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Last modified
7/14/2009 5:02:34 PM
Creation date
5/22/2009 5:20:50 PM
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UCREFRP
UCREFRP Catalog Number
8277
Author
Bauch, N. J. and N. E. Spahr.
Title
Pesticides in Surface Waters of the Upper Colorado River Basin, Colorado, 1996-98.
USFW Year
2000.
USFW - Doc Type
Water-Resources Investigations Report 00-4005,
Copyright Material
NO
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criteria during analysis, and only the concentration is <br />estimated, not the presence (National Water Quality <br />Laboratory, 1996). Throughout this report, estimated <br />concentrations above the MRL were treated as normal <br />concentrations, whereas estimated concentrations <br />below the MRL were treated as "less than" concentra- <br />tions. <br />Acknowledgments <br />We thank Bob Boulger, Jeff Foster, Dave Hartle, <br />Dennis Smits, and Rick Szmajter, USGS, for their <br />efforts in collecting the water samples for the data <br />analyzed here. Dave Butler, USGS, provided valuable <br />insight into site selection for the synoptic study of <br />agricultural drains in the Grand and Uncompahgre <br />River Valleys. Thanks also are extended to Joe Doma- <br />galski and Bob Kimbrough for technical review of the <br />manuscript and to Mary Kidd for editorial review, <br />John Evans for design, and Alene Brogan for manu- <br />script and layout. <br />QUALITY-CONTROL METHODS AND <br />RESULTS <br />Quality-control (QC) samples were used to <br />assess the bias and variability of water-quality data <br />that may be introduced by sample collection, <br />processing, shipping, and analysis. Without QC <br />samples, the quality of the data collected cannot be <br />determined. Field-blank, replicate, and field-matrix- <br />spike samples were collected and processed as QC <br />samples using the same equipment and procedures as <br />the stream-water or environmental samples in order to <br />evaluate the bias and variability of the pesticide data. <br />Pesticide surrogate solutions were added to each envi- <br />ronmental and quality-assurance sample in the labora- <br />tory as an additional QC mechanism. The same QC <br />procedures were used in the fixed-station and synoptic <br />sampling. Quality-control data for both sampling <br />programs were analyzed together. Further information <br />on QC in the NAWQA Program and QC samples is <br />described in Shelton (1994). <br />Field-blank samples were used to test for bias, <br />the systematic error inherent in sampling and analyt- <br />ical methods (Spahr and Boulger, 1997). Blank <br />samples were organic-free water that did not contain <br />detectable concentrations of the pesticides of interest. <br />The blank water, Baker Analyzed HPLC (J.T. Baker <br />Company, Phillipsburg, New York), was processed <br />through the sampling equipment and handled as if it <br />were a typical stream sample. Because pesticides in a <br />water sample can be detected at low concentrations in <br />the laboratory, field blanks are important in deter- <br />mining possible contamination of a sample from <br />collection, processing, cleaning, shipping, and anal- <br />ysis procedures. <br />Replicate samples were two or four samples <br />collected simultaneously or in sequence in order to <br />yield samples of nearly identical composition. Repli- <br />cates provide information on the precision of concen- <br />tration values and the consistency in identifying <br />targeted pesticides. As such, replicate samples test for <br />variability, the degree of random error in independent <br />measurements of the same quantity (Spahr and <br />Boulger, 1997). Replicate analysis is based on the <br />comparison of the analytical results of the environ- <br />mental sample with the analytical results of the QC <br />sample or samples. Replicates were analyzed by the <br />relative percent difference between replicate samples, <br />calculated by dividing the difference in concentration <br />between two replicate samples by the mean concentra- <br />tion of the two replicate samples and multiplying the <br />result by 100. Where more than two samples were <br />collected at a site, a range of relative percent differ- <br />ences was calculated. <br />The field-matrix-spike sample was an environ- <br />mental sample that had been spiked with a solution <br />containing targeted pesticides and then analyzed as a <br />typical water-quality sample. Specifically, one liter of <br />each environmental sample to be analyzed by GC/MS <br />was spiked with the targeted pesticides at a concentra- <br />tion of 0.1 µg/L, while another liter, for HPLC anal- <br />ysis, was spiked with targeted pesticides at a <br />concentration of 1 µg/L. The spiked samples were <br />used to identify the recoverability of pesticides in the <br />environmental samples. Pesticide recovery can be <br />affected by pesticide degradation, interference from <br />other organic substances or matter in the sample, and <br />laboratory analysis. Spike solutions were provided by <br />the USGS NWQL. <br />Pesticide-spike-recovery data were calculated in <br />three steps. First, the expected or theoretical concen- <br />tration of the spiked sample was determined by multi- <br />plying the concentration of the spike solution with the <br />amount of spike added to the environmental sample <br />and then dividing the result by the sample volume. <br />QUALITY-CONTROL METHODS AND RESULTS 13 <br />
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