离子色谱法测定变质烟用浸膏中硫化氢的含量

Determination of Hydrogen Sulfide in Deteriorated Extracts for Tobacco by Ion Chromatography

提出了测定变质烟用浸膏中硫化氢含量的离子色谱法。通过改进的蒸馏装置,在酸化条件下,对变质浸膏采取水蒸气蒸馏法分离,馏出的硫化氢气体用5%(质量分数)氢氧化钠溶液吸收。以IonPac AS7阴离子交换柱为分离柱,以1.5mol·L-1氢氧化钠-1mol·L-1乙酸钠-2%(体积分数)乙二胺(40+50+10)混合液为流动相,采用离子色谱-脉冲安培检测法测定其中硫化氢的含量。硫化氢的质量浓度在0.05~10mg·L-1范围内与对应的峰面积呈线性关系,检出限(3S/N)为3.2μg·L-1,加标回收率为92.0%~95.4%,日内相对标准偏差(n=7)和日间相对标准偏差(n=7)均小于4.0%。

A method of ion chromatography was proposed for determination of hydrogen sulfide in deteriorated extracts for tobacco. Under the conditions of acidification, H2S was separated by water vapor distillation from deteriorated extracts for tobacco with the improved distillation device, and then absorbed by 5% （w） NaOH solution. H2 S was determined by ion chromatography with pulsed amperometric detection, IonPae AS7 anion exchange column as separation column, and the mixture of 1.5 mol·L^-1 NaOH-1 mol·L^-1 CH3 COONa-2 （9） ethylenediamine （40＋50＋10） as the mobile phase. Linear relationship between values of peak area and mass concentration of H2S was obtained in the range of 0. 05-10 mol·L^-1, with detection limits （3S/N） of 3.2μg·L^-1. Values of the spiked recovery were found in the range of 92. 0%--95. 4%, and RSDs （n=7） of intra-day and RSDs （n=7） of inter-day were all less than 4. 0%.