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作 者:王志萍 王巧 孙洪涛 胡远霞 WANG Zhiping;WANG Qiao;SUN Hongtao;HU Yuanxia(State Key Laboratory of Rare Metal Special Materials,Northwest Rare Metal Materials Research Institute Ningxia Co.,Ltd.,Shizuishan 753000,China;Huizhou Top Metal Materials Co.,Ltd.,Huizhou 516000,China)
机构地区:[1]稀有金属特种材料国家重点实验室西北稀有金属材料研究院宁夏有限公司,宁夏石嘴山753000 [2]惠州拓普金属材料有限公司,广东惠州516000
出 处:《冶金分析》2021年第11期78-83,共6页Metallurgical Analysis
摘 要:高铍铍铝合金是一种重要的结构材料,杂质元素含量会影响其结构性能,因此需要准确测定其含量。样品采用硫酸-硝酸分解,优选了Fe 238.204nm、Mn 257.610nm、Cr 267.716nm、Ni 216.555nm、Mg 279.553nm作为分析谱线,采用标准加入法(MSA)绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铁、锰、铬、镍和镁,从而建立了高铍铍铝中铁、锰、铬、镍、镁等杂质元素的分析方法,各待测元素校准曲线线性相关系数r均大于0.9999,方法中各元素的检出限为0.0002%~0.0036%(质量分数,下同),定量限为0.0007%~0.0119%。按照实验方法测定1个高铍铍铝合金中的铁、锰、铬、镍、镁,结果的相对标准偏差(RSD,n=11)为1.2%~4.6%,加标回收率为93%~105%;选择1个样品与辉光放电质谱法(GD-MS)比对,测定结果基本一致。High-beryllium beryllium-aluminum alloy is an important structural material.The contents of impurity elements will affect its structural properties.Therefore,it is necessary to determine the impurity contents accurately.The samples were decomposed by sulfuric acid and nitric acid.Fe 238.204 nm,Mn 257.610 nm,Cr 267.716 nm,Ni 216.555 nm and Mg 279.553 nm were selected as the analytical lines.The method of standard addition(MSA)was used to draw calibration curves to eliminate the influence of matrix effect.The contents of iron,manganese,chromium,nickel,and magnesium were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Consequently,the analysis method of impurities in high-beryllium beryllium-aluminum alloy,including iron,manganese,chromium,nickel,and magnesium,was established.The linear correlation coefficients(r)of calibration curves of testing elements were all greater than 0.9999.The limits of detection of elements were between 0.0002% and 0.0036%(mass fraction,similarly hereinafter).The limits of quantification were between 0.0007% and 0.0119%.The contents of iron,manganese,chromium,nickel,and magnesium in one high-beryllium beryllium-aluminum alloy sample were determined according to the experimental method.The relative standard deviations(RSD,n=11)of determination results were between 1.2% and 4.6%.The spiked recoveries were between 93% and 105%.Another sample was used to compare with glow discharge mass spectrometry(GD-MS),and the determination results were basically consistent.
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