Grantee Research Project Results
1998 Progress Report: Rapid Field Determination of Organic Contaminants in Water by Solid Phase Microextraction and Infrared Spectroscopy
EPA Grant Number: R825343Title: Rapid Field Determination of Organic Contaminants in Water by Solid Phase Microextraction and Infrared Spectroscopy
Investigators: Tilotta, David C.
Institution: University of North Dakota
Current Institution: Columbia University in the City of New York
EPA Project Officer: Chung, Serena
Project Period: January 1, 1997 through December 31, 1998 (Extended to December 31, 1999)
Project Period Covered by this Report: January 1, 1998 through December 31, 1999
Project Amount: $205,350
RFA: Analytical and Monitoring Methods (1996) RFA Text | Recipients Lists
Research Category: Ecological Indicators/Assessment/Restoration , Environmental Statistics , Water , Air , Land and Waste Management
Objective:
The objectives of this research project are to: (1) identify suitable solid phase films for determining organic contaminants in water by solid phase microextraction coupled with infrared spectroscopy (SPME/IR), (2) determine which organic contaminants are amenable to the SPME/IR method, and (3) adapt the basic methodology to field use.Progress Summary:
Progress on this research project was slowed last year because of the severe flooding that occurred in Grand Forks, but since then it has begun to progress normally. We anticipate that this project will be completed at the end of 1999.Solid Phases. Of the many solid phases examined to date, four polymers have been found to be useful: Parafilm MTM (a wax-impregnated polymer/rubber composite), Poly(dimethylsiloxane) (PDMS, an important solid phase material of the SPME syringe technology), Teflon PFATM (a perfluoroalkoxy teflon polymer), and a poly(dimethylsiloxane)/polycarbonate copolymer.
Analyte Classes. Four classes of compounds have been examined for their suitability as analytes for SPME/IR using the aforementioned films: crop protection chemical, petroleum hydrocarbons, chlorinated hydrocarbons, and nitroaromatic explosives. Formal equilibration times, linear dynamic ranges, detection limits, and precision data for these classes for the appropriate solid phase film have been acquired.
The bulk of this last year was spent developing and testing a SPME/IR field method for determining total gasoline-range organics (TGRO) in water. In this method, the organic compounds are extracted from 250 mL of water into a small square (3.2 cm x 3.2 cm x 130 mm thick) of Teflon PFATM film. This film, a poly(perfluoroalkoxyethylene) polymer, lacks C-H bonds and makes it possible to quantitate the extracted organics directly in it through their C-H stretching vibrations. Three gasoline-range fuels?unleaded gasoline, aviation gas, and lighter fuel (petroleum naphtha)?were chosen to evaluate the SPME/IR procedure. Preliminary experiments show that method detection limits are in the 0.5-1.5 ppm range for spiked solutions, and precision is relatively good (6-11 percent relative standard deviations [RSDs]). Linear dynamic ranges of calibration extend to the water solubility limits for all fuels studied. The potential of this SPME/IR method for determining TGRO in natural "real world" water samples was investigated by extracting wastewater contaminated with gasoline. In this procedure, a commercially available gas chromatography standard was used to calibrate the SPME/IR method. The results obtained from the SPME/IR determination of the TGRO in two wastewater samples were in reasonable agreement with those obtained from standard purge-and-trap gas chromatographic analysis. Finally, preliminary application of this method in the field (at a petroleum tank farm) for TGRO analysis of contaminated water yielded excellent results.
Analysis of nitroaromatic explosive-related compounds (e.g., trinitrotoluene, aminonitrotoluenes, dinitrotoluenes, etc.) currently is ongoing using the SPME/IR approach. A poly(dimethylsiloxane)/polycarbonate copolymer has been identified as a selective and sensitive (e.g., detection limits in the ppb range) solid phase for this application.
Future Activities:
Future SPME/IR work will involve: (1) continuing the identification of suitable solid phase films, (2) expanding the basic methodology to explosive-related compounds, and (3) demonstrating the approach in field environments.Journal Articles on this Report : 2 Displayed | Download in RIS Format
| Other project views: | All 6 publications | 4 publications in selected types | All 3 journal articles |
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Merschman SA, Lubbad SH, Tilotta DC. Poly(dimethylsiloxane) films as sorbents for solid-phase microextraction coupled with infrared spectroscopy. Journal of Chromatography 1998;829(1-2):377-384. |
R825343 (1998) R825343 (Final) |
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Stahl DC, Tilotta DC. Partition infrared method for total gasoline range organics in water based on solid phase microextraction. Environmental Science & Technology 1999;33(5):814-819. |
R825343 (1998) R825343 (Final) |
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Supplemental Keywords:
analytical, measurement method, monitoring, water, gasoling, fuels, nitroaromatics, explosives, petroleum hydrocarbons, chlorinated hydrocarbons., Scientific Discipline, Ecosystem Protection/Environmental Exposure & Risk, Engineering, Chemistry, Environmental Chemistry, Monitoring/Modeling, Physics, hydrocarbons, chromatograph, Fourier transform infrared, gas chromatography, environmental monitoring, solid phase microextraction, spectroscopic, organic contaminants, solvents, FTIR, PAH, rapid field determinationProgress and Final Reports:
Original AbstractThe perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Conclusions drawn by the principal investigators have not been reviewed by the Agency.