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中国无机分析化学:2011,1(4):64-67
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电感耦合等离子体质谱法(ICP-MS)测定油品中铁、铜、铅、锡、砷、银、铬、镍、钒
(攀钢集团研究院有限公司,成都 611731)
Determination of Iron, Copper, Lead, Tin, Arsenic, Silver, Chromium, Nickel and Vanadium in Oil by Inductively Coupled Plasma Mass Spectrometry
(Panzhihua Iron and Steel Group Research Institute Co., Ltd , Chengdu, Sichuan 611731,China)
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投稿时间:2011-08-15    修订日期:2011-10-11
中文摘要: 以电感耦合等离子体质谱法(ICP-MS)测定油品中痕量元素铁、铜、铅、锡、砷、银、铬、镍、钒。油品于铂金坩埚中,在马弗炉内进行亚沸加热,首先蒸发除去有机物质直至仅剩余无机物残渣,然后在500 ℃灼烧灰化残渣,再加入硝酸、过氧化氢在电热板上加热浸取消解反应至完全,并煮沸分解过氧化氢,彻底消除了有机物对质谱测定的影响,试液组成简单,基体效应小,无需内标校正等技术措施,方法以纯溶液校准曲线直接进行测定。优选了消解试剂和用量、分析同位素、仪器工作条件等用以消除质谱干扰和空白本底的影响,测定高压变压器用绝缘油品中超痕量杂质元素的结果表明: 回收率为91%~110%,RSD <3%,检测限为0.0059~0.0099 μg/L,背景等效浓度为0.0003~0.0012 μg/L。
中文关键词: ICP-MS  油品分析                  
Abstract:Trace elements iron, copper, lead, tin, arsenic, silver, chromium, nickel and vanadium in oil sample were determined by inductively coupled plasma mass spectrometry (ICP-MS). The oil sample in the crucible was sub-boiling distilled in a muffle furnace until organic materials completely were evaporated. At 500 ℃ the residue was burned to form ashes. The ashes were soaked in the mixture of nitric acid and hydrogen peroxide, and dissolution was completed on heating plates. The sample solution was heated to boiling point in order to decompose hydrogen peroxide. Above sample treatment completely eliminated the interference of organic matter on mass spectrometry measurement. Additionally, after the sample treatment composition of the testing solution became simple and the matrix effects were reduced. Internal standard correction was not necessary but instead, the sample could be determined directly by the calibration curve of a pure solution. Optimization of the type and amount of digestion reagents, isotope usage and working conditions of equipment were completed in order to eliminate spectral interferences and blank background effect. The super trace impurities in high-voltage transformer insulating oil were determined and the results showed that: the recovery: 91% ~110 %, relative standard deviation(RSD) <3%, detection limit: 0.0059~0.0099 μg/L, BEC: 0.0003~0.0012μg/L.
keywords: ICP-MS  oil analysis  Fe  Cu  Pb  Sn  As  Ag  Cr  Ni  V
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成 勇.电感耦合等离子体质谱法(ICP-MS)测定油品中铁、铜、铅、锡、砷、银、铬、镍、钒[J].中国无机分析化学,2011,1(4):64-67.
CHENG Yong.Determination of Iron, Copper, Lead, Tin, Arsenic, Silver, Chromium, Nickel and Vanadium in Oil by Inductively Coupled Plasma Mass Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(4):64-67.

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