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      Hydride generation-in situ trapping-flame atomic absorption spectrometry hybridization for indium and thallium determination

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          Abstract

          The analytical performance of coupled hydride generation-integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of In and Tl in reference material. Indium, using formation of InH3 and TlH vapors were atomized in air-acetylene flame-heated IAT. A new design of HG-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 limits was achieved compared with that obtained using either of the atom trapping techniques, presented above, separately. The detection limits, defined as 3 times the blank standard deviation (3sigma), were 0.60 and 0.40 ng mL-1 for In and Tl, respectively. For a 120 s in situ pre-concentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, were 417 and 450 folds for In and Tl, respectively, using hydride generation-atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed by RSD, was 4.4% and 5.2% (n = 6) for In and Tl, respectively. The designs studied included slotted tube, single silica tube and integrated atom trap-cooled atom traps. The accuracy of the method was verified by the use of certified reference material (GBW 07302 Stream Sediment) and by aqueous standard calibration solutions. The measured In and Tl contents, in reference material, were in satisfactory agreement with the certified or information values.

          Translated abstract

          O desempenho analítico do acoplamento de geração de hidretos com sistema de aprisionamento de átomos (HG-IAT) em espectrometria de absorção atômica com chama (FAAS) foi avaliado para determinação de In e Tl em material de referência. Hidretos de índio (InH3) e tálio (TlH) foram atomizados em sistema IAT aquecido em chama ar-acetileno. Investigou-se um novo arranjo da técnica hifenizada HG-IAT-FAAS, que superaria a capacidade operacional dos arranjos existentes (tubo de sílica resfriado com água, tubo de quartzo com dupla fenda ou "aprisionamento integrado"). Obteve-se significativa melhora nos limites de detecção, em relação às técnicas de aprisionamento de átomos acima citadas. Os limites de detecção, definidos como 3 vezes o desvio padrão do branco (3sigma), foram 0,60 e 0,40 ng mL-1 para In e Tl, respectivamente. Para um tempo de pré-concentração de 120 s in situ (volume da amostra de 2 mL), a melhora na sensibilidade, comparando-se com espectrometria de absorção atômica com chama foi de 417 e 450 para In e Tl, respectivamente, usando a técnica de geração de hidretos e aprisionamento de átomos. A sensibilidade pode ser ainda melhorada aumentando-se o tempo de coleta. A precisão, expressa por RSD, foi de 4,4% e 5,2% (n = 6) para In e Tl, respectivamente. Os arranjos estudados incluíram tubo com fenda, tubo simples de sílica e aprisionamento de átomos resfriado e integrado. A precisão e exatidão do método foram verificadas pelo uso do material de referência certificado (GBW 07302 Sedimento) e soluções analíticas de calibração em meio aquoso. Os teores de In e Tl determinados no material de referência apresentaram adequada concordância com os valores certificados ou indicativos.

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          Most cited references 26

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          Anal. Chem.

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            J. Anal. At. Spectrom.

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                Author and article information

                Affiliations
                [1 ] Poznań University of Technology Poland
                Contributors
                Role: ND
                Role: ND
                Journal
                jbchs
                Journal of the Brazilian Chemical Society
                J. Braz. Chem. Soc.
                Sociedade Brasileira de Química (São Paulo )
                1678-4790
                April 2007
                : 18
                : 2
                : 304-311
                S0103-50532007000200010 10.1590/S0103-50532007000200010

                http://creativecommons.org/licenses/by/4.0/

                Product
                Product Information: SciELO Brazil
                Categories
                CHEMISTRY, MULTIDISCIPLINARY

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