吗啉产品纯度及杂质的气相色谱分析  

Determination of purity and impurities of morpholine by gas chromatography

作　　者：石占崇[1] 王松芝[1] 刘昱[2] 

机构地区：[1]中国石油吉林石化公司研究院,吉林吉林132021 [2]中国石油吉林石化公司,吉林吉林132021

出　　处：《化工科技》2013年第1期41-47,共7页Science & Technology in Chemical Industry

基　　金：国家标准工作委员会项目(20080734-T-606)

摘　　要：采用以改性的石墨化碳黑为色谱柱进行分离、热导检测器进行检测、校正面积归一化法进行定量的分析方法,同时对吗啉产品纯度及杂质进行气相色谱分析。对色谱柱的选择、操作条件的优化、定性分析、进样量和线性范围、最低检测限、校正因子、重复性和再现性实验结果、比对性实验结果等实验项目进行了考察,实验结果表明:吗啉产品纯度在产品质量检验指标范围内[w(吗啉)>98.0%;w(水)=0.10%～0.50%;w(乙二醇单甲醚)、w(N-甲基吗啉)和w(N-乙基吗啉)均<0.20%],经统计2次测定结果之差w(吗啉)<0.06%,w(水)<0.02%,乙二醇单甲醚等w(其它杂质)<0.01%;保留时间的相对标准偏差小于5%;方法最低检测浓度:进样量为1μL时,w(水)=0.02%,w(N-甲基吗啉)和w(乙二醇单甲醚)均为0.002%、w(N-乙基吗啉)=0.005%;此法具有操作简单,分析速度快、分析成本较低、重复性与准确性较好等特点,能够满足产品检验需要。The purity and impurities of morpholine were determined by gas chromatography using modified graphitized carbon black as chromatographic column. The thermal conductivity detector and the correct normalization area method were applied in the analytic method. The choose of the chroma- tographic column, the optimization of operating conditions, qualitative analysis, sampling amounts, the linearity range, the lowest detectable limit, corrected factors, repeatablility, reproducibility and the con- trast tests results were studied. In the product testing index range（the weight percent of morpholine was more than 98,of water was 0. 10-0. 50,of ethylene glycol monomethyl ether, N-methyl morpho- line and N-ethyl morpholine was all less than 0.20, respectively）, it was found that, the difference of the content of morpholine of the two experimental results was less than 0.06%, of water was less than 0.02% ,of impurities including ethylene glycol monomethyl ether etc. was less than 0.01%;the relative standard deviation of the retention time was less than 5% the lowest detectable limit of water was 0. 02%,of N-methyl morpholine and of ethylene glycol monomethyl ether was both 0. 002%, respectively, and of N-ethyl morpholine was 0. 005% with 1μL injecting volume. This method has the advantages of short analysis time, simple operation,low cost, good repeativity and excellent accuracy, which could meet the needs of products detection.

关 键 词：吗啉 1 4-氧氮杂环己烷 气相色谱法 纯度 杂质 最低检测浓度 

分 类 号：O657.71[理学—分析化学]