摘要
高纯铬作为钢铁的添加材料,其杂质含量关系到材料的性能,高效、准确测定其杂质元素的含量至关重要。试验将粒度为150μm的高纯铬粉压制成片,建立了辉光放电质谱法(GD-MS)测定高纯铬中Na、Mg、Al、Si等68种杂质元素的方法。试验表明:通过优化仪器工作条件,铬压片放电信号稳定且强度可满足测试要求;高分辨模式下测定K、Zn、Ga、Ge、Se、Mo、Ru、Rh、Pd、Ag、Sn元素,其余元素则在中分辨模式下消除质谱干扰。Na、Al、Si、P、S等13个元素采用校正后的相对灵敏度因子(RSF)进行测定,其余元素则采用仪器预设标准RSF(std-RSF)进行测定。方法检出限为0.001~0.50μg/g。按照实验方法测定两个高纯铬中杂质元素,其中56种常见元素的测定结果与采用电感耦合等离子体质谱法(ICP-MS)、电感耦合等离子体原子发射光谱法(ICP-AES)、原子吸收光谱法(AAS)、原子荧光光谱法(AFS)、红外光谱法(IR)的测定结果相一致;其余12种元素的测定结果也与ICP-MS半定量参考值相吻合。
High-purity chromium is an additive for iron and steel,and contents of impurities are related to the performance of iron and steel materials.Therefore,it is very important to determine the content of impurity elements efficiently and accurately.In experiments,the high purity chromium powder with particle size of 150μm was pressed into pieces,and a method for the determination of 68 impurity elements(such as Na,Mg,Al and Si)in high purity chromium by glow discharge mass spectrometry(GD-MS)was established.The results showed that the discharge signal of chromium piece was stable and the intensity could meet the test requirements by optimizing the working conditions of the instrument.The mass specal interference could be eliminated by determining K,Zn,Ga,Ge,Se,Mo,Ru,Rh,Pd,Ag and Sn at high resolution mode,while determining other elements at medium resolution mode.13 elements such as Na,Al,Si,P and S were determined by relative sensitivity factor(RSF)after correction,while other elements were determined using standard RSF.The limits of detection were between 0.001μg/g and 0.50μg/g.The contents of impurity elements in two high purity chromium samples were determined according to the experimental method.The found results of 56 common elements were consistent with those obtained by inductively coupled plasma mass spectroscopy(ICP-MS),inductively coupled plasma atomic emission spectrometry(ICP-AES),atomic absorption spectrometry(AAS),atomic fluorescence spectrometry(AFS)and infrared absorption(IR).The determination results of other 12 elements were also consistent with the semi-quantitative reference values obtained by ICP-MS.
作者
邵秋文
胡净宇
侯艳霞
杨国武
SHAO Qiu-wen;HU Jing-yu;HOU Yan-xia;YANG Guo-wu(Central Iron & Steel Research Institute, Beijing 100081, China;NCS Testing Technology Co., Ltd., Beijing 100081, China)
出处
《冶金分析》
CAS
北大核心
2020年第9期10-17,共8页
Metallurgical Analysis
基金
钢研纳克检测技术股份有限公司自立课题(ZNCS142)。
