氧弹燃烧-ICP-OES用于柴油标准物质中硫含量的定值

本文是柴油系列标准物质研究课题中的子课题,研究了用氧弹燃烧-电感耦合等离子发射光谱法对柴油中硫系列标准物质的定值。通过实验条件的最佳化,包括氧弹燃烧消解样品的影响因素、仪器分析的最佳条件等,利用新型的电感耦合等离子发射光谱仪器(SPECTRO CIROS)真空紫外谱线灵敏高,重现性好的优点,测量两个水平的硫标准物质,使用内标元素Y和进行基体匹配达到消除基体影响而提高测量准确度的目的。该方法展伸不确定度优于2％,测定的结果与其它的不同方法测定的结果一致。

Determination of Sulfur in Diesel Oil Certified Reference Materials by Oxygen-bomb-combustion ICP-OES

This paper describes the CRM (certified reference materials)-sulfur in diesel oil determination by ICP-OES after oxygen bomb combustion. The diesel oil is ignition by electrical circle then combusted in the bomb full of oxygen. Sulfur is translated into sulfur trioxide, which is absorbed by sodium hydroxide solution quantity. The latest ICP-OES instrument has perfectly sensitivity on vacuum UV spectrum, which has wide wavelength spectrum from 120 to 766 nm, with such ICP-OES instrument it is possible to analyze non-metal elements such as Br, Cl, S etc. after instrument optimized and by using inner standard material Y, we improve the repeatability, and long time stability. The extend uncertainty is less than 2% , and the last results of the determination is consistent with other methods (ICP-MS, IC). ICP-OES analysis method is rapid and widely used, but for non-metal element analysis ICP-OES is rarely used, the latest ICP-OES can analyze many non-metal elements as halogen and sulfur for its outing VUV spectrum analysis capacity. For such non-metal element analysis application, this paper gives the optimization parameter and key conditions.