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Application of hydrocyanic acid vapor generation via focused microwave radiation to the preparation of industrial effluent samples prior to free and total cyanide determinations by spectrophotometric flow injection analysis

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Abstract

A sample preparation procedure for the quantitative determination of free and total cyanides in industrial effluents has been developed that involves hydrocyanic acid vapor generation via focused microwave radiation. Hydrocyanic acid vapor was generated from free cyanides using only 5 min of irradiation time (90 W power) and a purge time of 5 min. The HCN generated was absorbed into an accepting NaOH solution using very simple glassware apparatus that was appropriate for the microwave oven cavity. After that, the cyanide concentration was determined within 90 s using a well-known spectrophotometric flow injection analysis system. Total cyanide analysis required 15 min irradiation time (90 W power), as well as chemical conditions such as the presence of EDTA–acetate buffer solution or ascorbic acid, depending on the effluent to be analyzed (petroleum refinery or electroplating effluents, respectively). The detection limit was 0.018 mg CN l−1 (quantification limit of 0.05 mg CN l−1), and the measured RSD was better than 8% for ten independent analyses of effluent samples (1.4 mg l−1 cyanide). The accuracy of the procedure was assessed via analyte spiking (with free and complex cyanides) and by performing an independent sample analysis based on the standard methodology recommended by the APHA for comparison. The sample preparation procedure takes only 10 min for free and 20 min for total cyanide, making this procedure much faster than traditional methodologies (conventional heating and distillation), which are time-consuming (they require at least 1 h). Samples from oil (sour and stripping tower bottom waters) and electroplating effluents were analyzed successfully.

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Acknowledgements

The authors are grateful to Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) and Fundação Carlos Chagas Filho de Amparo a Pesquisa do Estado do Rio de Janeiro (FAPERJ) for grants and fellowships.

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Authors and Affiliations

  1. Departamento de Geoquímica, Universidade Federal Fluminense, Outeiro de São João Batista s/n, Centro, 24020-150, Niterói, RJ, Brazil

    Maria Cristina Baptista Quaresma, Francis Assis Meirelles & Ricardo Erthal Santelli

  2. PETROBRAS/CENPES/Avaliação e Monitoramento Ambiental, Cidade Universitária, Qd. 7, 21949-900, Rio de Janeiro, RJ, Brazil

    Maria de Fátima Batista de Carvalho

  3. PETROBRAS/CENPES/Biotecnologia e Tratamentos Ambientais, Cidade Universitária, Qd. 7, 21949-900, Rio de Janeiro, RJ, Brazil

    Vânia Maria Junqueira Santiago

Authors
  1. Maria Cristina Baptista Quaresma
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  2. Maria de Fátima Batista de Carvalho
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  3. Francis Assis Meirelles
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  4. Vânia Maria Junqueira Santiago
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  5. Ricardo Erthal Santelli
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Correspondence to Ricardo Erthal Santelli.

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Quaresma, M.C.B., de Carvalho, M.d.F.B., Meirelles, F.A. et al. Application of hydrocyanic acid vapor generation via focused microwave radiation to the preparation of industrial effluent samples prior to free and total cyanide determinations by spectrophotometric flow injection analysis. Anal Bioanal Chem 387, 1017–1025 (2007). https://doi.org/10.1007/s00216-006-0985-1

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  • DOI: https://doi.org/10.1007/s00216-006-0985-1

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