摘要
建立了X射线荧光光谱法测定钼精矿中Mo,Si,Ca,Cu,Pb,W,Bi,P,As,Sn的分析方法。通过固体纯物质机械混合研磨配制了校准曲线所用的12个标准样品。钼精矿样品在600℃进行了灼烧处理。采用混合熔剂(Li2B4O7:LiBO2:LiF=10:2. 5:1,m/m/m)加氧化剂LiNO3,并且以低稀释比(混合熔剂:LiNO3:灼烧后试样=4:0. 6:0. 8,m/m/m)熔融制备了X射线荧光法所用玻璃片样品。使用背景曲线法计算As元素的可靠背景强度;采用干扰曲线法校正MoL1对P Kα,Pb Lα对As Kα的谱线重叠干扰;采用经验系数法和Rh靶Compton内标法对各分析元素的基体效应影响进行了校正。钼精矿中微量元素检出限分别为:Cu(9. 4×10-4%),Pb(1. 8×10-3%),W (2. 2×10-3%),Bi(1. 9×10-3%),P(9. 0×10-4%),As(6. 1×10-4%),Sn(2. 3×10-3%)。
A determination method for 10 elements( Mo,Si,Ca,Cu,Pb,W,Bi,P,As,Sn) in molybdenum concentrates by X-ray fluorescence analysis was established. 12 standard samples for calibration curves were prepared by the mechanical mixing and grinding of solid pure substances.Fused glass disc samples for X-ray fluorescence analysis were prepared at 600 ℃ with a low dilution ratio of mixed flux/Li NO3/sample = 4: 0. 6: 0. 8( m/m/m),where a mixed flux of Li2 B4 O7: Li BO2: Li F was 10: 2. 5: 1( m/m/m). Background adsorption curve was used to calculate reliable background strength of element As. Interfering curve method was employed to correct spectral line interference.The interference curve corrections were chosen to the spectral overlaps between Mo L1 and P Kα,Pb Lα and As Kα,respectively. The experiential coefficient method and interior labels of Rh K Compton scattered line were employed for matrix effect correction of other elements. Detection limits of different elements in molybdenum concentrates were Cu( 9. 4 × 10^4%),Pb( 1. 8 × 10^3%),W( 2. 2 × 10^3%),Bi( 1. 9 × 10^3%),P( 9. 0 × 10^4%),As( 6. 1 × 10^4%) and Sn( 2. 3 × 10^3%),respectively.
作者
童晓民
王楠
董再蒸
TONG Xiao-min;WANG Nan;DONG Zai-zheng(Analytical and Test Research Center, Northeast University, Shenyang 110819)
出处
《分析试验室》
CAS
CSCD
北大核心
2019年第3期369-373,共5页
Chinese Journal of Analysis Laboratory
关键词
X射线荧光光谱
钼精矿
低稀释比
X-ray fluorescence
Molybdenum Concentrates
Low dilution ratio
作者简介
通信作者:童晓民,E-mail:tong1969@163.com.
