters. Conclusions None of the detectors evaluated met the performance goal of universal, linear, organic carbon response. While some suc- cess was realized for many classes of organic compounds, oxygenated com- pounds presented the strongest challenge to the detection systems evaluated. Within an individual chemical class, a 1:1 linear carbon response relationship was achieved, but a linear carbon response relationship was not achieved when com- paring one chemical class to another. These detectors are useful for selective applications, but they do not meet the needs of an universal detector for total carbon in a sample containing a mixture of compounds from various chemical classes. Information in this document has been funded wholly by the U.S. Environmental Protection Agency under Contract 68-D1- 0010 to Eastern Research Group. It has been subjected to Agency review and ap- proved for publication. Mention of trade names or commercial products does not constitute endorsement or recommenda- tion for use. ------- Dave-Paul Dayton, Joan T. Bursey, and Stephanie B. Philipp are with Eastern Research Group, Inc., Morrisville, NC 27526. Merrill D. Jackson is the EPA Project Officer (see below). The complete report, entitled "Investigation of Selected Detectors for Application on Hydrocarbons Continuous Emissions Monitoring Systems," (Order No. PB97- 143168; Cost: $21.50, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: National Exposure Research Laboratory U. S. 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