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Determination of Antimony, Tin, and Arsenic in Antimonial Lead Alloys by X-Ray Fluorescence

Volume 23, Number 5 (Oct. 1969) Page 502-507

Fillmore, C.L.; Eckert, A.C.; Scholle, J.V.

Savings in man-hours of approximately 50% were gained with even greater reduction in elapsed time when fluorescent x-ray emission replaced classical wet methods to determine Sb (2%-7%), Sn (0.15%-0.75%) and As (0.05%-0.60%). No statistically significant differences were found in results, and scatter was less with the x-ray method. The problem of segregation in the sample was eliminated, and a surface of the required quality was obtained by a special method of sample preparation in which 5-20 ml of molten lead was poured into 1 liter of water, and the resulting granules were pressed to 95% density briquettes at 50 000 psi. The working curves, linear in the ranges stated, were established from alloys calibrated by the classical methods. Standard deviations were calculated from repeated x-ray determinations on a reference alloy (Sb: 5.89%±0.043; Sn: 0.36%±0.012; As: 0.175%±0.008).