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建立了氢还原重量法测定三氯化钌产品大样中钌含量的新方法,研究并优化了测定条件,结合原子吸收光谱法(AAS)、电感耦合等离子体原子发射光谱法(ICP-AES)和氯化铵纯度考察了杂质元素对了分析结果的误差影响。结果表明,钌含量为0.3~0.6g的三氯化钌与5~7g氯化铵能完全形成(NH4)2RuCl6配合物,于约100℃烘干水分、350℃分解铵盐、750℃氢还原为海绵钌和105℃干燥水气的条件下,测定3.94%,5.88%,7.32%,9.47%,10.84%和12.93%含量的钌,极差、标准偏差(S)、相对标准偏差(RSD,n=22)和重复性限(r)分别为±0.01%,0.0030%~0.0050%,0.0369%~0.0761%和0.008%~0.014%。样品加标回收率99.96%~99.98%。方法的结果准确,精密度好,且与YS/T562—2009标准分析方法的吻合。
A new method for the determination of ruthenium in a large sample of ruthenium trichloride by hydrogen reduction gravimetry was established. The conditions for the determination of ruthenium in a large sample of ruthenium trichloride were established. The conditions of the determination were optimized. The atomic absorption spectrometry (AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) And the purity of ammonium chloride investigated the impact of impurity elements on the analysis of the error. The results show that ruthenium trichloride with ruthenium content of 0.3 ~ 0.6g and ammonium chloride with 5 ~ 7g can completely form (NH4) 2RuCl6 complex, drying at about 100 ℃, decomposing ammonium salt at 350 ℃, reducing hydrogen at 750 ℃ Ruthenium, very poor, standard deviation (S), relative standard deviations (RSDs) of 3.94%, 5.88%, 7.32%, 9.47%, 10.84% and 12.93% were measured under the conditions of sponge ruthenium and 105 ℃ dry moisture. n = 22) and repeatability (r) were ± 0.01%, 0.0030% ~ 0.0050%, 0.0369% ~ 0.0761% and 0.008% ~ 0.014%, respectively. The recoveries of spiked samples ranged from 99.96% to 99.98%. The method has accurate result and good precision, and is consistent with YS / T562-2009 standard analysis method.