顶空气相色谱法测定氯乙烯生产过程产生的盐酸溶液中的乙炔和氯乙烯  

Determination of Acetylene and Vinyl Chloride in Hydrochloric Acid from Producing Vinyl Chloride by Headspace Gas Chromatography

作　　者：申书昌[1] 张文治[1] 王文波[1] 

机构地区：[1]齐齐哈尔大学化学化工学院,黑龙江齐齐哈尔161006

出　　处：《色谱》2002年第3期269-271,共3页Chinese Journal of Chromatography

基　　金：黑龙江省自然科学基金资助课题 (编号 :B0 1 0 3 )

摘　　要：采用顶空气相色谱法测定了氯乙烯生产过程产生的盐酸溶液中的乙炔和氯乙烯。使用氢氧化钠将试样中的氯化氢中和 ,从而消除其在气相色谱分析乙炔和氯乙烯中的影响。顶空平衡温度为 35℃ ,平衡时间为 4 5min ,色谱柱为填充了GDX 2 0 2固定相的 2m× 3mmi d 不锈钢柱 ,柱温 14 0℃。顶空气体进样量为 1mL。以外标法定量 ,乙炔含量测定结果的相对标准偏差为 0 85 % ;当其含量为 30 0 μg/g～ 15 0 μg/g时 ,回收率为 98 9%～10 3%。氯乙烯含量测定结果的相对标准偏差为 1 4 % ;当其含量为 2 0 0 μg/g～ 10 0 μg/g时 ,回收率为 98 8%～10 2 %。A headspace gas chromatographic method was used for determining acetylene and vinyl chloride in hydrochloric acid from vinyl chloride production. Hydrogen chloride was neutralized by sodium hydroxide, so its effect on determining acetylene and vinyl chloride was eliminated. The headspace bottle was put in a water bath at 35 ℃ for 45 min. The GC column was a 2 m×3 mm i d stainless steel tube packed with GDX 202 stationary phase. The column temperature was 140 ℃. Injection volume was 1 mL. External standard method was used for quantitation. The relative standard deviation was 0 85% and the recoveries in the range of 30 0 μg/g-150 μg/g were 98 9%-103% for acetylene. The relative standard deviation was 1 4% and the recoveries in the range of 20 0 μg/g-100 μg/g were 98 8%-102% for vinyl chloride.

关 键 词：测定 生产过程 盐酸溶液 顶空气相色谱法 乙炔 氯乙炔 

分 类 号：TQ222.423[化学工程—有机化工]