磷矿石化学成分分析标准物质研制

曾美云; 刘金; 邵鑫; 邹棣华

doi:10.15898/j.cnki.11-2131/td.201705170082

磷矿石化学成分分析标准物质研制

中国地质调查局武汉地质调查中心, 湖北武汉 430205

基金项目:
中国地质调查局矿评专项（12120113022200）

详细信息

作者简介: 曾美云, 硕士, 高级工程师, 从事岩矿测试及标准化研究工作。E-mail:ld_2002@sina.com

中图分类号: P578.92;TQ421.31

收稿日期: 2017-05-17

修回日期: 2017-09-08

录用日期: 2017-10-20

Preparation of Phosphate Ore Reference Materials for Chemical Composition Analysis

Wuhan Center of Geological Survey, China Geological Survey, Wuhan 430205, China

Received Date: 17 May 2017

Revised Date: 08 September 2017

Accepted Date: 20 October 2017

摘要

摘要: 磷矿的开发与综合利用不仅需要分析磷等主要元素，也需要准确地测定稀土元素和微量元素。分析测试过程需要含量适中、定值组分全的磷矿石标准物质进行质量监控，国内外现有的磷矿石标准物质无论是从定值指标还是含量梯度范围等方面均无法满足此需求。本文研制了4个不同类型磷矿石成分分析标准物质。样品采集自河北张家口钒山磷矿、贵州织金新华磷矿、云南昆阳磷矿、湖北神农架火炼坡磷矿4个典型矿区，其中张家口钒山磷矿和织金新华磷矿为含稀土的磷矿。检验结果表明样品的均匀性、稳定性良好；通过11家实验室协作定值，定值元素包括造岩主量元素、稀土元素和痕量元素共37项，其中3个组分为参考值，其余均给出标准值和不确定度。4个磷矿石标准物质形成了一个从边界品位、工业品位到磷精矿较为完整的含量系列，P₂O₅的含量分别为10.57%、18.91%、27.78%、39.40%，稀土元素总量分别为0.16%、0.11%、0.032%、0.0083%，可满足磷矿勘查、评价和综合利用开发中对标准物质的需求。
- 磷矿石 /
- 标准物质 /
- 均匀性 /
- 稳定性 /
- 标准值
Abstract: For the development and comprehensive utilization of phosphate ore it is not only necessary to analyze the main elements such as phosphorus, but it is also necessary to determine accurately the rare earth, trace and other elements. Phosphate Ore Reference Materials (PORMs) with numbers of components and suitable contents can be used for quality control during analysis. However, available PORMs in China and abroad do no meet the requirements in terms of the element contents and the content range. Four different types of PORMs have been developed and are described in this study. The samples of phosphate ores were collected from the Zhangjiakou Fanshan phosphate mine in Hebei province, Xinhua phosphate mine in Zhijin of Guizhou Province, Kunyang phosphate mine in Yunnan Province, and Huolian phosphate mine in Shennongjia of Hubei Province. Zhangjiakou Fanshan phosphate mine and Xinhua phosphate mine are rich in rare earth elements (REEs). Four samples were homogeneous and stable. The results from 11 laboratories were combined to confirm certified values and uncertainty of 37 components, which include major elements, REEs, and trace elements. Three components were taken as reference values and the rest were characterized as certified values. The four PORMs cover a complete content series from cut-off grade, production-grade, to phosphate concentrate with P₂O₅ contents of 10.57%, 18.91%, 27.78% and 39.40%, respectively, and the total REEs contents of 0.16%, 0.11%, 0.032% and 0.0083%, respectively. The developed PORMs meet the requirements for exploration, evaluation, and comprehensive utilization of phosphate ores.
- phosphate ore /
- reference materials /
- uniformity /
- stability /
- certified values

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表 1 样品矿物组成和结构特征

Table 1. Mineral composition and structural characteristics of the samples

样品编号	采样地点	岩性描述	矿物组成	P₂O₅品位
G-1	河北矾山磷矿区	深灰色条纹状超基性-碱性岩 (岩浆岩型)	磷灰石50%，金属矿物30%，角闪石10%，黑云母5%，榍石1%，绿泥石少量(金属矿物有：磁铁矿、黄铁矿、磁黄铁矿、黄铜矿、褐铁矿)	10%~11% (四级品)
G-2	贵州织金新华磷矿区	浅灰色块状海相沉积磷块岩 (沉积型)	胶磷矿50%，白云石35%，方解石10%，褐铁矿2%，石英3%，白云母少量	18%~20% (三级品)
G-3	云南昆阳磷矿区	深灰色层状海相沉积磷块岩 (沉积型)	胶磷矿30%，白云石50%，褐铁矿5%，石英5%，方解石5%，白云母2%	27%~28% (二级品)
G-4	湖北神农架火炼坡磷矿区	乳白色层状海相沉积磷块岩 (沉积型)	胶磷矿75%，方解石15%，白云石5%，石英3%，白云母2%	39%~40% (一级品)

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表 2 磷矿石样品粒度分布

Table 2. Grain distribution of phosphate rock samples

样品粒径 (μm)	G-1		G-2		G-3		G-4
样品粒径 (μm)	区间百分含量(%)	累积百分含量(%)	区间百分含量(%)	累积百分含量(%)	区间百分含量(%)	累积百分含量(%)	区间百分含量(%)	累积百分含量(%)
1.00~1.30	23.42	23.42	22.51	22.51	19.05	19.05	24.12	24.12
1.30~2.50	14.67	38.09	12.96	35.47	12.59	31.64	13.99	38.11
2.50~5.00	17.99	56.08	13.84	49.31	13.45	45.09	12.78	50.89
5.00~6.50	7.40	63.48	5.72	55.03	5.71	50.8	5.00	55.89
6.50~10.00	11.47	74.95	9.12	64.15	10.22	61.02	8.09	63.98
10.00~13.00	6.17	81.12	5.61	69.76	7.20	68.22	5.25	69.23
13.00~18.00	6.65	87.77	7.34	77.1	9.23	77.45	6.57	75.8
18.00~20.00	1.70	89.47	2.39	79.49	2.99	80.44	2.04	77.84
20.00~23.00	1.75	91.22	3.10	82.59	3.94	84.38	2.55	80.39
23.00~28.00	1.75	92.97	4.28	86.87	5.32	89.7	3.37	83.76
28.00~32.00	1.18	94.15	2.95	89.82	3.30	93.0	2.29	86.05
32.00~38.00	1.89	96.04	3.80	93.62	3.39	96.39	3.05	89.1
38.00~45.00	2.00	98.04	3.33	96.95	2.21	98.6	3.16	92.26
45.00~53.00	1.21	99.25	1.92	98.87	0.94	99.54	2.94	95.2
53.00~63.00	0.57	99.82	0.86	99.73	0.38	99.92	2.60	97.8
63.00~75.00	0.15	99.97	0.23	99.96	0.08	100	1.49	99.29

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表 3 均匀性检验结果

Table 3. Analytical results of the homogeneity test

元素	G-1			G-2			G-3			G-4
元素	含量测定平均值	RSD (%)	F	含量测定平均值	RSD (%)	F	含量测定平均值	RSD (%)	F	含量测定平均值	RSD (%)	F
P₂O_5*	10.5	0.64	1.03	18.6	0.67	1.00	27.5	0.62	1.01	39.5	0.77	1.00
SiO₂^*	29.7	0.84	1.01	2.95	1.21	1.01	11.1	1.00	1.02	1.62	2.54	1.15
TFe₂O₃^*	15.3	0.93	1.16	0.676	2.02	1.06	0.525	1.84	1.19	0.195	2.11	1.34
CaO^*	24.3	0.63	1.08	40.6	0.70	1.00	43.4	0.45	1.00	54.0	0.69	1.03
MgO^*	6.78	1.12	1.08	10.1	1.08	1.00	3.41	1.09	1.04	0.444	1.09	1.10
TiO₂^*	1.80	0.73	1.34	0.022	4.77	1.50	0.040	2.58	1.42	0.080	1.69	1.35
MnO^*	0.151	1.21	1.12	0.066	1.97	1.33	0.035	1.57	1.15	0.002	3.77	1.12
K₂O^*	2.52	1.01	1.06	0.096	1.71	1.03	0.488	1.75	1.11	0.165	1.08	1.51
Na₂O^*	0.435	1.53	1.19	0.096	1.65	1.83	0.279	2.22	1.03	0.100	1.57	1.57
SrO^*	0.253	1.36	1.09	0.054	3.23	1.19	0.095	1.22	1.25	0.054	1.47	1.21
S^*	0.472	1.52	1.27	0.045	2.48	1.46	0.130	2.57	1.39	0.047	4.02	1.26
F^*	0.557	2.16	1.01	1.83	1.99	1.09	2.59	2.08	1.08	3.09	1.66	1.14
U	2.00	4.66	1.20	11.8	3.26	1.02	15.4	2.02	1.04	6.16	1.57	1.02
La	224	2.98	1.03	192	2.04	1.00	49.0	2.51	1.00	16.6	3.36	1.01
Ce	518	2.74	1.01	102	2.10	1.02	39.9	3.97	1.00	13.2	3.76	1.00
Pr	72.9	2.55	1.01	31.3	2.59	1.00	8.12	2.94	1.01	2.57	4.11	1.01
Nd	335	1.54	1.03	136	2.15	1.04	32.7	2.77	1.01	11.5	4.13	1.01
Sm	59.6	4.08	1.02	25.5	3.30	1.03	5.96	3.93	1.03	2.10	2.91	1.02
Gd	41.2	4.79	1.02	27.1	4.06	1.01	7.13	3.85	0.80	2.11	2.20	1.02
Dy	18.9	3.68	1.11	26.4	3.79	1.03	7.32	3.65	1.07	1.93	3.43	1.01
Y	65.9	4.02	1.01	298	2.84	1.02	90.5	2.07	1.01	15.0	3.06	1.01
注：表中带“*”成分的测定平均值单位为10^-2，其他成分的测定平均值单位为10^-6。

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表 4 长期稳定性检验结果

Table 4. Analytical results of the long-term stability test

元素	G-1			G-2			G-3			G-4
元素	平均值	b₁	t_0.05×s(b₁)	平均值	b₁	t_0.05×s(b₁)	平均值	b₁	t_0.05×s(b₁)	平均值	b₁	t_0.05×s(b₁)
P₂O₅^*	10.6	0.0013	0.0072	18.6	0.0012	0.0013	27.5	0.0004	0.0135	39.5	0.0008	0.0110
SiO₂^*	29.7	-0.0038	0.0131	2.82	0.0004	0.0101	11.1	0.0001	0.0096	1.59	0.0018	0.0031
TFe₂O₃^*	15.1	0.0031	0.0137	0.689	-0.0007	0.0012	0.559	-0.0001	0.0015	0.165	0.0002	0.0004
CaO^*	24.1	-0.0030	0.0090	40.8	0.0028	0.0182	43.5	0.0001	0.0035	54.1	0.0060	0.0222
MgO^*	6.61	-0.00004	0.0065	10.1	-0.0009	0.0113	3.42	0.0012	0.0030	0.447	-0.0001	0.0006
TiO₂^*	1.79	-0.0004	0.0017	0.022	0.0001	0.0003	0.041	0.00007	0.0004	0.081	0.00018	0.00019
MnO^*	0.143	0.0001	0.0004	0.065	0.0001	0.0001	0.036	-0.00001	0.0001	0.002	-0.00002	0.00004
K₂O^*	2.53	-0.00001	0.0037	0.099	0.00005	0.0001	0.479	-0.0008	0.0015	0.172	0.0001	0.0002
Na₂O^*	0.431	0.0005	0.0010	0.093	-0.00001	0.0002	0.274	0.0003	0.0009	0.1	-0.0001	0.0003
SrO^*	0.255	0.00012	0.00014	0.054	0.00001	0.0001	0.096	0.00004	0.0002	0.054	0.0001	0.0002
S^*	0.454	-0.0007	0.0033	0.04	0.0002	0.0003	0.138	0.0005	0.0018	0.048	0.0002	0.0004
F^*	0.58	-0.0002	0.0008	1.78	0.0023	0.0044	2.53	0.0016	0.0093	3.13	0.0051	0.0104
U	2.19	-0.0001	0.0044	11.7	0.0058	0.0336	15.6	-0.0003	0.0014	6.09	0.0001	0.0029
La	224	0.1390	0.2622	191	0.1094	0.1862	49.3	0.0900	0.1412	16.6	0.0101	0.0162
Ce	526	0.1347	0.3563	103	-0.0322	0.1004	40.2	-0.0694	0.1014	13.6	-0.0116	0.0127
Pr	73.6	0.0264	0.0514	30.4	0.0113	0.0586	8.1	-0.0022	0.0178	2.57	0.0035	0.0078
Nd	337	0.0381	0.2649	136	-0.0622	0.0880	33.3	0.0057	0.0331	11.6	0.0123	0.0296
Sm	57.3	-0.0216	0.1476	24.2	-0.0001	0.0311	6.1	0.0012	0.0137	2.09	-0.0002	0.0033
Gd	41.5	-0.0086	0.0945	28.4	-0.0243	0.0857	7.17	-0.0006	0.0238	2.02	0.0005	0.0016
Dy	19.2	-0.0125	0.0577	27.4	-0.0390	0.0618	7.49	0.0066	0.0261	1.95	0.0008	0.0059
Y	64.6	0.0486	0.1238	294	0.0354	0.1979	90.7	-0.1026	0.1669	14.7	-0.0177	0.0544
注：表中带“*”成分的测定平均值单位为10^-2，其他成分的测定平均值单位为10^-6。

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表 5 磷矿石各元素定值分析方法

Table 5. Analytical methods of elements in phosphate rock samples

元素	分析方法
La	ICP-MS
Ce	ICP-MS
Pr	ICP-MS
Nd	ICP-MS
Sm	ICP-MS
Eu	ICP-MS
Gd	ICP-MS
Tb	ICP-MS
Dy	ICP-MS
Ho	ICP-MS
Er	ICP-MS
Tm	ICP-MS
Yb	ICP-MS
Lu	ICP-MS
Y	ICP-MS
I	ICP-MS, COL
As	AFS
Cr	ICP-MS，ICP-OES
S	COV，GR，CS
SiO₂	GR，COV，COL，ICP-OES
Al₂O₃	COV，COL，ICP-OES
TFe₂O₃	COV，COL，ICP-OES，FAAS
MgO	COV，ICP-OES，FAAS
CaO	COV，ICP-OES
Na₂O	ICP-OES，FAAS
K₂O	ICP-OES，FAAS
TiO₂	ICP-OES，COL
MnO	ICP-MS，ICP-OES，FAAS
P₂O₅	GR，COV，COL，ICP-OES
SrO	ICP-MS，ICP-OES
BaO	ICP-MS，ICP-OES
V	ICP-MS，ICP-OES
Cd	ICP-MS，GAAS
Pb	ICP-MS，ICP-OES
U	ICP-MS，ICP-OES
F	ISE，IC
CO₂	COV，CS
注：ICP-MS—电感耦合等离子体质谱法；ICP-OES—电感耦合等离子体发射光谱法；FAAS—火焰原子吸收光谱法；GAAS—石墨炉原子吸收光谱法；AFS—原子荧光光谱法；XRF—X射线荧光光谱法；CS—高频红外吸收光谱法；COL—比色法；COV—容量法；GR—重量法；ISE—离子选择电极法；IC—离子色谱法。

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表 6 磷矿石标准物质的标准值及扩展不确定度

Table 6. Certified values and expanded uncertainty of the phosphate rock standard samples

元素	标准值与扩展不确定度
元素	G-1	G-2	G-3	G-4
P₂O₅^*	10.57±0.12	18.91±0.10	27.78±0.16	39.40±0.22
SiO₂^*	29.70±0.20	2.92±0.13	10.64±0.20	1.55±0.07
TFe₂O₃^*	15.32±0.18	0.705±0.015	0.548±0.019	0.180±0.01
CaO^*	24.13±0.2	41.41±0.28	43.50±0.05	53.27±0.40
MgO^*	6.68±0.1	10.10±0.14	3.49±0.07	0.437±0.009
Al₂O₃^*	5.58±0.14	0.293±0.005	1.33±0.04	0.685±0.015
K₂O^*	2.49±0.05	0.099±0.003	0.513±0.017	0.156±0.007
Na₂O^*	0.427±0.016	0.096±0.006	0.283±0.011	0.111±0.006
TiO₂^*	1.79±0.03	0.022±0.004	0.042±0.005	0.079±0.004
MnO^*	0.148±0.005	0.069±0.003	0.034±0.002	0.002±0.001
F^*	0.569±0.018	1.78±0.07	2.64±0.13	3.24±0.19
S^*	0.438±0.040	-0.043	0.150±0.024	0.046±0.008
CO₂^*	0.717±0.040	23.42±0.40	8.48±0.11	-1.53
SrO^*	0.252±0.005	0.055±0.002	0.091±0.003	0.056±0.002
As	0.58±0.06	12.2±0.5	12.4±0.5	1.72±0.15
Cr	28.5±1.3	7.50±0.80	23.7±0.9	20.4±1.6
I	0.27±0.02	1.80±0.22	22.1±0.8	0.94±0.16
BaO	1024±9	979±10	951±13	29.7±1.2
V	331±12	7.83±0.29	17.4±0.5	16.2±0.4
Cd	0.29±0.03	0.28±0.03	0.13±0.01	-0.023
Pb	37.5±1.7	283±9	58.3±1.9	6.48±0.50
U	2.17±0.13	12.3±0.4	16.3±0.5	6.51±0.18
La	224±6	189±3	49.7±1.9	16.3±0.6
Ce	511±10	106±2	43.2±1.5	13.4±0.5
Pr	72.8±1.0	31.9±0.7	7.75±0.23	2.55±0.10
Nd	333±5	139±3	33.6±1.0	11.3±0.5
Sm	59.6±2.0	24.8±0.7	5.89±0.19	2.15±0.06
Eu	14.6±0.7	5.69±0.14	1.30±0.07	0.93±0.04
Gd	41.3±1.5	27.3±1.2	7.10±0.40	2.13±0.03
Tb	4.72±0.27	4.50±0.22	1.16±0.07	0.35±0.02
Dy	19.3±1.1	26.6±1.3	7.35±0.40	1.94±0.10
Ho	2.67±0.14	5.60±0.22	1.71±0.10	0.39±0.03
Er	5.97±0.04	15.0±0.6	4.79±0.20	1.02±0.06
Tm	0.64±0.04	1.92±0.08	0.63±0.03	0.15±0.01
Yb	3.35±0.12	9.36±0.40	3.13±0.15	0.74±0.05
Lu	0.43±0.03	1.13±0.06	0.40±0.02	0.094±0.007
Y	67.1±2.0	297±7	94.2±2.0	15.5±0.7

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磷矿石化学成分分析标准物质研制

中国地质调查局武汉地质调查中心, 湖北 武汉 430205

作者简介: 曾美云, 硕士, 高级工程师, 从事岩矿测试及标准化研究工作。E-mail:ld_2002@sina.com

Preparation of Phosphate Ore Reference Materials for Chemical Composition Analysis

Wuhan Center of Geological Survey, China Geological Survey, Wuhan 430205, China

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中国地质调查局武汉地质调查中心, 湖北武汉 430205