Spectroscopy and Spectral Analysis, Volume. 42, Issue 7, 2169(2022)
Determination of Nb and Re in High Purity Tungsten by Precipitation Separation-Inductively Coupled Plasma Mass Spectrometry
Figures & Tables(10)
Fig. 1. The interference on Nb and Re of W standard solution with different concentrations
Fig. 2. The influence of the amount of precipitant on the residual amount of tungsten
Fig. 3. The effect of the amount of buffer solution on the residual amount of tungsten
Fig. 4. The effect of aging time on the residual amount of tungsten
Table 1. Operation parameters of ICP-MS and ICP-OES
View tableView in ArticleTable 1. Operation parameters of ICP-MS and ICP-OES
ICP-MS工作仪器参数 数值 ICP-OES工作仪器参数 数值 RF功率/W 1 550 RF功率/W 1 200 采样深度/mm 8.0 等离子体气流量/(L·min-1) 15.0 载气流量/(L·min-1) 0.90 辅助气流量/(L·min-1) 1.00 稀释气流量/(L·min-1) 0.35 雾化气流量/(L·min-1) 0.70 泵速/(r·s-1) 0.20 泵速/(r·min-1) 12 测量方式 跳峰 观测高度/mm 8 扫描次数 3 积分时间/s 5 积分时间/s 0.1 - -
Table 2. The mass spectrum interference of the determination of Nb and Re in high-purity tungsten by ICP-MS
View tableView in ArticleTable 2. The mass spectrum interference of the determination of Nb and Re in high-purity tungsten by ICP-MS
同位素 干扰离子 93Nb 186W++ 185Re 184W1H+, 183W1 187Re 186W1H+
Table 3. The selection of internal standard elements
View tableView in ArticleTable 3. The selection of internal standard elements
待测元素 回收率/% 无内标 Sc Cs Tl Nb 101(121) 90.1(103) 103(111) 110(115) Re 97.9(119) 90.2(86.1) 100(93.5) 107(113)
Table 4. The limits of detection and quantitation(μg·g-1)
View tableView in ArticleTable 4. The limits of detection and quantitation(μg·g-1)
待测元素 直接测定 基体分离后测定 检出限 定量限 检出限 定量限 Nb 0.81 2.70 0.007 0.023 Re 0.61 2.02 0.036 0.12
Table 5. Precision and recovery of the method
View tableView in ArticleTable 5. Precision and recovery of the method
待测
元素测定值/
(μg·g-1)RSD/
%加标量/
(μg·g-1)回收值/
(μg·g-1)回收
率/%Nb 0.024 12 0.050 0.078 108 Re 0.21 4.8 0.20 0.42 105
Table 6. The analytical results of sample
View tableView in ArticleTable 6. The analytical results of sample
待测元素 测定值/
(μg·g-1)RSD/% 加标量/
(μg·g-1)加标
回收率/%Nb 0.021 8.8 0.050 109 Re 9.42 1.0 10.00 100
Tools
Get Citation
Copy Citation Text
. Determination of Nb and Re in High Purity Tungsten by Precipitation Separation-Inductively Coupled Plasma Mass Spectrometry[J]. Spectroscopy and Spectral Analysis, 2022, 42(7): 2169
Paper Information
Category: Orginal Article
Received: Jun. 10, 2021
Accepted: --
Published Online: Nov. 16, 2022
The Author Email:
© Copyright 2018-2021 | Chinese Laser Press.
All Rights Reserved 沪ICP备15018463号-20