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反相可切换亲水性溶剂液-液微萃取/电感耦合等离子体质谱法测定变压器油中铜和铁离子含量
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作者单位
付宇超,杨珍,李吟霜,李海燕 1. 中南民族大学 化学与材料科学学院湖北 武汉 430074 2. 中南民族大学 分析化学国家民委重点实验室湖北 武汉 430074 
基金项目:中央高校基本科研业务费专项资金项目(CZY19037)
中文摘要:以电感耦合等离子体质谱(ICP-MS)为检测手段,研究了反相可切换亲水性溶剂液-液微萃取(SHS-LLME)同时分离富集变压器绝缘油中Cu2+和Fe3+的方法。优化的萃取条件为:以50 μL三乙胺(TEA)萃取25 mL变压器油样,0.60 mol/L硝酸溶液为触发剂,TEA和HNO3摩尔比为1∶1.5,涡旋萃取反应5 min,亲水切换反应5 min,经离心分离后,取水萃取相直接进样测定。变压器油中Cu2+和Fe3+的质量浓度在0.100~10.0 μg/L范围内线性关系良好,线性系数(r2)均为0.999 6,检出限分别为16.8 ng/L和29.0 ng/L,富集倍数分别为23.7和24.1倍。对模拟老化变压器油样中Cu2+和Fe3+的含量进行测定,其加标回收率为93.3%~112%,相对标准偏差(n = 6)为3.6%~5.6%。该文所建立的样品前处理方法与现行标准所用的灰化法无显著性差异,可实现老化变压器油中痕量Cu2+和Fe3+的同时测定。
中文关键词:反相可切换亲水性溶剂  液-液微萃取  铜和铁离子  变压器油  电感耦合等离子体质谱(ICP-MS)
 
Determination of Contents of Copper and Iron Ions in Transformer Oil by Inductively Coupled Plasma Mass Spectrometry with Reversed Phase Switchable Hydrophilic Solvent Liquid-Liquid Microextraction
Abstract:Increase in the concentration of metal copper and iron ions in the insulation oil for running transformer not only leads to the deepening of the corrosion of the high-voltage copper windings and iron cores immersed in the transformer oil and reduction of insulation performance of the transformer oil,but also causes the increase in the insulation aging ability of transformer oil-paper of metal ion catalysis.In order to track the concentration of copper and iron ions in the transformer oil in operation,and reduce sudden transformer insulation failures caused by the accelerated aging of transformer oil-paper insulation,an inductively coupled plasma mass spectrometry(ICP-MS) with reverse phase switchable hydrophilic solvent liquid-liquid microextraction was developed for the simultaneous separation,enrichment and determination of Cu2+ and Fe3+ in transformer insulating oil.The switchable hydrophilic solvent triethylamine(TEA) was used as the extractant,and nitric acid solution was used as the trigger. The extraction conditions were optimized as follows:50 μL of TEA was used to extract 25 mL of transformer oil sample,the molar ratio of TEA to HNO3 was 1∶1.5,the concentration of HNO3 was 0.60 mol/L,the reaction time of vortex extraction and the hydrophilicity switching reaction were both 5 min,the lower water extract phase could be directly injected for determination after centrifugation was performed at 4 500 r/min for 5 min. There were good linearities for Cu2+ and Fe3+ in the range of 0.100-10.0 μg/L,with their correlation coefficients(r2) of 0.999 6.The detection limits for Cu2+ and Fe3+ were 16.8 ng/L and 29.0 ng/L,respectively,and the enrichment factors were about 24 times.The concentration of Cu2+ and Fe3+ in the oil samples of the simulated aging transformer were determined.And the spiked recoveries of Cu2+ and Fe3+ ranged from 93.3% to 112%,with relative standard deviations(RSDs) of 3.6%-5.6%.There is no significant difference between the sample pretreatment method established in this paper and the ashing method used in the current standard,and it is helpful for the online tracking determination of trace Cu2+ and Fe3+ in the operating transformer insulating oil.
Key Words:reversed phase switchable hydrophilicity solvent  liquid-liquid microextraction  copper and iron ions  transformer oil  inductively coupled plasma mass spectrometry(ICP-MS)
引用本文:付宇超,杨珍,李吟霜,李海燕.反相可切换亲水性溶剂液-液微萃取/电感耦合等离子体质谱法测定变压器油中铜和铁离子含量[J].分析测试学报,2022,41(7):1078-1082.
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