高分辨电感耦合等离子体质谱(HR-ICP-MS)测定毫克级柴(煤)油中硫含量的方法研究

Determination of Total Sulfur in Milligram Diesel Fuel and Kerosene Samples by High Resolution ICP-MS

本文建立了一种适合毫克级柴 (煤 )油样品中硫含量的高分辨电感耦合等离子体质谱 (HR -ICR -MS)分析方法。本法使用专门设计的HNO3 -HC1-H2 O2 密封消解溶样体系 ,能使柴 (煤 )油样品中的硫化合物完全转化成水相中的硫酸根离子 ,使用HR -ICP -MS技术能够克服氧分子离子的质谱干扰 ,从而实现毫克级柴 (煤 )油样品中硫含量的测定。本方法对水溶液的检出限为 0 .0 19μg/mL ,回收率达到 97%～ 10 3% ,取样量为 0 .0 10～ 0 .10 0 0g时的分析范围为0 0 0 0 0 6 %～ 1% ,测量的相对不确定度不盱 7%。

A method was presented for the determination of total sulfur in milligram diesel fuel and kerosene samples by HNO 3-HCL-H 2O 2 sealed digestion system using high-resolution Inductively Coupled Plasma-Mass Spectrometry.In the special designed sealed digestion vessel,sulfur from diesel and kerosene samples could completely be transformed to sulfate in aqueous solution.Furthermore,the sulfate in aqueous solution was able to be measured by HR-ICP-MS at medium resolution 3000 to separate the interferences from 16 O 16 O + and 14 N 18 O +ions.As a result,the method has a recovery of 97%～103%,range of 0.00006%～1% for 30 to 100 mg sample,uncertainty of 7% less.