敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪

门倩妮; 沈平; 甘黎明; 冯博鑫

doi:10.15898/j.cnki.11-2131/td.201905100060

敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪

1.
中国人民武装警察部队黄金部队第五支队, 陕西西安 710100

2.
甘肃智广地质工程勘察设计有限公司, 甘肃兰州 730010

详细信息

作者简介: 门倩妮, 硕士, 从事地质样品的分析测试工作。E-mail:menqianni-6019@163.com

中图分类号: O614.33;O657.63

收稿日期: 2019-05-10

修回日期: 2019-07-05

录用日期: 2019-07-19

Determination of Rare Earth Elements and Nb, Ta, Zr, Hf in Polymetallic Mineral Samples by Inductively Coupled Plasma-Mass Spectrometry Coupled with Open Acid Dissolution and Lithium Metaborate Alkali Fusion

1.
No.5 Gold Geological Party, Chinese People's Armed Police Force, Xi'an 710100, China

2.
Gansu Zhiguang Geological Engineering Survey and Design Co. LTD., Lanzhou 730010, China

Received Date: 10 May 2019

Revised Date: 05 July 2019

Accepted Date: 19 July 2019

摘要

摘要: 用电感耦合等离子体质谱法（ICP-MS）测定地质样品中的稀土及难熔元素，混合酸敞开酸溶法和碱熔融法是两种主要的溶样方法。但地质样品组分复杂，元素之间存在相互共生的现象，对于特殊元素、特殊样品用传统酸溶法会造成部分元素消解不完全，使测定结果不准确；而碱熔法的操作过程繁琐，且溶液盐度高，易产生基体干扰和堵塞仪器进样系统。本文改进了传统四酸和五酸体系，采用氢氟酸-硝酸-硫酸敞开酸溶体系，用国家一级标准物质制作标准曲线测定15种稀土元素，方法准确度（ΔlgC）为0.001~0.027。同时改进了偏硼酸锂碱熔法，样品用偏硼酸锂碱熔提取，加入氢氧化钠调节溶液至碱性条件，所测元素与偏硼酸锂共沉淀后过滤分离熔剂，再用硝酸复溶测定15种稀土元素及铌钽锆铪。两种溶样方法的测定值与认定值的相对误差为1.09%~9.30%。将混合酸敞开酸溶法测定稀土元素、偏硼酸锂碱熔法测定铌钽锆铪的结果与其他实验室密闭酸溶法相比，两组数据的相对偏差为0.13%~15.32%。本实验表明，混合酸敞开酸溶法适用于测定地质样品中的稀土元素，偏硼酸锂碱熔法不仅适用于测定地质样品中的稀土元素及铌钽锆铪，也适用于测定如古老高压变质岩石及铝含量高的样品中的铌钽锆铪。
- 多金属矿 /
- 稀土元素 /
- 铌 /
- 钽 /
- 锆 /
- 铪 /
- 氢氟酸-硝酸-硫酸敞开酸溶 /
- 偏硼酸锂碱熔 /
- 氢氧化钠 /
- 电感耦合等离子体质谱法
Abstract: BACKGROUNDMixed acid open acid dissolution and alkali fusion methods are the two main dissolution methods for determination of rare earth and refractory elements in geological samples by inductively coupled plasma-mass spectrometry (ICP-MS). However, the composition of geological samples is complex. For special elements and special samples, the traditional acid-dissolving method will cause incomplete digestion of some elements, which makes the measurement results inaccurate. The operation process of the alkali fusion method is cumbersome. The solution has high salinity, which can easily cause matrix interference and block the sample introduction system. OBJECTIVESTo improve the traditional four-acid and penta-acid systems in the determination of rare earth elements. METHODSThe hydrofluoric acid-nitric acid-sulfuric acid open acid solution system was used to determine the 15 rare earth elements by using the national standard material to prepare a standard curve. At the same time, the lithium metaborate alkali fusion method was improved. The sample was extracted with lithium metaborate alkali, and the solution was added to the alkaline condition by adding sodium hydroxide. The measured element was coprecipitated with lithium metaborate, and the flux was separated and filtered, and then reconstituted with nitric acid. Nineteen elements such as rare earth and lanthanum zirconium were measured. RESULTSThe relative deviations between the measured value and the certified value of the two dissolution methods were 1.09%-9.30%. The results of determination of Nb, Ta, Zr and Hf by mixed acid open dissolution method and rare earth element by lithium metaborate alkali fusion method were compared with those of another laboratory that used closed acid dissolution methods. The relative deviations between the two groups were 0.13%-15.32%. CONCLUSIONSThe mixed acid open dissolution method is suitable for the determination of rare earth elements in geological samples, whereas the lithium metaborate alkali fusion method is not only suitable for the determination of rare earth elements and Nb, Ta, Zr and Hf in geological samples, but also for the determination of Nb, Ta, Zr and Hf in ancient high pressure metamorphic rock samples and the sample with a high Al content.
- polymetallic ores /
- rare earth elements /
- Nb /
- Ta /
- Zr /
- Hf /
- HF-HNO₃-H₂SO₄ open dissolution /
- lithium metaborate alkali fusion /
- sodium hydroxide /
- inductively coupled plasma-mass spectrometry

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表 1 混合酸敞开酸溶法的测定结果

Table 1. Analytical results of elements treated with the mixed acid open dissolution

元素	GBW07328					GBW07107					GBW07450					GBW07311
元素	认定值 (μg/g)	分步骤加酸法 (μg/g)	直接加混合酸法 (μg/g)	混合酸溶解两次法 (μg/g)	直接加混合酸相对误差 (%)	认定值 (μg/g)	分步骤加酸法 (μg/g)	直接加混合酸法 (μg/g)	混合酸溶解两次法 (μg/g)	直接加混合酸相对误差 (%)	认定值 (μg/g)	分步骤加酸法 (μg/g)	直接加混合酸 (μg/g)	混合酸溶解两次法 (μg/g)	直接加混相对误差 (%)	认定值 (μg/g)	分步骤加酸法 (μg/g)	直接加混合酸 (μg/g)	混合酸溶解两次法 (μg/g)	直接加混合酸相对误差 (%)
Y	15.3	12.1	11.9	12.5	-22.2	26	20.4	18.9	22.8	-27.3	27	21.1	21.7	24.3	-19.6	43	38.2	37.1	38.9	-13.7
La	32.5	28.4	27.0	28.4	-16.9	62	53.6	53.7	55.2	-13.4	26	21.4	22.7	25.5	-12.7	30	24.4	23.2	27.1	-22.7
Ce	60.5	60.2	60.5	60.3	0.0	109	123	108	109	-0.9	52	48.1	52.4	53.4	0.8	58	52.5	54.1	57.1	-6.7
Pr	6.94	6.69	6.68	6.72	-3.7	13.6	12.6	12.9	13.2	-5.1	6.4	5.55	6.23	6.34	-2.7	7.4	6.18	7.06	7.19	-4.6
Nd	25.7	26.1	26.6	25.7	3.5	48	52.8	53.5	54.9	11.5	25	24.7	27.5	26.5	10.0	27	26.6	25.4	26.4	-5.9
Sm	4.49	4.64	4.75	4.39	5.8	8.4	8.37	8.32	8.41	-1.0	5.1	5.11	5.37	5.86	5.3	6.2	6.27	6.17	6.30	-0.5
Eu	0.96	0.847	0.853	0.867	-11.1	1.7	1.61	1.67	1.71	-1.8	1.13	0.966	1.02	1.06	-9.7	0.6	0.478	0.510	0.588	-15.0
Gd	3.74	3.53	3.50	3.63	-6.4	6.7	6.90	6.87	6.93	2.5	4.7	4.55	4.81	4.97	2.3	5.9	6.07	6.07	6.04	2.9
Tb	0.54	0.432	0.441	0.461	-18.3	1.02	0.899	0.917	0.933	-10.1	0.8	0.634	0.698	0.702	-12.8	1.13	0.996	1.06	1.03	-6.2
Dy	2.94	2.81	2.71	2.85	-7.8	5.1	5.39	5.45	5.60	6.9	4.8	4.33	4.62	4.60	-3.7	7.2	7.26	7.30	7.30	1.4
Ho	0.58	0.437	0.455	0.464	-21.6	0.98	0.928	0.945	0.961	-3.6	0.98	0.785	0.819	0.838	-16.4	1.4	1.37	1.45	1.36	3.6
Er	1.64	1.46	1.43	1.49	-12.8	2.7	2.83	2.78	2.87	3.0	2.8	2.48	2.63	2.66	-6.1	4.6	4.41	4.37	4.42	-5.0
Tm	0.25	0.133	0.134	0.138	-46.4	0.43	0.302	0.328	0.324	-23.7	0.47	0.284	0.308	0.314	-34.5	0.74	0.623	0.631	0.722	-14.7
Yb	1.63	1.41	1.40	1.46	-14.1	2.6	2.59	2.61	2.69	0.4	3	2.42	2.55	2.59	-15.0	5.1	4.90	5.07	5.07	-0.6
Lu	0.25	0.124	0.137	0.179	-45.2	0.41	0.33	0.31	0.32	-24.4	0.47	0.286	0.304	0.306	-35.3	0.78	0.643	0.660	0.754	-15.4
Nb	10.5	5.79	6.02	7.20	-42.7	14.3	10.1	9.19	11.3	-35.7	11.4	9.28	8.96	9.25	-21.4	25	19.7	22.8	22.2	-8.8
Ta	1.2	0.667	1.06	0.924	-11.7	1	0.436	0.488	0.722	-51.2	0.84	0.582	0.617	0.514	-26.5	5.7	5.31	5.33	5.44	-6.5
Zr	184	108	115	128	-37.5	96	47.3	53.2	57.7	-44.6	190	162	157	164	-17.4	153	132	138	140	-9.8
Hf	5.5	1.99	2.02	2.65	-63.3	2.9	1.45	1.36	1.62	-53.1	5.5	3.22	3.58	4.22	-34.9	5.4	4.76	4.43	4.52	-18.0

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表 2 采用国家一级标准物质制作标准曲线的测定结果

Table 2. Analytical results of elements using the national standard reference materials as standard curve

元素	GBW07328			GBW07107			GBW07450			GBW07311
元素	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)
⁸⁹Y	15.3	14.9	0.012	26	27.1	0.018	27	26.4	0.010	43	43.2	0.002
¹³⁹La	32.5	32.7	0.003	62	63.1	0.008	26	25.9	0.002	30	29.6	0.006
¹⁴⁰Ce	60.5	60.4	0.001	109	109	0.001	52	53.1	0.009	58	57.9	0.001
¹⁴¹Pr	6.94	6.84	0.006	13.6	13.6	0.001	6.4	6.39	0.000	7.4	7.51	0.007
¹⁴⁶Nd	25.7	25.7	0.001	48	49.0	0.009	25	26.0	0.017	27	27.0	0.000
¹⁴⁷Sm	4.49	4.50	0.000	8.4	8.41	0.001	5.1	5.14	0.004	6.2	6.31	0.007
¹⁵³Eu	0.96	0.957	0.001	1.7	1.71	0.003	1.13	1.09	0.014	0.6	0.613	0.009
¹⁵⁷Gd	3.74	3.68	0.007	6.7	6.80	0.006	4.7	4.76	0.006	5.9	6.04	0.010
¹⁵⁹Tb	0.54	0.56	0.017	1.02	0.989	0.013	0.8	0.782	0.010	1.13	1.03	0.012
¹⁶³Dy	2.94	2.95	0.002	5.1	5.10	0.000	4.8	4.74	0.006	7.2	7.31	0.006
¹⁶⁵Ho	0.58	0.591	0.008	0.98	0.975	0.002	0.98	0.988	0.004	1.4	1.39	0.005
¹⁶⁶Er	1.64	1.64	0.000	2.7	2.87	0.027	2.8	2.76	0.006	4.6	4.59	0.001
¹⁶⁹Tm	0.25	0.248	0.003	0.43	0.423	0.007	0.47	0.474	0.004	0.74	0.725	0.009
¹⁷²Yb	1.63	1.65	0.006	2.6	2.68	0.013	3	2.99	0.001	5.1	5.06	0.004
¹⁷⁵Lu	0.25	0.249	0.002	0.41	0.409	0.001	0.47	0.486	0.015	0.78	0.75	0.015

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表 3 偏硼酸锂作为熔剂的测定结果

Table 3. Analytical results of elements using lithium metaborate as flux

元素	GBW07328			GBW07107			GBW07450			GBW07311
元素	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC
⁸⁹Y	15.3	16.2	0.025	26	27.1	0.018	27	27.8	0.013	43	42.8	0.002
¹³⁹La	32.5	33.5	0.013	62	64.2	0.015	26	27.3	0.022	30	31.3	0.018
¹⁴⁰Ce	60.5	61.8	0.009	109	110	0.005	52	51.3	0.006	58	56.3	0.013
¹⁴¹Pr	6.94	6.72	0.014	13.6	11.3	0.080	6.4	6.27	0.009	7.4	7.61	0.012
¹⁴⁶Nd	25.7	24.4	0.023	48	46.5	0.014	25	27.3	0.039	27	28.4	0.023
¹⁴⁷Sm	4.49	4.61	0.012	8.4	8.56	0.008	5.1	5.02	0.007	6.2	6.11	0.006
¹⁵³Eu	0.96	0.949	0.005	1.7	1.78	0.021	1.13	1.12	0.004	0.6	0.623	0.016
¹⁵⁷Gd	3.74	3.86	0.014	6.7	6.78	0.005	4.7	4.39	0.029	5.9	6.18	0.020
¹⁵⁹Tb	0.54	0.561	0.017	1.02	1.14	0.049	0.8	0.822	0.012	1.13	1.32	0.068
¹⁶³Dy	2.94	3.07	0.018	5.1	5.36	0.022	4.8	4.98	0.016	7.2	7.44	0.014
¹⁶⁵Ho	0.58	0.596	0.012	0.98	1.01	0.014	0.98	0.999	0.008	1.4	1.33	0.023
¹⁶⁶Er	1.64	1.66	0.004	2.7	2.59	0.017	2.8	2.92	0.018	4.6	4.77	0.015
¹⁶⁹Tm	0.25	0.233	0.031	0.43	0.411	0.020	0.47	0.455	0.014	0.74	0.772	0.018
¹⁷²Yb	1.63	1.64	0.003	2.6	2.78	0.028	3	2.88	0.018	5.1	5.14	0.004
¹⁷⁵Lu	0.25	0.238	0.021	0.41	0.424	0.015	0.47	0.488	0.016	0.78	0.733	0.027
⁹³Nb	10.5	4.72	0.347	14.3	8.53	0.224	11.4	6.16	0.267	25	11.4	0.343
¹⁸¹Ta	1.2	0.812	0.170	0.9	0.657	0.137	0.84	0.431	0.290	5.7	2.74	0.318
⁹⁰Zr	184	98.2	0.273	96	45.1	0.328	190	97.5	0.290	153	68.2	0.351
¹⁷⁸Hf	5.5	2.99	0.265	2.9	1.08	0.430	5.5	2.14	0.409	5.4	3.27	0.218

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表 4 偏硼酸锂为熔剂时加氢氧化钠碱化后的测定结果

Table 4. Analytical results of elements using lithium metaborate as flux and adding sodium hydroxide to alkalization

元素	GBW07328			GBW07107			GBW07450			GBW07311
元素	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC	认定值 (μg/g)	测定值 (μg/g)	ΔlgC
⁸⁹Y	15.3	14.8	0.014	26	26.3	0.005	27	27.4	0.006	43	41.8	0.012
¹³⁹La	32.5	33.7	0.016	62	61.3	0.005	26	24.8	0.020	30	28.5	0.023
¹⁴⁰Ce	60.5	58.6	0.014	109	107	0.007	52	50.3	0.014	58	57.8	0.002
¹⁴¹Pr	6.94	6.74	0.013	13.6	14.8	0.036	6.4	6.51	0.008	7.4	7.65	0.015
¹⁴⁶Nd	25.7	26.2	0.009	48	50.2	0.020	25	24.9	0.000	27	26.5	0.007
¹⁴⁷Sm	4.49	4.34	0.015	8.4	8.33	0.004	5.1	5.21	0.010	6.2	6.41	0.014
¹⁵³Eu	0.96	0.962	0.001	1.7	1.67	0.007	1.13	1.23	0.036	0.6	0.631	0.022
¹⁵⁷Gd	3.74	3.88	0.016	6.7	6.78	0.005	4.7	4.54	0.015	5.9	6.05	0.011
¹⁵⁹Tb	0.54	0.519	0.017	1.02	0.992	0.012	0.8	0.778	0.012	1.13	1.14	0.005
¹⁶³Dy	2.94	2.72	0.033	5.1	5.32	0.018	4.8	4.76	0.004	7.2	7.12	0.005
¹⁶⁵Ho	0.58	0.566	0.011	0.98	0.973	0.003	0.98	0.973	0.003	1.4	1.44	0.012
¹⁶⁶Er	1.64	1.71	0.018	2.7	2.55	0.024	2.8	2.93	0.020	4.6	4.75	0.014
¹⁶⁹Tm	0.25	0.233	0.029	0.43	0.452	0.022	0.47	0.455	0.014	0.74	0.731	0.005
¹⁷²Yb	1.63	1.67	0.011	2.6	2.76	0.027	3	2.87	0.019	5.1	5.38	0.023
¹⁷⁵Lu	0.25	0.273	0.038	0.41	0.408	0.002	0.47	0.462	0.007	0.78	0.765	0.008
⁹³Nb	10.5	9.38	0.049	14.3	13.8	0.016	11.4	10.9	0.020	25	24.3	0.013
¹⁸¹Ta	1.2	1.30	0.035	0.9	0.879	0.010	0.84	0.794	0.024	5.7	5.54	0.013
⁹⁰Zr	184	187	0.008	96	95.8	0.001	190	194	0.010	153	152	0.003
¹⁷⁸Hf	5.5	5.25	0.021	2.9	2.86	0.007	5.5	5.33	0.014	5.4	5.37	0.002

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表 5 方法检出限

Table 5. Detection limit of the method

元素	检出限(μg/g)
元素	混合酸敞开酸溶法	改进的偏硼酸锂碱熔法
⁸⁹Y	0.101	0.038
¹³⁹La	0.095	0.087
¹⁴⁰Ce	0.163	0.519
¹⁴¹Pr	0.018	0.032
¹⁴⁶Nd	0.084	0.066
¹⁴⁷Sm	0.014	0.037
¹⁵³Eu	0.003	0.023
¹⁵⁷Gd	0.003	0.106
¹⁵⁹Tb	0.01	0.085
¹⁶³Dy	0.009	0.044
¹⁶⁵Ho	0.058	0.09
¹⁶⁶Er	0.007	0.033
¹⁶⁹Tm	0.002	0.087
¹⁷²Yb	0.005	0.036
¹⁷⁵Lu	0.001	0.072
⁹³Nb	-	0.221
¹⁸¹Ta	-	0.073
⁹⁰Zr	-	0.926
¹⁷⁸Hf	-	0.063

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表 6 混合酸敞开酸溶和偏硼酸锂碱熔法的准确度和精密度

Table 6. Accuracy and precision tests of the mixed acid open dissolution method and lithium metaborate alkali fusion method

元素	混合酸敞开酸溶法
	GBW07328				GBW07107				GBW07450				GBW07311
	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)
⁸⁹Y	15.3	14.7	0.017	1.14	26	24.6	0.024	3.11	27	25.7	0.021	2.26	43	45.7	0.026	1.97
¹³⁹La	32.5	30.1	0.033	7.91	62	60.9	0.008	4..26	26	26.9	0.015	1.80	30	28.6	0.021	2.21
¹⁴⁰Ce	60.5	63.2	0.019	6.32	109	113	0.016	2.16	52	54.7	0.022	2.16	58	56.9	0.008	1.73
¹⁴¹Pr	6.94	6.78	0.010	6.64	13.6	13.2	0.013	4.57	6.4	6.29	0.008	1.93	7.4	7.19	0.013	1.46
¹⁴⁶Nd	25.7	24.1	0.028	4.37	48	47.1	0.008	1.58	25	23.6	0.025	5.63	27	25.6	0.023	1.92
¹⁴⁷Sm	4.49	4.62	0.012	8.85	8.4	8.16	0.013	3.72	5.1	5.24	0.012	3.71	6.2	6.06	0.010	1.47
¹⁵³Eu	0.96	0.993	0.015	2.57	1.7	1.57	0.035	7.96	1.13	1.23	0.037	4.30	0.6	0.717	0.077	2.95
¹⁵⁷Gd	3.74	3.56	0.021	7.92	6.7	6.83	0.008	4.34	4.7	4.59	0.010	2.25	5.9	5.76	0.010	2.24
¹⁵⁹Tb	0.54	0.522	0.015	3.84	1.02	0.984	0.016	4.62	0.8	0.773	0.015	3.16	1.13	1.21	0.030	1.14
¹⁶³Dy	2.94	2.73	0.032	6.26	5.1	5.24	0.012	2.93	4.8	4.67	0.012	2.81	7.2	7.04	0.010	1.72
¹⁶⁵Ho	0.58	0.551	0.022	8.24	0.98	0.952	0.013	4.29	0.98	1.06	0.034	4.94	1.4	1.32	0.026	1.57
¹⁶⁶Er	1.64	1.61	0.008	7.22	2.7	2.56	0.023	4.40	2.8	2.89	0.014	4.64	4.6	4.71	0.010	3.08
¹⁶⁹Tm	0.25	0.234	0.029	2.43	0.43	0.417	0.013	5.51	0.47	0.493	0.021	5.76	0.74	0.729	0.007	2.57
¹⁷²Yb	1.63	1.60	0.008	2.15	2.6	2.49	0.019	4.17	3	2.82	0.026	4.19	5.1	4.84	0.023	1.09
¹⁷⁵Lu	0.25	0.227	0.042	2.59	0.41	0.424	0.015	4.92	0.47	0.492	0.020	2.63	0.78	0.746	0.019	3.56
元素	偏硼酸锂碱熔法
	GBW07328				GBW07107				GBW07450				GBW07311
	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)	认定值 (μg/g)	测定平均值 (μg/g)	ΔlgC	RSD (%)
⁸⁹Y	15.3	14.7	0.017	1.46	26	25.4	0.010	2.71	27	25.7	0.021	2.51	43	41.6	0.014	4.40
¹³⁹La	32.5	31.1	0.019	2.52	62	60.6	0.010	3.94	26	25.4	0.010	1.74	30	31.7	0.024	2.62
¹⁴⁰Ce	60.5	59.1	0.011	1.27	109	105	0.016	2.77	52	49.5	0.021	3.07	58	59.3	0.010	1.95
¹⁴¹Pr	6.94	6.62	0.021	1.76	13.6	14.4	0.025	3.82	6.4	6.28	0.008	2.19	7.4	7.51	0.006	1.41
¹⁴⁶Nd	25.7	25.9	0.003	4.52	48	46.1	0.018	2.81	25	27.3	0.038	2.50	27	26.3	0.011	1.79
¹⁴⁷Sm	4.49	4.37	0.012	1.97	8.4	8.07	0.017	4.73	5.1	5.33	0.019	6.48	6.2	6.08	0.008	3.77
¹⁵³Eu	0.96	0.906	0.025	6.49	1.7	1.75	0.013	1.79	1.13	1.21	0.030	3.63	0.6	0.571	0.022	2.23
¹⁵⁷Gd	3.74	3.77	0.003	3.73	6.7	6.46	0.016	2.08	4.7	4.58	0.011	2.97	5.9	6.23	0.024	5.01
¹⁵⁹Tb	0.54	0.556	0.013	1.53	1.02	0.944	0.034	1.17	0.8	0.831	0.017	1.81	1.13	1.24	0.040	4.33
¹⁶³Dy	2.94	3.12	0.026	4.63	5.1	5.26	0.013	5.17	4.8	4.56	0.022	3.41	7.2	7.02	0.011	2.19
¹⁶⁵Ho	0.58	0.543	0.029	8.52	0.98	0.947	0.015	7.90	0.98	1.02	0.019	2.92	1.4	1.51	0.033	1.75
¹⁶⁶Er	1.64	1.62	0.005	3.79	2.7	2.74	0.007	6.46	2.8	2.84	0.006	6.09	4.6	4.68	0.007	3.10
¹⁶⁹Tm	0.25	0.262	0.020	2.58	0.43	0.449	0.019	2.60	0.47	0.445	0.024	2.33	0.74	0.771	0.018	1.29
¹⁷²Yb	1.63	1.6	0.008	5.71	2.6	2.82	0.035	4.68	3	3.16	0.023	4.83	5.1	5.18	0.007	3.03
¹⁷⁵Lu	0.25	0.235	0.027	3.08	0.41	0.441	0.032	5.22	0.47	0.459	0.010	2.98	0.78	0.792	0.007	2.24
⁹³Nb	10.5	11.2	0.028	2.25	14.3	13.1	0.038	4.70	11.4	10.7	0.028	9.45	25	26.1	0.019	1.33
¹⁸¹Ta	1.2	1.22	0.007	5.82	0.9	0.921	0.010	8.72	0.84	0.822	0.009	9.73	5.7	5.82	0.009	1.80
⁹⁰Zr	184	179	0.012	2.12	96	92.7	0.015	6.71	190	197	0.016	3.45	153	147	0.017	4.37
¹⁷⁸Hf	5.5	5.36	0.011	9.30	2.9	2.63	0.043	5.60	5.5	5.28	0.018	5.93	5.4	4.89	0.043	5.81

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敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪

1. 中国人民武装警察部队黄金部队第五支队, 陕西 西安 710100 2. 甘肃智广地质工程勘察设计有限公司, 甘肃 兰州 730010

作者简介: 门倩妮, 硕士, 从事地质样品的分析测试工作。E-mail:menqianni-6019@163.com

Determination of Rare Earth Elements and Nb, Ta, Zr, Hf in Polymetallic Mineral Samples by Inductively Coupled Plasma-Mass Spectrometry Coupled with Open Acid Dissolution and Lithium Metaborate Alkali Fusion

1. No.5 Gold Geological Party, Chinese People's Armed Police Force, Xi'an 710100, China 2. Gansu Zhiguang Geological Engineering Survey and Design Co. LTD., Lanzhou 730010, China

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中国人民武装警察部队黄金部队第五支队, 陕西西安 710100

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甘肃智广地质工程勘察设计有限公司, 甘肃兰州 730010

1.
No.5 Gold Geological Party, Chinese People's Armed Police Force, Xi'an 710100, China

2.
Gansu Zhiguang Geological Engineering Survey and Design Co. LTD., Lanzhou 730010, China