地表水中四乙基铅分析方法及样品保存

Method Discussion about Determination and Sample Preserve of Tetraethyl Lead in Surface Water

在文献调研基础上对地表水中四乙基铅的色谱法、光度法和光谱法适用情况，萃取、消解和浓缩等不同前处理方法对分析结果的影响以及样品保存条件进行了验证和研究。结果表明，测定水中四乙基铅的光谱和色谱方法均有其适用的特点，可以满足不同条件的实验室和水样的分析，改进后的双硫腙方法检出限可达到I．5μg／L，精密度15％，回收率88％～110％；ICP—MS法检出限可达0．01μg／L，精密度6％，回收率95％一101％；液液萃取一GC—MS检出限达0．1μg／L，精密度12％，回收率65％～78％；自动顶空一气相色谱法检出限可达0．05μg／L，精密度3％，回收率98％～100％；浓缩较消解和萃取更容易造成四乙基铅的损失；没有保护剂的条件下四乙基铅最好在8h内分析完毕，加入甲醇和NaCl可以使采用顶空分析的样品保存3d。其他不同保护剂的保存效果有待进一步研究。

This paper is ahout the Method study of Tetraethyl Lead in surface water,including chromatography and spectroscopic methodology and double sulphur hydrazone colorimetry. It has been discussed how the difference pretreatment process how to influence the anylsis results, such as extraction, digestion and concentration. The results of studies show that the MLD of the improved double sulphur hydrazone colorimetry is reached 1.5 μg/L, RSD is 15% , the recovery rates can be changed between 88% and 110%. The MLD of ICP-MS is 0.01 μg/L,RSD is 6% , the recovery rates is 95% -101%. The same dates of Liquid- Liquid extraction-GC-MS are the MLD O. 1 Ixg/L,RSD is 12% , the recovery rates is 65% -78%. The Tetraethyl Lead loss in the cours of concentrateion per-trement is easier and much more than extraction or digestion. In 4℃without protecting agent the experiment of Tetraethyl Lead should be finished within 8 hours. With CH2OH and NaC1 in samples it can be keept in 3 days but only in Auto-Inspace-GC method. Much more thoroughly studies should be carry on.