材料期刊网

矿产品种类多样,硫含量范围较广.以硫酸钾建立校准曲线,建立了高频感应燃烧红外吸收法测定矿产品中硫含量的检测方法.确定的最佳实验条件如下:硫质量分数小于10%时,选择称样量为0.1 g;硫质量分数为10%~20%时,选择称样量为0.05 g;硫质量分数为20%~40%时,选择称样量为0.025 g;硫质量分数在40%~55%时,采用高纯二氧化硅粉将样品稀释约8倍后,选择称样量为0.1 g,再测定.试样加入方式为:先将试样放入到预先加有0.2 g锡粒的瓷坩埚内,再覆盖0.5 g纯铁和1.6 g钨粒.结果表明,校准曲线的线性相关系数大于0.99,硫质量在0.004 8~11.0 mg之间与吸收峰面积呈良好的线性关系.对于硫质量分数低于0.05%的样品,结果计算时要考虑扣除试剂空白值的影响,而对于硫质量分数高于0.05%的样品,试剂空白值(包括使用高纯二氧化硅粉时)可忽略不计.将实验方法应用于硫质量分数在0.01%~53%之间不同含量水平矿产品标准样品的分析,测得结果与认定值基本一致,相对标准偏差(RSD,n=5)均小于2.6%,加标回收率在97%~120%之间.

There are various kinds of mineral products, meanwhile, the range of sulfur content is wide.The calibration curve was prepared with potassium sulfate.The determination method of sulfur content in mineral products by high frequency combustion infrared absorption was established.The optimal experimental conditions were obtained as below: the sample mass was 0.1 g when the mass fraction of sulfur was less than 10%;the sample mass was 0.05 g when the mass fraction of sulfur was in range of 10%-20%;the sample mass was 0.025 g when the mass fraction of sulfur was in range of 20%-40%;when the sulfur content in sample was in range of 40%-55%, the sample was diluted by about 8 times using high-purity silicon dioxide powder, and then the sample mass was 0.1 g for determination.The sample addition was described as follows: the sample was transferred into porcelain crucible containing 0.2 g of tin particles followed by covering with 0.5 g of pure iron and 1.6 g of tungsten particles.The results indicated that the linear correlation coefficient of calibration curve was higher than 0.99.The mass of sulfur in range of 0.004 8-11.0 mg showed good linearity to the absorption peak area.For the sample with sulfur content lower than 0.05%, the influence of reagent blank should be deducted during calculation.For the sample with sulfur content higher than 0.05%, the reagent blank (including the condition using high-purity silicon dioxide powder) could be ignored.The proposed method was applied to the analysis of standard mineral samples with different sulfur contents in range of 0.01%-53%.The found results were basically consistent with the certified values.The relative standard deviations (RSD, n=5)were less than 2.6%, and the recoveries were between 97% and 120%.