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1.
J AOAC Int ; 93(3): 985-91, 2010.
Artigo em Inglês | MEDLINE | ID: mdl-20629404

RESUMO

An effective and environmentally friendly single-drop microextraction method was developed for the preconcentration of ultratraces of cobalt before its determination by electrothermal atomic absorption spectrometry (ETAAS). A microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate, [C6MIM][PF6], was used to extract Co(II) ions as an ammonium pyrroldinedithiocarbamate (APDC) complex. The sensitivity was improved by increasing the volume of the suspended drop. Several variables affecting microextraction efficiency and the ETAAS signal-such as pyrolysis and atomization temperature, pH, APDC concentration, extraction time, drop volume, and stirring rate-were investigated and optimized. Under the optimum experimental conditions, the detection limit (3 SD) was 0.04 microg/L, and the enrichment factor was 120. The RSD for five replicate determinations of Co(II) at 0.5 microg/L was 4.5%. The developed method was validated by analysis of a Standard Reference Material and applied to the determination of cobalt in water samples.


Assuntos
Cobalto/análise , Líquidos Iônicos/química , Espectrofotometria Atômica/métodos , Poluentes Químicos da Água/análise
2.
J Hazard Mater ; 176(1-3): 481-6, 2010 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-19962233

RESUMO

A simple and effective hollow fiber based-liquid phase microextraction (HF-LPME) technique by using ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate, [C(6)MIM][PF(6)], coupled with electrothermal atomic absorption spectrometry (ETAAS) was developed for the determination of lead and nickel in environmental and biological samples. Ammonium pyrroldinedithiocarbamate (APDC) was used as chelating agent. Several factors that influence the microextraction efficiency and ETAAS signal, such as pH, APDC concentration extraction time, amounts of ionic liquid, stirring rate, pyrolysis and atomization temperature were investigated and the microextraction conditions were established. In the optimum experimental conditions, the detection limits (3 s) of the method were 0.03 and 0.02 microg L(-1), for Ni and Pb, respectively and corresponding relative standard deviations (0.5 microg L(-1), n=6) were 4.2% and 5%. The developed method was validated by the analysis of certified reference materials and applied to the determination of lead and nickel in real samples.


Assuntos
Líquidos Iônicos/química , Chumbo/isolamento & purificação , Níquel/isolamento & purificação , Espectrofotometria Atômica/métodos , Quelantes , Fluoretos/química , Concentração de Íons de Hidrogênio , Limite de Detecção , Fosfatos/química , Padrões de Referência , Solventes , Temperatura
3.
Anal Chim Acta ; 644(1-2): 48-52, 2009 Jun 30.
Artigo em Inglês | MEDLINE | ID: mdl-19463561

RESUMO

An improved single drop microextraction procedure was developed for the preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry. Ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6], was used as an alternative to volatile organic solvents for extraction. Lead was complexed with ammonium pyrroldinedithiocarbamate (APDC) and extracted into a 7-microL ionic liquid drop. The extracted complex was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, APDC concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.015 microg L(-1) and 76, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.2 microg L(-1) Pb was 5.2%. The developed method was validated by the analysis of certified reference materials and applied successfully to the determination of lead in several real samples.

4.
Talanta ; 77(4): 1539-44, 2009 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-19084676

RESUMO

Room temperature ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C(4)MIM][PF(6)], was used as an alternative to volatile organic solvents in single drop microextraction-electrothermal atomic absorption spectrometry (SDME-ETAAS). Manganese was extracted from aqueous solution into a drop of the ionic liquid after complextaion with 1-(2-thiazolylazo)-2-naphthol (TAN) and the drop was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, TAN concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.024 microg L(-1) and 30.3, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.5 microg L(-1) Mn(II) was 5.5%. The developed method was validated by the analysis of a certified reference material (NIST SRM 1643e) and applied successfully to the determination of manganese in several natural water samples.


Assuntos
Técnicas de Química Analítica/métodos , Eletroquímica/métodos , Líquidos Iônicos/análise , Manganês/análise , Poluentes Químicos da Água/análise , Métodos Analíticos de Preparação de Amostras/métodos , Concentração de Íons de Hidrogênio , Íons , Metais/análise , Reprodutibilidade dos Testes , Água/análise , Purificação da Água
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