United States Environmental Protection Agency Environmenta/ Monitoring Systems Laboratory Las Vegas NV 89193-3478 Research and Development EPA/540/SR-93/518 September 1993 EPA Project Summary Superfund Innovative Technology Evaluation (SITE) Program Evaluation Report For Antox BTX Water Screen (BTX Immunoassay) R.W. Gerlach, R.J. White, N.F.D. O'Leary, and J.M. Van Emon The results of a demonstration of a portable immunoassay for the detec- tion of benzene, toluene, and xylene(s) (BTX) are described in this report The BTX immunoassay was developed by Antox, Inc., (South Portland, ME) and is intended as a screening technology. Seventy-nine field samples were ob- tained from monitoring wells at several sites with gasoline-contaminated ground water. Sample splits were ana- lyzed on-site by the BTX immunoassay and in the laboratory by gas chroma- tography (GC) using EPA Method 8020. The BTX immunoassay was rapid and simple to use. It performed well in iden- tifying high-level contamination and gasoline-contaminated samples having BTX concentrations greater than 100 ppb. It did not fully meet the claims of the developer of identifying contamina- tion levels down to 25 ppb BTX. Two field samples determined by GC to have between 25 and 100 ppb BTX failed to be classified correctly by the immu- noassay. Results from quality assur- ance samples with BTX concentrations of 2.5, 25, and 100 ppb also showed that false negative results would be expected at higher than a 5 percent rate when BTX contamination levels were between 25 and 100 ppb. How- ever, for samples with higher BTX lev- els, the immunoassay gave excellent results. Two field samples yielded false positive results compared to GC val- ues, but these samples showed signs of low-level gasoline contamination. This technology could provide cost-ef- fective screening or monitoring func- tions at sites with ground water con- taminated by gasoline or other fuels. It could also be used in a laboratory set- ting to select samples for further analy- sis. This Project Summary was developed by EPA's En vironmental Monitoring Sys- tems Laboratory, Las Vegas, NV, to an- nounce 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 The performance of an immunoassay field kit technique was evaluated during a U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) demonstration. This semi-quantitative method was developed by Antox Inc. (South Portland, ME), to detect benzene, toluene, and xylene (BTX) contaminant levels in environmental water samples. The evaluation compared results from BTX immunoassays performed in the field to quantitative results obtained by laboratory-based gas chromatography (GC) using EPA Method 8020. Technology Description The BTX immunoassay is a competitive enzyme-linked immunosorbent assay (ELISA), which uses an antibody-coated polystyrene cuvette as the solid phase. A hapten-enzyme conjugate mimics the free analyte (BTX compounds) and competes with aromatic compounds in the sample for binding sites on the immobilized anti- body. The test is performed by placing Printed on Recycled Paper ------- reference and test solutions in separate coated cuvettes in which competition for binding to the antibody occurs. After a 10- minute Incubation step, substrate and chro- mogen are added, and a colored enzymatic reaction product is formed. The optical density (OD) of the reference and sample cuvettes Is determined using a portable colorimeter, and the ratio of sample to reference OD values is deter- mined. The color intensity is inversely pro- portional to the BTX hydrocarbon level in the test sample. Low sample-to-reference ratios are associated with high BTX con- centrations and high ratios with low BTX concentrations. The developer had se- lected a ratio of 0.85 as the decision level, with all samples having a ratio less than 0.85 being labeled as having 25 ppb BTX or greater. The laboratory confirmatory method was gas chromatography following EPA Method 8020 using the purge-and-trap sample preparation technique in EPA Method 5030. Demonstration Design Seventy-nine field samples were ob- tained from four separate monitoring well- fields in the Las Vegas valley during the first quarter of 1992. Three of these sites represented gasoline sources and the fourth site had wells that might also be contaminated with other hydrocarbon mix- tures, such as jet fuel or diesel fuel. Each sample well was purged of three well- volumes prior to sampling to remove stag- nant water from the well and surrounding aquifer. Sample splits were placed in clear 40-mL volatile organic analysis (VOA) vi- als with Teflon septums. The field immu- noassay sample split was run in duplicate on-site and the other sample splits were maintained at 4°C until analysis. In addi- tion to sample blanks, a variety of quality assurance samples were prepared having concentrations from 2.5 to 100 ppb BTX. These samples were used to check for sample stability, transportation and stor- age problems, and to verify the perfor- mance characteristics of the GC method. Results and Discussion Of the 79 field samples, 36 were deter- mined to be above 25 ppb BTX by GC analysis while 43 samples had concentra- tions below the 25 ppb criteria of the im- munoassay. Two (six percent) of the positive samples gave false negative re- sults on both replicate analyses. One of these samples had 35.5 ppb and the other had 74.8 ppb BTX. Two (five percent) of the negative samples gave false positive results on both replicate analyses. How- ever, each of these samples was associ- ated with minor levels of gasoline contamination. A plot of sample to reference OD ratios vs. BTX concentration as determined from GC analysis revealed the expected sigmoidal curve shape. However, there was significant variability in the S/R ratio. for a given concentration level. In the re- gion of 25 to 100 ppb BTX, this variability hindered the immunoassay from perform- ing up to the developer's expectations. Evaluation of quality assurance samples having concentrations from 2.5 to 100 ppb BTX also showed that a greater than five percent chance of false negatives would be expected up to approximately 100 ppb BTX. For higher level samples, the immu- noassay worked quite well. Conclusions and Recommendations The BTX immunoassay performed well for most samples evaluated in this study. The immunoassay was portable, easy to use, inexpensive, and provided a rapid estimate of BTX concentration that would prove useful in certain applications. For instance, this method could prove useful in mapping the distribution of contami- nants at a site or for monitoring changes in contaminant levels over time. Samples with BTX concentrations above 100 ppb were accurately identified. Only five per- cent of the samples were misclassified based on replicate determinations. The false negative and quality assurance re- sults suggest that the current formulation of the BTX immunoassay is riot robust enough to accurately deal with samples in the range of 25 to 100 ppb BTX (as the manufacturer claims). If one wants to be very accurate in this range, a more sensi- tive format should be developed. An addi- tional area for development that was identified by this demonstration was the need for a stable low-level performance standard or a simple procedure for gener- ating these types of standards. The information in this document has been funded wholly or in part by the U.S. Environmental Protection Agency under Contract Number 68-CO-0049 to Lockheed Engineering & Sciences Company. It has been subjected to the Agency's peer and administrative review, and it has been ap- proved for publication as an EPA docu- ment. Mention of trade names and commercial products does not constitute endorsement or recommendation for use. •fru.S. GOVERNMENT PRINTING OFFICE: I9t3 - 75O-07I/8O078 ------- ------- R.W. Gerlach, R.J. White, and N.F.D. O'Leary are with Lockheed Engineering & Sciences Company, Las Vegas, NV 89119. The EPA author, J.M. Van Emon, (also the EPA Project Officer, see below) is with Environmental Monitoring Systems Laboratory, Las Vegas NV 89193-3478. Ths complete report, entitled "Superfund Innovative Technology Evaluation (SITE) Program Evaluation Report For AntoxBTX Water Screen (BTX immunoassay)," (Order No. PB93-218337; Cost: $27.00; 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: Environmental Monitoring Systems Laboratory U.S. Environmental Protection Agency Las Vegas NV 89193-3478 United States Environmental Protection Agency Center for Environmental Research Information Cincinnati, OH 45268 Official Business Penalty for Private Use $300 BULK RATE POSTAGE & FEES PAID EPA PERMIT No. G-35 EPA/540/SR-93/518 ------- |