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Mobile and persistent chemicals that are present in urban wastewater, such as pharmaceuticals, may survive on-site or municipal wastewater treatment and post-discharge environmental processes. These pharmaceuticals have the potential to reach surface and groundwaters, essential drinking-water sources. A joint, two-phase U.S. Geological Survey-U.S. Environmental Protection Agency study examined source and treated waters from 25 drinking-water treatment plants from across the United States. Treatment plants that had probable wastewater inputs to their source waters were selected to assess the prevalence of pharmaceuticals in such source waters, and to identify which pharmaceuticals persist through drinking-water treatment. All samples were analyzed for 24 pharmaceuticals in Phase I and for 118 in Phase II. In Phase I, 11 pharmaceuticals were detected in all source-water samples, with a maximum of nine pharmaceuticals detected in any one sample. The median number of pharmaceuticals for all 25 samples was five. Quantifiable pharmaceutical detections were fewer, with a maximum of five pharmaceuticals in any one sample and a median for all samples of two. In Phase II, 47 different pharmaceuticals were detected in all source-water samples, with a maximum of 41 pharmaceuticals detected in any one sample. The median number of pharmaceuticals for all 25 samples was eight. For 37 quantifiable pharmaceuticals in Phase II, median concentrations in source water were below 113ng/L. For both Phase I and Phase II campaigns, substantially fewer pharmaceuticals were detected in treated water samples than in corresponding source-water samples. Seven different pharmaceuticals were detected in all Phase I treated water samples, with a maximum of four detections in any one sample and a median of two pharmaceuticals for all samples. In Phase II a total of 26 different pharmaceuticals were detected in all treated water samples, with a maximum of 20 pharmaceuticals detected in any one sample and a median of 2 pharmaceuticals detected for all 25 samples. Source-water type influences the presence of pharmaceuticals in source and treated water. Treatment processes appear effective in reducing concentrations of most pharmaceuticals. Pharmaceuticals more consistently persisting through treatment include carbamazepine, bupropion, cotinine, metoprolol, and lithium. Pharmaceutical concentrations and compositions from this study provide an important base data set for further sublethal, long-term exposure assessments, and for understanding potential effects of these and other contaminants of emerging concern upon human and ecosystem health.
This report presents precision and accuracy data for volatile organic compounds (VOCs) in the nanogram-per-liter range, including aromatic hydrocarbons, reformulated fuel components, and halogenated hydrocarbons using purge and trap capillary-column gas chromatography/mass spectrometry. One-hundred-four VOCs were initially tested. Of these, 86 are suitable for determination by this method. Selected data are provided for the 18 VOCs that were not included. This method also allows for the reporting of semiquantitative results for tentatively identified VOCs not included in the list of method compounds. Method detection limits, method performance data, preservation study results, and blank results are presented.The authors describe a procedure for reporting low-concentration detections at less than the reporting limit. The nondetection value (NDV) is introduced as a statistically defined reporting limit designed to limit false positives and false negatives to less than 1 percent. Nondetections of method compounds are reported as "less than NDV." Positive detections measured at less than NDV are reported as estimated concentrations to alert the data user to decreased confidence in accurate quantitation. Instructions are provided for analysts to report data at less than the reporting limits. This method can support the use of either method reporting limits that censor detections at lower concentrations or the use of NDVs as reporting limits. The data-reporting strategy for providing analytical results at less than the reporting limit is a result of the increased need to identify the presence or absence of environmental contaminants in water samples at increasingly lower concentrations.Long-term method detection limits (LTMDLs) for 86 selected compounds range from 0.013 to 2.452 micrograms per liter (ug/L) and differ from standard method detection limits (MDLs) in that the LTMDLs include the long-term variance of multiple instruments, multiple operators, and multiple calibrations over a longer time. For these reasons, LTMDLs are expected to be slightly higher than standard MDLs. Recoveries for all of the VOCs tested ranged from 36 (tert-butyl formate) to 155 percent (pentachlorobenzene). The majority of the compounds ranged from 85 to 115 percent recovery and had less than 5 percent relative standard deviation for concentrations spiked between 1 to 500 (o,g/L in volatile blank-, surface-, and ground-water samples. Recoveries of 60 set spikes at low concentrations ranged from 70 to 114 percent (1,2,3trimethylbenzene and acetone). Recovery data were collected over 6 months with multiple instruments, operators, and calibrations.In this method, volatile organic compounds are extracted from a water sample by actively purging with helium. The VOCs are collected onto a sorbent trap, thermally desorbed, separated by a Megabore gas chromatographic capillary column, and finally determined by a full-scan quadrupole mass spectrometer. Compound identification is confirmed by the gas chromatographic retention time and by the resulta...
A combined field and laboratory study was conducted to compare purge and trap gas chromatography/mass spectrometry (PT‐GC/MS) and purgeable organic chloride (POC1) analysis for measuring volatile chlorinated hydro‐carbons (VCH) in ground water. Distilled‐water spike and recovery experiments using 10 VCH indicate that at concentrations greater than 1 /ig/1 recovery is more than 80 percent for both methods with relative standard deviations of about 10 percent. Ground‐water samples were collected from a site on Cape Cod, Massachusetts, where a shallow unconfined aquifer has been contaminated by VCH, and were analyzed by both methods. Results for PT‐GC/MS and POC1 analysis of the ground‐water samples were not significantly different (alpha = 0.05, paired t‐test analysis) and indicated little bias between the two methods. Similar conclusions about concentrations and distributions of VCH in the ground‐water contamination plume were drawn from the two data sets. However, only PT‐GC/MS analysis identified the individual compounds present and determined their concentrations, which was necessary for toxicological and biogeochemical evaluation of the contaminated ground water. POC1 analysis was a complimentary method for use with PT‐GC/MS analysis for identifying samples with VCH concentrations below the detection limit or with high VCH concentrations that require dilution. Use of POC1 as a complimentary monitoring method for PT‐GC/MS can result in more efficient use of analytical resources.
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