Determinação direta e simultânea de 'AL', 'AS', 'CU', 'FE', 'MN' e 'NI' em álcool etílico hidratado combustível por espectrometria de absorção atômica em forno de grafite
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Data
2002-07
Autores
Oliveira, Adriana Paiva de [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
Este trabalho propõe um método para a determinação direta e simultânea de Al, As, Cu, Fe, Mn e Ni em álcool etílico hidratado combustível (AEHC) por espectrometria de absorção atômica em forno de grafite (GFAAS), empregando tubo de grafite com aquecimento transversal (THGA) e corretor de fundo por efeito Zeeman longitudinal. Foram avaliados dois tipos de modificadores: a mistura nitrato de paládio + nitrato de magnésio, e o modificador permanente W/Rh. No primeiro caso, as curvas analíticas foram obtidas injetando-se 10 mL das soluções de referência (2,0, 5,0, 10, 20, 30, 40 e 50 mg L-1 Al, As, Cu, Fe, Mn e Ni em meio 0,28 mol L-1 HNO3 ) + 10 mL de etanol P.A. + 5 mL Pd(NO3)2+ 3 mL Mg(NO3)2. Para determinar os analitos, foram injetados 10 mL de amostra + 10 mL de solução 0,28 mol L-1 HNO3 + 5 mL Pd(NO3)2 + 3 mL Mg(NO3)2. No teste de adição e recuperação, foram injetados 10 mL de amostra + 10 mL de solução 60 mg L-1 Al, As, Cu, Fe, Mn e Ni em meio 0,28 mol L-1 HNO3+ 5 mL Pd(NO3)2 + 3 mL Mg(NO3)2. Todas as medidas foram feitas em absorbância integrada e em triplicata. O programa de aquecimento otimizado (temperatura, tempo de rampa, tempo de patamar) foi o seguinte: secagem 1 (120oC, 1 s, 10 s); secagem 2 (150oC, 5 s, 25 s); pirólise (1200oC, 10 s, 20 s); atomização (2200oC, 1 s, 6 s) e limpeza (2550oC, 1 s, 3 s). As massas características foram 37 pg Al, 73 pg As, 31 pg Cu, 16 pg Fe, 9 pg Mn e 44 pg Ni e o tempo de vida do atomizador foi equivalente a aproximadamente 250 ciclos de aquecimento. Os desvios padrões relativos (n=12) foram £3%, £6%, £2%, £3,4%, £1,3% e £2% para Al, As, Cu, Fe, Mn e Ni, respectivamente. As recuperações dos analitos adicionados às amostras coletadas em postos de abastecimento da cidade de Araraquara variaram entre 77-112%, 92-114%, 104-113%, 91-116%, 91-122% e 93-116% para Al, As, Cu, Fe, Mn e Ni, respectivamente...
This work describes a method for direct and simultaneous determination of Al, As, Cu, Fe, Mn and Ni in fuel ethanol by electrothermal atomic absorption spectrometry (GFAAS) with transversely heated graphite atomizer (THGA) and longitudinal Zeeman-effect background corrector. The following modifiers were evaluated: a) the mixture Pd(NO3)2 + 3 æL Mg(NO3)2; b) W/Rh as permanent modifier. Regards to Pd/Mg(NO3)2, analytical curves were obtained by injecting 10 æL of each analytical solutions (2.0, 5.0, 10, 20, 30, 40 and 50 æg L-1 Al, As, Cu, Fe, Mn, Ni in 0.28 mol L-1 HNO3) plus 10 æL of ethanol P.A. plus 5 æL Pd(NO3)2 plus 3 æL Mg(NO3)2. For determination, 10 æL of samples plus 10 æL of 0.28 mol L-1 nitric acid solution plus 5 æL Pd(NO3)2 + 3 æL Mg(NO3)2 were sequentially injected. For analyte addition tests, 10 æL sample plus 10 æL of 60 æg L-1 Al, As, Cu, Fe, Mn e Ni containing 0.28 mol L-1 HNO3 plus 5 æL Pd(NO3)2 plus 3 æL Mg(NO3)2 were sequentially injected. All measurements were carried out in triplicate and integrated absorbance. The optimized heating program of graphite tube (temperature, ramp time, hold time) was: dry 1 (120oC, 1 s, 10 s); dry 2 (150oC, 5 s, 25 s); pirolysis (1200oC, 10 s, 20 s); atomization (2200oC, 1 s, 6 s) and clean (2550oC, 1 s, 3 s). The characteristic masses were calculated as 37 pg Al, 73 pg As, 31 pg Cu, 16 pg Fe, 9 pg Mn and 44 pg Ni. The lifetime of atomizer was equivalent to ca. 250 heating cycles. Relative standard deviations (n=12) were =3%, =6%, =2%, =3.4%, =1.3% and =2% for Al, As, Cu, Fe, Mn and Ni, respectively. The recoveries of Al, As, Cu, Fe, Mn and Ni added to fuel ethanol samples varied from 77 to 112%, 92 to 114%, 104 to 113%, 91 to 116%, 91 to 122% and 93 to 116%, respectively. Accuracy was checked for Al, As, Cu, Fe, Mn and Ni determination in 20 samples purchased at a local gas stations in Araraquara city, Brazil... (Complete abstract, access undermentioned electronic address)
This work describes a method for direct and simultaneous determination of Al, As, Cu, Fe, Mn and Ni in fuel ethanol by electrothermal atomic absorption spectrometry (GFAAS) with transversely heated graphite atomizer (THGA) and longitudinal Zeeman-effect background corrector. The following modifiers were evaluated: a) the mixture Pd(NO3)2 + 3 æL Mg(NO3)2; b) W/Rh as permanent modifier. Regards to Pd/Mg(NO3)2, analytical curves were obtained by injecting 10 æL of each analytical solutions (2.0, 5.0, 10, 20, 30, 40 and 50 æg L-1 Al, As, Cu, Fe, Mn, Ni in 0.28 mol L-1 HNO3) plus 10 æL of ethanol P.A. plus 5 æL Pd(NO3)2 plus 3 æL Mg(NO3)2. For determination, 10 æL of samples plus 10 æL of 0.28 mol L-1 nitric acid solution plus 5 æL Pd(NO3)2 + 3 æL Mg(NO3)2 were sequentially injected. For analyte addition tests, 10 æL sample plus 10 æL of 60 æg L-1 Al, As, Cu, Fe, Mn e Ni containing 0.28 mol L-1 HNO3 plus 5 æL Pd(NO3)2 plus 3 æL Mg(NO3)2 were sequentially injected. All measurements were carried out in triplicate and integrated absorbance. The optimized heating program of graphite tube (temperature, ramp time, hold time) was: dry 1 (120oC, 1 s, 10 s); dry 2 (150oC, 5 s, 25 s); pirolysis (1200oC, 10 s, 20 s); atomization (2200oC, 1 s, 6 s) and clean (2550oC, 1 s, 3 s). The characteristic masses were calculated as 37 pg Al, 73 pg As, 31 pg Cu, 16 pg Fe, 9 pg Mn and 44 pg Ni. The lifetime of atomizer was equivalent to ca. 250 heating cycles. Relative standard deviations (n=12) were =3%, =6%, =2%, =3.4%, =1.3% and =2% for Al, As, Cu, Fe, Mn and Ni, respectively. The recoveries of Al, As, Cu, Fe, Mn and Ni added to fuel ethanol samples varied from 77 to 112%, 92 to 114%, 104 to 113%, 91 to 116%, 91 to 122% and 93 to 116%, respectively. Accuracy was checked for Al, As, Cu, Fe, Mn and Ni determination in 20 samples purchased at a local gas stations in Araraquara city, Brazil... (Complete abstract, access undermentioned electronic address)
Descrição
Palavras-chave
Espectroscopia de absorção atomica, Álcool como combustível, Fuel ethanol
Como citar
OLIVEIRA, Adriana Paiva de. Determinação direta e simultânea de 'AL', 'AS', 'CU', 'FE', 'MN' e 'NI' em álcool etílico hidratado combustível por espectrometria de absorção atômica em forno de grafite. 2002. 93 f. Dissertação (mestrado) - Universidade Estadual Paulista, Instituto de Química, 2002.