高频燃烧红外吸收法测定氟化镨钕-氟化锂电解质中碳  

Determination of carbon in praseodymium neodymium fluoridelithium fluoride electrolyte by high-frequency combustion infrared absorption method

作　　者：郝慧聪 杨帆 张秀艳[1,2] 范小龙[1,2] 任旭东 HAO Huicong;YANG Fan;ZHANG Xiuyan;FAN Xiaolong;REN Xudong(Baotou Research Institute of Rare Earths,State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou O14030,China;Ruike National Engineering Research Center of Rare Earths Metallurgy and Function Materials,Baotou 014030,China)

机构地区：[1]包头稀土研究院,白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]瑞科稀土冶金及功能材料国家工程研究中心,内蒙古包头014030

出　　处：《冶金分析》2024年第8期53-58,共6页Metallurgical Analysis

摘　　要：准确测定和控制氟化镨钕-氟化锂电解质中的碳含量,对监测镨钕合金中生产工艺流程及最终产品的质量具有重要意义。控制分析时间为35 s,称样量为0.20~0.30 g,用钢铁标准样品进行单点校正曲线,选择钨、锡、铁为助熔剂,建立了高频燃烧红外吸收法测定氟化镨钕-氟化锂电解质中碳含量的测定方法。以钨质量、锡质量、铁质量,助熔剂和试样的加入顺序为考察因素,设计了4因素3水平的正交试验,确定助熔剂和试样的加入顺序为纯铁+试样+钨、锡,助熔剂用量为0.60 g纯铁、1.20 g钨、0.40 g锡。方法检出限为0.000 255%(质量分数,下同),定量限为0.000 85%。按照实验方法对3个不同批次的氟化镨钕-氟化锂电解质试样进行测定,11次测定结果的相对标准偏差(RSD)为2.8%~3.3%。使用格拉布斯异常值判断法进行异常值判别,3个试样测定结果的格拉布斯G_(Max)分别为1.463、1.503、1.335,G_(Min)分别为1.704、1.639、1.669,均小于格拉布斯临界值G_((0.05,11))=2.234(显著水平α=0.05),表明测定结果均不存在异常值。在这3个试样中加入钢铁标准样品进行加标回收试验,回收率介于96%~105%之间。Accurate determination and control of carbon content in praseodymium neodymium fluoride-lithi-um fluoride electrolytes is of great significance for the monitoring of praseodymium neodymium alloy pro-duction process and the quality of finished products.A method for the determination of carbon content in praseodymium neodymium fluoride-lithium fluoride electrolyte by high-frequency combustion infrared ab-sorption was established.The analytical time was controlled at 35 s,and the sampling mass was 0.20-0.30 g.The standard sample of steel was used for the preparation of single-point calibration curve.Tungsten,tin,and iron were selected as the flux.An orthogonal experiment with four factors and three levels was designed,and the investigation factors includes the mass of tungsten,the mass of tin,the mass of iron,and the adding sequence of flux and sample.Through the experiments,the adding sequence of flux and sample was pure iron+sample+tungsten and tin.The dosage of flux was 0.60 g of iron,1.20 g of tungsten,and 0.40 g of tin.The limit of detection of method was 0.000255%(mass fraction,the same below),and the limit of quantification was 0.00085%.Three different batches of praseodymium neodymium fluoride-lithium fluoride electrolyte samples were measured according to the experimental method,and the relative standard deviations(RSD,n=11)of determination results were between 2.8% and 3.3%.The Grubbs outlier judgment method was used to identify the outliers.The Grubbs G_(Max) of measurement results of three batches was 1.463,1.503,and 1.335,and the G_(Min) was 1.704,1.639,and 1.669,respectively.They were all less than the Grubbs critical value G(0.05.11)=2.234(significant level α=0.05),indicating that there were no abnormal values in the measurement results.The standard steel sample was used into the sample for spiked recovery tests,and the recoveries were between 96% and 105%.

关 键 词：高频燃烧红外吸收法 氟化镨钕-氟化锂电解质 助熔剂 钨 锡 铁 碳 

分 类 号：O659.2[理学—分析化学] TF031[理学—化学]