分离硅、磷快速定量测定砷的探讨

Rapid Quantitative Determination of Arsenic by Separation of Silicon and Phosphorus

砷是钢铁成分中的有害元素，当砷含量较高时，会使钢的脆性增加，延伸率，断面收缩率及冲击韧性降低。测定钢铁中砷的含量对炼钢十分重要，为实现砷的快速测定，本文深入探讨分离硅、磷，用砷钼蓝比色法，实现砷定量的快速测定。提出用高氯酸冒烟分离钢铁样品中的硅，用硝酸溶解残留物，在酸性介质中，加入钼酸铵溶液和乙酸丁酯萃取生成磷钼酸，砷与钼酸铵生成砷钼黄，再加入酒石酸钾纳掩蔽磷，加入抗败血酸和氯化亚锡混合液还原，使砷钼黄还原为砷钼蓝，然后用此砷钼蓝比色法快速定量测定砷。此方法的加标准回收率94.74％～108.0％.检出限为0.005％。

Arsenic was a harmful ingredient in steel.The high degree of arsenic content increased the brittleness of steel, and decreased the elongation , section shrinkage rate and impact toughness.For the rapid determination of arsenic , the separation of silicon in steel samples with perchloric acid smoking , dissolved in nitric acid residued in acidic medium , adding ammonium molybdate solution and butyl acetate extraction form phosphomolybdic acid , arsenic and ammonium molybdate formed molybdenum yellow arsenic , adding tartaric acid potassium sodium masking P , anti septic acid and stannous chloride mixture reduction , the reduction of arsenic molybdenum yellow arsenic molybdenum blue , and then used the arsenic molybdenum blue colorimetric method for rapid quantitative determination of arsenic.