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本文报导磷钒钼和磷钒杂多化合物的合成和元素分析法。对合成磷钒钼杂多酸的传统方法——乙醚萃取法作了改进,合成了传统法未能合成的 H_8PV_5M_(07)O_(40),其中三种杂多酸(n=1～3)的产量和文献值相比分别提高了185.7%、42.9%、483%,并通过元素分析,确证得到了较纯的产品。对磷钒杂多酸盐,在 pH=1～4、原料中磷、钒的摩尔比为1:11.8的条件下,制得了 Na_(12)PV_(13)O_(41)和Na_3PV_(14)O_(42),在酸度更高的条件下,合成了尚未见报导的 Na_6H_3PV_(14)O_(42)。同时,将磷钒钼黄分光光度法应用到杂多化合物体系,分析了磷和钒的含量,确定了它们的组成。
This paper reports the synthesis and elemental analysis of phosphorus, vanadium and phosphorus-vanadium heteropoly compounds. H_8PV_5M_ (07) O_ (40) synthesized by the traditional method was synthesized by the traditional method of ether-heteropolyphosphatadolybdovanadate-ether extraction, in which three kinds of heteropoly acids (n = 1-3) Compared with the literatures, the yields of the products increased by 185.7%, 42.9% and 483% respectively, and the pure products were confirmed by elemental analysis. (12) PV_ (13) O_ (41) and Na_3PV_ (14) were prepared on the phosphovanadate heteropolyacid salt under the condition of pH = 1 ~ 4 and the molar ratio of phosphorus and vanadium in the raw material was 1: 11.8. O_ (42), Na_6H_3PV_ (14) O_ (42) has not been reported yet under the conditions of higher acidity. At the same time, the phosphomoly vanadium molybdenum yellow spectrophotometry was applied to the heteropoly compound system, and the contents of phosphorus and vanadium were analyzed to determine their composition.