Determination of Sulfide in Geothermal Water by Inductively Coupled Plasma-Optical Emission Spectrometry
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摘要: 地热水中的硫化物（H2S、HS-和S2-）通常受到硫酸根、亚硫酸根、硫代硫酸根等硫元素的共存干扰，并且硫化物具有热、光、氧不稳定性，在水样保存、前处理、标准溶液配制等环节影响着测试的准确度和精密度。本文在现场采集的地热水水样中加入乙酸锌及氢氧化钠，使硫化物形成硫化锌沉淀而与溶液分离，将此沉淀溶于双氧水和逆王水，使低价态的S2-氧化成稳定的SO42-，选择易于纯化且性质稳定的硫酸钠配制硫标准储备液，以182.624 nm谱线作为硫元素分析谱线，应用电感耦合等离子体发射光谱法测定出地热水样中的硫化物含量。硫的浓度在0.1~100 mg/L范围内与其发射强度呈线性（相关系数为0.9994）；方法检出限为0.009 mg/L，相对标准偏差（n=11）低于1.80%，实际水样中硫化物的加标回收率介于99.0%~103.0%。与前人相关测试方法相比，本方法的技术指标具有优势。
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关键词:
- 硫化物 /
- 地热水 /
- 硫酸钠 /
- 电感耦合等离子体发射光谱法
Abstract: Existing sulfur-containing compounds, such as sulfate, sulfite and thiosulfate, can affect the determination of sulfide (H2S, HS- and S2-) in geothermal water. In addition, the detection accuracy and precision may also be influenced by sample treatment processes such as sample collecting, sample pretreatment, and standard solution preparation. Zinc acetate and sodium hydroxide were added to water samples collected at the site in which sulfide would be precipitated as zinc sulfide and separated from water. The precipitation was further dissolved in hydrogen peroxide and Lefort aqua regia in which S2- would be oxidized to SO42-. The standard stock solution was prepared by using sodium sulfate, which was stable and easily purified. Sulfur content in water was determined by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) using the spectrum of 182.624 nm as the sulfur element analysis line. It was found that S2- concentration ranging between 0.1 and 100 mg/L was linearly correlated with emission intensity with a correlation coefficient of 0.9994. Detection limit of the method was 0.009 mg/L, relative standard deviation (n=11) was less than 1.80%, and standard addition recovery was 99.0%-103.0%. The technical indicators in this method are superior to previous analytical methods. -
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表 1 ICP-OES仪器工作参数
Table 1. Operating parameters for ICP-OES determination
工作参数 设定值 垂直观测高度 15 mm 蠕动泵泵速 50 r/min 冷却气流量 一般 辅助气流量 1.0 L/min 发射功率 1250 W 载气压强 0.22 MPa 冲洗时间 30 s 短波积分时间 20 s 
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