色谱2024，Vol.42Issue(8)：766-772,7.DOI:10.3724/SP.J.1123.2023.10028
离子色谱-脉冲安培法测定空气中微量硫化氢
Ion chromatography-pulsed amperometry method for determination of trace hydrogen sulfide in air
摘要
Abstract
Hydrogen sulfide(H2S)is a pervasive gaseous pollutant that emits the characteristic odor of rotten gas,even at low concentrations.It is generated during various industrial proces-ses,including petroleum and natural gas refining,mining operations,wastewater treatment ac-tivities,and refuse disposal practices.According to statistics from the World Health Organiza-tion(WHO),over 70 occupations are exposed to H2S,rendering it a key monitoring factor in occupational disease detection.Although H2S has legitimate uses in the chemical,medical,and other fields,prolonged exposure to this gas can cause severe damage to the respiratory and central nervous systems,as well as other organs in the human body.Moreover,the substantial release of H2S into the environment can lead to significant pollution.This noxious substance has the potential to impair soil,water,and air quality,while disrupting the equilibrium of the sur-rounding ecosystems.Therefore,sulfide has become one of the most commonly measured sub-stances for environmental monitoring worldwide.Achieving the stable enrichment and accurate detection of low-level H2S is of great significance.Common methods for detecting this gas in-clude spectrophotometry,chemical analysis,gas chromatography,rapid field detection,and ion chromatography.Although these methods provide relatively reliable results,they suffer from limitations such as high detection cost,low recovery,lack of environmental friendliness,and imprecise quantification of low-concentration H2S.Furthermore,the sampling processes in-volved in these methods are complex and require specialized equipment and electrical devices.Additionally,approximately 20％of the sulfides in a sample are lost after 2 h in a conventional alkaline sodium hydroxide solution,causing difficulties in preservation and detection. In this study,an accurate,efficient,and cost-saving method based on ion chromatography-pulse amperometry was developed for H2S determination.A conventional IonPac AS7(250 mm ×4 mm)anion-exchange column was employed,and a new eluent based on sodium hydroxide and sodium oxalate was used to replace the original sodium hydroxide-sodium acetate eluent.The main factors influencing the separation and detection performance of the proposed method,including the pulse amperage detection potential parameters and integration time,as well as the type and content of additives in the stabilizing solution,were optimized.The results showed that the proposed method had a good linear relationship between 10 and 3 000 μg/L,with cor-relation coefficients(r2)of up to 0.999.The limits of detection(S/N=3)and quantification(S/N=10)were 1.53 and 5.10 μg/L,respectively.The relative standard deviations(RSDs)of the peak area and retention time of sulfides were less than 0.2％(n=6).The new method ex-hibited excellent stability,with up to 90％reduction in reagent costs.Compared with conven-tional ion chromatography-pulse amperometry,this method is more suitable for detecting low concentrations of sulfides in actual samples.Sulfides in a 250 mmol/L sodium hydroxide-0.8％(mass fraction)ethylenediaminetetraacetic acid disodium salt solution were effectively main-tained for over 10 h.The new stabilizer significantly improved the reliability of both large-scale and long-term detection.The recovery of the proposed method was investigated by combining the system with a badge-type passive sampler.This sampling method requires no power de-vices;it is inexpensive,simple to operate,and can realize long-term sampling without the need for skilled personnel.Moreover,it can overcome the influence of short-term changes in pollu-tant concentration.The sampling results have high reference value for large-scale intervention-less pollutant monitoring in ultraclean rooms,museum counters,and other places.The results demonstrated that the recovery of the proposed method was greater than 95％for the blank sample and 80％for the sample plus standard solution.Finally,the newly established method was applied to determine H2S levels in air samples collected via passive sampling at school gar-bage stations.The measured results did not exceed the national limit.关键词
离子色谱/安培检测/硫化物/电位/草酸钠Key words
ion chromatography(IC)/amperometric detection/sulfide/potential/sodium oxalate分类
化学化工引用本文复制引用
高晓静,倪彤,沈睿,施超欧..离子色谱-脉冲安培法测定空气中微量硫化氢[J].色谱,2024,42(8):766-772,7.基金项目
馆藏文物预防性保护风险防控关键技术研发示范项目(2020YFC1522500).Research and Development Demonstration of Key Technologies for Risk Prevention and Control in the Pre-ventive Protection of Cultural Relics(No.2020YFC1522500). （2020YFC1522500）
