4.7 Article

Determination of cadmium and lead in reference materials by volatile species generation with in situ trapping flame atomic absorption spectrometry

Journal

MICROCHEMICAL JOURNAL
Volume 83, Issue 1, Pages 17-23

Publisher

ELSEVIER
DOI: 10.1016/j.microc.2006.01.001

Keywords

reference materials; in situ trapping; volatile species generation; cadmium; lead; flame atomic absorption spectrometry

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The analytical performance of coupled volatile species generation-integrated atom trap (VSG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Cd and Ph in reference materials. Lead using formation of PbH4 and Cd-0 vapors are atomized in air-acetylene flame-heated IAT. A new design of VSG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube or an integrated trap) was investigated. A dramatic improvement in detection limit was achieved compared with that obtained using either of the above atom trapping techniques separately. The concentration detection limits, defined as 3 times the blank standard deviation (3 sigma), were 0.05 and 0.40 ng mL(-1) for Cd and Pb, respectively. For a 120 s in situ pre-concentration time, sensitivity enhancement compared to flame AAS, was 500 and 575 folds for Cd and Pb, respectively, using volatile species generation-atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 4.4% and 4.1% (n = 6) for Cd and Pb, respectively. The designs studied include slotted tube, single silica tube and integrated atom trap-cooled atom traps. The accuracy of method was verified using certified reference materials (PLANTS 3 and IAEA/W-4) by standard addition calibration technique. The measured Cd and Pb contents in two reference materials were in satisfactory agreement with the certified values. (c) 2006 Elsevier B.V. All rights reserved.

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