Garcia Sanchez F, Navas Diaz A, Medinilla J
University of Malaga, Faculty of Sciences, Department of Analytical Chemistry, Spain.
J Assoc Off Anal Chem. 1990 Sep-Oct;73(5):764-70.
A mineralization procedure is proposed for copper aerosols in which samples are mineralized by wet-ashing with HNO3 + HCIO4 mixture. Copper content is determined by a photometric method based on formation of a complex between copper and benzyl 2-pyridyl ketone 2-quinolylhydrazone (BPKQH). The influence of pH, ethanol content, and reagent concentration is studied. Copper determination at pH = 7.3, in the range 0.05 to 3 ppm is proposed. Mineralization with HNO3 is carried out in different conditions of evaporation (with or without dryness) and manipulation. Analysis of variance by the (ANOVA) single factor method shows that digestion conditions significantly increase the variability of results. Repeatability assays suggest that nitric acid alone gives low precision. Recovery assays reveal that the HNO3 digestion process causes copper loss by volatilization. Mineralization with HNO3 + HCIO4 is optimized on the basis of the accuracy and precision obtained. The ANOVA method suggests that mineralization conditions significantly increase total variability of results and also that results of the photometric method are not significantly different from those of the AAS method. The optimum mineralization procedure gave an RSD of 0.63% and a copper recovery of 98.4%. The combined digestion and quantification method was applied to determination of copper in aerosol samples obtained during leaf spraying operations of olive trees in the field.
