负载型季鏻盐高分子聚合物催化剂中氯和磷的测定

摘要

The contents of chlorine and phosphorus in polymer-supported quaternary phosphonium catalysts were determined by oxygen flask combustion and then by means of IC or ICP-OES method. The accuracy of the methods was investigated with benzyltriphenylphosphonium chloride as simulate sample. The results showed that when the IC method was used,the recoveries of chlorine and phosphorus were 95.3% and 73.9% respectively. After being treated with H2O2,the recovery of phosphorus didn’t increase. When the contents of chlorine and phosphorus in the polymer supported catalysts were analyzed by IC,the relative standard deviation(RSD)<4%,the addition standard recovery of chlorine was in the range of 97.4%-98.6% and the addition standard recovery of phosphorus was in the range of 104.5%-106.9%. The simulate samples without treatment and treated with H2O2 were analyzed by means of ICP-OES,and the recoveries of phosphorus were 98.2%and 97.1%,respectively. When the polymer supported catalysts were analyzed by means of ICP-OES, RSD<2%and the addition standard recovery of phosphorus was in the range of 96.8%-97.0%. The results were compared with the analytical results by XRF without standard sample. The method could be used to accurately analyze the contents of chlorine and phosphorus in catalysts.%采用氧瓶燃烧试样前处理，结合IC法和ICP-OES法测定了负载型季鏻盐高分子聚合物催化剂中氯和磷的含量。以苄基三苯基氯化鏻为模拟试样，考察了方法的回收率。实验结果表明，模拟试样用IC法分析时氯回收率为95.3%，磷回收率为73.9%。采用H2O2预处理后，磷回收率未提高。催化剂试样采用IC法测定氯和磷含量时，相对标准偏差小于4%，氯的加标回收率在97.4%～98.6%之间，磷的加标回收率在104.5%～106.9%之间。用ICP-OES法分析模拟试样，不加或加入H2O2预处理时，磷的回收率分别为98.2%和97.1%。催化剂试样采用ICP-OES法分析磷含量时，相对标准偏差小于2%，磷的加标回收率在96.8%～97.0%之间。与无标样XRF法测定氯和磷含量比较，该方法可用于聚合物催化剂中氯和磷含量的准确分析。