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 m L盐酸,2 m L硝酸和1 m L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。
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.
作者
姚慧
王坤
杨惠玲
YAO Hui;WANG Kun;YANG Huiling(China Automotive Technology and Research Center,Tianjin 300300,China)
出处
《中国测试》
CAS
北大核心
2018年第8期47-51,共5页
China Measurement & Test
关键词
SCR
钒
钨
钛
电感耦合等离子体质谱法
selective catalyst reduction
vanadium
tungsten
titanium
inductively coupled plasma mass spectrometry
