A heated purge-and-trap gas chromatography/mass spectrometry method was used to determine the cis- and trans-isomers of (4-methylcyclohexyl)methanol (4-MCHM), the reported major component of the Crude MCHM/Dowanol™ PPh glycol ether material spilled into the Elk River upriver from Charleston, West Virginia, on January 9, 2014. The trans-isomer eluted first and method detection limits were 0.16-μg L(-1)trans-, 0.28-μg L(-1)cis-, and 0.4-μg L(-1) Total (total response of isomers) 4-MCHM. Estimated concentrations in the spill source material were 491-g L(-1)trans- and 277-g L(-1)cis-4-MCHM, the sum constituting 84% of the source material assuming its density equaled 4-MCHM. Elk River samples collected⩽3.2 km downriver from the spill on January 15 had low (⩽2.9 μg L(-1) Total) 4-MCHM concentrations, whereas the isomers were not detected in samples collected 2 d earlier at the same sites. Similar 4-MCHM concentrations (range 4.2-5.5 μg L(-1) Total) occurred for samples of the Ohio River at Louisville, Kentucky, on January 17, ∼630 km downriver from the spill. Total 4-MCHM concentrations in Charleston, WV, office tap water decreased from 129 μg L(-1) on January 27 to 2.2 μg L(-1) on February 3, but remained detectable in tap samples through final collection on February 25 indicating some persistence of 4-MCHM within the water distribution system. One isomer of methyl 4-methylcyclohexanecarboxylate was detected in all Ohio River and tap water samples, and both isomers were detected in the source material spilled.

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...

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Twenty-two bottom-sediment samples were collected from Town Lake in Austin, Texas, in 1991 and 1992 and analyzed for chlorinated insecticides by a reconnaissance-quality, electron-capture gas chromatography screening method developed by the U.S. Geological Survey (USGS). Four different chlorinated insecticides (aldrin, chlordane, dieldrin, and p,p'-DDT) and two degradation products of p,p'-DDT (p,p'-DDD and p,p'-DDE) were detected in these samples. The most significant insecticides detected were chlordane, which was detected in 20 of the 22 samples at concentrations that ranged from 26 to 140 micrograms per kilogram, and p,p'-DDT, which was detected in all 22 samples at concentrations that ranged from 5 to 40 micrograms per kilogram. Degradation products of p,p'-DDT were detected in all 22 samples. Concentrations of p,p'-DDD ranged from not detected to 117 micrograms per kilogram and for p,p'-DDE from 9 to 97 micrograms per kilogram. Of the 22 samples collected, 15 also were analyzed by the standard USGS laboratory analytical method for chlorinated insecticides to determine the comparability of the two methods. Correlation coefficients were calculated for chlordane (0.8662), p,p'-DDT (0.6393), p,p'-DDD (0.9401), p,p'-DDE (0.8595), and dieldrin (0.3819). A paired sign test at the 95 percent confidence level showed no significant difference between the screening method and the laboratory analytical method for all detected insecticides except aldrin. P-values were calculated from the data for chlordane (1.0000), p,p'-DDT (0.1796), p,p'-DDD (1.0000), p,p'-DDE (0.1796), and dieldrin (0.2891).