摘要
本实验采用氢氟酸溶解样品,滴加硝酸氧化不溶碳化物或氮化物,用饱和硼酸溶液络合氟离子。在酸性介质中,磷酸离子与钼酸铵形成磷钼杂多酸,用正丁醇-三氯甲烷萃取分离,再用氯化亚锡还原成钼蓝并反萃取至水相中,以分光光度法测定铪中磷含量。试验考察了溶解酸用量、显色酸酸度、萃取次数、共存元素干扰等因素对分析结果的影响。最佳分析条件如下:用4mL氢氟酸溶解1g样品,显色时硝酸的加入量为4~8mL,采用两次萃取。此法应用于海绵铪模拟样品磷量的测定,方法的RSD(n=11)均小于5.00%,具有较高的准确性和良好的稳定性。
Samples were dissolved with hydrofluoric acid, insoluble carbides or nitrides was oxidized with nitric acid , fluorine ions were complexed with a saturated boric acid solution, in an acidic medium, phosphoric acid ions and ammonia molybdate formed phosphomolybdenum heteropoly acid, it was separated by n-butane-chloroform and reduced to molybdenum blue with stannous chloride, molybdenum blue was back-extracted to water phase, the phosphorus content was detected by spectrophotometry. The effects of acid amount, color acidity, extraction times, and coexistence elements were studied. The optical analysis conditions were as follows: 4ml fluorine was used to resolve 1gram sample ,4~8ml nitric acid was used for color reaction, the solution was extracted twice. The method was used for the phosphorus content detection in sponge hafnium, the relative deviation of the results was less than 5%, and the results were accurate and stable.
作者
魏东
翟通德
李佗
刘厚勇
WEI Dong;ZHAI Tongde;LI Tuo;LIU Houyong(Xi'an Hantang Analysis and Testing Co., Ltd., Xi'an 710016, China)
出处
《四川有色金属》
2019年第2期63-66,共4页
Sichuan Nonferrous Metals
关键词
萃取
分光光度法
铪
磷
extraction spectrophotomety
hafnium
phosphorus
