Avaliação da espectrometria de absorção atômica com fonte contínua e de alta resolução no desenvolvimento de métodos analíticos para diagnóstico foliar de cana-de-açucar e laranjeira
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Data
2010-09-23
Autores
Oliveira, Silvana Ruella de [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
A diagnose foliar é uma ferramenta para avaliar o estado nutricional das plantas, corrigir deficiências ou excessos de nutrientes, otimizar a produção e avaliar os requerimentos de fertilizantes. Desenvolver novas metodologias analíticas para determinações multielementares de macro (Ca, K, Mg, P e S) e micronutrientes (B, Cu, Fe, Mn, Mo e Zn) em folhas de cana-de-açúcar e de laranjeira por espectrometria de absorção atômica com fonte contínua e de alta resolução (HR-CS FAAS) foi o objetivo deste trabalho. A determinação multielementar de Cu, Fe, Mn, Zn, Ca, Mg e K em folhas de cana-de-açúcar por HR-CS FAAS foi feita após digestão das folhas em forno de micro-ondas. Usando linhas atômicas principais para Cu (324,754 nm), Fe (248,327 nm), Mn (279,482 nm) e Zn (213,857 nm), linhas secundárias para Ca (239,856 nm) e K (404,414 nm) e linha adjacente (202,588 nm) a linha secundária (202,582 nm) para Mg, curvas analiticas nos intervalos 0,1–0,5 mg L−1 Cu, 0,5–4,0 mg L−1 Fe, 0,5–4,0 mg L−1 Mn, 0,2–1,0 mg L−1 Zn, 10,0–100,0 mg L−1 Ca, 5,0–40,0 mg L−1 Mg e 50,0–250,0 mg L−1 K foram obtidas. A interferência espectral causada pela molécula de NO na linha principal do Zn (213,857 nm) foi removida com correção pelo algoritmo dos mínimos quadrados (LSBC). Exatidão e precisão foram avaliadas pela análise de 5 materiais de referência certificados e os resultados foram concordantes ao nível de 95% de confiança. Folhas de cana-de-açúcar foram analisadas e os resultados foram próximos dos obtidos por LS FAAS. As recuperações variaram de 84-114% para todos os analitos. Os limites de detecção foram 0,6 mg L-1 Ca, 0,4 mg L-1 Mg, 0,4 mg L-1 K, 7,7 μg L-1 Cu, 7,7 μg L-1 Fe, 1,5 μg L-1 Mn e 5,9 μg L-1 Zn. Um preparo de amostras alternativo foi proposto para determinar B, Ca, Cu, Fe, K, Mg, Mn, Mo, P, S e Zn por HR-CS FAAS...
Foliar diagnosis is a tool for evaluating nutritional state of plants, correcting nutrient deficiencies or excesses, optimizing crop production and evaluating fertilizer requirements. The goal of this work was to develop new methodologies for multielement determination of macro (Ca, K, Mg, P and S) and micronutrients (B, Cu, Fe, Mn, Mo, and Zn) in sugarcane and orange leaves by high resolution continuum source atomic absorption spectrometry (HR-CS FAAS). The multielement determination of Cu, Fe, Mn, Zn, Ca, Mg and K in sugarcane leaves by HR-CS FAAS was carried out after microwave-assisted sample digestion. Using main lines for Cu (324.754 nm), Fe (248.327 nm), Mn (279.482 nm) and Zn (213.857 nm), secondary lines for Ca (239.856 nm) and K (404.414 nm), and side line (202.588 nm) at wing of secondary line (202.582 nm) for Mg, analytical curves in the 0.1–0.5 mg L−1 Cu, 0.5- 4.0 mg L−1 Fe, 0.5-4.0 mg L−1 Mn, 0.2-1.0 mg L−1 Zn, 10.0-100.0 mg L−1 Ca, 5.0-40.0 mg L−1 Mg e 50.0-250.0 mg L−1 K intervals were obtained. Spectral interference caused by NO molecule on the main line for Zn (213.857 nm) was removed with least squares background correction (LSBC). Accuracy and precision were evaluated by analysis of 5 certified reference materials and the results were in agreement at 95% confidence level. Sugarcane leaves were analyzed and the results were close to those obtained by LS FAAS. Recoveries varied from 84 to 114% for all analytes. The limits of detection were 0.6 mg L-1 Ca, 0.4 mg L-1 Mg, 0.4 mg L-1 K, 7.7 μg L-1 Cu, 7.7 μg L-1 Fe, 1.5 μg L-1 Mn and 5.9 μg L-1 Zn. An alternative sample preparation was proposed for determining B, Ca, Cu, Fe, K, Mg, Mn, Mo, P, S and Zn by HR-CS FAAS. Sugarcane and orange leaves were submitted to dry ashing and solubilized in hydrochloric acid. This digest was divided in 3: one for B, P and S determination; other for Cu, Fe, Mn, Zn, Ca... (Complete abstract click electronic access below)
Foliar diagnosis is a tool for evaluating nutritional state of plants, correcting nutrient deficiencies or excesses, optimizing crop production and evaluating fertilizer requirements. The goal of this work was to develop new methodologies for multielement determination of macro (Ca, K, Mg, P and S) and micronutrients (B, Cu, Fe, Mn, Mo, and Zn) in sugarcane and orange leaves by high resolution continuum source atomic absorption spectrometry (HR-CS FAAS). The multielement determination of Cu, Fe, Mn, Zn, Ca, Mg and K in sugarcane leaves by HR-CS FAAS was carried out after microwave-assisted sample digestion. Using main lines for Cu (324.754 nm), Fe (248.327 nm), Mn (279.482 nm) and Zn (213.857 nm), secondary lines for Ca (239.856 nm) and K (404.414 nm), and side line (202.588 nm) at wing of secondary line (202.582 nm) for Mg, analytical curves in the 0.1–0.5 mg L−1 Cu, 0.5- 4.0 mg L−1 Fe, 0.5-4.0 mg L−1 Mn, 0.2-1.0 mg L−1 Zn, 10.0-100.0 mg L−1 Ca, 5.0-40.0 mg L−1 Mg e 50.0-250.0 mg L−1 K intervals were obtained. Spectral interference caused by NO molecule on the main line for Zn (213.857 nm) was removed with least squares background correction (LSBC). Accuracy and precision were evaluated by analysis of 5 certified reference materials and the results were in agreement at 95% confidence level. Sugarcane leaves were analyzed and the results were close to those obtained by LS FAAS. Recoveries varied from 84 to 114% for all analytes. The limits of detection were 0.6 mg L-1 Ca, 0.4 mg L-1 Mg, 0.4 mg L-1 K, 7.7 μg L-1 Cu, 7.7 μg L-1 Fe, 1.5 μg L-1 Mn and 5.9 μg L-1 Zn. An alternative sample preparation was proposed for determining B, Ca, Cu, Fe, K, Mg, Mn, Mo, P, S and Zn by HR-CS FAAS. Sugarcane and orange leaves were submitted to dry ashing and solubilized in hydrochloric acid. This digest was divided in 3: one for B, P and S determination; other for Cu, Fe, Mn, Zn, Ca... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Diagnose foliar, Macronutrientes, Elementos traços na nutrição, Foliar diagnosis, Macronutrients, Micronutrients
Como citar
OLIVEIRA, Silvana Ruella de. Avaliação da espectrometria de absorção atômica com fonte contínua e de alta resolução no desenvolvimento de métodos analíticos para diagnóstico foliar de cana-de-açucar e laranjeira. 2010. 162 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Quimica de Araraquara, 2010.