微波消解ICP法测定硅铁中钛元素的含量

DETERMINATION OF TITANIUM CONTENT IN FERROSILICON BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY AFTER MICROWAVE DIGESTION

以微波消解的方式溶解硅铁及氮化硅铁样品,并采用电感耦合等离子体光谱仪进行微量钛元素含量的测定,研究溶解参数、酸试剂选择、元素波长对硅铁及氮化硅铁中微量钛元素含量测定的影响。结果表明,使用盐酸-氢氟酸以微波消解的方式溶解硅铁及氮化硅铁样品,通过基体匹配配制系列标准校正溶液,钛元素质量分数范围为0.0002%~0.1%、0.0001%~0.5%,线性相关系数均大于0.999;钛的检出限≤0.0002%,结果相对标准偏差(RSD,n=6)<5%,加标回收率为97.8%~105%,结果满足预期要求。

The samples of ferrosilicon and ferrosilicon nitride were dissolved by microwave digestion,and the content of trace titanium was determined by inductively coupled plasma spectrometer.The effects of dissolution parameters,acid reagent selection and element wavelength on the determination of trace titanium in ferrosilicon and ferrosilicon nitride were studied.The results showed that the samples of ferrosilicon and ferrosilicon nitride were dissolved by hydrochloric acid-fluorhydric acid through microwave digestion,and a series of standard calibration solutions were prepared by matrix matching,the mass fraction of titanium was in the range of 0.0002%~0.1%,0.0001%~0.5%,and the linear correlation coefficients was greater than 0.999;the detection limit of titanium was≤0.0002%,the relative standard deviation(RSD,n=6)was<5%,and the recovery was 97.8%~105%.The results meet the expected requirements.