摘要
为了建立辉光放电质谱法(GD-MS)测定颗粒状高纯铬中痕量元素的方法,深入研究了颗粒状高纯铬样品的制备方案。比较了不同研磨方式和压片方案,考察了不同粒度、模具或压力下压制的高纯铬样品片中基体铬在不同放电参数下的信号强度。实验表明,当样品粒度为100目(150μm),采用铝杯模具在75t压力下压制时,样品成形效果较好,且对应基体铬信号强度与放电电压、放电气流和脉冲时间的线性关系较好,信号强度最高可达到5×1010 cps以上,较为理想;采用研磨仪自动研磨50～100g样品1min,100目(150μm)样品产率可达90%以上,因此采用此种方式处理样品。采用实验方法制备样品,用GD-MS分析颗粒状高纯铬中主要痕量元素的结果与电感耦合等离子体原子发射光谱法(ICP-AES)、电感耦合等离子体质谱法(ICP-MS)和原子吸收光谱法(AAS)测定值吻合较好,μg/g含量级别的钠、铝、硅、钙、钛、钒、锰、铁、镍、铜这10个杂质元素测定值的相对标准偏差(RSD,n=7)在0.80%～11.6%之间,ng/g含量级别的钼、锑、铅这3个杂质元素的RSD(n=7)则在3.7%～13.6%之间。方法为进一步研究颗粒状高纯铬样品全元素分析和纯度分析提供了可靠的试验方案。
In order to establish the determination method of trace elements in granular high-purity chromium by glow discharge mass spectrometry (GD-MS), the preparation scheme of granular high-purity chromium samples was systemically studied. Various grinding methods and pressing schemes were compared. The signal intensity of matrix chromium in high purity chromium samples prepared under different experimental conditions (including particle size, mould and pressure) was investigated with different discharge parameters. The experimental results showed that the forming effect of sample was good when the sample granularity was 100-mesh (150 μm) and the aluminum cup mould was pressed at 75 t pressure. Moreover, the corresponding signal intensity of matrix chromium had good linear relationship with discharge voltage, discharge gas flow and pulse duration. The maximum signal intensity was higher than 5×10^10 cps, which was satisfactory. In experiments, 50-100 g of samples were automatically ground by a grinder for 1 minute, and the yield of 100-mesh (150 μm) sample was more than 90%. Therefore, this method was adopted for sample preparation.The granular high-purity chromium sample was prepared according to the experimental method and then determined by GD-MS. The found results of trace elements were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectroscopy (AAS). For ten impurity elements with content level at μg/g (including Na, Al, Si, Ca, Ti, V, Mn, Fe, Ni and Cu), the relative standard deviations (RSD, n =7) were in range of 0.80%-11.6%. For three impurity elements with content level at ng/g (including Mo, Sb and Pb), the RSDs were in range of 3.7%-13.6%. The proposed method provided a reliable experimental scheme for the further study of all-element analysis and purity analysis of granular high-purity chromium samples.
作者
邵秋文
胡净宇
侯艳霞
杨国武
贾德健
SHAO Qiu-wen;HU Jing-yu;HOU Yan-xia;YANG Guo-wu;JIA De-jian(Central Iron & Steel Research Institute, Beijing 100081, China;NCS Testing Technology Co., Ltd., Beijing 100081, China;Ruishenbao Analytical (Shanghai) Co., Ltd., Shanghai 200237, China)
出处
《冶金分析》
CAS
北大核心
2019年第5期1-7,共7页
Metallurgical Analysis
基金
中国钢研科技集团有限公司青年创新专项基金(ZNCS098)
关键词
辉光放电质谱法(GD-MS)
颗粒状样品
高纯铬
样品制备
glow discharge mass spectrometry (GD-MS)
granular sample
high purity chromium
sample preparation
