摘要
建立了辉光放电质谱（GD-MS）法测定镍锌铁氧体中22种杂质元素（Li,Be,Na,Mg,Si,P,K,Ca,Ti V,Cr,Mn,Co,Ga,Sr,Mo,Ag,Cd,Sn,Sb,W,Pb）的分析方法。以铜粉为导电材质,与镍锌铁氧体粉末混合均匀后压片,考察了样品的制备条件以及辉光放电电流、放电电压、放电气体流量以及预溅射时间等放电参数对分析信号灵敏度和稳定性的影响,通过同位素的选择、质谱中分辨率模式和高分辨率模式的应用消除了质谱干扰,将Fe,Ni,Zn,O和Cu,5种元素的总信号作归一化处理,利用差减法计算获得镍锌铁氧体中杂质元素的含量。研究结果表明,22种待测元素的检出限在0.001~0.29μg/g之间,相对标准偏差为3.5%~18.6%,样品测定结果与采用ICP-MS法分析的分析结果基本一致,表明本方法具有较好的准确度和精密度。
A direct current glow discharge mass spectrometry （GD-MS） for the determination of Li, Be, Na, Mg, Si, P, K, Ca, Ti, V, Cr, Mn, Co, Ga, St, Mo, Ag, Cd, Sn, Sb, W and Pb in nickel-zinc ferrites was developed. Copper powder as the conductive medium was evenly mixed with nickel-zinc ferrites powder for tableting, and then the impurity elements in nickel-zinc ferrites were determined by GD-MS. The influence of sample preparation and the glow discharge conditions including discharge current, discharge voltage, discharge gas flow rate and pre-sputter time on discharge stability and analysis sensitivity were investigated. The mass spectrometry interferences of analytes were investigated, as well as appropriate isotopes were selected. Most of the mass spectrometry interferences were avoided by measuring in medium resolution mode and high resolution mode. Total signal of Fe, Ni, Zn, O and Cu normalization was adopted, and the impurity elements in nickel- zinc ferrites were calculate in subtraction. The results showed that the detection limits for the investigated elements were in the range of 0.001-0.29 μg/g, the relative standard deviations of each element were within 3.5%-18.6%. The analysis results were consistent with those obtained by inductively coupled plasma mass spectrometry.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2015年第9期1366-1370,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.21271187)
湖南省自然科学基金(No.14JJ5032)
重庆市高校优秀成果转化资助项目(No.KJZH14217)
湖南省教育厅重点科研项目(No.14A035)
湖南省重点学科建设项目(湘教发[2011]76号)资助~~
关键词
辉光放电质谱法
镍锌铁氧体
杂质元素
铜粉
归一化
Glow discharge mass spectrometry
Nickel-zinc ferrites
Impurity elements
Copper powder
Normalization
