Abstract:The calibration curve was prepared by standard reagent of potassium sulfate. The sample was placed onto porcelain crucible containing 0.50 g of pure iron followed by covering 3.0 g of pure tungsten. The determination method of trace sulfur in tin-lead solder by high frequency combustion infrared absorption method was established. The optimal experimental conditions obtainedwere listed as below: the sample mass was 1.0 g when S≤0.001 0%; the sample mass was 0.50 g when 0.001 0%<S≤0.010%; the sample mass was 0.20 g when 0.010%<S≤ 0.025%. The results indicated that the sulfur content in range of 0.001 0-0.050 mg showed good linearity to the absorbance. The correlation coefficient was r=0.999 7. The detection limit of method was 0.000 021%, and the low limit of determination was 0.000 084 %. Four internal control samples of tin-lead solder with different content of sulfur were determined for 11 times. The found results were basically consistent with the reference values. The relative standard deviation (RSD) was between 7.3% and 15.0%. The recoveries were between 96% and 115%. When the mass fraction of sulfur was in range of 0.000 10%-0.025%, the repeatability standard deviation was Sr=0.064 6 x+0.000 01, the repeatability limit was r=0.181 2 x+0.00 003, the reproducibility standard deviation was SR=0.081 9 x-0.000 002, and the reproducibility limit was R=0.229 7x-0.000 006.
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