ICP-AES法测定红土镍矿中镍、钙、钛、锰、铜、钴、铬、锌与磷的含量

Determination of Ni,Ca,Ti,Mn,Cu,Co,Cr,Zn and P in laterite-nickel ores by inductively coupled plasma-atomic emission spectrometry

建立了ICP-AES法测定红土镍矿中Ni;Ca;Ti;Mn;Cu;Co;Cr;Zn和P含量的方法。样品用HCl、HNO3溶解,加入HF和HClO4,加热至HClO4烟冒尽,用HCl溶解盐类,过滤,采用ICP-AES法同时测定滤液中Ni、Ca、Mn、Cu、Co、Zn、P;残渣经灼烧、挥硅、K2S2O7熔融、HCl浸取,所得溶液与滤液合并,测定溶液中Cr和Ti含量。方法检出限:P为0.022μg/mL,其它元素在0.0032～0.0085μg/mL之间,方法的精密度(n=7)在1.4%～2.9%之间。分析结果与分光光度法、XRF法和AAS法分析结果的相对误差:Ni、Cu、Co、Cr小于5%,Ti和Mn小于10%,Zn小于15%,Ca和P小于19%。

An ICP-AES method was established for the determination of nickel in nickel laterite ore, calcium, titanium, manganese, copper, cobalt, chromium, zinc and phosphorus contents. Samples were dissolved with hydrochloric acid and nitric acid, and then hydrofluoric acid and perchloric acid were added and heated till the smoke disappeared. The salt was dissolved in hydrochloric acid, followed by filtering, calcium, manganese, nickel, copper, cobalt, zinc, phosphorus in filter were simultaneously determined using ICP-AES method ; the residue was processed by burning, volatile silicon, potassium pyrosulfate fusion, hydrochloric acid leaching to obtain the solution, and chromium and titanium contents in the solution were determined. The detection limits of the method were 0.022 g/mL for P and in range of 0. 0032 - 0. 0085 g/mL for other elements. The precisions of the method （ RSD, n = 7 ） were in range of 1. 4% - 2. 9%. Compared with the results of spectrophotometric method, XRF method and AAS method, the relative errors of the results were less than 5% for nickel, copper, cobalt, chromium, less than 10% for manganese and titanium, less than 15% for Zinc and less than 19% for calcium and phosphorus.