期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 405, 期 21, 页码 6761-6769出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-013-7111-y
关键词
In-syringe magnetic-stirring-assisted dispersive liquid-liquid microextraction; Chromate; Lab-in-a-syringe; Diphenylcarbazide
资金
- Spanish Ministry of Science and Innovation [CTQ2010-15541]
- Conselleria d'Economia, Hacienda, e Innovacio of the Government of the Balearic Islands [43/2011]
- Conselleria d Educacio, Cultura I Universitat
- European Social Fund
- Education for Competitiveness Operational Program [CZ.1.07/2.3.00/30.0022]
- state budget of the Czech Republic
A fully automated method for the determination of chromate is described. It is based on the selective reaction of Cr(VI) with diphenylcarbazide in acidic media to form a colored complex of Cr(III) with the oxidation product diphenylcarbazone. The reaction was performed within the syringe of an automatic burette containing a magnetic stirrer for homogenization of the sample and the required reagents. In-syringe stirring was made possible using a specially designed driving device placed around the syringe barrel to achieve a rotating magnetic field in the syringe, forcing the stirrer to spin. In a second step, the reaction mixture in the syringe was neutralized to allow in-syringe magnetic-stirring-assisted dispersive liquid-liquid microextraction of the complex into 125 mu L of n-hexanol. After phase separation by droplet flotation over 30 s, the organic phase was propelled into a coupled spectrophotometric detection cell. The entire multistep procedure including in-system standard preparation was done within 270 s. The method was used for the analysis of natural waters, achieving average analyte recovery of 103 %, a limit of detection of 0.26 mu g L-1, and a repeatability of less than 4 % relative standard deviation.
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