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在盐酸介质中及55℃加热条件下,铋与硫脲形成黄色络合物,从而建立了用分光光度法比较铋、氧化铋、硫化铋在盐酸-硫脲中溶解性的新方法。研究了反应介质、试剂浓度、加热时间、加热温度、震荡速率等因素的影响。在最佳实验条件下,溶液的质量浓度为0.04~0.24 mg/mL时符合比尔定律。相关系数R=0.999 9,检出限为1.05×10-2μg/mL,标准偏差SD=0.003 5,相对标准偏差RSD=2.42%,摩尔吸收系数为1.515×105L/(mol·cm),加标回收率为96.7%~98.8%。实验结果表明,铋、氧化铋、硫化铋的溶解性顺序大小为:铋>氧化铋>硫化铋。
In the medium of hydrochloric acid and heating at 55 ℃, bismuth and thiourea form a yellow complex, thus establishing a new spectrophotometric method to compare the solubility of bismuth, bismuth oxide and bismuth sulfide in hydrochloric acid - thiourea. The effects of reaction medium, reagent concentration, heating time, heating temperature, shaking rate and other factors were studied. Under the best experimental conditions, Beer’s law is obeyed when the mass concentration of solution is 0.04 ~ 0.24 mg / mL. The correlation coefficient R = 0.999 9, the detection limit was 1.05 × 10-2μg / mL, the standard deviation SD was 0.003 5, the relative standard deviation RSD was 2.42% and the molar absorption coefficient 1.515 × 105L / (mol · cm) The recovery rate was 96.7% ~ 98.8%. The experimental results show that the order of solubility of bismuth, bismuth oxide and bismuth sulfide is: bismuth> bismuth oxide> bismuth sulfide.