气相色谱三内标法同时测定苯甲醚产品中五种成分的含量
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摘要
针对新型"环境友好型"工艺生产的苯甲醚产品特性,特建立了同时测定其主含量与杂质含量的气相色谱内标分析法。分别以1,4-二氧六环、乙基环己烷、4-乙基甲苯为碳酸二甲酯、苯甲醚、苯酚、邻甲基苯甲醚与对甲基苯甲醚的内标物,各物质色谱峰12分钟内可以完全分离; 5种组分和内标物的峰面积比值与其质量浓度比有良好的线性关系,线性相关系数0. 9994～1. 0000,方法检出限0. 0029 g/L～0. 033 g/L,定量限为0. 0097 g/L～0. 11 g/L;方法重复性相对标准偏差(RSD)为0. 074%～2. 9%;对平行六组相同样品进行三水平加标试验,其平均回收率为98. 7%～105. 0%,RSD为0. 33%～2. 19%;将此方法应用于苯甲醚产品的定性与定量检测,并采用格布鲁斯检验法对各组分含量进行显著性评价。本方法简单、快速、准确,可同时测定苯甲醚产品中主产物与特征杂质的含量,为质量控制提供可靠的依据。
A new internal standard analysis method for the simultaneous determination of the main products and impurities of anisole by gas chromatography was established due to the features of components obtained through environment-friendly technology. Specifically,1,4-dioxane,ethylcyclohexane and 4-ethyltoluene were selected as the internal standard substances for dimethyl carbonate; anisole; phenol,o-methyl anisole and p-methyl anisole,respectively and these components were separated completely from each other within 12 min. The calibration curve of peak area ratio on the mass concentration ratio was linear with a correlation coefficient from 0. 9994 to 1. 0000,limits of detection and quantification ranged from 0. 0029 g/L to 0. 033 g/L and0. 0097 g/L to 0. 11 g/L,respectively; The relative standard deviation of method repeatability ranged from 0. 074% to 2. 9%.Three different spiked levels were measured with 6 parallel test samples,and the average recovery is 98. 7% ～ 105. 0% with RSD0. 33% ～ 2. 19%. This method had been applied to commercial anisole products for qualitative and quantitative analysis,and Grubbs tests were used to pick up outliers for evaluating every sample. This method is simple,fast,accurate and suitable for simultaneous determination of principle products and impurities of anisole,providing reliable support for quality control process.
A new internal standard analysis method for the simultaneous determination of the main products and impurities of anisole by gas chromatography was established due to the features of components obtained through environment-friendly technology. Specifically,1,4-dioxane,ethylcyclohexane and 4-ethyltoluene were selected as the internal standard substances for dimethyl carbonate; anisole; phenol,o-methyl anisole and p-methyl anisole,respectively and these components were separated completely from each other within 12 min. The calibration curve of peak area ratio on the mass concentration ratio was linear with a correlation coefficient from 0. 9994 to 1. 0000,limits of detection and quantification ranged from 0. 0029 g/L to 0. 033 g/L and0. 0097 g/L to 0. 11 g/L,respectively; The relative standard deviation of method repeatability ranged from 0. 074% to 2. 9%.Three different spiked levels were measured with 6 parallel test samples,and the average recovery is 98. 7% ～ 105. 0% with RSD0. 33% ～ 2. 19%. This method had been applied to commercial anisole products for qualitative and quantitative analysis,and Grubbs tests were used to pick up outliers for evaluating every sample. This method is simple,fast,accurate and suitable for simultaneous determination of principle products and impurities of anisole,providing reliable support for quality control process.
引文
[1]Kirichenko G N,Glazunova V I,Balaev A V,et al.Catalytic vapor phase alkylation of phenol with methanol[J].Petroleum Chemistry,2008,48(5):389-392.
[2]Samolada M C,Grigoriadou E,Kiparissides Z,et al.Selective o-alkylation of phenol with methanol over sulfates supported onγ-Al2O3[J].Journal of Catalysis,1995,152(1):52-62.
[3]Lee S C,Lee S W,Kim K S,et al.O-alkylation of phenol derivatives over basic zeolites[J].Catalysis Today,1988,44(1/4):253-258.
[4]宋锡瑾,王常申.合成苯甲醚的新工艺[J].精细化工,2000,17(1):42-44.
[5]Dang D,Wang Z,Lin W G,et al.Synthesis of anisole by vapor phase methylation of phenol with methanol over catalysts supported on activated alumina[J].Chinese Journal of Catalysis,2016,37(5):720-726.
[6]唐黎华,张成芳,陈玲君,等.碳酸二甲酯水解反应的研究[J].华东理工大学学报,1998,24(2):243-245.
[7]胡永刚,张生万.苯甲醚中苯酚气相色谱测定的研究[J].山西大学学报(自然科学版),1997,20(1):70-72.
[8]陈燕.气相色谱法测定苯甲醚中杂酚杂醚[J].科技视界,2015,22:324-325.
[9]侯倩倩,张文申,许峰,等.气相色谱内标法测定偏二甲肼纯度[J].化学推进剂与高分子材料,2016,14(6):88-90.
[10]郭伟强,张培敏,边平凤.分析化学手册(第三版)基础知识与安全知识[M].北京:化学工业出版社,2016:893.
[2]Samolada M C,Grigoriadou E,Kiparissides Z,et al.Selective o-alkylation of phenol with methanol over sulfates supported onγ-Al2O3[J].Journal of Catalysis,1995,152(1):52-62.
[3]Lee S C,Lee S W,Kim K S,et al.O-alkylation of phenol derivatives over basic zeolites[J].Catalysis Today,1988,44(1/4):253-258.
[4]宋锡瑾,王常申.合成苯甲醚的新工艺[J].精细化工,2000,17(1):42-44.
[5]Dang D,Wang Z,Lin W G,et al.Synthesis of anisole by vapor phase methylation of phenol with methanol over catalysts supported on activated alumina[J].Chinese Journal of Catalysis,2016,37(5):720-726.
[6]唐黎华,张成芳,陈玲君,等.碳酸二甲酯水解反应的研究[J].华东理工大学学报,1998,24(2):243-245.
[7]胡永刚,张生万.苯甲醚中苯酚气相色谱测定的研究[J].山西大学学报(自然科学版),1997,20(1):70-72.
[8]陈燕.气相色谱法测定苯甲醚中杂酚杂醚[J].科技视界,2015,22:324-325.
[9]侯倩倩,张文申,许峰,等.气相色谱内标法测定偏二甲肼纯度[J].化学推进剂与高分子材料,2016,14(6):88-90.
[10]郭伟强,张培敏,边平凤.分析化学手册(第三版)基础知识与安全知识[M].北京:化学工业出版社,2016:893.