摘要
高频红外碳硫仪测定不同矿石种类中的硫含量,测定速度快,稳定性好,但当测定范围宽、样品种类多时,受助熔剂、氧化温度和氧化时间影响较大。本文应用高频红外碳硫分析仪,研究了实验条件对分析结果的影响,通过优化样品称样量、助熔剂添加量和分析时间,建立了矿石样品中质量分数为0.74%~32.0%的硫含量检测方法,分析条件为:分析氧气流速2.8L/min,样品称样量0.0400g,纯铁助熔剂0.50g,纯钨助熔剂2.0g,分析时间45s。通过国家标准物质验证该方法的检出限为0.185%,定量限为0.739%,标准曲线线性相关系数大于0.9995,测定结果的相对标准偏差小于3%(n=11),与标准值的相对误差小于2%,且均小于DZ/T 0130—2006中对矿石样品分析要求的相对误差允许限。采用本方法与传统燃烧碘量法对实际样品进行测定,两种方法测定值的绝对误差小于0.5%,测定结果之间呈极显著线性关系(R^(2)=0.9995),表明两种方法具有良好的一致性。
BACKGROUND:High-frequency infrared carbon and sulfur analyzer can be used to rapidly analyze the sulfur content in different ores with good stability.However,the analysis is greatly affected by the flux type,oxidation temperature and time for various sulfur contents and sample types.OBJECTIVES:To expand the detection range of sulfur and improve the detection efficiency.METHODS:A high-frequency infrared carbon and sulfur analyzer was used to study the influence of experimental conditions on the analysis results.By optimizing the sample weight,the amount of flux,and the analysis time,a method for determination of sulfur with a content of 0.74%to 32.0%in ore samples was established.RESULTS:The optimized conditions were 2.8L/min oxygen flow,45s analysis time,sample weight of 0.0400g,0.50g pure iron and 2.0g pure tungsten as flux.The detection limit of the method verified by national standard material was 0.185%,and the limit of quantification was 0.739%.The linear correlation coefficient of calibration curve was better than 0.9995,the relative standard deviations were less than 3%(n=11)and the relative errors were less than 2%.The relative errors were all less than the allowance limit for the ores analysis of relative error obtained in accordance with DZ/T 0130—2006.The actual samples of the laboratory were determined by this method and the traditional iodine combustion method.The absolute error of the measured values between the two methods was less than 0.5%,with an extremely significant linear relationship(R^(2)=0.9995),indicating good agreement between the two methods.CONCLUSIONS:The method has high precision and low relative error.The detection limit,precision and accuracy of the established method meet the analytical requirements of the ores.
作者
耶曼
李婧
马怡飞
柯艳
李小桂
YE Man;LI Jing;MA Yifei;KE Yan;LI Xiaogui(Xi’an Northwest Geological Institute for Nonferrous Metals Co.,Ltd.,Xi’an 710054,China)
出处
《岩矿测试》
CAS
CSCD
北大核心
2022年第4期680-687,共8页
Rock and Mineral Analysis
基金
国家重点研发计划项目(2021YFC1808800)。
关键词
镍矿石
铅矿石
锌矿石
硫
高频燃烧-红外吸收光谱法
nickel ore
lead ore
zinc ore
sulfur
high frequency combustion-infrared absorption spectrometry
