4.7 Article

On-line filtration system for determining total chromium and chromium in the soluble fraction of industrial effluents by flow injection flame atomic absorption spectrometry

Journal

ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 373, Issue 1-2, Pages 98-102

Publisher

SPRINGER-VERLAG BERLIN
DOI: 10.1007/s00216-002-1289-8

Keywords

chromium determination; flow injection; flame atomic absorption spectrometry; FI-AAS; AAS

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Two manifolds were assessed for the purpose of determining both the total chromium content and that present as a soluble form in industrial effluents by flow injection flame atomic absorption spectrometry (FI-FAAS). To determine the chromium content in the soluble fraction the samples were used without additional treatment, a 0.45 mum filter being included in the FI system. To determine the total chromium content, the samples were acidified with nitric acid 20% (v/v) and heated for 30 s in a microwave oven (temperatures of about 70degreesC were reached). The problem posed by the very different concentration range in which total and soluble chromium are present was overcome by using programmed flow rate methodology and by only partially emptying the sample loop. A personal computer controlled both the rotation speed of a peristaltic pump and the volume of sample injected into the system, thus obtaining the dispersion degree required. Using the manifold proposed, the chromium content in the soluble fraction can be determined in the 0.5-20 mug mL(-1) range using a 10 mug mL(-1) single standard for calibration. To determine the total chromium content, a calibration line in the 20-200 mug mL(-1) range was obtained using a single 50 mug, mL(-1) chromium standard solution. The reliability of the semi-automatic devices was verified by comparing the results obtained with those found by treating the samples and using both FAAS in a conventional way and a spectrophotometric method using diphenylcarbazide at the 95% confidence level (ANOVA test). The proposed procedures showed a RSD lower than +/-3%.

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