Determination of Trace Elements in Water by Inductively Coupled Plasma–Mass Spectrometry: Collaborative Study

Abstract

A joint U.S. Environmental Protection Agency (U.S. EPA)—AOAC interlaboratory method validation study was conducted on U.S. EPA method 200.8, Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma–Mass Spectrometry. The purpose of the study was to determine and compare the mean recovery and precision of the inductively coupled plasma–mass spectrometry (ICP–MS) analyses for 20 trace elements in reagent water, drinking water, and groundwater. The formal study was based on Youden’s nonreplicate plan for collaborative tests of analytical methods. The test waters were spiked with the 20 trace elements at 6 concentration levels in the 0.8–200 μg/L range, prepared as 3 Youden pairs. Thirteen collaborators spiked 100 mL aliquots of the test waters, acidified them with 1 mL concentrated HNO3 and 0.5 mL concentrated HCl, reduced the volume to 20 mL by heating in an open beaker at 85°C, refluxed them for 30 min at 95°C, and diluted them to 50 mL. After centrifuging or settling the samples, a 20 mL portion of the supernatant was diluted to 50 mL and analyzed by ICP–MS. Related experiments evaluated the method performance in wastewater and wastewater digestate at a single concentration pair, and an alternative nitric acid digestion procedure. Mean recoveries for reagent water, drinking water, and groundwater were generally 95–105% with between-laboratory relative standard deviations about 4–8%. The method also worked well with wastewaters and digestate, with between-laboratory relative standard deviations averaging 8% and recoveries averaging 100%. Recoveries of silver, however, were low in all matrixes at concentrations over 100 μg/L. The nitric acid digestion procedure was comparable in accuracy and precision to the mixed-acid digestion in U.S. EPA method 200.8. The method was adopted first action by AOAC INTERNATIONAL.