高频燃烧红外吸收法测定二硼化钛中硫

doi:10.13228/j.boyuan.issn1000-7571.012115

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摘要硫的存在会降低二硼化钛的硬度,因此准确测定二硼化钛中硫的含量显得尤为必要。称取(0.300±0.001) g样品于预先铺有1.50 g钨锡助熔剂的坩埚中,再加入0.50 g纯铁助熔剂,设定分析功率为1.98 kW,建立了高频燃烧红外吸收法测定二硼化钛中硫含量的分析方法。结果表明:校准曲线线性相关系数为0.999 5,方法检出限为0.000 9%,定量限为0.003%。按照实验方法对3个不同硫含量的二硼化钛样品进行测定,并分别加入不同含量的硫酸钾基准试剂进行加标回收试验,测定结果的相对标准偏差(RSD,n=8)为0.9%～1.5%,加标回收率在96%～104%之间。根据二硼化钛成分配比,称取一定量的高纯硼粉和钛铁标准样品混合配制二硼化钛模拟样品,按照实验方法进行测定,测定值与理论值基本吻合。

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	张高庆
	王录锋

关键词 ：二硼化钛, 硫, 高频燃烧红外吸收法, 钨锡, 纯铁

Abstract：The presence of sulfur will decrease the hardness of titanium diboride, so it is particularly necessary to accurately determine the content of sulfur in titanium diboride. (0.300±0.001) g of sample was transferred into a crucible containing 1.50 g of tungsten-tin flux. Then 0.50 g of pure iron flux was added. The analytical power was set at 1.98 kW. The analysis method for the determination of sulfur in titanium diboride by high frequency combustion infrared absorption was established. The results showed that the linear correlation coefficient of calibration curve was 0.999 5. The limit of detection was 0.000 9%, and the limit of quantification was 0.003%. Three titanium diboride samples with different sulfur contents were determined according to the experimental method. Various contents of potassium sulphate standard reagent were added for the recovery tests.The relative standard deviations(RSD, n=8) of determination results were between 0.9% and 1.5%, and the recoveries were between 96% and 104%. Certain amounts of high purity boron powder and ferrotitanium certified reference materials were used to prepare titanium diboride simulated samples according to the composition of titanium diboride.The synthetic samples were determined according to the experimental method, and the found results were basically consistent with the theoretical values.

Key words： titanium diboride sulfur high frequency combustion infrared absorption method tungsten-tin pure iron

收稿日期: 2023-02-09

ZTFLH:	O657.33
	TF125.4

基金资助:四川省科技厅项目(2022NSFSC0307);攀枝花学院校级项目(035200137,035000742,025501953)

作者简介: 张高庆(1991—),男,讲师,博士,主要研究方向为钒钛产品检测技术的开发;E-mail:zhanggaoqing111@163.com

引用本文:

张高庆, 王录锋. 高频燃烧红外吸收法测定二硼化钛中硫[J]. 冶金分析, 2023, 43(10): 41-46. ZHANG Gaoqing, WANG Lufeng. Determination of sulfur in titanium diboride by high frequency combustion infrared absorption method. , 2023, 43(10): 41-46.

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