激光剥蚀-电感耦合等离子体质谱法测定高纯铪中10种杂质元素

doi:10.3964/j.issn.1000-0593(2019)02-0571-06

Abstract
References
Related Citation (15)

Download: PDF (3422 KB)
Export: BibTeX | EndNote (RIS)

Abstract High purified hafnium has important applications in nuclear reactor, plasma cutting machine, optical element and so on, because of its unique physical and chemical properties. The type and content of impurities in high purity hafnium affect the physical and chemical properties of high purity hafnium, and the purity requirement of high-purity hafnium is also higher and higher. This requires higher requirements for the analysis and detection technology of high-purity hafnium. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a combination of laser ablation sampling technique and inductively coupled plasma mass spectrometry. The advantage of this method is that impurities can be avoided in the preprocessing, and the solid sample can be analyzed directly. So, this method is an efficient, fast and precise analytical technology, widely applied in the fields of environment, geology, metallurgy, fuel energy, materials, biomedicine, archaeology and so on. However, the application of testing high purity hafnium by LA-ICP-MS has not been reported while LA-ICP-MS is one of the best methods for the detection of high purity metallic impurities. Ten kinds of impurities (Al，Sc，Ti，Fe，Ni，Cu，Mo，Ag，Sn，W) in high purified hafnium were quantitatively analyzed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). In order to reduce the fractionation effect of elements in the laser ablation process and improve the signal sensitivity and stability, the laser denudation parameters were optimized. Experiments showed that the optimal laser ablation parameters were that He flow rate was 600 mL·min^-1, energy 90%, spot size 150 μm, scan rate 60 μm·s^-1and pulse repetition 20 Hz. The working parameters of ICP-MS instrument after experimental optimization were that RF power was 1 450 W, RF matching voltage 1.8 V, carrier gas flow rate 0.85 L·min^-1, cooling gas flow rate 0.85 L·min^-1, sample depth 7.5 mm. Under the best experimental conditions, internal control standard samples were used to establish working curves; the linear correlation coefficients of impurities were between 0.993 6 and 0.999 8. The signal intensity of the blank carrier gas was collected and measured for 11 times. The content of the standard deviation of the 3 times blank signal was taken as the detection limit of the elements. The detection limits of each element were from 0.001 to 0.08 μg·g^-1. High purified hafnium was made into a suitable sample of size. The oxide on the surface of the sample was washed with nitric acid. The sample was loaded into ablation pool, and laser ablated by line scanning. Under the best experimental conditions, ten kinds of impurities in three high purified hafnium samples were determined by LA-ICP-MS. The content of impurity elements was 0.17~36.76 μg·g^-1. Relative standard deviations were from 1.4% to 20%, which showed that the method has good precision. In the case of W, Student’s t test was made between the determination of LA-ICP-MS and ICP-MS. Student’s t test shows that the t values of the three samples were 2.14, 1.64 and 2.11, which were lower than the critical value of the significant level of 0.05 (t_{0.05, 12}=2.18), so there was no significant difference between the results of LA-ICP-MS method and ICP-MS method. The trueness and precision were favorable, which showed that this method can be used for quantitative analysis of impurities in high pure hafnium.

Key words：High purified hafnium; LA-ICP-MS; Laser ablation parameter

Received: 2018-01-04 Accepted: 2018-05-20

ZTFLH:

O657.6

Corresponding Authors: LIU Ying E-mail: css2@grinm.com

Cite this article:

URL:

https://www.gpxygpfx.com/EN/10.3964/j.issn.1000-0593(2019)02-0571-06 OR https://www.gpxygpfx.com/EN/Y2019/V39/I02/571

[1] YAN Guang-jiong, TONG Jian, LI Na，et al（颜广炅, 童坚, 李娜，等）. Chinese Journal of Analysis Laboratory（分析实验室）, 2008, 27(12): 107.
[2] MO Shu-min, PAN Yuan-hai, WANG Chang-hua（墨淑敏, 潘元海, 王长华）. Chinese Journal of Spectroscopy Laboratory（光谱实验室）, 2012, 29(3): 1455.
[3] QIAN Rong, SI Qin-bi-li-ge, ZHUO Shang-jun，et al（钱荣, 斯琴毕力格, 卓尚军, 等）. Chinese Journal of Analytical Chemistry（分析化学）, 2011, 39(5): 700.
[4] General Research Institute for Nonferrous Metals（北京金属研究总院）. GYB 15—2014，2014.
[5] WANG Wei（王炜）. Environmental Protection and Circular Economy（环境保护与循环经济）, 2014, 34(6): 56.
[6] Burakov V S, Raikov S N , Tarasenko N V, et al. Journal of Applied Spectroscopy, 2010, 77(5): 595.
[7] Gaudiuso R, Aglio L D, De Pascale O, et al. Sensors, 2010, 10(8): 7434.
[8] WANG Hua-jian, ZHANG Shui-chang, YE Yun-tao, et al（王华建, 张水昌, 叶云涛, 等）. Chinese Journal of Analytical Chemistry（分析化学）, 2016, 44(11): 1665.
[9] KE Yu-qiu, ZHANG Lu-yuan, CHAI Xin-na, et al（柯于球, 张路远, 柴辛娜, 等）. Chemical Journal of Chinese Universities（高等学校化学学报）, 2012, 33(2): 257.
[10] FAN Chen-zi, HU Ming-yue, ZHAO Ling-hao, et al（范晨子，胡明月, 赵令浩, 等）. Rock and Mineral Analysis（岩矿测试）, 2013, 32(3): 383.
[11] Bengtson A, Thomas B. Metallurgical Analysis（冶金分析）, 2009, 29(2): 8.
[12] XIE Cheng-li, LU Ji-dong, LI Peng-yan，et al（谢承利, 陆继东, 李鹏艳, 等）. Journal of Engineering Thermophysics（工程热物理学报）, 2009, 30(2): 329.
[13] LI Tian-yi, ZHOU Yan, FANG Shi, et al（李天义, 周雁, 方石, 等）. Oil & Gas Geology（石油与天然气地质）, 2013, 34(4): 550.
[14] Herrera K K, Tognoni E, Gornushkin I B, et al. Anal. At. Spectrom., 2009, 24: 426.
[15] ZHOU Hui, WANG Zheng, ZHU Yan, et al（周慧, 汪正, 朱燕, 等）. Chinese Journal of Analytical Chemistry（分析化学）, 2014, 42(1): 123.
[16] GUO Liang, LI Xue-lian, JIN Xian-zhong（郭亮, 李雪莲, 金献忠）. Physical Testing and Chemical Analysis(Part B: Chemical Analysis)（理化检验：化学分册）, 2016, 52(2): 151.
[17] LI Qing, ZHANG Guo-xia, CHEN Yi-rui, et al（李青, 张国霞, 陈奕睿, 等）. Chinese Journal of Analytical Chemistry（分析化学）, 2017, 45(6): 868.
[18] LING Xue, JIA La-jiang, LIU Xiao-ming, et al（凌雪, 贾腊江, 柳小明, 等）. Journal of Lanzhou University·Natural Sciences（兰州大学学报·自然科学版）, 2012, 48(1): 8.