CaO-SiO_2-P_2O_5-H_2O系统材料中磷的分光光度法测定  

Spectrophotometric Determination of Phosphor in CaO SiO 2 P 2O 5 H 2O System

作　　者：陈悦[1] 祝孝丰[1] 杨南如[1] 

机构地区：[1]南京化工大学材料科学与工程系

出　　处：《硅酸盐通报》1998年第1期50-53,共4页Bulletin of the Chinese Ceramic Society

基　　金：国家自然科学基金

摘　　要：将采用溶胶—凝胶法合成的ＣａＯ－ＳｉＯ２－Ｐ２Ｏ５－Ｈ２Ｏ系统材料在５～１０℃、１＋１的ＨＮＯ３介质中分解。于１．０ｍｏｌ／Ｌ的ＨＮＯ３介质中，正磷酸根和钼酸铵及钒酸铵形成Ｐ∶Ｍｏ∶Ｖ＝１∶１∶１１的黄色三元杂多酸。在４２０ｎｍ波长处测量三元杂多酸的吸光度，求出未知试样中ＰＯ４３－的含量。聚磷酸根的含量则在１ｍｏｌ／Ｌ的ＨＮＯ３介质中于沸水浴中水解后同法测总ＰＯ４３－，用差减法求出。工作曲线的线性范围为０～５０μｇ／ｍｌ（ＰＯ４３－）。十倍于ＰＯ４３－量的ＳｉＯ４４－离子对本方法不产生干扰。方法准确度较高，Ｐ２Ｏ７４－的加料回收率为９４％～１０４％。分别测试了合成试样中水化前后磷的浓度，与３１Ｐ－ＮＭＲ测试结果相吻合。Samples of CaO SiO 2 P 2O 5 system were decomposed in (1+1) nitric acid at 5～10℃. The yellow heteropoly acid of P∶Mo∶V=1∶1∶11 was formed from the reaction of phosphate with (NH 4) 6Mo 6O 24 and NH 4VO 3. Absorbance of hetropoly acid at the wave length of 420nm was measured. The content of phosphate anion in unknown samples was obtained by working curve method. The total phosphate hydrolysed from polyphosphate in 1.0mol/L nitric acid at 100℃ was measured with the same method, so the content of phosphate could be achieved by subtraction method. The linear range of working curve was 0～50μg/ml (PO 4 3- ). 4- anions of ten time content of PO 4 3- didnt cause disturbance in this method. This method has higher accuracy. The feed recovery for P 2O 7 4- was 94%～104%, which has met the analysis requirement.

关 键 词：测定 分光光度法 分光光度法 磷酸根 氧化物 

分 类 号：O657.3[理学—分析化学]