薄层色谱与红外光谱联用中新型固定相氟化钡的制备及应用  

Preparation and Application of Barium Fluoride Particles as Stationary Phase for TLC-FTIR Analysis

作　　者：刘微[1,2] 吴海军[2,3] 王修鹏[4] 祝青[5] 康廷国[1] 贺安琪[2] 翁诗甫[2] 杨展澜[2] 夏锦明[6] 徐怡庄[2] 吴瑾光[2] 

机构地区：[1]辽宁中医药大学药学院,大连116600 [2]北京大学化学与分子工程学院,稀土材料化学与应用国家重点实验室,北京100871 [3]内蒙古民族大学蒙医药学院,通辽028000 [4]山东省临沂市技术监督信息所,临沂276004 [5]北京大学工学院工程技术研究所,北京100871 [6]沈阳度太生物制药研究中心,沈阳110031

出　　处：《高等学校化学学报》2013年第6期1347-1352,共6页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金(批准号:50973003);国家“八六三”计划项目(批准号:2010AA03A406);科技部平台项目(批准号:2005DKA32800);北京市专利基金和北京大学先进技术研究院培育项目资助

摘　　要：采用氟化钠与氯化钡反应制备了满足薄层色谱-红外光谱联用要求的氟化钡颗粒.该方法虽然可以避免产生干扰红外光谱分析的碳酸钡杂质,但氟化钡的产率偏低.通过电感耦合等离子体(ICP)和X射线粉末衍射(XRD)分析证实,氟化钠与氯化钡反应同时会生成氟氯化钡,在沉淀洗涤过程中,氟氯化钡的溶解会造成钡离子的流失和氟化钡产率的下降.本文采用氟化钠溶液洗涤沉淀制备氟化钡,可使氟氯化钡转化为氟化钡,使氟化钡产率得到明显提高.扫描电子显微镜和纳米粒度仪分析结果表明,制备的氟化钡颗粒的粒径约为100 nm.利用沉降挥发法制备了以氟化钡颗粒为固定相的薄层色谱板,实验结果表明用该薄层色谱板可成功分离罗丹明B和孔雀石绿,分离所得样品可被红外光谱检测且不受固定相的干扰.In this study,we modified the preparation of barium fluoride fine particles by a reaction between sodium fluoride and barium chloride.However,the experimental result turned out that the yield of BaF2 is rather low.By inductive coupled plasma（ICP） and X-ray diffraction（XRD） analysis,we found barium fluorochloride was produced with barium fluoride in the reaction.During the washing of precipitates,barium fluorochloride was dissolved in water with low concentration of Cl-and F-,leading to the lost of barium ions and low yield of BaF2.To solve the problem,aqueous solution of NaF was used to wash the product of the reaction between barium chloride and sodium fluoride.Both XRD and ICP results confirmed that barium fluorochloride converted into barium fluoride.Hence,the yield of barium fluoride increases significantly.The average diameter of the BaF2 particles is around 100 nm by SEM and nanometer particle size analyzer.We used settlement volatilization method to prepare TLC plate without using polymeric adhesive.TLC experiments prove that the TLC plate using BaF2 fine particles as stationary phase can separate the mixture of Rhodamine B and Malachite green.FTIR analysis confirms that the FTIR spectra of the separated Rhodamine B and Malachite green spots are in good agreement with the FTIR spectra of pure Rhodamine B and Malachite green.

关 键 词：氟化钡 固定相 薄层色谱 红外光谱 联用 

分 类 号：O657[理学—分析化学] O614.23[理学—化学]