电感耦合等离子体原子发射光谱法测定钒铁中硫含量

Determination of sulfur in ferrovanadium by inductively coupled plasma atomic emission spectrometry

采用硝酸(1+2)和盐酸(1+1)的混酸(VHNO3∶VHCl=3∶2)溶解样品,选择S180.731nm或S182.034nm的光谱线作为硫的分析线,建立了电感耦合等离子体原子发射光谱法测定钒铁中硫含量的方法。采用在标准溶液中补加基体溶液绘制校准曲线来消除基体干扰。结果表明,采用S180.731nm(185)作分析线时线性回归方程为I=3.033 9ρ+0.337 8,线性相关系数大于0.999,检出限为0.009 4μg/mL;采用S182.034nm(184)作分析线时线性回归方程为I=2.586 3ρ-0.296 5,线性相关系数也大于0.999,检出限为0.020μg/mL。方法应用于钒铁标样GSBH42004-92和钒铁内控样ET-FT-04中硫的测定,测定值与认定值或红外法测定值一致,相对标准偏差(n=7)分别为5.9%和2.7%。

After the sample was dissolved with nitric acid and hydrochloric acid（VHNO3 ： VHCl=3 ： 2）, sulfur in ferrovanadium was determined by inductively coupled plasma-atomic emission spectrometry with S 180. 731 nm and S 182. 034 nm as analytical line. Calibration curve was made by adding matrix solution in the standard solution to eliminate matrix interference. The results showed that when S 180. 731 nm（185） was used as analytical line, the linear regression equation was I=3. 033 9pq- 0. 337 8 with linear correlation coefficient over 0. 999 and detection limit of 0. 009 4 μg/mL; when S 182.034 nm（184） was used as analytical line, the linear regression equation was I=2. 586 3p--0.296 5 with linear correlation coefficient over 0. 999 and detection limit of 0. 020 μg/mL. Proposed method was applied to determination of sulfur in ferrovanadium certified reference material GSBH42004-92 and internal control sample ET-FT-04. The results were consistent with the certified values or those ob- tained by infrared method. The relative standard deviation （n=7） was 5.9% and 2.7 %, respectively.