National Water Quality Laboratory

Friday October 19, 2018

USGS Open-File Report 99-464

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory — Determination of Whole-Water Recoverable Arsenic, Boron, and Vanadium Using Inductively Coupled Plasma-Mass Spectrometry

John R. Garbarino


Analysis of in-bottle digestate by using the inductively coupled plasma-mass spectrometric (ICP-MS) method has been expanded to include arsenic, boron, and vanadium. Whole-water samples are digested by using either the hydrochloric acid in-bottle digestion procedure or the nitric acid in-bottle digestion procedure. When the hydrochloric acid in-bottle digestion procedure is used, chloride must be removed from the digestate by subboiling evaporation before arsenic and vanadium can be accurately determined. Method detection limits for these elements are now 10 to 100 times lower than U.S. Geological Survey (USGS) methods using hydride generation-atomic absorption spectrophotometry (HG-AAS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES), thus providing lower variability at ambient concentrations. The bias and variability of the methods were determined by using results from spike recoveries, standard reference materials, and validation samples. Spike recoveries in reagent-water, surface-water, ground-water, and whole-water recoverable matrices averaged 90 percent for seven replicates; spike recoveries were biased from 25 to 35 percent low for the ground-water matrix because of the abnormally high iron concentration. Results for reference material were within one standard deviation of the most probable value. There was no significant difference between the results from ICP-MS and HG-AAS or ICP-AES methods for the natural whole-water samples that were analyzed.

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