Je. Longbottom et al., DETERMINATION OF TRACE-ELEMENTS IN WATER BY INDUCTIVELY-COUPLED PLASMA-MASS SPECTROMETRY - COLLABORATIVE STUDY, Journal of AOAC International, 77(4), 1994, pp. 1004-1023
A joint U.S. Environmental Protection Agency (U.S. EPA)-AOAC interlabo
ratory method validation study was conducted on U.S. EPA method 200.8,
Determination of Trace Elements in Waters and Wastes by Inductively C
oupled Plasma-Mass Spectrometry. The purpose of the study was to deter
mine and compare the mean recovery and precision of the inductively co
upled plasma-mass spectrometry (ICP-MS) analyses for 20 trace elements
in reagent water, drinking water, and ground-water. The formal study
was based on Youden's nonreplicate plan for collaborative tests of ana
lytical methods. The test waters were spiked with the 20 trace element
s at 6 concentration levels in the 0.8-200 mug/L range, prepared as 3
Youden pairs. Thirteen collaborators spiked 100 mL aliquots of the tes
t waters, acidified them with 1 mL concentrated HN03 and 0.5 mL concen
trated HCl, reduced the volume to 20 mL by heating in an open beaker a
t 85-degrees-C, refluxed them for 30 min at 95-degrees-C, and diluted
them to 50 mL. After centrifuging or settling the samples, a 20 mL por
tion of the supernatant was diluted to 50 mL and analyzed by ICP-MS. R
elated experiments evaluated the method performance in wastewater and
wastewater digestate at a single concentration pair, and an alternativ
e nitric acid digestion procedure. Mean recoveries for reagent water,
drinking water, and groundwater were generally 95-105% with between-la
boratory relative standard deviations about 4-8%. The method also work
ed well with wastewaters and digestate, with between-laboratory relati
ve standard deviations averaging 8% and recoveries averaging 100%. Rec
overies of silver, however, were low in all matrixes at concentrations
over 100 mug/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.