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Mercury determinations in biohazard samples by GFAAS using Noviplex card sampling.

O artigo descreve um novo método para coleta de amostras de risco biológico (sangue/plasma humano e de peixe contaminados com mercúrio e homogeneizados de tecido muscular e hepático) usando percolação em cartões Noviplex para determinação de mercúrio total por espectrometria de absorção atômica com forno de grafite (GFAAS). Para o processo de amostragem, 50 µL das amostras biológicas foram filtradas no disco de amostragem do cartão Noviplex. Três minutos após a percolação da alíquota da amostra, a amostra adsorvida no disco amostrador do cartão já está seca e apresenta estabilidade à temperatura ambiente por seis meses. Após o processo de amostragem, os discos amostrais do cartão com as amostras percoladas foram mineralizados em meio ácido contendo 18 mol L-1 de H2SO4 e 0,02 mol L-1 de KMnO4 na proporção de 1,0:0,50 (v/v). As determinações de mercúrio nos extratos ácidos foram realizadas via GFAAS, injetando 15 µL de amostra + 5 µL de nitrato de zircônio (modificador químico) no tubo de grafite do espectrômetro, cuja parede interna foi revestida com carboneto de tungstênio (modificador químico permanente). As condições de reação proporcionaram estabilização térmica do mercúrio em temperaturas de atomização de até 1700°C. O método foi validado para determinações de mercúrio total em extratos de materiais de referência DORM-4 e DOLT-4. O LOD e LOQ calculados form de 12 a 43 µg kg-1, respectivamente. O método de amostragem provou ser bastante robusto para determinações de mercúrio em amostras de risco biológico.
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Mercury determinations in biohazard samples by GFAAS using Noviplex card sampling.

  • DOI: https://doi.org/10.22533/at.ed.1652412074

  • Palavras-chave: Noviplex cards, mercury in biological samples, electrothermal atomization, chemical modifier.

  • Keywords: Noviplex cards, mercury in biological samples, electrothermal atomization, chemical modifier.

  • Abstract: This paper presents a new method for sampling biohazard samples (mercury-contaminated human and fish blood/plasma and muscle and liver tissue homogenates) using percolation on Noviplex cards for total mercury determination by graphite furnace atomic absorption spectrometry (GFAAS). For the sampling process, 50 µL of the biological samples was percolated onto the sampling disk of the Noviplex card. Three minutes after percolation of the sample aliquot, the sample adsorbed on the card-sampling disk was already dry and showed stability at room temperature for six months. After the sampling process, the card sampling discs with the percolated samples were mineralized in an acidic medium containing 18 mol L-1 H2SO4 and 0.02 mol L-1 KMnO4 in a 1.0:0.50 (v/v) ratio. Mercury determinations of the acid extracts were performed via GFAAS by injecting 15 µL of sample + 5 µL of zirconium nitrate (chemical modifier) into the graphite tube of the spectrometer, in which the inner wall was coated with tungsten carbide (permanent chemical modifier). The reaction conditions provided thermal stabilization of mercury at atomization temperatures up to 1700 °C. The method was validated for total mercury determinations with extracts from DORM-4 and DOLT-4 reference materials. The calculated LOD and LOQ ranged from 12 to 43 µg kg-1, respectively. The sampling method proved to be quite robust for mercury determinations for biohazard samples. This paper presents a new method for sampling biohazard samples (mercury-contaminated human and fish blood/plasma and muscle and liver tissue homogenates) using percolation on Noviplex cards for total mercury determination by graphite furnace atomic absorption spectrometry (GFAAS). For the sampling process, 50 µL of the biological samples was percolated onto the sampling disk of the Noviplex card. Three minutes after percolation of the sample aliquot, the sample adsorbed on the card-sampling disk was already dry and showed stability at room temperature for six months. After the sampling process, the card sampling discs with the percolated samples were mineralized in an acidic medium containing 18 mol L-1 H2SO4 and 0.02 mol L-1 KMnO4 in a 1.0:0.50 (v/v) ratio. Mercury determinations of the acid extracts were performed via GFAAS by injecting 15 µL of sample + 5 µL of zirconium nitrate (chemical modifier) into the graphite tube of the spectrometer, in which the inner wall was coated with tungsten carbide (permanent chemical modifier). The reaction conditions provided thermal stabilization of mercury at atomization temperatures up to 1700 °C. The method was validated for total mercury determinations with extracts from DORM-4 and DOLT-4 reference materials. The calculated LOD and LOQ ranged from 12 to 43 µg kg-1, respectively. The sampling method proved to be quite robust for mercury determinations for biohazard samples. This paper presents a new method for sampling biohazard samples (mercury-contaminated human and fish blood/plasma and muscle and liver tissue homogenates) using percolation on Noviplex cards for total mercury determination by graphite furnace atomic absorption spectrometry (GFAAS). For the sampling process, 50 µL of the biological samples was percolated onto the sampling disk of the Noviplex card. Three minutes after percolation of the sample aliquot, the sample adsorbed on the card-sampling disk was already dry and showed stability at room temperature for six months. After the sampling process, the card sampling discs with the percolated samples were mineralized in an acidic medium containing 18 mol L-1 H2SO4 and 0.02 mol L-1 KMnO4 in a 1.0:0.50 (v/v) ratio. Mercury determinations of the acid extracts were performed via GFAAS by injecting 15 µL of sample + 5 µL of zirconium nitrate (chemical modifier) into the graphite tube of the spectrometer, in which the inner wall was coated with tungsten carbide (permanent chemical modifier). The reaction conditions provided thermal stabilization of mercury at atomization temperatures up to 1700 °C. The method was validated for total mercury determinations with extracts from DORM-4 and DOLT-4 reference materials. The calculated LOD and LOQ ranged from 12 to 43 µg kg-1, respectively. The sampling method proved to be quite robust to mercury determinations in biohazard samples.

  • Emerson Carlos de Almeida
  • Nubya Gonçalves Cavallini
  • Joyce Andrade da Silva
  • Luane Benedita Gonçalves Andrade
  • Camila Pereira Braga
  • Jiri Adamec
  • Pedro de Magalhães Padilha
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