洗涤剂中含磷化合物的^(31)P NMR快速检测方法  

Analysis of Phosphorus-containing Compounds in Detergents by ^(31)P Nuclear Magnetic Resonance

作　　者：叶汝汉[1] 陈泳[2] 柳亚玲[1] 朱黎明[2] 李正全[2] 孙一峰[2] 潘文龙[2] 

机构地区：[1]广东工业大学轻工化工学院,广东广州510090 [2]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,广东广州510070

出　　处：《分析测试学报》2011年第6期624-628,共5页Journal of Instrumental Analysis

基　　金：广东省科技计划资助项目(2002C1030601)

摘　　要：收集了常见的31种含磷无机化合物和84种含磷有机化合物,首次建立了含磷化合物的核磁共振谱图库,并以此为依据建立了31P NMR技术快速检测洗涤剂中含磷化合物的方法。对洗衣粉、金属清洗剂和除油剂样品进行31P NMR分析,经与31P谱图库比对,可快速确定含磷化合物的结构。结果表明,10种洗衣粉中仅有1种检出含磷化合物,其成分为三聚磷酸钠、焦磷酸钠及磷酸氢二钠;3种金属清洗剂中的含磷成分均为磷酸;而3种除油剂的含磷成分分别为壬基酚聚氧乙烯醚磷酸酯、三聚磷酸钠和磷酸氢二钠,三聚磷酸钠和磷酸钠,磷酸氢二钾。该法相对简便、准确、快速,适用于其他含磷精细化工产品的分析。31 inorganic phosphorus-containing compounds and 84 organic phosphorus-containing compounds were collected, and the 31p NMR spectra database of phosphorus-containing compounds was established for the first time. A method based on the spectra database was developed for the rapid determination of phosphorus-containing compounds in detergents by 31p NMR. Phosphorus-containing compounds in several kinds of washing powder, metal cleaning agents and deoiling agents were detected by NMR. By comparing the 31p NMR spectra of the tested samples with that of the standard, the structures of phosphorus-containing compounds in detergents were identified. The results showed that, under the presented conditions, three phosphorus-containing compounds e. g. sodium tripolyphosphate, sodium pyrophosphate and disodium hydrogen phosphate were detected in one kind of washing powder. Only one phosphorus-containing component （phosphoric acid） was detected in all three metal cleaning agents. And the phosphorus-containing components of three deoiling agents were detected to be phosphate polyoxyethylene nonylphenol, sodium tripolyphosphate and disodium hydrogen phosphate, as well as sodium tripolyphosphate, sodium phosphate and dipotassium hydrogen phosphate, respectively. The proposed method could also be applied in the analysis of other phosphorus-containing fine chemical products with the advantages of simplicity, accuracy and rapidity.

关 键 词：31P NMR 含磷化合物 洗涤剂 化学位移 

分 类 号：O482.532[理学—固体物理] TS192.26[理学—物理]