Field and Laboratory Quality Assurance

Citation

Elliott, S.M., Lee, K.E., Brigham, M.E., Langer, S.K., Trombley, M.M., Menheer, M.A., Furlong, E.T., Foreman, W.T., Jorgenson, Z.G., Choy, S.J., Moore, J.N., Banda, J.B., and Gefell, D.J., 2015, Chemicals of Emerging Concern in Water and Bottom Sediment in Great Lakes Areas of Concern, 2013—Analytical Methods, Collection Methods, Environmental Data, and Quality Assurance: U.S. Geological Survey Data Release, https://doi.org/10.5066/F7DF6P9D.

Summary

Several quality-control measures were implemented both in the field and at the laboratory to evaluate the integrity of the data being generated. Sample replicates and blank samples were collected in the field. Surrogate standards, isotope dilution standards, matrix spikes, reagent blank-water spikes, and reagent blank-sediment samples were prepared in the laboratory. Quality control measures used in 2013 were similar to those used in previous years of the study. Detailed descriptions and how the quality-assurance data are used can be found in Lee and others (2012) for data collected in 2010-11 and in Lee and others (2015) for data collected in 2012 for the same study. References: Lee, K.E., Langer, S.K., Menheer, M.A., [...]

Summary

Several quality-control measures were implemented both in the field and at the laboratory to evaluate the integrity of the data being generated. Sample replicates and blank samples were collected in the field. Surrogate standards, isotope dilution standards, matrix spikes, reagent blank-water spikes, and reagent blank-sediment samples were prepared in the laboratory. Quality control measures used in 2013 were similar to those used in previous years of the study. Detailed descriptions and how the quality-assurance data are used can be found in Lee and others (2012) for data collected in 2010-11 and in Lee and others (2015) for data collected in 2012 for the same study.

References:

Lee, K.E., Langer, S.K., Menheer, M.A., Foreman, W.T., Furlong, E.T., and Smith, S.G., 2012, Chemicals of emerging concern in water and bottom sediment in Great Lakes areas of concern, 2010 to 2011—Collection methods, analyses methods, quality assurance, and data: U.S. Geological Survey Data Series 723, 26 p., http://pubs.usgs.gov/ds/723/.

Lee, K.E., Langer, S.K., Menheer, M.A., Hansen, D.S., Foreman, W.T., Furlong, E.T., Jorgenson, Z.G., Choy S.J., Moore, J.N., Banda, JoAnn, Gefell, D.J., 2015, Chemicals of emerging concern in water and bottom sediment in the Great Lakes Basin, 2012—Collection methods, analytical methods, quality assurance, and study data: U.S. Geological Survey Data Series 910, 14 p., http://dx.doi.org/10.3133/ds910.

Field Quality Assurance

Field blank water samples were collected to assess potential contamination sources introduced during sample collection and processing. Three field blank water samples were collected in 2013; analytical results are included in "2013WaterData" in the   'Environmental Data' section of this directory. Seven pharmaceuticals were detected in one of the field blank samples; no compounds were detected in the other two field blank samples. Environmental concentrations less than three times the highest field blank concentration were considered to be affected by blank-related contamination and assigned a 'Cf' qualifier, which is located immediately after the value in "2013WaterData" and "2013Data_by_Result" in the 'Environmental Data' section of this directory. For the seven compounds detected in field blank samples, 12 samples were considered affected by blank-related contamination for 1,7-dimethylxanthine; 42 samples for caffeine; 2 samples for glipizide; 37 samples for lidocaine; 19 samples for metformin; 0 samples for sulfadimethoxine; and 14 samples for sulfamethoxazole.

Field replicate samples (see spreadsheet file) were collected to assess variability in results from point of sample collection through analysis. Variability was characterized by calculating the relative percent difference for each compound between each replicate pair. A summary of relative percent difference and detection consistency for water and sediment field replicate samples is provided in "2013Replicates". Relative percent difference is calculated by dividing the absolute difference in environmental concentrations between the environmental and replicate samples by the mean concentration of the two samples and multiplying by 100.

Five water replicate sample pairs were collected for analysis of wastewater compounds (schedule 4433) and pharmaceuticals in filtered water (schedule 2440), 1 replicate sample pair for analysis of pharmaceuticals in unfiltered water (schedule 8244), and 6 replicate sample pairs for analysis of steroid hormones, sterols, and bisphenol A (schedule 4434) during 2013 ("2013WaterData"). Mean relative percent differences ranged from 0 to 66.7 for wastewater compounds (schedule 4433) in unfiltered water, 3.4 to 19 for steroid hormones, sterols, and bisphenol A (schedule 4434) in unfiltered water, and 7 to 74 for pharmaceuticals (schedule 2440) in filtered water. Only one replicate sample pair was analyzed by research method 8244 for pharmaceuticals in unfiltered water, relative percent difference ranged from 25 to 121 for all compounds.

Four bottom-sediment replicate sample pairs were collected during 2013 ("2013SedimentData"). Mean relative percent differences ranged from 6 to 73 for wastewater compounds (schedule 5433) and 12 to 128 for steroid hormones, sterols, and bisphenol A (research method 6434). Seventeen replicate sample pairs were analyzed for human-use pharmaceuticals and antidepressants (research method 9008). Mean relative percent differences ranged from 20 to 94 for human-use pharmaceuticals and 20 to 43 for antidepressants.

Laboratory Quality Assurance

This directory also includes summaries of percent recovery of laboratory matrix-spike samples, compound detections in laboratory-blank samples, percent recovery of laboratory reagent-matrix spike samples, surrogate standards, and isotope dilution standard (IDS) compounds that were analyzed with environmental samples.

Laboratory-matrix spike samples for water and bottom sediment were prepared to evaluate recovery performance of compounds in samples collected at specific sites. Recovery of target analytes and statistics for laboratory-matrix spike samples are provided in "2013WaterMatrixSpikeRecovery" and "2013SedimentMatrixSpikeRecovery" in this directory.

Three laboratory-matrix spike water samples were collected during 2013. Mean percent recovery for wastewater compounds (schedule4433) in unfiltered water ranged from 33 to 195. Mean percent recovery for steroid hormones, sterols, and bisphenol A (schedule 4434) in unfiltered water ranged from 74 to 111. Mean percent recovery for pharmaceuticals (schedule 2440) in filtered water ranged from 53 to 394. No field-matrix spike water samples were analyzed for schedule 8244. Mean recoveries for most compounds in these methods were within the range (60-120) of what is typically deemed to be acceptable recovery rates (W.T. Foreman and R.B. Green, U.S. Geological Survey National Water Quality Laboratory, written communication, 2014).

Two laboratory-matrix spike bottom-sediment samples were prepared during 2013 to evaluate recovery of compounds using laboratory schedules 5433 and 6434. Mean percent recovery of wastewater compounds (schedule 5433) ranged from 15 to 157. Mean percent recovery of steroid hormones. sterols, and bisphenol A (research method 6434) ranged from 38 to 117. Fourteen laboratory-matrix spike bottom-sediment samples were prepared during 2013 to evaluate recovery of human-use pharmacetuicals and antidepressants (research method 9008). Mean percent recovery of pharmaceuticals in bottom sediment ranged from 3 to 24. Mean percent recovery of antidepressants in bottom sediment ranged from 3 to 31. Pharmaceutical recoveries of laboratory-matrix spike bottom-sediment samples were substantially lower than anticipated; experiments to identify the reason for this drop in performance are underway (E.T. Furlong, U.S. Geological Survey National Water Quality Laboratory, written communication, 2015).

Laboratory blank-water samples are reagent-water samples or baked reagent-sand matrix simultaneously analyzed with environmental samples that provide information about potential contamination introduced during sample preparation and analysis at the laboratory. "2013LabBlankDetections" provides a summary of compounds detected in laboratory blank-water and blank-sediment samples analyzed with environmental samples collected during 2013. Thirty compounds were detected in at least one laboratory blank-water sample analyzed for wastewater compounds in unfiltered water (schedule 4433), several of which were detected at concentrations that may have affected some environmental sample results. The only compound detected in laboratory blank-water samples analyzed for steroid hormones, sterols, and bisphenol A (schedule 4434) was cholesterol, which was detected in two laboratory blank-water samples. Detected concentrations of cholesterol in the laboratory blank-water samples were substantially lower than environmental concentrations ("2013WaterData") and were assumed to not have affected environmental sample results. Thirty-eight compounds were detected in at least one laboratory blank-water sample analyzed for pharmaceuticals in filtered water (schedule 2440), several of which were detected at concentrations that may have affected some environmental sample results. Thirty-three compounds were detected in at least one laboratory blank-sediment sample analyzed for wastewater compounds (schedule 5433), several of which were detected at concentrations that may have affected some environmental results. No compounds were detected in laboratory blank-sediment samples analyzed for steroid hormones, sterols, and bisphenol A (schedule 6434) or human-use pharmaceuticals and antidepressants (research method 9008).

Laboratory reagent-spike samples are reagent-water and ashed sand-matrix samples spiked with a known concentration of select chemicals that provide information about method performance with time, in the absence of sample matrix. Summaries of recoveries in laboratory reagent-water and reagent-sediment spikes are provided in "2013WaterLaboratoryReagentSpikes" and "2013SedimentLaboratoryReagentSpikes". In water, mean percent recovery of waste water compounds (schedule 4433) ranged from 32 to 143. Mean percent recovery of steroid hormones, sterols, and bisphenol A (schedule 4434) ranged from 80 to 112. Mean percent recovery of pharmaceuticals (schedule 2044) ranged from 50 to 104. In bottom-sediment samples, mean percent recovery of wastewater compounds (schedule 5433) ranged from 15 to 114. Mean percent recovery of 18 wastewater compounds (schedule 5433) was less than 60 percent, and environmental sample results associated with those compounds should be interpreted with caution. Mean percent recovery of steroid hormones, sterols, and bisphenol A (research method 6434) ranged from 83 to 108; all within acceptable range of recovery. Mean percent recovery of human-use pharmaceuticals and antidepressants (research method 9008) ranged from 8 to 22 and 6 to 20, respectively. Pharmaceutical recoveries of laboratory reagent-spike ashed sand matrix samples were substantially lower than anticipated; experiments to identify the reason for this drop in performance are underway (E.T. Furlong, U.S. Geological Survey National Water Quality Laboratory, written communication, 2015).

Surrogate standards and IDS compounds are similar in structure to several of the target method compounds and are used to monitor sample-specific laboratory procedural performance. Additionally, IDS compounds are used to correct chemical concentrations of steroid hormones, sterols, and bisphenol A in unfiltered water (schedule 4434) and bottom sediment (schedule 6434). Mean recoveries, standard deviations, and relative standard deviations (absolute value of the coefficient of variation) for surrogate standards and IDS compounds are provided in "SurrogateRecoveries". Mean percent recovery of surrogate compounds analyzed for wastewater compounds in unfiltered water (schedule 4433) ranged from 47 to 92. Decafluorobiphenyl was the only surrogate standard with a mean percent recovery less than 60. Mean percent recovery of IDS compounds analyzed for steroid hormones, sterols, and bisphenol A in unfiltered water (schedule 4434) ranged from 26 to 84. Progesterone-2,3,4-13C3 was the only IDS compound with a mean percent recovery less than 60. Mean percent recovery of surrogate standards analyzed for pharmaceuticals in filtered water (schedule 2440) ranged from 75 to 119; all within the acceptable range of recovery. In bottom-sediment samples, mean percent recovery of surrogate standard analyzed for wastewater compounds (schedule 5433) ranged from 23 to 73. Mean percent recoveries for bisphenol A-d3 and decafluorobiphenyl were below 60. Mean percent recovery of IDS compounds analyzed for steroid hormones, sterols, and bisphenol A (schedule 6434) ranged from 8 to 63. All compounds except bisphenol A-d16 and mestranol-2,4,16,16-d4 had mean percent recoveries less than 60. Mean percent recovery of surrogate standards analyzed for human-use pharmaceuticals and antidepressants (research method 9008) were all less than 40. Pharmaceutical recoveries of surrogate compounds in bottom-sediment samples were substantially lower than anticipated; experiments to identify the reason for this drop in performance are underway (E.T. Furlong, U.S. Geological Survey National Water Quality Laboratory, written communication, 2015).

Contacts

Author :: Sarah M Elliott, Kathy E Lee, Sue Langer, Molly M Trombley, Michael A Menheer, Mark E Brigham, Edward T Furlong, William T Foreman, Zachary Jorgenson, Steven Choy, Jeremy Moore, JoAnn Banda, Daniel J. Gefell
Point of Contact :: Sarah M Elliot
Distributor :: U.S. Geological Survey - ScienceBase
Metadata Contact :: Sarah M Elliott
USGS Mission Area :: Water Resources
SDC Data Owner :: Upper Midwest Water Science Center

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2013LabBlankDetections.xlsx “Laboratory QA: compound detections in laboratory-blank samples”		20.86 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
2013Replicates.xlsx “Field QA: Replicates Samples”		27.9 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
2013SedimentLaboratoryReagentSpikes.xlsx “Lab QA: percent recovery of laboratory reagent-matrix spike samples for sediment”		22.62 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
2013SedimentMatrixSpikeRecovery.xlsx “Laboratory QA: laboratory matrix-spike samples for sediment”		28.1 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
2013SurrogateRecoveries.xlsx “Laboratory QA: surrogate standards”		18.16 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
2013WaterLaboratoryReagentSpikes.xlsx “Lab QA: percent recovery of laboratory reagent-matrix spike samples for water”		27.18 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
2013WaterMatrixSpikeRecovery.xlsx “Laboratory QA: laboratory matrix-spike samples for water”		28.89 KB	application/vnd.openxmlformats-officedocument.spreadsheetml.sheet
Chemicals_of_Emerging_Concern_in_Sediment_in_Great_Lakes_2013_FieldLabQualityAssurance.xml Original FGDC Metadata	View	31.57 KB	application/fgdc+xml

Field and Laboratory Quality Assurance

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