1. 安徽省产品质量监督检验研究院，合肥 230051； 2. 安徽省生态环境监测中心，合肥 230071
Rapid determination of sulfide in industrial wastewater by gas phase molecular absorption
WANG Zhao1, ZHAO Bin2, YAO Bangben1
1. Anhui Institute of Product Quality Supervision and Inspection, Hefei 230051, China; 2. Anhui Ecological Environment Monitoring Center, Hefei 230071, China
摘要：建立气相分子吸收法快速测定工业废水中硫化物的方法。 水样经乙酸锌溶液固定后转化成硫化锌沉淀，硫化锌沉淀与盐酸反应转化成硫化氢，用载气将硫化氢气体载入气相分子吸收光谱仪的吸光管中，于 202.6 nm 波长处测定吸光度，吸光度与硫化物质量浓度之间的关系符合朗伯-比尔定律。 硫化物质量浓度在 0.02～10.0 mg/L 范围内与吸光度线性关系良好，相关系数为 0.999 6，方法检出限为 0.005 mg/L。采用所建方法分别对水质硫化物标准样品、硫化物标准溶液和加标工业废水平行测定 6 次，测定值的相对标准偏差为 1.3%～7.9%。对水质硫化物标准样品和硫化物标准溶液进行测定，测定值与标准值基本一致，相对误差为-5.0%～2.3%。含硫和不含硫工业废水实际样品的加标回收率分别为 85.6% 和 80.1%。该方法快速 、灵敏、准确，可用于工业废水中硫化物的检测。
Abstract：A method for the rapid determination of sulfides in industrial wastewater by gas phase molecular absorption was established. The water sample was fixed in zinc acetate solution and converted into zinc sulfide precipitate. The zinc sulfide precipitate reacted with hydrochloric acid to convert into hydrogen sulfide. The hydrogen sulfide gas was loaded into the absorption tube of the gas phase molecular absorption spectrometer by using carrier gas, and the absorbance was determined at the wavelength of 202.6 nm. The relationship between absorbance and the mass concentration of sulfide followed Lambert-Beer's law. The mass concentration of sulfides had a good linear relationship with absorbance in the range of 0.02-10.0 mg/L, with the correlation coefficient of 0.999 6, and the detection limit was 0.005 mg/L. Six measurements were conducted by using the established method on water quality sulfide standard samples, sulfide standard solutions, and spiked industrial waste levels, the relative standard deviation of the determination results was 1.3%-7.9%. The determination of water quality sulfide standard samples and sulfide standard solutions showed that the determination values were basically consistent with the standard values, with the relative error of -5.0% to 2.3%. The actual recovery rates of sulfur containing and non sulfur containing industrial wastewater samples were 85.6% and 80.1%, respectively. This method is fast, sensitive, and accurate, and it can be used for the detection of sulfides in industrial wastewater.
Keywords：sulfide; gas phase molecular absorption spectrometry; industrial wastewater
WANG Zhao，ZHAO Bin，YAO Bangben. Rapid determination of sulfide in industrial wastewater by gas phase molecular absorption[J].Chemical Analysis and Meterage，2023，32(10)：39.