波长色散X射线荧光光谱无标分析法检测树脂中的铅  

Determination of Lead in Resin by Wavelength Dispersive X–Ray Fluorescence Spectrometry with Standard–Sample–Free Quantitative Analysis

作　　者：窦怀智[1] 洪华[1] 王红卫[1] 江涛[1] 侯晋[1] 

机构地区：[1]南通出入境检验检疫局,江苏南通226004

出　　处：《化学分析计量》2014年第3期14-17,共4页Chemical Analysis And Meterage

基　　金：江苏出入境检验检疫局科研项目(2012KJ25)

摘　　要：建立波长色散X射线荧光光谱检测树脂中重金属元素的无标样分析方法。热塑性塑料在200℃热压成样片;热固性塑料取平面直接测量;涂料研磨成粉末后用硼酸镶边、衬底,经过压样机20 t压力30 s压制成样片。所有样品在真空模式下,以激发电流为50 mA,激发电压为60 kV,分光晶体为LiF(200),准直器为0.23°,测量谱线为Pb Lβ1,峰位(2θ)为28.258的仪器工作条件下测定树脂中铅的含量,通过康普顿比率判断结果的可信度。测定值与标准方法检测值相比,偏差小于10%,测定结果的相对标准偏差小于1%(n=6)。结果表明,波长色散荧光光谱无标分析方法可以快速准确地分析树脂样品中的铅含量。Determination of heavy metals in resin by wavelength dispersive X-Ray fluorescence spectrometry with standard-sample-free quantitative analysis was established. Thermoplastics was pressed into pellets at 200℃. Thermosetting plastics was detected directly. Paints were grinded into powder and pressed into pellets by 20 t power for 30 s with boric acid as a bottom. The condition of equipment was set vacuum, inspire current of 50 mA, inspire voltage of 60 kV, LiF（200） for beam splitter, collimator of 0.23°, spectral line of Pb Lβ1 and peak（2θ） at 28.258. The results determined by standard-sample-free quantitative analysis were in accordance with the results detected by standard method within deviation of 10%. The relative standard deviation of determination results was less than 1%（n=6）. The Compton Ratio was used to judge the accuracy of results. The study confirmed the content of lead in resin could be determined quickly and accurately by wavelength dispersive X-Ray fluorescence spectrometry with standard-sample-free quantitative analysis.

关 键 词：X射线荧光光谱 树脂 铅 

分 类 号：O657.3[理学—分析化学]