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大量锆存在对稀土元素的测定有干扰。因此含锆矿石中分离大量锆是准确测定稀土元素总量的关键。鉴于锆在硫酸介质中分配系数很低,据此,我们采用国产732阳离子交换树脂对交换介质、洗脱条件、稀土元素的分离、回收及矿石分析等进行了试验,从而拟订了含锆矿石中稀土元素总量的分析方法。试验结果表明:锆量少于1毫克时,可用100毫升硫酸(2+98)洗脱,然后用100毫升1.2M盐酸洗脱钛、铁、铝等干扰元素;用200毫升3—4M盐酸洗脱稀土元素。锆含量高时,可在2—4％(V/V)硫酸介质中进行交换,以120毫升6％硫酸进行洗脱,能有效地分离高达100毫克锆及常量的钛、铁、铝及钍等干扰元素。再用80毫升1.2M盐酸洗脱残留的铝。最后以200毫升3M或4M盐酸洗脱稀土元素,然后分取适量试液用偶氮胂Ⅲ光度法或其它方法进行测定。试验结果表明,按上述条件对相应元素进行洗脱,洗脱曲线形状较好。稀土元素从500微克至200毫克能定量回收。方法的精密度符合要求。
The presence of a large amount of zirconium interfered with the determination of rare earth elements. Therefore, zirconium ore containing a large amount of zirconium is the key to accurately determine the total amount of rare earth elements. In view of the very low partition coefficient of zirconium in sulfuric acid medium, we tested the exchange medium, elution conditions, the separation and recovery of rare earth elements and ore analysis using domestic 732 cation exchange resin, Analysis of total rare earth elements. The test results show that when the amount of zirconium is less than 1 mg, it can be eluted with 100 ml of sulfuric acid (2 + 98) and then with 100 ml of 1.2M hydrochloric acid to elute the interfering elements such as titanium, iron and aluminum; with 200 ml of 3-4M hydrochloric acid Rare earth elements. High levels of zirconium can be exchanged between 2-4% (V / V) sulfuric acid and eluted with 120 ml of 6% sulfuric acid to effectively separate up to 100 milligrams of zirconium and titanium, iron, aluminum and thorium Interference elements. Remaining aluminum was eluted with 80 ml of 1.2 M hydrochloric acid. Finally, 200 milliliters of 3M or 4M hydrochloric acid elution of rare earth elements, and then the right amount of test solution with arsenazo Ⅲ spectrophotometry or other methods were measured. The experimental results show that according to the above conditions, the corresponding elements are eluted and the shape of the elution curve is good. Rare earth elements from 500 micrograms to 200 milligrams can be quantitative recovery. The precision of the method meets the requirements.