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Registro Completo |
Biblioteca(s): |
Embrapa Pecuária Sudeste. |
Data corrente: |
18/08/2005 |
Data da última atualização: |
08/05/2023 |
Tipo da produção científica: |
Artigo em Periódico Indexado |
Autoria: |
NOMURA, C. S.; SILVA, C. S.; NOGUEIRA, A. R. de A.; OLIVEIRA, P. V. |
Afiliação: |
CASSIANA S. NOMURA, Universidade de São Paulo; CINTIA S. SILVA, Universidade de São Paulo; ANA RITA DE ARAUJO NOGUEIRA, CPPSE; PEDRO V. OLIVEIRA, Universidade de São Paulo. |
Título: |
Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. |
Ano de publicação: |
2005 |
Fonte/Imprenta: |
Spectrochimica Acta Part B, v. 60, p. 673-680, 2005. |
DOI: |
https://doi.org/10.1016/j.sab.2005.02.021 |
Idioma: |
Inglês |
Conteúdo: |
This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 ?g of W + 200 ?g of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 ?g for Cu and 30 ?g for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg? 1 and 128 mg kg? 1, respectively. The relative standard deviations were lower than 6% (n = 5). The accuracy of the entire procedure was checked with bovine liver from NIST (1577b) and determination of Cu and Zn using flame atomic absorption spectrometry after microwave-assisted sample digestion. MenosThis work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 ?g of W + 200 ?g of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatm... Mostrar Tudo |
Palavras-Chave: |
Bovine liver; Electrothermal atomic absorption spectrometry; Homogeneity; Sample preparation; Solid sampling. |
Categoria do assunto: |
W Química e Física |
Marc: |
LEADER 02967naa a2200229 a 4500 001 1047180 005 2023-05-08 008 2005 bl uuuu u00u1 u #d 024 7 $ahttps://doi.org/10.1016/j.sab.2005.02.021$2DOI 100 1 $aNOMURA, C. S. 245 $aBovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry.$h[electronic resource] 260 $c2005 520 $aThis work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 ?g of W + 200 ?g of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 ?g for Cu and 30 ?g for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg? 1 and 128 mg kg? 1, respectively. The relative standard deviations were lower than 6% (n = 5). The accuracy of the entire procedure was checked with bovine liver from NIST (1577b) and determination of Cu and Zn using flame atomic absorption spectrometry after microwave-assisted sample digestion. 653 $aBovine liver 653 $aElectrothermal atomic absorption spectrometry 653 $aHomogeneity 653 $aSample preparation 653 $aSolid sampling 700 1 $aSILVA, C. S. 700 1 $aNOGUEIRA, A. R. de A. 700 1 $aOLIVEIRA, P. V. 773 $tSpectrochimica Acta Part B$gv. 60, p. 673-680, 2005.
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