顶空气相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

 采用顶空气相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 ,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 %。

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

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 degrees C for 45 min. The GC column was a 2 m x 3 mm i.d. stainless steel tube packed with GDX-202 stationary phase. The column temperature was 140 degrees C. 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 micrograms/g-150 micrograms/g were 98.9%-103% for acetylene. The relative standard deviation was 1.4% and the recoveries in the range of 20.0 micrograms/g-100 micrograms/g were 98.8%-102% for vinyl chloride.