|
|
|
|
|
|
| Analysis of Ultra-Trace Impurities in High Purity Molybdenum Powder through Inductively Coupled Plasma Tandem Mass Spectrometry |
| FU Liang1, 2, SHI Shu-yun2*, TANG You-gen2, WANG Hai-yan2 |
1. Collaborative Innovation Center of Green Development for Wuling Mountain Areas, Yangtze Normal University, Chongqing 408100, China
2. School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China |
|
|
|
|
Abstract An analytical method for the determination of ultra-trace impurities in high purity molybdenum was established by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). In MS/MS mode, H2 was used as the reaction gas to measure Si and Ca through the H2 on-mass method. O2 was employed as the reaction gas to measure the Cd via the O2 on-mass method, and P, As, Se, Ta, Sn, Sb, Ba, and W were measured by the O2 mass-shift method. NH3/He was adopted as the reaction gas, so that Na, Mg, Al, K, and V could be measured by NH3/He on-mass method, and Ti, Cr, Mn, Fe, Co, Ni, Cu, and Zn could be measured by the NH3/He mass- shift method. Pb, Bi, Th, and U were measured in single quadropole (SQ) mode without gas. Compared with conventional collision/reaction cell (CRC) inductively coupled plasma mass spectrometry (ICP-MS), the background equivalent concentration (BEC) and detection limit of analyte in this method were lower, and the mass spectrum interference could be eliminated more thoroughly. Under optimized working conditions, the calibration curves of analytes showed good linearity with linear correlation coefficient (R2)≥0.999 7. The detection limit was 0.04～50.1 ng·L-1, the spike recoveries were 92.2%～107.4% and the relative standard deviation (RSD) was ≤4.3%, indicating that the proposal method has excellent accuracy and precision. The results of the sample analysis showed that the method can be used for the determination of 28 impurity elements in high purity molybdenum powder with purity of 5N (≥99.999%).
|
|
Received: 2017-09-18
Accepted: 2018-02-02
|
|
|
|
Corresponding Authors:
SHI Shu-yun
E-mail: syshicsu@163.com
|
|
[1] WANG Dong-hui, YUAN Xiao-bo, LI Zhong-kui, et al(王东辉, 袁晓波, 李中奎, 等). Rare Metals Letters(稀有金属快报), 2006, 25(12): 1.
[2] AN Geng, LI Jing, LIU Ren-zhi, et al(安 耿, 李 晶, 刘仁智, 等)．China Molybdenum Industry(中国钼业), 2011, 35(2): 45.
[3] YANG Fan, WANG Kuai-she, HU Ping, et al(杨 帆, 王快社, 胡 平, 等). Hot Working Technology(热加工工艺), 2013, 42(24): 10.
[4] Saito M, Hirose F, Okochi Haruno. Anal. Sci., 1995, 11(4): 695.
[5] Theimer K H, Krivan V. Anal. Chem., 1990, 62(24): 2722.
[6] Docekal B, Krivan V. J. Anal. Atom. Spectrom., 1993, 8(4): 637.
[7] Docekal B, Krivan V, Franek M. Spectrochim. Acta B, 1994, 49(6): 577.
[8] Docekal B, KrivanV. Spectrochim. Acta B, 1995, 50(4-7): 517.
[9] Nakashima R, Sasaki S. Anal. Chim. Acta, 1976, 85(1): 75.
[10] LI Lin-yuan, PENG Yu, YAN Xiao-hua, et al(李林元, 彭 宇, 颜晓华, 等). Cemented Carbide(硬质合金), 2016, 33(2): 119.
[11] Mogi F, Itoh K, Okamoto N, et al. Denki Seiko, 1988, 59(4): 263.
[12] Kujirai O, Yamada K, Kohri M, et al. Fresen. J. Anal. Chem., 1991, 339(3): 133.
[13] Krivan V, TheimerK H. Spectrochim. Acta B, 1997, 52(14): 2061.
[14] Hasegawa S I, Yamaguchi H, Yamada K, et al. Mater. Trans., 2004, 45(3): 925.
[15] Kipphardt H, Czerwensky M, Matschat R. J. Anal. Atom. Spectrom., 2005, 20(1-1): 28.
[16] WANG Chang-hua, LI Ji-dong, PAN Yuan-hai(王长华, 李继东, 潘元海). Chinese Journal of Analysis Laboratory(分析试验室), 2011, 30(7): 18.
[17] FU Liang, SHI Shu-yun(符 靓, 施树云). Chinese Journal of Analytical Chemistry(分析化学), 2017, 45(8): 1222.
[18] Fu L, Shi S Y, Chen X Q. Spectrochim. Acta B, 2017, 133: 34.
[19] He Q, Xing Z, Wei C, et al. Chem. Commun., 2016, 52(69): 10501.
[20] Quemet A, Brennetot R, Chevalier E, et al. Talanta, 2012, 99: 207.
[21] Deitrich C L, Cuello-Nunez S, Kmiotek D, et al. Anal. Chem., 2016, 88(12): 6357. |
| [1] |
CAI Song-tao1, XIE Hua-lin2, HUANG Jian-hua3*. Analysis of Heavy Metal Cd in Cereal-Based Complementary Foods for
Infants and Young Children by Inductively Coupled Plasma Tandem
Mass Spectrometry (ICP-MS/MS)[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2022, 42(09): 2818-2823. |
| [2] |
LIU Hong-wei1,3, FU Liang2*. Analysis of Metal Impurity Elements in Li4Ti5O12 Through Microwave Plasma Atomic Emission Spectroscopy[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2021, 41(10): 3021-3025. |
| [3] |
LI Tan-ping, LI Ai-yang. Analysis of Ultra-Trace Metal Impurity Elements in Proprylene Glycol Monomethyl Ether Using Inductively Coupled Plasma Tandem Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2021, 41(02): 618-623. |
| [4] |
ZHANG Liang-liang, WANG Chang-hua, HU Fang-fei, MO Shu-min, LI Ji-dong*. Determination of Trace Impurity Elements in Zircaloy by Ion Exchange-Inductively Coupled Plasma Mass Spectroscopy[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2020, 40(08): 2622-2628. |
| [5] |
WANG Zi-ren, WANG Chang-hua, HU Fang-fei, LI Ji-dong*. Quantification of Trace Impurities in Graphite by Glow Discharge Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2019, 39(04): 1256-1261. |
| [6] |
LIU Hong-wei, NIE Xi-du*. Analysis of Trace Elements in Wild Artemisia Selengensis Using Inductively Coupled Plasma Tandem Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(12): 3923-3928. |
| [7] |
ZHOU Xue-zhong, LIU Hong-wei*. Accurate Determination of Calcium and Chlorine in Food with Inductively Coupled Plasma Tandem Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(11): 3567-3571. |
| [8] |
FU Liang1,3, ZHAO Feng-xuan2, WANG Hai-yan3, WANG Huan-zhe2, CHEN Tao2, XU Jian-hua1, LI Bing1, XIE Hua-lin1*. Impurity Elements Analysis of Catalyst Precursor Ruthenium Nitrosyl Nitrate Using Inductively Coupled Plasma Tandem Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(11): 3572-3577. |
| [9] |
JIANG Bo1,3, HUANG Jian-hua2*. Multi-Element Analysis of Jatropha curcas L. Oil Using Inductively Coupled Plasma Tandem Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(09): 2937-2942. |
| [10] |
WANG Jin-lei1, 2, QIAN Jun-min2, LI Bo1, LUO Lin1*, SUN Bao-lian1, XU Wei-jun2, CUI Ning2. Chloroformylation-Separation of Matrix and Determination of Trace Impurities in High Purity Chromium by ICP-MS[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2017, 37(09): 2896-2899. |
| [11] |
NIE Xi-du1, FU Liang2* . Simultaneous Determination of Impurity Elements in N-Methyl-2- Pyrrolidone (NMP) with Direct Injection Inductively Coupled Plasma Optical Emission Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2017, 37(03): 910-913. |
| [12] |
LIU Hong-wei1, XIE Hua-lin2*, NIE Xi-du1 . Determination of Impurity Elements in Rosin with Inductively Coupled Plasma Mass Spectrometry [J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2017, 37(02): 603-606. |
| [13] |
NIE Xi-du1, FU Liang2* . Determination of Trace Impurity Elements in Food Grade Chitosan with Inductively Coupled Plasma Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2016, 36(08): 2621-2624. |
| [14] |
ZHU Qian-hua . Determination of Impurity Elements in the Positive Electrode Material LiMn2O4 by Inductively Coupled Plasma Mass Spectrometry [J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2013, 33(05): 1350-1353. |
| [15] |
LI Tan-ping1, XIE Hua-lin2*. Determination of Impurity Elements in Edible Phosphate by ICP-MS [J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2012, 32(10): 2834-2837. |
|
|
|
|
