二次热解析-气相色谱法测定含氰废气中的氰化物
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摘要
建立了以Tenax-TA吸附管为吸附剂,采用二次热解析-气相色谱联用技术测定相关含氰废气处理装置试样中丙烯腈、乙腈含量的方法,通过对热解析和色谱条件进行优化,使用标准试样测定了线性范围和工作曲线,考察了方法的精密度和准确度,并采用该方法对含氰废气中的丙烯腈、乙腈进行了测定。实验结果表明,丙烯腈、乙腈的质量浓度在各自配制的质量浓度范围内呈现良好的线性关系,相关系数为0.999 9。标样回收率在99%～104%之间,6次重复测定的相对标准偏差均小于3%,两种物质的热解析效率均高于98%,丙烯腈检出限为3.12×10~(-4) mg/m~3。该方法具有良好的准确性、精密度和灵敏度,能很好地适用于含氰废气检测。
A method of determining acrylonitrile and acetonitrile contents in CN-containing waste gas was developed by a two-time thermal desorption/gas chromatography combined technique using Tenax-TA adsorption tube as adsorbent. The thermal desorption/gas chromatography conditions were optimized,and the precision and accuracy of this method were investigated by determining the linear range and working curve using standard samples. The method was applied to the determination of acrylonitrile and acetonitrile contents in the CN-containing waste gas. The experimental results showed that the mass concentrations of acrylonitrile and acetonitrile exhibited a good linear relationship within each formulaed mass concentration range,with correlation coefficients of 0.999 9. The recoveries of standards samples were from 99% to 104%,and the relative standard deviations of six repeated measurements are within 3%. Thermal desorption efficiency of the two components were above98%,and the detection limit of acrylonitrile was 3.12×10~(-4) mg/m~3. The method has good accuracy,precision and sensitivity,and is suitable for the detection of CN-containing waste gas.
A method of determining acrylonitrile and acetonitrile contents in CN-containing waste gas was developed by a two-time thermal desorption/gas chromatography combined technique using Tenax-TA adsorption tube as adsorbent. The thermal desorption/gas chromatography conditions were optimized,and the precision and accuracy of this method were investigated by determining the linear range and working curve using standard samples. The method was applied to the determination of acrylonitrile and acetonitrile contents in the CN-containing waste gas. The experimental results showed that the mass concentrations of acrylonitrile and acetonitrile exhibited a good linear relationship within each formulaed mass concentration range,with correlation coefficients of 0.999 9. The recoveries of standards samples were from 99% to 104%,and the relative standard deviations of six repeated measurements are within 3%. Thermal desorption efficiency of the two components were above98%,and the detection limit of acrylonitrile was 3.12×10~(-4) mg/m~3. The method has good accuracy,precision and sensitivity,and is suitable for the detection of CN-containing waste gas.
引文
[1]黄金霞,张润春,陆书来.2017年丙烯腈生产与市场[J].化学工业,2018,36(3):35-41.
[2]黄金霞,张润春,陆书来.2016年丙烯腈生产与市场[J].化学工业,2017,35(3):45-49.
[3]崔小明.我国丙烯腈生产技术进展及市场分析[J].化工市场,2015,40(11):32-36.
[4]张林伟.我国丙烯腈行业现状及发展前景[J].石油化工技术与经济,2014(1):53-57.
[5]纪立春,刘权益,孙亚斌,等.丙烯腈生产技术进展及国内外市场动态[J].弹性体,2009,19(6):69-74.
[6]姜其舟.丙烯腈行业生产现状分析[J].山东化工,2018,47(7):56-59.
[7]何学萍,董艳华,孙洪辉.消除含氰废气隐患,提高丙烯腈装置安全环保水平[J].中国高新技术企业,2011(22):102-104.
[8]杨郁满,孙铁,张素香,等.丙烯腈装置废气污水处理技术与设备改进[J].现代化工,2014,34(1):126-128.
[9]国家环境保护局.GB 16297-1996大气污染物综合排放标准[S].北京:中国标准出版社,1997.
[10]国家环境保护局.GB 31571-2015石油化学工业污染物排放标准[S].北京:中国标准出版社,2015.
[11]国家环境保护局.HJ/T 37-1999固定污染源排气中丙烯腈的测定气相色谱法[S].北京:中国标准出版社,1999.
[2]黄金霞,张润春,陆书来.2016年丙烯腈生产与市场[J].化学工业,2017,35(3):45-49.
[3]崔小明.我国丙烯腈生产技术进展及市场分析[J].化工市场,2015,40(11):32-36.
[4]张林伟.我国丙烯腈行业现状及发展前景[J].石油化工技术与经济,2014(1):53-57.
[5]纪立春,刘权益,孙亚斌,等.丙烯腈生产技术进展及国内外市场动态[J].弹性体,2009,19(6):69-74.
[6]姜其舟.丙烯腈行业生产现状分析[J].山东化工,2018,47(7):56-59.
[7]何学萍,董艳华,孙洪辉.消除含氰废气隐患,提高丙烯腈装置安全环保水平[J].中国高新技术企业,2011(22):102-104.
[8]杨郁满,孙铁,张素香,等.丙烯腈装置废气污水处理技术与设备改进[J].现代化工,2014,34(1):126-128.
[9]国家环境保护局.GB 16297-1996大气污染物综合排放标准[S].北京:中国标准出版社,1997.
[10]国家环境保护局.GB 31571-2015石油化学工业污染物排放标准[S].北京:中国标准出版社,2015.
[11]国家环境保护局.HJ/T 37-1999固定污染源排气中丙烯腈的测定气相色谱法[S].北京:中国标准出版社,1999.