贵州织金磷矿床中离子吸附型稀土的存在及初步定量

段凯波; 王登红; 熊先孝; 连卫; 高鹏; 王英林; 张杨

贵州织金磷矿床中离子吸附型稀土的存在及初步定量

1.
中化地质矿山总局化工地质调查总院, 北京 100013

2.
中国地质科学院矿产资源研究所, 北京 100037

基金项目:
中国地质大调查项目-我国三稀金属资源战略调查计划项目(1212011220803)

详细信息

作者简介: 段凯波，博士，高级工程师，主要从事沉积矿床地质学研究。E-mail: kaiboduan@aliyun.com

中图分类号: O614.33

收稿日期: 2013-07-02

录用日期: 2013-08-17

A Review of a Preliminary Quantitative Study and Genetic Analysis for Rare Earth Elements of Ionic Adsorption State in Phosphate Ore Deposit in Zhijin, Guizhou Province

1.
General Institute of Chemical Geolog Survey, China Chemical Geology and Mine Bureau, Beijing 100013, China

2.
Institute of Mineral Resources, Chinese Academy of Geological Sciences, Beijing 100037, China

Received Date: 02 July 2013

Accepted Date: 17 August 2013

摘要

摘要: 近年来研究表明贵州织金磷块岩矿床中伴生丰富的稀土主要以类质同象形式存在，其主要依据为稀土总量与磷含量的正相关性，而对独立稀土矿物与离子吸附型稀土两种赋存状态的认识目前仍然不清楚。本文通过利用电感耦合等离子体质谱(ICP-MS)稀土元素全分析、磷钼酸喹啉重量法磷分析、岩矿鉴定与实验室选矿试验等方法对该矿床中伴生稀土的赋存规律进行了研究。岩矿鉴定表明矿石中主要矿物成分为胶磷矿并含少量黏土矿物，但未发现独立的稀土矿物；磷与稀土全分析显示稀土总量及各分量都与磷含量呈正相关，从而验证并进一步表明了稀土主要以类质同象形式存在于胶磷矿中。通过研究原矿经选别后稀土与磷在精矿、尾矿和选液(尾矿水)中的分配对比及两者的含量关系来探讨稀土的赋存规律，结果显示磷仅分配于精矿和尾矿中未发生损失，而11.98%的稀土在强电解质硫酸盐的作用下从原矿中解离出来进入了选液，推断这部分稀土在原矿中未进入矿物晶格，而是呈离子态吸附于矿物表面，初步认为漫长时限与潮湿条件下的充分风化作用以及胶磷矿与黏土矿物所充当的吸附载体发挥了作用，表明织金磷矿中稀土总量的11.98%以离子吸附状态存在。综合各分析结果，织金磷矿伴生稀土各赋存状态中类质同象占主导，未发现独立稀土矿物，而离子吸附型稀土占一定的比例，故将稀土的离子吸附形式列为仅次于类质同象的第二大赋存状态。
- 稀土磷块岩 /
- 赋存状态 /
- 独立稀土矿物 /
- 类质同象 /
- 离子吸附
Abstract: Recent studies on rare earth elements (REEs) for the Phosphate Deposit in Zhijin, Guizhou show that the occurrence state of REEs is dominated by isomorphism on the basis of the positive correlation between ∑REEs content and phosphorus content. However, the understanding for the independent REE minerals state and the ionic adsorption REE state is still not clear at present. Methods of Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) analysis for REEs, quinoline phosphomolybdate gravimetry analysis for phosphorus, rock-mineral identification and laboratory beneficiation test have been carried out for the study of REE occurrence state in the deposit. The results from rock-mineral identification show the REE-phosphate ore are composed of collophane dominantly and a small quantity of clay minerals, but no independent REEs minerals have been observed. Element content analytical results indicate a positive correlation between ΣREEs and phosphorus, and even between each single REE and phosphorus, which confirm REEs occur in collophane as isomorphism state dominantly. The REEs distribution was studied by allocation and content correlation of REEs and phosphorus in the concentration, tailings and processing solution (tailing water). As a result, phosphorus only collects in the concentrate and tailings without any loss, while 11.98% of ΣREEs dissociates from ore under the reaction of strong sulfate electrolyte and enters the processing solution. It indicated that this part of REEs was adsorbed on the surface of minerals instead of in mineral crystal lattice. 11.98% of REEs are ionic adsorption REEs. The complete weathering on the condition of eternity and moisture and adsorption carriers played by collophane and clay minerals contributed to the genesis of the ionic adsorption state REEs. In summary, the occurrence state of REEs hosted in the deposit is dominated by isomorphism and partly is in an ionic adsorption state and not an independent REE mineral. Therefore, ionic adsorption is the second primary occurrence state after the isomorphism state.
- REE-phosphate ore /
- occurrence state /
- independent REEs minerals /
- isomorphism /
- ionic adsorption

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图 1 偏光显微镜下磷块岩矿物组合特征

Figure 1.

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图 2 ΣREEs与P₂O₅含量正相关关系

Figure 2.

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图 3 Y与P₂O₅含量正相关关系

Figure 3.

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图 4 Tm与P₂O₅含量正相关关系

Figure 4.

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图 5 La与P₂O₅含量正相关关系

Figure 5.

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图 6 反浮选试验闭路流程及数据信息

Figure 6.

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表 1 磷块岩矿石的矿物组成

Table 1. Mineral composition of phosphate ore

矿物种类	含量w/%	矿物种类	含量w/%
胶磷矿	50～55	方解石	3
白云石	30～35	碳质物	2
石英、玉髓	5	金属矿物	2
黏土矿物	3

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表 2 磷块岩矿石中P₂O₅和REEs含量分析结果

Table 2. Analytical results of P₂O₅ and REEs in phosphate ores

样品编号	w/%	w/10^-6
样品编号	P₂O₅	La	Ce	Pr	Nd	Sm	Eu	Gd	Tb	Dy	Ho	Er	Tm	Yb	Lu	Y	ΣREEs	La+Ce+Nd+Y
XH-001	19.42	199.90	109.40	30.46	129.90	22.35	5.27	23.90	3.78	22.20	4.53	12.51	1.61	8.13	1.16	277.40	852.50	716.60
XH-002	33.76	432.20	222.60	60.97	257.00	42.50	10.32	47.82	7.88	44.91	9.28	25.37	3.20	15.41	2.20	582.30	1763.96	1494.10
XH-003	19.51	209.70	106.60	30.43	132.50	23.50	5.26	25.41	4.23	25.55	5.38	15.05	1.85	9.28	1.34	327.90	923.97	776.70
XH-004	21.61	254.70	129.10	37.80	164.30	28.77	6.60	31.76	5.31	31.84	6.59	17.91	2.34	11.34	1.57	405.50	1135.43	953.60
XH-005	36.90	446.50	216.70	61.17	256.60	43.17	9.93	48.68	7.96	45.98	9.56	26.13	3.20	15.95	2.24	625.00	1818.76	1544.80
XH-006	27.80	276.70	178.60	49.32	225.30	41.16	11.70	44.72	7.13	40.20	8.09	21.55	2.70	13.19	1.78	497.80	1419.94	1178.40
XH-007	31.12	316.00	153.30	43.86	187.20	32.06	7.62	37.58	6.25	36.96	7.88	22.04	2.88	13.88	1.89	513.70	1383.10	1170.20
XH-008	20.83	224.00	112.00	32.64	139.00	24.67	6.06	28.07	4.63	27.92	6.02	16.16	2.14	10.14	1.46	368.10	1003.01	843.10
XH-009	13.95	163.10	83.23	24.29	105.70	18.64	4.28	20.62	3.47	20.89	4.24	11.48	1.48	7.49	1.01	261.50	731.42	613.53
XH-010	11.32	116.00	62.21	18.00	78.63	13.60	3.23	15.04	2.55	15.28	3.12	8.57	1.11	5.50	0.78	187.70	531.33	444.54
XH-011	34.07	562.00	209.30	58.07	246.00	41.12	9.69	43.72	6.65	37.74	7.47	20.08	2.48	12.02	1.71	504.30	1762.35	1521.60
XH-012	17.68	203.00	107.50	31.71	137.20	23.72	6.11	27.06	4.39	26.02	5.38	14.70	1.87	9.06	1.20	327.10	926.03	774.80
XH-013	23.67	244.80	129.60	39.29	168.50	29.98	6.87	33.26	5.53	32.21	6.89	18.57	2.33	11.41	1.64	427.70	1158.59	970.60
XH-014	21.46	217.50	116.00	32.67	138.60	24.96	5.93	27.89	4.57	27.84	5.75	15.67	1.97	9.39	1.37	365.70	995.80	837.80
XH-015	12.51	142.00	75.82	21.94	96.41	16.84	4.13	18.66	3.16	18.71	3.99	11.03	1.45	7.61	1.05	240.00	662.81	554.23
XH-016	15.53	194.70	100.80	28.58	122.90	21.77	5.00	24.17	4.04	24.27	4.91	13.41	1.71	8.74	1.18	304.10	860.27	722.50
XH-017	15.11	194.40	101.80	28.54	121.00	22.03	5.07	24.21	4.00	23.48	4.93	13.04	1.69	8.40	1.20	300.20	853.99	717.40
XH-018	17.29	216.10	111.20	31.33	134.50	23.86	5.33	26.10	4.41	25.60	5.28	14.72	1.78	8.89	1.23	331.30	941.63	793.10
XH-019	9.77	140.50	69.90	19.70	81.04	14.37	3.53	15.96	2.78	16.24	3.43	9.36	1.24	5.83	0.83	211.00	595.71	502.44
XH-020	11.73	263.30	139.90	37.63	158.50	27.44	6.10	29.40	5.00	28.68	6.08	16.39	2.10	9.83	1.40	388.70	1120.44	950.40
XH-021	5.08	82.18	47.55	12.16	52.75	8.93	2.08	10.67	1.78	11.34	2.37	6.81	0.95	4.63	0.69	147.10	391.98	329.58
XH-022	4.50	78.52	44.74	12.38	52.93	9.18	2.21	10.35	1.78	10.40	2.19	6.20	0.87	4.05	0.62	128.10	364.52	304.29
XH-023	6.49	95.30	51.98	14.44	61.22	11.09	2.53	11.66	1.98	11.73	2.45	6.83	0.92	4.65	0.70	144.70	422.18	353.20
XH-024	6.52	82.08	53.09	14.51	63.59	11.98	3.38	13.37	2.04	11.46	2.39	6.21	0.81	4.00	0.60	135.20	404.72	333.96
XH-025	5.84	83.86	48.74	12.18	51.80	9.21	2.36	10.90	1.77	10.45	2.31	6.60	0.85	4.57	0.67	141.90	388.16	326.30
XH-026	16.18	231.60	137.80	32.62	139.70	24.24	5.95	28.04	4.59	27.48	5.88	16.31	2.10	9.57	1.34	372.90	1040.12	882.00
XH-027	9.68	128.60	70.41	19.57	83.80	14.75	3.70	16.29	2.60	15.96	3.32	9.07	1.11	5.45	0.76	200.60	575.99	483.41
XH-028	2.80	17.86	12.32	2.87	12.29	2.13	0.59	2.30	0.42	2.57	0.52	1.43	0.19	0.94	0.13	27.67	84.22	70.14
XH-029	9.04	106.10	57.76	16.05	67.63	12.35	2.87	13.25	2.23	13.20	2.78	7.67	1.05	5.15	0.72	163.50	472.30	394.99
XH-030	9.85	104.80	55.41	16.12	68.10	11.96	2.99	13.25	2.23	13.72	2.87	7.87	1.06	5.16	0.77	170.60	476.91	398.91
XH-031	13.77	144.50	80.03	22.36	94.91	17.35	4.43	18.88	2.99	17.87	3.59	9.81	1.24	5.99	0.90	220.00	644.84	539.44
XH-032	18.11	200.30	117.90	31.91	140.00	26.58	8.64	28.43	4.61	26.29	5.31	14.34	1.87	8.58	1.24	336.40	952.39	794.60
XH-033	2.34	58.57	78.04	11.62	45.62	8.30	2.28	8.06	1.38	7.74	1.58	4.54	0.64	3.91	0.61	63.77	296.65	246.00
XH-034	26.95	359.60	202.50	53.61	232.70	40.94	10.81	46.22	7.39	43.84	9.01	24.89	3.14	15.61	2.20	580.30	1632.76	1375.10
XH-035	25.25	357.40	199.60	52.83	225.30	40.34	10.20	45.91	7.35	43.24	8.90	24.26	3.05	15.39	2.17	559.00	1594.94	1341.30
XH-036	35.09	504.60	247.20	68.20	287.30	48.77	10.96	54.85	9.05	53.69	10.92	29.70	3.75	17.94	2.51	738.10	2087.55	1777.20
XH-037	15.56	184.80	101.30	27.71	120.70	21.56	5.21	22.37	3.84	21.89	4.46	12.26	1.59	7.77	1.17	279.90	816.53	686.70
XH-038	7.74	99.60	59.35	16.20	70.95	12.67	3.75	13.76	2.26	12.88	2.67	7.52	0.98	5.02	0.75	160.40	468.76	390.30
XH-039	4.75	59.84	38.95	9.90	42.99	7.58	2.68	9.17	1.49	8.67	1.92	5.49	0.67	3.43	0.49	113.00	306.27	254.78
XH-040	2.22	41.37	24.15	6.61	29.15	5.20	1.38	6.25	0.99	6.28	1.40	3.90	0.57	2.78	0.44	80.73	211.20	175.40
XH-041	34.08	385.70	200.50	54.19	223.20	34.71	8.84	35.89	5.48	29.65	5.82	16.04	2.01	9.72	1.50	415.30	1428.56	1224.70
XH-042	10.17	116.20	61.42	18.22	76.92	13.22	3.37	14.45	2.39	14.22	3.08	8.23	1.06	5.47	0.78	180.50	519.52	435.04
XH-043	24.51	308.20	147.50	43.07	184.10	30.04	6.73	32.04	5.24	30.12	6.22	16.64	2.14	10.64	1.45	589.90	1414.02	1229.70
XH-044	37.53	403.00	200.50	53.64	231.40	38.70	10.27	42.74	7.05	41.53	8.52	23.33	2.98	14.35	1.98	675.20	1755.20	1510.10
XH-045	19.32	241.70	119.40	35.19	147.30	25.35	5.97	27.05	4.57	27.32	5.75	15.71	2.02	9.68	1.35	375.70	1044.05	884.10
XH-046	15.51	178.00	92.80	25.70	107.00	17.90	3.87	19.60	3.14	18.60	3.89	10.70	1.35	6.96	1.04	248.00	738.55	625.80
XH-047	15.53	199.00	105.00	28.80	122.00	20.70	4.63	22.90	3.75	22.10	4.53	12.40	1.56	7.91	1.15	293.00	849.43	719.00
XH-048	5.57	71.30	40.50	9.77	41.30	7.15	1.67	8.30	1.42	8.74	1.94	5.39	0.72	3.69	0.55	130.00	332.44	283.10
XH-049	3.27	42.30	25.40	6.43	27.60	4.90	1.04	5.46	0.92	5.71	1.28	3.72	0.54	2.90	0.46	78.20	206.86	173.50
XH-050	32.25	369.00	194.00	50.80	212.00	35.70	9.02	38.80	6.30	37.00	7.71	20.60	2.62	12.80	1.79	606.00	1604.14	1381.00
XH-051	5.79	108.00	64.40	17.60	75.60	12.90	2.85	13.90	2.25	13.60	2.80	7.59	0.97	4.98	0.74	174.00	502.18	422.00
XH-052	2.04	42.30	25.30	6.75	28.10	5.06	1.19	5.46	0.90	5.71	1.26	3.71	0.54	3.08	0.48	74.50	204.34	170.20
XH-053	0.14	3.66	3.62	0.61	2.56	0.43	0.11	0.46	0.07	0.44	0.10	0.29	0.05	0.24	0.03	4.96	17.63	14.80
XH-054	17.74	191.00	99.70	29.00	121.00	20.90	4.64	22.50	3.71	22.20	4.75	12.80	1.64	8.10	1.18	301.00	844.12	712.70
XH-055	11.79	129.00	71.60	19.90	84.00	14.80	3.34	15.90	2.62	15.80	3.31	8.97	1.15	5.75	0.85	211.00	587.99	495.60
XH-056	12.96	165.00	107.00	25.70	111.00	19.20	5.43	20.70	3.35	20.00	4.18	11.40	1.46	7.28	1.03	273.00	775.73	656.00
XH-057	9.70	94.80	54.00	15.50	67.10	12.00	2.88	12.90	2.10	13.10	2.70	7.35	0.92	4.74	0.71	166.00	456.80	381.90
XH-058	18.90	217.00	110.00	31.30	134.00	22.50	4.88	24.40	3.94	24.20	5.01	13.80	1.77	9.20	1.34	334.00	937.34	795.00
XH-059	35.37	389.00	186.00	53.40	225.00	37.80	8.29	41.80	6.90	41.30	8.68	23.40	2.99	14.80	2.12	689.00	1730.48	1489.00
XH-060	9.19	93.30	48.90	14.50	61.60	10.70	2.32	11.30	1.90	11.30	2.39	6.56	0.87	4.36	0.68	151.00	421.68	354.80
XH-061	26.33	327.00	165.00	41.20	163.00	24.90	5.19	27.10	4.17	26.10	5.46	14.70	1.91	9.81	1.44	357.00	1173.98	1012.00

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表 3 原矿多项化学分析结果

Table 3. Chemical analytical results of main elements in ore sample

元素	含量w/%	元素	含量w/%
P₂O₅	23.39	FeO	0.075
MgO	6.01	Na₂O	0.058
CaO	44.87	K₂O	0.12
SiO₂	3.28	TiO₂	0.045
CO₂	16.35	MnO	0.058
F	2.38	SrO	0.072
Al₂O₃	0.20	酸不溶物	3.18
Fe₂O₃	1.12	烧失量	16.99

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表 4 原矿稀土全分析结果

Table 4. Analytical results of REEs in ore sample

元素	含量w/10^-6	元素	含量w/10^-6
La	285.00	Dy	27.14
Ce	140.00	Ho	5.78
Pr	40.04	Er	15.39
Nd	165.00	Tm	2.06
Sm	27.65	Yb	9.90
Eu	6.33	Lu	1.42
Gd	28.72	Y	429.00
Tb	4.76	ΣREEs	1188.19

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表 5 精矿中稀土及主要组分含量分析结果

Table 5. Analytical results of REEs and main elements in the concentrate

元素	含量w/10^-6	元素	含量w/10^-6
La	349.00	Er	18.58
Ce	197.00	Tm	2.36
Pr	54.68	Yb	11.41
Nd	227.00	Lu	1.61
Sm	36.30	Y	431.00
Eu	7.93	ΣREEs	1421.55
Gd	36.96
Tb	5.95	元素	含量w/%
Dy	34.74	P₂O₅	32.35
Ho	7.03	MgO	1.23

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表 6 尾矿中稀土及主要组分含量分析结果

Table 6. Analytical results of REEs and main elements in the tailings

元素	含量w/10^-6	元素	含量w/10^-6
La	56.90	Er	4.60
Ce	29.56	Tm	0.67
Pr	8.40	Yb	3.78
Nd	35.70	Lu	0.63
Sm	6.13	Y	88.60
Eu	1.35	ΣREEs	252.53
Gd	6.28
Tb	1.13	元素	含量w/%
Dy	7.17	P₂O₅	4.49
Ho	1.63	MgO	16.09

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表 7 试验后稀土的回收和流失

Table 7. Recovery and loss of REEs throughout beneficiation test

元素	原矿	精矿(产率67.86％)			尾矿(产率32.14％)			金属量损失w/10^-6	损失率/%
元素	含量w/10^-6	含量w/10^-6	金属量w/10^-6	回收率/%	含量w/10^-6	金属量w/10^-6	回收率/%	金属量损失w/10^-6	损失率/%
La	285.00	349.00	236.83	83.10	56.90	18.29	6.42	29.88	10.48
Ce	140.00	197.00	133.68	95.49	29.56	9.50	6.79	-3.18	-2.27
Pr	40.04	54.68	37.11	92.68	8.40	2.70	6.74	0.23	0.57
Nd	165.00	227.00	154.04	93.36	35.70	11.47	6.95	-0.51	-0.31
Sm	27.65	36.30	24.63	89.08	6.13	1.97	7.12	1.05	3.80
Eu	6.33	7.93	5.38	84.99	1.35	0.43	6.79	0.52	8.21
Gd	28.72	36.96	25.08	87.33	6.28	2.02	7.03	1.62	5.64
Tb	4.76	5.95	4.04	84.87	1.13	0.36	7.56	0.36	7.56
Dy	27.14	34.74	23.57	86.85	7.17	2.30	8.47	1.27	4.68
Ho	5.78	7.03	4.77	82.53	1.63	0.52	9.00	0.49	8.48
Er	15.39	18.58	12.61	81.94	4.60	1.48	9.62	1.30	8.45
Tm	2.06	2.36	1.60	77.67	0.67	0.22	10.68	0.24	11.65
Yb	9.90	11.41	7.74	78.18	3.78	1.21	12.22	0.95	9.60
Lu	1.42	1.61	1.09	76.76	0.63	0.20	14.08	0.13	9.15
Y	429.00	431.00	292.48	68.18	88.60	28.48	6.64	108.04	25.18
∑REEs	1188.19	1421.55	964.65	81.19	252.53	81.15	6.83	142.39	11.98

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表 8 尾矿水中稀土元素全分析结果

Table 8. Analytical results of REEs in the processing solution

元素	含量ρ/(μg·mL^-1)	元素	含量ρ/(μg·mL^-1)
La	0.011	Dy	0.002
Ce	0.005	Ho	0
Pr	0.001	Er	0
Nd	0.003	Tm	0
Sm	0.004	Yb	0.001
Eu	0	Lu	0.001
Gd	0.003	Y	0.02
Tb	0.002	ΣREEs	0.051

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表 9 精矿、尾矿与尾矿水中ΣREEs与P₂O₅的分配对比

Table 9. Correlation for allocation of ΣREEs and P₂O₅ in the concentration,tailings and processing solution

组分	原矿	精矿(产率67.86％)		尾矿(产率32.14％)		损失
组分	含量w/%	含量w/%	质量m/kg	含量w/%	质量m/kg	质量m/kg	比率/%
ΣREEs	0.118819	0.142155	0.00096465	0.025253	0.00008115	0.00014239	11.98
P₂O₅	23.39	32.35	0.2195271	4.49	0.01443086	-0.00006	0.026

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贵州织金磷矿床中离子吸附型稀土的存在及初步定量

1. 中化地质矿山总局化工地质调查总院, 北京 100013 2. 中国地质科学院矿产资源研究所, 北京 100037

作者简介: 段凯波，博士，高级工程师，主要从事沉积矿床地质学研究。E-mail: kaiboduan@aliyun.com

A Review of a Preliminary Quantitative Study and Genetic Analysis for Rare Earth Elements of Ionic Adsorption State in Phosphate Ore Deposit in Zhijin, Guizhou Province

1. General Institute of Chemical Geolog Survey, China Chemical Geology and Mine Bureau, Beijing 100013, China 2. Institute of Mineral Resources, Chinese Academy of Geological Sciences, Beijing 100037, China

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1.
中化地质矿山总局化工地质调查总院, 北京 100013

2.
中国地质科学院矿产资源研究所, 北京 100037

1.
General Institute of Chemical Geolog Survey, China Chemical Geology and Mine Bureau, Beijing 100013, China

2.
Institute of Mineral Resources, Chinese Academy of Geological Sciences, Beijing 100037, China