表面处理剂中含氟无机化合物^(19)F NMR检测方法  

Analysis of inorganic fluorine-containing compounds in surface treating agents by ^(19)F NMR

作　　者：仇镇武[1] 柳亚玲[1] 叶汝汉[1] 李正全[1] 陈泳[1] 朱黎明[1] 潘文龙[1] 

机构地区：[1]中国广州分析测试中心,广东省化学危害应急检测技术重点实验室,广州510070

出　　处：《分析试验室》2013年第12期70-73,共4页Chinese Journal of Analysis Laboratory

基　　金：广东省科技计划资助项目(2006B36302006)资助

摘　　要：根据19F NMR测试干扰因素少,谱图信息表征能力强的特点,以及NMR样品预处理方法相对简单的优点,建立了一种表面处理剂中含氟无机化合物的快速检测方法。首先,获取了27种常见含氟无机化合物的‘标准’19F NMR谱图,并根据含氟无机化合物的类型对谱学特征进行了分析和归纳;而后,对3种不同类型的表面处理剂实施了19F NMR测试,根据上述谱学特征分析的结果对样品中含氟无机化合物进行了甄别。结果表明,10种口腔护理用品中有9种检出含有氟化钠、单氟磷酸钠或三氟乙酸钠等含氟无机化合物;3种清洗剂中分别含有氢氟酸、氟硅酸或氟钛酸;而两种电镀添加剂中各含有两种含氟无机化合物,分别为氟硅酸钾/氟硅酸钠和氟锆酸/氟化钠。19F NMR分析方法同样适用于其他含氟无机化合物精细化工产品的分析。The19F NMR test is special for analyzing inorganic fluorine-containing compounds in surface treating agents because of some advantages such as the less interference, the powerful characterization capability of spectral information and the simple pretreatment method of NMR samples. First, 27 standard19F NMR spectra of inorganic fluorine-containing compounds were collected. The characteristics of 19F NMR spectra of various inorganic fluorine-containing compounds were carried on the summary analysis systematically. After that, three kinds of surface treating agents were detected by^gF NMR. On the basis of 19F NMR spectroscopic property, the inorganic fluorine-containing compounds were analyzed detailedly in samples. The results showed that, nine out of ten oral care products were detected to contain inorganic fluorine-containing compounds. The inorganic fluorine-containing compounds were sodium fluoride, sodium monofluorophosphate or sodium trifluoroaeetate, and so on. Three cleaning agents were detected to contain hydrofluoric acid, fluosilicic acid, hexafluorotitanic acid, respectively. And the inorganic fluorine-containing compounds of two plating additives one was detected to contain sodium fluorosilicate and potassium fluorosilicate, the other was detected to contain hexafluorozirconic acid and sodium fluoride. The proposed method could also be applied to the analysis of other inorganic fluorine- containing fine chemicals with the advantages of simplicity, accuracy and rapidity.

关 键 词：19^F NMR 含氟无机化合物 表面处理剂 化学位移 

分 类 号：O657.3[理学—分析化学]