电感耦合等离子体原子发射光谱法测定高纯石墨中9种元素  

Determination of nine elements in high purity graphite by inductively coupled plasma atomic emission spectrometry

作　　者：杨倩倩[1] 何石[1] 胡月[1] 彭霞[1] 李美玲[1] 

机构地区：[1]钢铁研究总院,北京100081

出　　处：《冶金分析》2016年第3期49-53,共5页Metallurgical Analysis

基　　金：国家科技部和国家重大科学仪器设备开发专项基金资助项目(No.2011YQ140147)

摘　　要：高纯石墨作为优异的功能材料被广泛应用于国防和航空航天等产业，其对痕量杂质元素含量的要求也逐年提高，目前所用的测试方法检出限都较高，已不能满足日益增长的测试需求。实验将1g高纯石墨样品置于1100℃马弗炉中灰化至完全；取出冷却，加入3g助熔剂（m（H3B03）：77／（Na2C03）=1：2），再次放入马弗炉中，在11OO℃下加热熔融40min至熔液澄清；取出冷却，使用盐酸（1＋1）溶解盐类。采用A1396．152nm、Ca396．847nlTl、Cr267．716nm、Cu324．754nm、Fe238．204nm、Mg279．553nm、Ni231．604nm、Si251．612nm、Zn213．856nm作为分析线，建立了使用电感耦合等离子体原子发射光谱法（ICP-AES）测定高纯石墨中铝、钙、铬、铜、铁、镁、镍、硅和锌等9种杂质元素的方法。结果表明，铝、钙、铬、铜、铁、镁、镍、硅和锌的质量浓度在O．5O～500μg／mL范围内与发射强度呈线性，校准曲线的线性相关系数均大于O．9995；方法中各元素的检出限为O．O37～O．87μg／g。将方法应用于高纯石墨样品中9种杂质元素的测定，测定结果与电感耦合等离子体质谱法的测定结果相吻合，相对标准偏差（RSD，n=7）均小于6．O％，回收率为93％～1O8％。The high purity graphite is a kind of excellent function materials and it has been widely used in national defense and aerospace industries.The determination requirements of trace impurities content are increasing year by year.At present,the detection limits of current testing methods are relatively high,which could not meet the increasing determination requirements.1g of high purity graphite sample was put into muffle furnace at 1 100 ℃ and completely ashed.After cooling,3g of flux(m(H3BO3)∶m(Na2CO3)=1∶2)was added.Then,the sample was put into muffle furnace again for melting at 1 100℃for 40 min.The cooled salts were dissolved with hydrochloric acid(1+1).Thus,a determination method of nine impurities including aluminum,calcium,chromium,copper,iron,magnesium,nickel,silicon and zinc in high purity graphite was established by inductively coupled plasma atomic emission spectrometry(ICP-AES)with Al 396.152 nm,Ca 396.847 nm,Cr 267.716 nm,Cu 324.754 nm,Fe 238.204 nm,Mg279.553 nm,Ni 231.604 nm,Si 251.612 nm and Zn 213.856 nm as analytical lines.The results showed that the mass concentration of aluminum,calcium,chromium,copper,iron,magnesium,nickel,silicon and zinc in range of 0.50-500μg/mL was linear to the emission intensity.The linear correlation coefficients of calibration curves were all higher than 0.999 5.The detection limits of elements were between0.037μg/g and 0.87μg/g.The proposed method was applied to the determination of nine impurities in high-purity graphite samples.The results were consistent with those obtained by inductively coupled plasma mass spectrometry.The relative standard deviations(RSD,n=7)were less than 6.0%.The recoveries were between 93% and 108%.

关 键 词：灰化 碱熔 电感耦合等离子体原子发射光谱法(ICP-AES) 高纯石墨 杂质元素 

分 类 号：O657.31[理学—分析化学]