Grantee Research Project Results
1997 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, 1997 through December 31, 1998
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: identify suitable solid phase films for determining organic contaminants in water by SPME/IR, determine which organic contaminants are amenable to the SPME/IR method, and adapt the basic methodology to field use.Progress Summary:
Progress on this research project was slowed because of the severe flooding that occurred in Grand Forks this last spring. Although only six weeks of actual time were lost, the unexpected loss of two students (because of further flood concerns) resulted in the additional loss of ca. 3 months. Nonetheless, reasonable progress has been made in attaining the goals outlined in the proposal.Accomplishments and Research Results:
Solid Phases. Of the many solid phases examined to date, three 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) and Teflon PFATM (a perfluoroalkoxy teflon polymer).Analyte Classes. To date, three classes of compounds have been examined for their suitability as analytes for SPME/IR using the three aforementioned films. Formal equilibration times, linear dynamic ranges, detection limits, and precision data, expressed as percent relative standard deviation (%RSD), for these classes for the appropriate solid phase film are shown in Table 1. Multiple entries in this table for a given analyte imply that more than one film is useful. Conversely, the absence of an entry for a given analyte/film combination indicates that that film is not suitable for the analysis.
Volatile organic compounds (VOCs) examined include the BTEX compounds (benzene, toluene, ethylbenzene, xylenes), and halocarbons such as carbon tetrachloride, chlorobenzene, chloroform, and p-chlorotoluene. Parafilm MTM and PDMS both have been useful for the analytical determination of these compounds. SPME/IR analyses using Parafilm has demonstrated the ability of SPME/IR in distinguishing four of the six alkylbenzenes (benzene, o-xylene, m-xylene, p-xylene) in a petroleum industry wastewater sample. Quantitation by simple univariate calibration based on absorbance band heights have provided good agreement with purge and trap GC/MS standard methods. Analytical determinations of ethylbenzene and toluene are, however, complicated by the spectral overlap of other components known to be in gasoline.
Gasoline fuels include the more volatile organics such as small-chain hydrocarbons and, as previously discussed, the BTEX compounds. Teflon PFATM has been found to successfully extract gasoline-range organics (GROs) from water and to provide a clear spectral region for identification and quantitation. SPME/IR analysis of the C-H stretching region provides a method for determining a group of substances. Whereas Parafilm and PDMS provides a means of identifying individual components of multicomponent mixtures, PFA is more useful for analysis of the mixture itself. The two films thus compliment one another in terms of the selectivity they provide.
Analysis of pesticides and herbicides are currently underway using the SPME/IR approach. Poly(dimethylsiloxane) has been identified as the only solid phase that can successfully be used to determine trifluralin in aqueous solutions by SPME/IR.
Future Activities:
Future SPME/IR work will involve: 1) continuing the identification of suitable solid phase films, 2) expanding the basic methodology to pesticides and herbicides, and 3) demonstrating the approach in field environments.Journal Articles:
No journal articles submitted with this report: View all 6 publications for this projectSupplemental Keywords:
chemicals, toxic substances, volatile organic compounds, VOCs, nonaqueous phase liquid, NAPL, clean technologies, waste minimization, analytical, measurement methods, agriculture, petroleum, environmental chemistry., 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.