Non-chromatographic speciation analysis of arsenic and antimony in milk hydride generation atomic fluorescence spectrometry
A rapid, high sensitivity method has been developed for the determination of As(III), As(V), Sb(III) and Sb(V) in milk samples by using hydride generation atomic fluorescence spectrometry. The method is based on the leaching of As and Sb from milk through the sonication of samples with aqua regia fo...
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Published in | Analytica chimica acta Vol. 493; no. 2; pp. 195 - 203 |
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Main Authors | , , , , |
Format | Journal Article |
Language | English |
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Amsterdam
Elsevier B.V
01.10.2003
Elsevier |
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Abstract | A rapid, high sensitivity method has been developed for the determination of As(III), As(V), Sb(III) and Sb(V) in milk samples by using hydride generation atomic fluorescence spectrometry. The method is based on the leaching of As and Sb from milk through the sonication of samples with aqua regia followed by direct determination of the corresponding hydrides both before and after reduction with KI. It was confirmed by recovery experiments on spiked commercially available samples that neither the reduced nor the oxidized forms of the elements under study or mixtures of the two oxidation states were modified by the room temperature sample treatment with aqua regia. The methodologies developed provided 3
σ limit of detection values of 8.1, 10.3, 5.4 and 7.7
ng
l
−1 for As(III), As(V), Sb(III) and Sb(V) in the diluted samples. Average relative standard deviation values of 5.7, 5.5, 8.2 and 4.7% were found for determination of As(III), As(V), Sb(III) and Sb(V) in commercially available samples of different composition and origin containing from 3.5 to 13.6
ng
g
−1 total As and from 4.9 to 11.8
ng
g
−1 total Sb, it being confirmed that As(V) and Sb(V) are the main species present in the samples analyzed (62±5 and 73±5%, respectively). The time required to determine As and Sb species in milk involves 10
min sonication and 30
min prereduction but these steps can be carried out for several sample simultaneously. Additionally the fluorescence measurement step involves less than 20
min for three replicates of all the four measurements required. So, in less than 2
h it is possible to determine the content of As(III), As(V), Sb(III) and Sb(V) in four samples. |
---|---|
AbstractList | A rapid, high sensitivity method has been developed for the determination of As(III), As(V), Sb(III) and Sb(V) in milk samples by using hydride generation atomic fluorescence spectrometry. The method is based on the leaching of As and Sb from milk through the sonication of samples with aqua regia followed by direct determination of the corresponding hydrides both before and after reduction with KI. It was confirmed by recovery experiments on spiked commercially available samples that neither the reduced nor the oxidized forms of the elements under study or mixtures of the two oxidation states were modified by the room temperature sample treatment with aqua regia. The methodologies developed provided 3
σ limit of detection values of 8.1, 10.3, 5.4 and 7.7
ng
l
−1 for As(III), As(V), Sb(III) and Sb(V) in the diluted samples. Average relative standard deviation values of 5.7, 5.5, 8.2 and 4.7% were found for determination of As(III), As(V), Sb(III) and Sb(V) in commercially available samples of different composition and origin containing from 3.5 to 13.6
ng
g
−1 total As and from 4.9 to 11.8
ng
g
−1 total Sb, it being confirmed that As(V) and Sb(V) are the main species present in the samples analyzed (62±5 and 73±5%, respectively). The time required to determine As and Sb species in milk involves 10
min sonication and 30
min prereduction but these steps can be carried out for several sample simultaneously. Additionally the fluorescence measurement step involves less than 20
min for three replicates of all the four measurements required. So, in less than 2
h it is possible to determine the content of As(III), As(V), Sb(III) and Sb(V) in four samples. |
Author | de la Guardia, Miguel Teutsch, Carmen Cava-Montesinos, Patricia Luisa Cervera, M de la Guardia, Alberto |
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Keywords | Antimony Arsenic Speciation Slurries and atomic fluorescence spectrometry Milk Trace analysis Sonication Antimony III Leaching Arsenic V Direct method Chemical reduction Antimony V Hydridation Sensitivity Atomic fluorescence spectrometry Detection limit Arsenic III Aqua regia Standard deviation Potassium iodide |
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SubjectTerms | Analytical chemistry Antimony Arsenic Chemistry Exact sciences and technology Milk Slurries and atomic fluorescence spectrometry Speciation Spectrometric and optical methods |
Title | Non-chromatographic speciation analysis of arsenic and antimony in milk hydride generation atomic fluorescence spectrometry |
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