锰硅合金中氮化钛的测定

DETERMINATION OF TITANIUM NITRIDE IN SILICOMANGANESE ALLOY

提出了一种测定锰硅合金中氮化钛的方法。试样用硫酸-氢氟酸分解基体,用氢氟酸-过硫酸铵破坏氮化钛,用二安替比啉甲烷光度法测定分离出的氮化钛中的钛。试验了分解基体及氮化钛的试剂、浓度、温度及时间;讨论了不同分离条件对氮化钛提取率的影响;根据氮化钛和碳化钛在不同试剂中的溶解特性,采用分离基体后,先分解碳化钛,再分解氮化钛的分离方法进行了测定,与所拟方法结果一致。通过测定试样中的总氮量及分离氮化钛后的残渣中氮含量进行计算,证明结果可靠。该方法操作简便,对于氮化钛含量小于0.002%的试样,相对标准偏差RSD小于20%。

This paper puts forward a determination method of titanium nitride in silicomanganese alloy.The sample decomposes matrix by sulfuric acid-hydrofluoric acid and then titanium nitride is destroyed by hydrofluoric acid-ammonium persulfate.Ttitanium in titanium nitride which is separated by diantipyryl methane photometry is determined.Matrix decomposition and the reagent,concentration,temperature and time of titanium nitride are tested,discussing the effect on extraction rate of titanium nitride in different separation conditions.According to characteristics of dissolution of titanium nitride and titanium carbide in the different reagent,after using matrix separation,first decomposing titanium carbide and then titanium nitride,the result measured is same with the plan after determination of separation method.Through calculation of total quantity of nitrogen in sample and the nitrogen content in residua after matrix separation,the result is reliable.This method is easy to operate for the sample containing less than 0.002%titanium nitride,and the relative standard deviation is less than 20%.