A method of x-ray fluorescence analysis for high antimonial lead alloys has been developed to cover antimony concentrations between 6 and 18%, a range not covered in previously published x-ray methods. The proposed method utilizes a General Electric XRD 6 VS spectrometer, chill-cast mold, and a special cutting bit to produce a smooth surface. Ten separate 10-sec counts are taken at 120° intervals to offset nonhomogeneity of the surface. Average counts vs concentration are plotted to obtain calibration curves and percentage concentration. The precision and accuracy of the proposed method compare favorably with the classical wet method. The average standard deviation of the proposed method in terms of the amount present is 1.19% for antimony, 2.03% for tin, and 2.37% for arsenic. These values are within the limits required in the specifications of most high antimonial lead alloys. A time saving of 2 h per sample is realized by the x-ray method over the classical wet method.
Donald L. McAlpin and Charles T. Kenner, "Determination of Antimony, Tin, and Arsenic in High Antimonial Lead Alloys by Vacuum X-ray Fluorescence," Appl. Spectrosc. 29, 481-485 (1975)