1. 中汽研汽车检验中心（天津）有限公司，天津 300300； 2. 中国汽车技术研究中心有限公司，天津 300300
Determination of Pt, Pd, Rh in automotive ceramic catalyst by super microwave digestion inductively coupled plasma mass spectrometry
Yao Hui1, Wang Yang2, Yang Huiling1
1. CATARC Automotive Test Center (Tianjin) Co., Ltd., Tianjin 300300; 2. China Automotive Technology and Research Center Co., Ltd., Tianjin 300300
摘要：建立了一种检测车用陶瓷催化剂中铂、钯、铑的超级微波消解电感耦合等离子体质谱法。通过单因素试验和正交试验优化酸配比、称样量、消解温度、消解时间及回流溶剂参数，确定了最佳消解方法：0.1 g 样品中加入1 mL 盐酸、5 mL 硝酸、1 mL 氢氟酸，在220 ℃的消解温度下保持30 min，赶酸后加入10 mL 逆王水于170 ℃回流60 min，以电感耦合等离子体质谱法进行测定。在优化的条件下，铂、钯、铑的质量浓度在20～1 000 μg/L 范围内与响应值线性关系良好，相关系数均为1.000 0，检出限分别为2.5、2.1、4.9 μg/L。铂、钯、铑测定结果的标准偏差分别为0.59%、1.15%、1.20%（n=7），加标回收率分别为99.6%、101.2%、102.7%。该方法具有较高的准确度，有望应用于HJ 509-2009 标准修订。
Abstract：A method for the determination of platinum, palladium and rhodium in automotive ceramic catalysts by super microwave digestion inductively coupled plasma mass spectrometry was established. Through single factor tests and orthogonal test, the acid ratio, sample weight, digestion temperature, digestion time and reflux solvent parameters were optimized, and the optimal digestion method was determined as follows: 1 mL hydrochloric acid, 5 mL nitric acid and 1 mL hydrofluoric acid were added to 0.1 g sample, and the digestion temperature was 220 ℃ for 30 min, 10 mL aqua regia was added after acid removal, and the reflux time was 60 min at 170 ℃, finally determined by inductively coupled plasma mass spectrometry. Under the optimized conditions, the mass concentration of platinum, palladium and rhodium had a good linear relationship with the response value 20-1 000 μg/L, the correlation coefficients were 1.000 0 and the detection limits of platinum, palladium and rhodium were 2.5, 2.1 and 4.9 μg/L, respectively. The relative standard deviation of determination results of platinum, palladium and rhodium were 0.59%, 1.15% and 1.20% (n=7), and the recoveries were 99.6%, 101.2% and 102.7%, respectively. The method has high accuracy and is expected to be applied to the revision of HJ 509-2009 standard.
Keywords：super microwave digestion; automotive ceramic catalyst; platinum; palladium; rhodium
姚慧，王阳，杨惠玲. 超级微波消解电感耦合等离子体质谱法测定车用陶瓷催化剂中铂、钯、铑[J]. 化学分析计量，2021，30(2)：41.
Yao Hui，Wang Yang，Yang Huiling. Determination of Pt，Pd，Rh in automotive ceramic catalyst by super microwave digestion inductively coupled plasma mass spectrometry[ J]. Chemical Analysis and Meterage，2021，30(2)：41.