碱液提取全基体进样-电感耦合等离子体串联质谱(ICP-MS/MS)法测定土壤中的六价铬  

Determination of Hexavalent Chromium in Soil by Inductively Coupled Plasma Tandem Mass Spectrometry(ICP-MS/MS)with Alkali Extraction Whole Matrix Injection

作　　者：张吴 徐义邦 高明 姜云娜 秦文 ZHANG Wu;XU Yibang;GAO Ming;JIANG Yunna;QIN Wen(Nanchang Ecological Environment Monitoring Centre in Jiangxi Province,Nanchang,Jiangxi 330038,China;Jiangxi Province Ecological Environmental Monnitoring Centre,Nanchang,Jiangxi 330039,China)

机构地区：[1]江西省南昌生态环境监测中心,南昌330038 [2]江西省生态环境监测中心,南昌330039

出　　处：《中国无机分析化学》2024年第9期1242-1247,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家环境保护重金属污染监测重点实验室开放基金资助项目(SKLMHM202317)。

摘　　要：针对HJ 1082—2019方法检出限高,高盐导致容易堵塞燃烧头,造成信号不稳定、结果漂移等问题。利用耐高盐全基体进样系统,通过引入稀释气降低高盐基体的影响,碱液提取后的样品可直接进样,结合ICP-MS/MS的低检出限,建立了碱液提取全基体进样-电感耦合等离子体串联质谱法准确测定土壤中低浓度六价铬的方法。对碱液提取条件、质谱仪器工作条件进行了优化,讨论质谱干扰对六价铬测定的影响,同时对标准样品和实际样品进行了精密度和正确度测试。方法检出限0.08 mg/kg,相对标准偏差在0.70%~4.2%、加标回收率在92.9%~107%。方法操作简便快速,检出限低,结果准确性高、重复性好。In response to the questions such as high detection limits,signal instability and result drift caused by blocking of the combustion head,which leaded by high salt content in HJ 1082—2019.By using a high salt resistant whole matrix injection system and introducing dilution gas to reduce the influence of high salt matrix,the sample extracted from alkaline solution can be directly injected.Combined with the low detection limit of ICP-MS/MS,an accurate method for the determination of low concentration hexavalent chromium in soil by alkaline digestion whole matrix injection inductively coupled plasma tandem mass spectrometry was established.The alkaline digestion conditions and the working conditions of the mass spectrometer were optimized.The influence of mass spectrometry interference on the determination of hexavalent chromium was discussed.At the same time,precision and accuracy tests were conducted on standard and actual samples.The detection limit of the method was 0.08 mg/kg,the relative standard deviation was between 0.70%and 4.2%,and the recovery of the added standard was between 92.9%and 107%.The method is easy and fast to operate,with low detection limit,high accuracy of results and good repeatability.

关 键 词：提取液温度 液固比 全基体进样 电感耦合等离子体串联质谱法 

分 类 号：O652[理学—分析化学]