X-Ray Absorption-Edge Determination of Cobalt in Complex Mixtures*

The application of the X-ray absorption-edge technique was extended to the determination of cobalt in aqueous and alcoholic solutions containing a wide variety of impurity elements. In the procedure developed, secondary radiation from a 50% copper-nickel alloy is passed through an absorption cell filled alternately with the solvent and the sample solution. The transmitted Intensities of the Kα lines for copper and nickel are measured, and the concentration of cobalt is determined using accepted absorption principles. The K absorption edge for cobalt occurs at 1.604 A, restricting cell construction materials and solvents to those containing light elements with low X-ray absorption characteristics and also limiting the path length of the cell.Cells of 0.16- and 0.34-cm path length were used in the analysis of aqueous and alcoholic solutions, respectively. With the 0.16-cm path-length cell, relative standard deviations of 4.6 to 0.5% were obtained for cobalt concentrations ranging from 1.00 to 10.00 mg/ml for known aqueous solutions that contain various known concentrations of nitric acid. With the longer path-length cell, relative standard deviations from 1.8 to 0.46% were obtained for cobalt concentrations in the same range in known alcoholic solutions containing various known concentrations of nitric acid. The standard deviation of determining the blank is 0.043 mg of cobalt per milliliter for the 0.16-cm cell and 0.016 mg of cobalt per milliliter for the longer cell.A Norelco X-ray spectrograph with a three-position head was used in these analyses. Less than 5 min is required to convert this instrument from normal fluorescence operation to absorption-edge analysis. Approximately 15 to 20 analyses can be performed daily.