CCQM-P

IAEA Seibersdorf

1. Analytical method 1.1. Sample decomposition Microwave assisted sample digestion at 200 C for 30 minutes. Average test portion: 0.5 g Acids used: 4 ml HNO3 (Merck Suprapur, 14.6 M), 0.5 ml H2O2 (Merck Suprapur, 30 %) 1.2. Dry weight determination Drying oven at 80 C for 4 h. Sample mass 0.6 g. 1.3. Analysis Inductively Coupled Plasma-Source Mass Spectrometry with conventional pneumatic nebulization (Perkin-Elmer Sciex Elan 6000, Quadrupole ICP-MS instrument). Calibration was achieved by preparing a standard stock solution containing the analytes of interest (in 4 % v/v HNO3), from mono elemental standards (1 0.005 g/l) on a gravimetric basis. The stock was further diluted (gravimetrically) to produce appropriate working standards (in 4% v/v HNO3). All working standards contained the internal standard (Sc, In, Rh, Tl) at 10 g/l. Five measurements were performed on each solution. Quantification was achieved using the isotopes 57Fe, 66Zn, 75As, 82Se, 111Cd and 208Pb.

2. Quantification of uncertainty [1] (Example for Se) 2.1. Measurand The mass fraction of Se (wSe) in bovine liver material is given by:

wSe [ mg / kg ] =
Where: c0 Vs ms fD R

c0 Vs ms f D R 1000

Concentration of Se in the sample solution [ng/ml] Volume of the sample solution (on gravimetric basis) [ml] Test portion [g] Dry mass factor Recovery

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2.2. Intermediate values and uncertainties

Abbr. c0 Vs ms fD R

Description Concentration of Se in sample sln. Volume of sample solution Test portion Dry mass factor Recovery

Value 20.38 ng/ml 49.91 ml 0.51207 g 0.9604 1.00

Standard uncertainty Relative std. uncertainty u(x) u(x)/x 0.283 ng/ml 0.0139 0.0005 ml 0.00001 0.000024 g 0.00005 0.0048 0.005 0.006 0.006

2.3. Spreadsheet calculation

value std. uncertainty c0 Vs ms fD R c u(y,xi) u(y)^2, u(y,xi)^2 u(cSe) U (k=2) 20.38 49.91 0.51207 0.9604 1.00 2.07

c0 20.38 0.283 20.663 49.91 0.51207 0.9604 1.00 2.10 0.03 0.0008

Vs 49.91 0.0005 20.38 49.9105 0.51207 0.9604 1.00 2.07 0.00 0.00000000

ms 0.51207 0.000024 20.38 49.91 0.512094 0.9604 1.00 2.07 0.00 0.000000

fD 0.9604 0.0048 20.38 49.91 0.51207 0.9652 1.00 2.06 -0.01 0.00011

R 1.00 0.006 20.38 49.91 0.51207 0.9604 1.01 2.06 -0.01 0.00015

0.0011 0.03 0.06

3. Literature [1] Guide for Quantifying Measurement Uncertainty issued by EURACHEM/CITAC (2000)