高钛冷固球团矿中全铁和TiO_2联合测定方法的研究

目的确定高钛冷固球团矿(以下简称钛球)中全铁和TiO2联合测定的简便可靠方法。方法采用无水Na2CO3和H3BO3(2+1)混合熔剂一次熔解样品,提取定容后分别移取一定量的试液。全铁采用K2Cr2O7溶液滴定法测定,TiO2采用二安替比林甲烷分光光度法测定。结果通过多种方式对比实验,27组测定结果显示,全铁测定结果绝对误差在-0.30%~0.18%之间,相对偏差在-0.59%~0.35%之间;TiO2测定结果绝对误差在-0.26%~0.40%之间,相对偏差在-2.03%~3.14%之间,表明实验结果准确可靠,完全可以代替传统分析方法;并给出了TiO2含量与吸光度(A)之间的线性关系式:A=1 307.35mTiO2-5.86或者mTiO2=7.649 1×10-4 A+0.004 5,此方程式的线性相关系数R2=0.999 9。结论本法通过一次熔样,可实现全铁和TiO2的联合测定,不仅节省大约2/3单位样品的分析时间,提高了工作效率,而且节约了大量试剂的使用量,降低了分析成本,过程分析准确可靠,可控性强,能够满足企业生产之需要。

Study on combined determination method of total iron and TiO2 in high titanium cold-bound pellets

Objective--To define simple and reliable combined determination methods of total iron and titanium dioxide（TiO2） in the high Ti cold-bound pellets （hereinafter referred to as the titanium ball）. Methods--The disposable dissolution sample was dissolved with the mixed solvent of anhydrous sodium carbonate and boric acid （2q-l）, then a certain amount of test solution was removed after be- ing extracted and diluted. Total iron was determined with potassium dichromate titration method and titanium dioxide with diantipyrylmethane spectrophotometric method. Results--By comparison test in various ways, the determination results of 27 groups showed the absolute errors of the determination results of total iron were--0.30-0.18%, and that of TiO2 was --0. 26-0. 40%. The compari- son test and paired t-test indicated that the experimental results were accurate and reliable and the method adopted herein could completely replace the original analysis method. In addition, the linear relational expression between the content of TiO2 and absorbance （A） （A= 1 307. 35rnTiO2 --5. 86 or mTiO2 = 7. 649 1 X 10-4A q-0. 004 5） was given, the linear correlation coefficient of the expression R2 is 0. 999 9. Conclusion--This method can simultaneously determine total iron and titanium dioxide with disposable dissolution samples, so it can save analysis time and reagent dosage, improve work efficien-cy and reduce the cost, the process analysis is not only accurate and reliable but also has good control- lability, so the method can meet the needs of enterprise production.