ICP-MS/MS测定高纯氧化钇的14种稀土杂质元素

doi:10.19964/j.issn.1006-4990.2021-0379

Abstract

Abstract:

Fourteen rare earth impurities in high purity yttrium oxide were determined by series triple quadrupole inductively coupled plasma mass spectrometry（ICP-MS/MS）.Under the best working conditions,the analytical mode of the sample was determined as the mode of TQ-He.The effect of He and O₂ as reaction gases on the detection limit and the equivalent background concentration（BEC） was investigated,which could eliminate the interference of polyatomic ions that produced by yttrium oxide matrix more effectively.The interference of collision mode could be eliminated to achieve the purpose of accurate determination of trace rare earth impurities in high purity yttrium.In the helium mode,the detection limit of rare earth elements was between 0.007 μg/L and 0.89 μg/L in experiment.The recovery was 97.93%~104.86% and the relative standard deviation was 0.78%~3.39%.The method had the advantages of simplicity and high precision,which could meet the direct determination of 14 rare earth impurity elements in high purity yttrium oxide with a purity of 99.999%~99.999 9% and above.

Key words: ICP-MS/MS, high purity yttrium oxide, rare earth impurities, elimination of interference

CLC Number:

TQ133.23

LIANG Yuyi,LI Bing,KONG Xiangfei,QIN Wenzhong,HU Zhenguang. Determination of 14 rare earth impurity elements in high-purity yttrium oxide by ICP-MS/MS[J]. Inorganic Chemicals Industry, 2022, 54(4): 165-168.

Figures/Tables 7

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References 17

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仪器模式	测量模式	RF功率/ W	采样深度/ mm	稀释气流量/ （L·min^-1）	载气流量/ （L·min^-1）	He流量/ （mL·min^-1）	O₂流量/ （mL·min^-1）	NH₃-He（1∶9）流量/（mL·min^-1）
He	SQ	1 550	8	0.5	0.6	—	—	—
O₂mass shift	MS/MS	1 550	8	0.5	0.6	—	0.3	—
NH₃ mass shift	MS/MS	1 550	8	0.5	0.6	—	—	—
NH₃ on mass	MS/MS	1 550	8	0.5	0.6	1	—	8.0

步骤	消解温度/℃	消解时间/min	消解功率/W
1	100	10	1 600
2	130	15	1 600
3	150	10	1 600

模式	响应强度/cps		模式	响应强度/cps
模式	Nd	Sm	模式	Nd	Sm
SQ-He	39 987	41 562	TQ-He	1 266	—
SQ-O₂	48 713	15	TQ-O₂	16	21

稀土元素	等效背景浓度
稀土元素	He	O₂ mass shift	NH₃ mass shift	NH₃ on mass
Nd	0.028	0.035	0.023	—
La	0.133	0.132	0.141	—
Ce	0.041	0.042	0.037	—
Pr	1.324	1.367	1.298	—
Sm	1.007	1.021	0.987	—
Eu	0.036	0.028	0.031	—
Gd	0.041	0.043	0.039	—
Tb	36.220	154.600	25.270	0.018
Dy	165.000	321.200	162.000	0.040
Ho	18.170	19.210	19.290	0.040
Er	0.038	0.056	0.059	—
Tm	0.652	0.771	0.716	—
Yb	0.254	0.313	0.423	—
Lu	0.073	0.025	0.008	—

模式	信号强度/cps
模式	Pr	Tm
TQ-He	4 341	3 761
TQ-O₂	4 102	3 675

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Determination of 14 rare earth impurity elements in high-purity yttrium oxide by ICP-MS/MS

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稀土元素	相关系数	等效背景质量浓度/ （ng·L^-1）	检出限/ （μg·L^-1）	稀土元素	相关系数	等效背景质量浓度/ （ng·L^-1）	检出限/ （μg·L^-1）
Nd	0.999 2	21.80	0.340	Tb	0.999 7	25.10	0.021
La	0.999 5	16.30	0.890	Dy	0.999 7	2.14	0.126
Ce	0.999 8	4.33	0.060	Ho	0.999 3	1.43	0.009
Pr	0.999 2	13.20	0.360	Er	0.999 2	5.67	0.032
Sm	0.999 9	7.31	0.017	Tm	0.999 4	3.21	0.007
Eu	0.999 9	4.63	0.008	Yb	0.999 1	4.34	0.010
Gd	0.999 8	18.90	0.012	Lu	0.999 3	1.98	0.011

稀土元素	质量数	内标 1	内标 2	400 mg/L Y₂O₃
稀土元素	质量数	内标 1	内标 2	强度/ cps	质量浓度/ （ng·mL^-1）	回收率/%	RSD/ %
Nd	144	103	115	256	0.412 1	101.35	1.34
La	139	103	115	423	0.495 8	98.84	0.83
Ce	140	103	115	375	0.005 1	100.46	0.78
Pr	141	103	115	267	0.021 1	100.19	1.29
Sm	152	103	115	71	0.084 1	97.93	2.45
Eu	153	103	115	487	0.001 1	100.36	1.73
Gd	155	103	115	289	0.002 4	100.06	3.39
Tb	159	103	115	1023	0.051 3	100.42	2.56
Dy	163	103	115	162	0.001 3	101.86	1.28
Ho	165	103	115	192	0.108 4	104.86	1.27
Er	170	103	115	27	0.252 3	101.42	1.56
Tm	169	103	115	426	0.002 2	99.88	1.65
Yb	174	103	115	123	0.001 5	101.65	1.23
Lu	175	103	115	672	0.025 6	101.47	2.97

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