气相色谱法测定煤制乙二醇粗产品的纯度及10种有机杂质
兰淑惠,叶德钧,杨俊,刘积位,黎福钊,周业婵
中国检验认证集团广西有限公司,南宁 530000
Determination of purity and 10 organic impurities of crude ethylene glycol products produced from coal by gas chromatography
LAN Shuhui, YE Dejun, YANG Jun, LIU Jiwei, LI Fuzhao, ZHOU Yechan
China Certification & Inspection Group Guangxi Co., Ltd., Nanning 530000, China
摘要:建立气相色谱法测定煤制乙二醇粗产品的纯度及甲醇、乙醇、1, 2-丙二醇、1, 2-丁二醇、1, 3-二氧杂烷-2-甲醇、1, 4-丁二醇、二乙二醇、碳酸乙烯酯、1, 2-己二醇、三乙二醇10种有机杂质的方法。对样品进行超声处理5 min,以DB-624色谱柱(30 m×0.32 mm, 1.8μm)为分析柱,采用FID检测器进行测定,校正色谱峰面积归一化法定量,样品应在采集后24 h内完成测定。该方法检出限为0.000 4%~0.001 0%(质量分数),加标回收率为86.0%~114.9%,测定结果的相对标准偏差为0.8%~5.5%(n=9)。该方法可用于煤制乙二醇生产工艺分析及过程监测。
Abstract:A method was established for the determination of the purity and 10 organic impurities such as methanol, ethanol, 1, 2-propylene glycol, 1, 2-butanediol, 1, 3-dioxane-2-methanol, 1, 4-butanediol, diethylene glycol, vinyl carbonate, 1, 2-hexanediol and triethylene glycol of crude ethylene glycol products produced from coal by gas chromatography. The samples were treated by ultrasonic for 5 min, DB-624 column (30 m×0.32 mm, 1.8μm) was used as the analytical column, FID detector was used for determination, and the chromatographic peak area normalization method was used for quanti fication. The sample should be determined within 24 h after collection. The detection limit of the method was 0.000 4%-0.001 0%(mass fraction), the recoveries were 86.0%-114.9%, and the relative standard deviations of the determination results were 0.8%-5.5%(n=9). The method can be used for process analysis and process monitoring of ethylene glycol production made from coal.
关键词:乙二醇;气相色谱法;纯度;杂质
Keywords:ethylene glycol; gas chromatography; purity; impurities
基金:中检集团研发项目(2021ZJYF002)
本文引用格式:
兰淑惠,叶德钧,杨俊,等.气相色谱法测定煤制乙二醇粗产品的纯度及10种有机杂质[J].化学分析计量,2022,31(7):13.
LAN Shuhui,YE Dejun,YANG Jun,et al. Determination of purity and 10 organic impurities of crude ethylene glycol products produced from coal by gas chromatography[J]. Chemical Analysis and Meterage,2022,31(7):13.
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