甲基异丁基甲酮萃取-火焰原子吸收光谱法测定氧化锑中的磷

研究了MIBK萃取-火焰原子吸收光谱法测定氧化锑中的磷。在盐酸介质中,磷酸根与钼酸铵形成磷钼物质的量之比为1∶12磷钼杂多酸,用酒石酸钾钠掩蔽锑,以甲基异丁基甲酮为萃取试剂,用火焰原子吸收光谱法测定有机相中磷钼杂多酸中的钼,据此建立了一种间接测定氧化锑中微量磷的新方法。在优化的实验条件下,当磷的含量在0.055~1.00 mg/L范围内时,其吸光度与浓度呈良好的线性关系;方法的检出限为0.011 mg/L;对4个样品进行测定的回收率在97.8%~106.2%之间;相对标准偏差为2.6%~4.2%。用于氧化锑中微量磷的测定,结果满意。

Methyl Isobutyl Ketone Extraction-Atomic Absorption Spectrometric Determination of Trace Phosphorus in Antimony Oxide

Determination of trace phosphorus in antimony oxide with flame atomic absorption spectrometry(FAAS) was investigated.After the antimony oxide sample was digested,the phosphorus in sample was converted to phosphate.Then,phosphate reacted with molybdic acid to produce phosphomolybdate complex and extracted by methyl isobutyl ketone.The phosphorus was determined indirectly by FAAS.The dynamic calibration curve ranged from 0.055 to 1.00 mg/L.The detection limit was 0.011 mg/L.The recovery of determining four samples was obtained within 97.8%-106.2%.The relative standard deviation was between 2.6% and 4.2%.This method was applied to determine trace phosphorus in Sb2O3 with satisfactory results.