摘要
建立了高频燃烧红外吸收法测定金属矿产品中硫含量的方法。当样品中硫含量为0.004 6%～3.96%时可以直接测量,当硫含量高于3.96%时采用高纯二氧化硅进行10倍稀释后测定,最终确定了铁矿的称样质量为10～800 mg之间,铜精矿和锌精矿的称样质量均为50 mg。样品中依次加入0.4 g铁和1.5 g钨作为助熔剂。通过分析称样质量、助熔剂的种类和用量等因素确定了最佳分析条件:工作电流为40μA,氧气压力为172.375 kPa,载气压力为482.65 kPa,分析时间为40 s,硫释放时间为50 s。结果表明,此时试料燃烧完全,硫释放曲线平滑。硫的含量在0.009 6～8.0 mg范围内与红外吸收峰面积呈良好的线性关系,线性相关系数为0.999,方法检出限为0.003 19 g。金属矿标准物质测定结果与标准值基本一致,相对误差为–0.018%～0.01%,测定结果的相对标准偏差为0.79%～2.53%(n=6)。该方法操作简单,重现性好,适用于金属矿产中硫含量的准确测定。
A high frequency combustion infrared absorption method for the determination of sulfur content in metallic mineral products was established. When the sulphur content in the sample was 0.004 6%–3.96%, it can be measured directly. When the sulfur content was higher than 3.96%, high purity silicon dioxide was used for 10 times dilution. Finally, the sample mass of iron ore was determined to be 10–800 mg, and the samples of copper concentrate and zinc concentrate were all 50 mg. 0.4 g iron and 1.5 g tungsten were added as flux in the samples. The optimum analytical conditions were determined by analyzing the amount of sample, the type and dosage of flux. The working current was 40 μA, the oxygen pressure was 172.375 kPa, the carrier gas pressure was 482.65 kPa, the analysis time was 40 s, and the sulfur release time was 50 s. The results showed that the combustion of the sample was complete and the sulfur release curve was smooth. The sulfur mass had a good linear relationship with the peak area in the range of 0.009 6–8.0 mg, the linear correlation coefficient was 0.999, and the detection limit was 0.003 19 g. The detection results of metal ore standard material were basically consistent with the certified value, the relative errors were –0.018%–0.01%, and the relative standard deviations of the results were 0.79%–2.53% （n=6）. The method is simple and reproducible, and it is suitable for the accurate determination of sulphur content in metallic mineral products.
作者
王巧玲
张志峰
肖宇
刘利波
宋玥玮
WANG Qiaoling, ZHANG Zhifeng, XIAO Yu, LIU Libo, SONG Yuewei(Erlian Customs, Erlianhot011100, China)
出处
《化学分析计量》
CAS
2018年第4期89-93,共5页
Chemical Analysis And Meterage
关键词
高频燃烧红外吸收法
金属矿产品
硫
high frequency combustion infrared absorption
metallic mineral products
sulfur
