氢还原重量法测定三氯化钌产品中钌的含量  

Determination of Ruthenium in Ruthenium Trichloride by Hydrogen Reduction Gravimetric Method

作　　者：郭俊梅 韩守礼 谭文进 贺小塘 李琨 刘文 李勇 王欢 吴喜龙 

机构地区：[1]贵研资源(易门)有限公司,云南易门651100 [2]贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,昆明650106

出　　处：《中国无机分析化学》2014年第3期44-51,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家高技术研究发展计划基金(863计划)(2012AA063203;2012AA063207)资助;云南省科技创新强省计划项目(2011AA004)资助;云南省地方标准制(修)订基金项目(K24-2013)资助

摘　　要：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0.3～0.6 g的三氯化钌与5～7 g氯化铵能完全形成（NH4）2 RuCl6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 the production of ruthenium trichloride by hydrogen reduction gravimetrie method was established. Analytical conditions were investigated and optimized. Combining with AAS, ICP-AES and considering the purity of ammonia chloride, the effeet of impurities on the determination of ruthenium content was investigated. The results indicated that the （NH4）2RuC16 complex was formed completely using ruthenium trichloride （containing 0.3 - 0.6 g ruthenium） and ammonium chloride （5 - 7 g）, then it was reduced to sponge ruthenium under the conditions （1. water drying at 100℃, 2. decomposition of ammonium salt at 350℃, 3. hydrogen reduction at 750 ℃, 4. vapor drying at 105 ~C）. Ruthenium contents of 3.94%, 5.88%, 7.32%, 9.47%, 10. 84% and 12.93% in above-mentioned samples were measured. The ranges, standard deviations（S）, relative standard deviations （RSD, n = 22） and repeatability limits （r） were ± 0.01%, 0. 0030% 0.0050G, 0. 0369% -0. 0701% and 0. 008%-0. 014% , respectively. Comparing with YS/T 562-2009, the method is more accurate and precise.

关 键 词：三氯化钌产品 钌 氢还原重量法 

分 类 号：O655.1[理学—分析化学]