Analytisch-chemische aspecten van de bepaling van As, Ca, Cd, Sb, Sn, Pb, Zn in MVS-filterdestruaten met ICP-MS
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Type
Report
Language
nl
Date
1995-03-31
Research Projects
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Title
Analytisch-chemische aspecten van de bepaling van
As, Ca, Cd, Sb, Sn, Pb, Zn in MVS-filterdestruaten met
ICP-MS
Translated Title
Analytical chemical aspects of the determination
of As, Ca, Cd, Sb, Sn, Pb, Zn in MVS filterdigests by
ICP-MS
Published in
Abstract
In dit onderzoek werd een ICP-MS-methode ontwikkeld
voor de bepaling van Ca, Zn, As, Cd, Sb, Sn en Pb in filterdestruaten. De
onderste analysegrens is 30 ng/l Sb, 60 ng/l Cd, 200 ng/l As, 300 ng/l Sn,
400 ng/l Pb, 4 mug/l Zn en 20 mug/l Ca ; de precisie is beter dan 7% RSD
voor Ca, 4% RSD voor As, Cd, 3% RSD voor Zn, 2% RSD voor Pb en 1% RSD voor
Sn, Sb bij concentraties hoger dan 25 maal de onderste analysegrens. De
kalibratielijn is lineair tot tenminste 20 mug/l As, Cd, Sb, 50 mug/l Sn,
100 mug/l Pb, 200 mug/l Zn, 1000 mug/l Ca. Spectrale storingen en
matrixeffecten zijn afwezig of kunnen gereduceerd worden tot verwaarloosbare
niveaus indien de monsters verdund worden tot minder dan 20 muM Al, 0,3 muM
Ba, 20 muM Fe, 0,07 mM K, 0,08 mM Mg, 4 muM Mn, 2 mM Na, 0,4 mM Si, 0,6 mM
Cl, 3 mM S. Voor Sn, Sb en Pb werden lichte matrixeffecten gevonden (5-10%).
Een wiskundige correctieprocedure voor de storing van ArCl+ op As was niet
noodzakelijk tot een nivo van 0,6 mM Cl. De ICP-MS-methode werd toegepast
bij de analyse van filterdestruaten. De recovery van een analyt-spike lag
tussen 90 - 110%. De Ca, Zn, As, Cd en Pb resultaten met ICP-MS zijn in
overeenstemming met de resultaten met ICP-AES (Ca, Zn), GFAAS (Cd, Pb) en
hydride-FI-AAS (As). De resultaten voor Ca, Zn en Pb met ICP-MS waren
echter significant verschillend van die met XRF.
In this study an ICP-MS method was developed for the determination of Ca, Zn, As, Cd, Sb, Sn and Pb in filter digests. Detection limits are 30 ng/l Sb, 60 ng/l Cd, 200 ng/l As, 300 ng/l Sn, 400 ng/l Pb, 4 mug/l Zn and 20 mug/l Ca ; the precision amounts to 7% RSD for Ca, 4% RSD for As, Cd, 3% RSD for Zn, 2% RSD for Pb and 1% RSD for Sn, Sb at concentrations above 25 times the detection limit. The calibration curve is linear up to at least 20 mug/l As, Cd, Sb, 50 mug/l Sn, 100 mug/l Pb, 200 mug/l Zn, 1000 mug/l Ca. Spectral interferences and matrix effects are absent or are reduced to negligible levels after dilution of the samples to less than 20 muM Al, 0.3 muM Ba, 20 muM Fe, 0.07 mM K, 0.08 mM Mg, 4 muM Mn, 2 mM Na, 0.4 mM Si, 0.6 mM Cl, 3 mM S. For Sn, Sb and Pb slight matrix effects were found (5-10%). A mathematical correction procedure for the interference of ArCl+ on As was not necessary at levels up to 0.6 mM Cl. The ICP-MS method was applied to the analysis of filter digests. The recovery for an analyte spike was between 90 - 110%. The Ca, Zn, As, Cd and Pb results for ICP-MS were in agreement with the results for ICP-AES (Ca, Zn), GFAAS (Cd, Pb) and hydride-FI-AAS (As). The Ca, Zn and Pb results for ICP-MS and XRF were significantly different.
In this study an ICP-MS method was developed for the determination of Ca, Zn, As, Cd, Sb, Sn and Pb in filter digests. Detection limits are 30 ng/l Sb, 60 ng/l Cd, 200 ng/l As, 300 ng/l Sn, 400 ng/l Pb, 4 mug/l Zn and 20 mug/l Ca ; the precision amounts to 7% RSD for Ca, 4% RSD for As, Cd, 3% RSD for Zn, 2% RSD for Pb and 1% RSD for Sn, Sb at concentrations above 25 times the detection limit. The calibration curve is linear up to at least 20 mug/l As, Cd, Sb, 50 mug/l Sn, 100 mug/l Pb, 200 mug/l Zn, 1000 mug/l Ca. Spectral interferences and matrix effects are absent or are reduced to negligible levels after dilution of the samples to less than 20 muM Al, 0.3 muM Ba, 20 muM Fe, 0.07 mM K, 0.08 mM Mg, 4 muM Mn, 2 mM Na, 0.4 mM Si, 0.6 mM Cl, 3 mM S. For Sn, Sb and Pb slight matrix effects were found (5-10%). A mathematical correction procedure for the interference of ArCl+ on As was not necessary at levels up to 0.6 mM Cl. The ICP-MS method was applied to the analysis of filter digests. The recovery for an analyte spike was between 90 - 110%. The Ca, Zn, As, Cd and Pb results for ICP-MS were in agreement with the results for ICP-AES (Ca, Zn), GFAAS (Cd, Pb) and hydride-FI-AAS (As). The Ca, Zn and Pb results for ICP-MS and XRF were significantly different.
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