作者：姚慧, 王坤, 杨惠玲
作者单位：中国汽车技术研究中心, 天津 300300
关键词：SCR;钒;钨;钛;电感耦合等离子体质谱法
摘要：
试验首先采用6种不同酸配比的酸溶法和2种碱熔法对SCR催化剂进行前处理，采用电感耦合等离子体质谱法测定样品中钒、钨、钛含量。实验发现：需添加氢氟酸，否则钨、钛溶出率极低，钨在高温下易挥发，采用碱熔法溶出率低。试验通过对酸添加量，微波消解温度和消解时间的考察，进一步优化酸溶法，并以电感耦合等离子体质谱法测定样品中钒、钨、钛含量。结果显示：采用8 mL盐酸，2 mL硝酸和1 mL氢氟酸，在180℃下微波消解30 min，为SCR最佳前处理方案，钒钨钛的回收率分别为101.0%，100.7%，101.7%，相对标准偏差分别为1.0%，2.2%，0.3%，结果满意。
Determination of vanadium, tungsten and titanium content in SCR catalyst
YAO Hui, WANG Kun, YANG Huiling
China Automotive Technology and Research Center, Tianjin 300300, China
Abstract: Firstly, 6 acid solution methods and 2 alkali fusion methods were used to compare the pretreatment of SCR catalyst, and the content of vanadium, tungsten and titanium in the sample was determined by inductively coupled plasma mass spectrometry (ICP MS). The results showed that hydrofluoric acid was needed, otherwise the dissolution rate of tungsten and titanium was very low, tungsten was easy to volatilize at high temperature, and the dissolution rate was low by alkali fusion methods. The amount of acid added, the temperature of microwave digestion and the time of microwave digestion were investigated to further optimize the acid dissolution method, and the content of vanadium, tungsten and titanium in the sample was determined by ICP MS. The results show that the best method for SCR catalyst degestion was using 8 mL hydrochloric acid, 2 mL nitric acid and 1 mL hydrofluoric acid, microwave digestion of 30 min at 180℃. The recoveries of vanadium, tungsten and titanium were 101%, 100.7% and 101.7%, respectively. The relative standard deviations were 1%, 2.2% and 0.3%, respectively. The results were satisfactory.
Keywords: selective catalyst reduction;vanadium;tungsten;titanium;inductively coupled plasma mass spectrometry
2018, 44(8): 47-51 收稿日期: 2018-02-04;收到修改稿日期: 2018-03-16
基金项目:
作者简介: 姚慧(1984-),女,天津市人,工程师,硕士,主要从事车用催化剂贵金属检测研究工作
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