高频燃烧红外吸收法测SCR脱硝催化剂中的硫含量
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摘要
采用高频燃烧红外吸收法测定SCR脱硝催化剂中硫的含量,讨论了试样预处理、助熔剂用量及加入顺序、称样量三个方面对硫测量结果的影响,仪器校准曲线采用光谱纯二氧化钛作基体,基准硫酸钾作校准物质,减少由校准引入的系统误差,校准曲线的线性方程为y=0.081 5x+0.004 9,相关系数为0.999 6。结果表明:本方法对硫的检出限为1.4×10-5%,方法测定下限为5.6×10-5%,对四个硫含量不同的试样进行分析,相对标准偏差小于2%(n=7),方法加标回收率在95.7%~102%之间。本方法操作简单,检测速度快,检出限低,结果准确可靠,可以满足SCR脱硝催化剂分析要求。
The determination of sulfur content in SCR denitrification catalyst by high frequency combustion infrared absorption method was carried out.The influence on sulfur measurement results was discussed from three aspects:sample pretreatment,flux and addition order,sample quantity selection.The instrument calibration curve uses spectral pure titanium dioxide as the matrix,and the base potassium sulfate as the calibration material,reducing the system error introduced by the calibration.The linear equation of the calibration curve is y=0.081 5 x+0.004 9,and the correlation coefficient is 0.999 6.The results show that the detection limit of sulfur in this method is 1.4×10-5%,the lower limit of the method is 5.6×10-5%,and the relative standard deviation of four samples with different sulfur content is less than 2%(n=7).The method recovery rate was between 95.7% and 102%.The method has simple operation,fast detection speed,low detection limit,and accurate and reliable results,which can meet the requirements of SCR denitrification catalyst analysis.
The determination of sulfur content in SCR denitrification catalyst by high frequency combustion infrared absorption method was carried out.The influence on sulfur measurement results was discussed from three aspects:sample pretreatment,flux and addition order,sample quantity selection.The instrument calibration curve uses spectral pure titanium dioxide as the matrix,and the base potassium sulfate as the calibration material,reducing the system error introduced by the calibration.The linear equation of the calibration curve is y=0.081 5 x+0.004 9,and the correlation coefficient is 0.999 6.The results show that the detection limit of sulfur in this method is 1.4×10-5%,the lower limit of the method is 5.6×10-5%,and the relative standard deviation of four samples with different sulfur content is less than 2%(n=7).The method recovery rate was between 95.7% and 102%.The method has simple operation,fast detection speed,low detection limit,and accurate and reliable results,which can meet the requirements of SCR denitrification catalyst analysis.
引文
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15 庄艾春.高频燃烧红外吸收法测定锡锌铅青铜中硫[J].冶金分析,2017(4):33.
16 傅明,黄志强,杨万彪,等.高频红外碳硫仪快速测定金属硅中的碳和硫[J].分析科学学报,2003(2):199.
17 张鑫.高频燃烧红外吸收光谱法测定铀矿石中的硫[J].湿法冶金,2017(2):156.
18 刘攀,唐伟,张斌彬,等.高频感应燃烧-红外吸收光谱法在测定无机非金属样品中碳、硫的应用[J].理化检验(化学分册),2016(4):487.
19 环境保护部.HJ 168-2010环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.
2 卢晗,郑鑫,李薇,等.燃煤电厂脱硫技术及超低排放改造费效分析[J].环境工程,2018(1):97.
3 张效铭,程敢,张传祥.燃煤烟气氧化脱硫脱硝技术进展[J].应用化工,2018(2):375.
4 杨旭,陈红萍,齐雪.脱硝催化剂的硫中毒机理研究[J].现代化工,2018(2):20.
5 王丽朋,陈宝康,姚燕,等.脱硝催化剂失活及再生实验[J].热力发电,2017(11):67.
6 陈艳萍,吴思明,卢慧剑,等.1000MW燃煤电厂钒钛系脱硝催化剂失活原因分析[J].浙江大学学报(工学版),2015(3):564.
7 印德俊.硫精砂中高硫的熔融重量法测定[J].分析试验室,1993(6):95.
8 张晨.燃烧-中和滴定法测定锌精矿焙砂中的硫[J].中国无机分析化学,2016(3):47.
9 严恒泰.氧化物助熔供氧-以氮气作载气-燃烧-碘量法测定硫量[J].理化检验(化学分册),2017(12):1474.
10 马兵兵.ICP-AES法测定铝酸钠溶液中的总硫和低价硫[J].湿法冶金,2017(1):78.
11 苏雄.X-荧光光谱法测定硫原矿、硫尾矿中硫含量[J].中国钼业,2016(4):49.
12 杨绍美,陆建平,曹家兴,等.离子色谱同时测定中草药中磷硫含量[J].分析试验室,2011(7):119.
13 刘玉龙,缪德仁.原子吸收光谱法间接测定萤石中的全硫[J].分析试验室,2009(8):19.
14 谢树军,杨理琼.二氧化铀粉末中硫的测定——感应炉燃烧红外吸收法[J].湿法冶金,2008(3):191.
15 庄艾春.高频燃烧红外吸收法测定锡锌铅青铜中硫[J].冶金分析,2017(4):33.
16 傅明,黄志强,杨万彪,等.高频红外碳硫仪快速测定金属硅中的碳和硫[J].分析科学学报,2003(2):199.
17 张鑫.高频燃烧红外吸收光谱法测定铀矿石中的硫[J].湿法冶金,2017(2):156.
18 刘攀,唐伟,张斌彬,等.高频感应燃烧-红外吸收光谱法在测定无机非金属样品中碳、硫的应用[J].理化检验(化学分册),2016(4):487.
19 环境保护部.HJ 168-2010环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.