气相色谱法分析聚甲醛二甲基醚合成产物中的甲醛含量.pdf

石油化工
2015年第44卷第9期
PETROCHEMICAL TECHNOLOGY
1127
气相色谱法分析聚甲醛二甲基醚
合成产物中的甲醛含量
许竟早,张育红,王川,高晓晨
(中国石化上海石油化工研究院,上海201208)
[摘要1采用CP-Wax毛细管柱(25mx0.25mmi.d.×0.2pm),建立测定聚甲醛二甲基瞇( PODE)合成产物中甲醛含量的
气相色谱法;针对该体系中难分离的甲醇和甲醛组分,优化了色谱条件,考察了方法的精密度和准确性,用该方法分析了
PODE实际试样。实验结果表明,使用CP-Wax毛细管色谱柱,实现了甲醛、甲缩醛、甲醇和水的完全分离;该方法测定
PODEっ合成产物中甲醛含量时, PODE1合成产物中的甲醛含量与峰面积呈良好的线性关系,线性相关系数为0.982~0.9995,
实际试样加标回收率为98%~101%,相对标准偏差小于3.0%(m=5),最低检测限为0.049%(w)。与传统的化学滴定法相比,
气相色谱法无需前处理,操作简便,测定结果准确、可靠。该方法可用于PODEっ合成产物中甲醛含量的定量分析,也可用于
含甲醇的体系中常量甲醛的分析。
L关鍵词」聚甲醛二甲基瞇;气相色谱法;甲醛;甲缩醛;甲醇
「文章编号]1000-8144(2015)09-1127-04
[中图分类号]0657.7
文献标志码]A
Analysis of Formaldehyde in Synthesized PODEM Products by Gas Chromatography
Xujingzao, Zhang Yuhong, Wang Chuan, Gao Xiaochen
SINOPEC Shanghai Research Institute of Petrochemical Technology, Shanghai 201208, China.
I Abstract A novel gas chromatography method for the analysis of formaldehyde in synthesized
polyoxymethylene dimethyl ethers(PODEM )products was established with a Cp-wax capillar
column(25 m x0.25 mm i.d. x0.2 wm)and TCD detector For methanol and formaldehyde separated
difficultly in the system, the chromatographic conditions were optimized. The repeatability and
accuracy of the method were investigated. The experimental results showed that four components in
the system, namely formaldehyde, methylal, methanol and water, were separated completely by
using the Cp-wax capillary column. The linear correlation coefficients of the standard curves were
0.9982-0.999 5. The addition standard recoveries of the method were in the range of 98-101
The relative standard deviations and the detection limit were less than 3.0%(n=5)and 0.049%(w)
respectively. Compared with the traditional chemical titration method, the gas chromato raphy method
without pre-treatment is simple and convenient, and the results are more accurate. It can also be used
for the analysis of formaldehyde in methanol system
I Keywords I polyoxymethylene dimethyl ether; gas chromatography; formaldehyde; methylal
methanol
聚甲醛二甲基( PODE,其中,m为整数,燃料添加组分虽能提高能源利用效率,减少尾气
1≤m<10)是一种新型清洁柴油添加组分1劉。当排放,但易造成气塞或气阻?。当m=2~10时
m=1时, PODE.即为甲缩醛,用甲缩醛作为车用 PODE.较适合用作柴油添加剂,在柴油中添加量
收稿日期12015-02-27;[修改稿日期12015-05-29。
作者简介]许竞早(1982-),女,安徽省庐江县人,硕土,工程师,电话021-68462197-6304,电邮xz.sshy@ sinopec, com