摘要
采用微波消解系统消解硅橡胶催化剂,再用火焰原子吸收法测定了其中铂的含量。考察了消解试剂种类、无机酸、共存离子对测定结果的影响及抑制方法。结果表明,采用HNO3+HF或HCl+HF或王水+HF为消解试剂对硅橡胶催化剂进行微波消解时效果好,消解时避免使用H2SO4;为防止消解液爆沸,需进行预消解。常见共存离子K^+、Na^+、Fe^2+、Cu^2+、Pb^2+、Zn^2+、Ca^2+、Mg^2+、Si对铂含量测定结果的影响很大,无机酸HCl、HNO3及HF对铂含量的测定结果也有一定的影响;采用CuSO4作干扰抑制剂不仅能有效抑制无机酸和共存离子的影响,而且具有明显的增敏作用:此方法的相对标准偏差小于2%,回收率为92.43%~109.05%.
The silicone rubber catalyzer was melted by microwave counteract system, and the platinum content in silicone rubber catalyzer was then measured by flame atomic absorption spectroscopy. The influence of different counteraction solvents, inorganic acid and coexist ions and restraining method were studied. The results showed that silicone rubber catalyzer was melted effectively with nitric acid plus hydrofluoric acid or hydrochloric acid plus hydrofluoric acid or aqua regia plus hydrofluoric acid. Sulfuric acid was avoided tp use in this experiment, and it was necessary to do preparative counteraction for preventing boil. The influence of K ^+ ,Na^ + ,Fe^2 + , Cu^2 + , Pb^2 + , Zn^2 + , Ca^2 + , Mg^2 + and Si ions in the experiment was great, and hydrofluoric acid, nitric acid and hydrofluoric acid had certain effects in flame atomic absorption spectroscopy. The effects of inorganic acid and coexist ions were restrained by using the release solvent of CuSO4, and at the same time the measure sensitivity was increased. The relative standard deviation of the method was less than 2%, and the recovery rate was 92.43% to 109.05%.
出处
《有机硅材料》
CAS
2010年第1期45-49,共5页
Silicone Material
关键词
微波消解
火焰原子吸收法
铂
硅橡胶
加成型
microwave digestion, flame atomic absorption, platinum, silicone rubber, addition type