石墨炉原子吸收法快速测定聚醚酮酮特种高分子材料中铝离子残留  

Fast Determination of Al Residue in Polyether Ketone Ketone by Graphite Furnace Atomic Absorption Spectrometry

作　　者：梅朋 徐俊俊[3,2] 郭俊芳[1] 段太成[2] 

机构地区：[1]武汉工程大学,武汉430074 [2]中国科学院长春应用化学研究所,电分析化学国家重点实验室,长春130022 [3]燕山大学,秦皇岛066004

出　　处：《分析化学》2014年第11期1702-1705,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.21275138)~~

摘　　要：建立了石墨炉原子吸收光谱(GF-AAS)快速测定聚醚酮酮特种高分子材料催化剂Al3+残留的方法。样品以浓H2SO4磺化后,以四氢呋喃溶解,直接进样,以GF-AAS测定铝含量。对样品处理方法进行了系统研究,结果表明,0.2 g样品以2 mL浓H2SO4在220℃溶解4 min即可获得澄清溶液,并可进一步与四氢呋喃形成稳定溶液或分散液,满足GF-AAS进样分析要求。优化了石墨炉升温程序,在400℃预灰化温度和40 s的总预灰化时间下显著提高了GF-AAS的测定稳定性。方法检出限(3σ)为38.5 ng/g,平行测定精密度RSD(n=6)为2.2%,加入回收率为99%和105%。相比传统高温灼烧法,本方法更简洁、快速,且大大降低了样品处理过程中的玷污风险。A new method was developed for fast determination of Al residue in polyether ketone ketone （ PEKK） special polymer material by graphite furnace atomic absorption spectrometry （ GF-AAS） . Instead of high temperature ashing, sample was dissolved in concentrated sulfuric acid and diluted by tetrahydrofuran, then was directly analyzed by GF-AAS. Systematical investigation was made on sample preparation, it was found that for 0. 2 g of sample weight, a clear sample solution could be obtained by heating at 220 ℃ with 2 mL of concentrated H2 SO4 for 4 min, and the obtained solution was ready for the subsequent mixing with tetrahydrofuran for sample dilution or dispersion before analysis. Redesign of the GF-AAS temperature program was also made, on the basis of the recommended program a pre-ashing step was added, which greatly helped increasing the analytical precision when the temperature was set at 400 ℃ and the total time was set at 40 s. The detection limits （ 3σ） were 38. 5 ng/g, the RSD for six parallel determinations of real samples was 2. 2%, and the recoveries for spiked tests were 99%-105%, respectively. In comparison with the traditional high-temperature ashing technique, the established method was more concise, faster and less exposed to contamination during sample preparation.

关 键 词：聚醚酮酮 铝离子残留 石墨炉原子吸收光谱法 

分 类 号：O657.31[理学—分析化学] O632.4[理学—化学]