矽线石成分分析标准物质研制

许春雪; 王亚平; 张旭; 董波; 孙德忠; 安子怡

doi:10.15898/j.cnki.11-2131/td.201608190123

矽线石成分分析标准物质研制

1.
国家地质实验测试中心, 北京 100037

2.
黑龙江省地质矿产测试应用研究所, 黑龙江哈尔滨 150036

基金项目:
中国地质调查局地质调查项目（DD20160095）；国土资源公益性行业科研专项（200911044-02）

详细信息

作者简介: 许春雪, 副研究员, 主要从事地球化学和地质分析标准化研究。E-mail:xuchunxue1980@163.com

通讯作者: 王亚平, 研究员, 研究方向为地球化学和分析化学。E-mail:wypsm@yeah.net

中图分类号: TQ421.31

收稿日期: 2016-08-19

修回日期: 2017-02-07

录用日期: 2017-02-15

Preparation of Certified Reference Materials of Sillimanite for Chemical Composition Analysis

1.
National Research Center for Geoanalysis, Beijing 100037, China

2.
Institute of Geology and Mineral Resources Testing & Application of Heilongjiang Province, Harbin 150036, China

More Information

Corresponding author: Ya-ping WANG, wypsm@yeah.net

Received Date: 19 August 2016

Revised Date: 07 February 2017

Accepted Date: 15 February 2017

摘要

摘要: 随着矽线石应用领域的逐步拓展，英国、南非和日本等国家已研制了4种矽线石标准物质，而我国仅有一种矽线石国家二级标准物质，无论从组分的浓度梯度范围还是定值指标等方面，均难以满足我国研究需求。本文针对我国矽线石的分布情况，在黑龙江林口县和河南内乡县采集典型矽线石原矿2种，在黑龙江林口县采集矽线石精矿1种，按照国家一级标准物质研制标准和规范要求，研制了3种矽线石成分分析国家一级标准物质（批准编号为GBW07843、GBW07844、GBW07845）。均匀性检验结果表明，除个别指标（Y-1的TFe₂O₃、Cu和J-1的MnO等）外，3种标准物质检测指标的F值均小于临界值F_{0.05（24，25）}=1.96，组内和组间无明显差异；Y-1的TFe₂O₃、Cu和J-1的MnO等指标的组内和组间差异主要来源于分析方法误差，由此表明此批标准物质均匀性良好。在14个月考察期内，3种标准物质计算得到的拟合直线斜率b₁均不显著，表明3种标准物质有较好的稳定性。经我国10家实验室使用多种分析方法对矿石中的主量元素、痕量元素和矽线石含量（硅铝，SAl₂O₃）等共计39种组分联合定值，各组分的相对扩展不确定度处于0.60%~29.9%区间，3种矽线石标准物质主量成分Al₂O₃的含量分别为25.85%、28.16%和55.06%。该系列矽线石标准物质可满足地质、环境等研究领域相关样品分析质量监控工作的需求。
- 矽线石 /
- 成分分析 /
- 物相分析 /
- 标准物质 /
- 标准值
Abstract: With an increasing utilization of sillimanite, some reference materials of sillimanite for chemical composition have been developed in countries such as the UK, South Africa and Japan. In China, there is only one national secondary standard material for chemical compositon of sillimanite. It is difficult to meet the research needs of the country in terms of the concentration gradient range and the value index. For this study, two sillimanite ores were collected from Linkou county in Heilongjiang and Leijiang county in Henan, and one sillimanite concentrate was collected from Linkou county in Heilongjiang. According to national primary reference materials specifications, 3 sillimanite CRMs have been developed and approved as national standard reference materials (GBW07843, GBW07844, GBW07845). For the homogeneity test, the calculated F values in 3 sillimanite CRMs obtained by analysis of variance (ANOVA) were less than the critical F values at the 95% confidence level, with the exception of TFe₂O₃ and Cu in Y-1, and MnO in J-1, indicating no obvious differences between units and within units. The differences of TFe₂O₃ and Cu in Y-1 and MnO in J-1 between units and within units resulted from the error in the analytical methods. The results showed that 3 sillimanite CRMs had good homogeneity. The calculated test statistic b₁ of 3 sillimanite CRMs during the 14-month observation period was statistically insignificant, indicating that 3 sillimanite CRMs were stable. 10 qualified laboratories were selected to give certified values and uncertainties of 39 components, including major elements, trace elements and sillimanite phases in ores. The relative expanded uncertainties of 39 components range from 0.60% to 29.9%. The content of Al₂O₃ in sillimanite reference materials is 25.85%, 28.16%, 55.06% for GBW07843, GBW07844, and GBW07845, respectively. 3 sillimanite CRMs meet the monitoring requirements of chemical composition analysis for sillimanite samples in geology and environment fields.
- sillimanite /
- chemical composition analysis /
- phase analysis /
- reference material /
- certified value

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表 1 国内外矽线石标准物质的研制情况

Table 1. The development information of the sillimanite standard materials at home and abroad

序号	标准物质编号	定值(参考值)指标	研制国家	研制年份
1	BCS-CRM 309	Si、Al、Fe、Ti、Ca、Mg、Na、K、Mn、Li、O、Sr、Ba等13项	英国	1974
2	JCRM R304	SiO₂、Al₂O₃、Fe₂O₃、TiO₂、ZrO₂、MnO、P₂O₅、CaO、MgO、Na₂O、K₂O等11项	日本	2003
3	SARM 44	Ba、Ce、Co、Cr、Cu、Ga、Mo、Nb、Ni、Pb、Rb、S、Sr、Th、V、Y、Zn、Zr、Fe、SiO₂、Al₂O₃、CaO、K₂O、MnO、TiO₂、P₂O₅、FeO、MgO、Na₂O等29项	南非	1989
4	CERAM 2CAS12	Al₂O₃、SiO₂、CaO、Fe₂O₃、K₂O、Li₂O、MgO、MnO、Na₂O、TiO₂、LOI等11项	英国	-
5	GBW(E)070061	SiO₂、Al₂O₃、TFe₂O₃、CaO、MgO、TiO₂、Na₂O、K₂O、MnO、P₂O₅、F、FeO、Ba、Co、Cr、Cu、La、Nb、Ni、Pb、Rb、S、Sr、Th、V、Y、Zn、Zr、LOI等29项	中国	-

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表 2 均匀性检验结果

Table 2. Analytical results of the homogeneity tests

样品编号	项目	组分含量(%)
样品编号	项目	TAl₂O₃	SAl₂O₃	Na₂O	MgO	SiO₂	P₂O₅	K₂O	CaO	TiO₂	MnO	TFe₂O₃	FeO
Y-1	平均值	25.6	13.7	0.45	0.95	56.2	0.092	2.45	0.26	1.26	0.0863	9.45	4.66
	RSD(%)	0.65	0.82	4.09	1.47	0.40	9.72	2.06	3.38	1.73	2.01	0.85	0.48
	F实测值	1.15	0.99	0.78	0.52	0.96	1.48	1.10	1.67	0.68	1.28	3.05	0.84
	u_bb	0.0431	0.0424	0.0072	0.0060	0.0846	0.0039	0.0108	0.0044	0.0089	0.0006	0.0571	0.0087
Y-2	平均值	28.4	11.4	0.06	1.02	46.9	0.128	1.84	0.26	1.55	0.067	13.3	6.80
	RSD(%)	0.44	0.59	10.34	2.74	0.24	3.62	0.91	3.89	1.63	2.91	0.62	0.36
	F实测值	0.17	1.02	1.05	0.60	0.70	0.16	0.89	0.57	0.81	0.33	0.19	1.06
	u_bb	0.0617	0.0067	0.0009	0.0117	0.0457	0.0023	0.0065	0.0042	0.0100	0.0009	0.0400	0.0040
J-1	平均值	54.9	46.7	0.06	0.125	40.8	0.123	0.36	0.12	0.15	0.011	1.26	0.18
	RSD(%)	0.17	0.39	6.91	3.50	0.29	3.93	3.52	5.66	4.56	8.49	1.94	6.09
	F实测值	2.80	0.35	1.13	1.61	1.02	0.63	0.97	1.77	0.48	6.69	1.08	0.44
	u_bb	0.0639	0.0824	0.0010	0.0021	0.0122	0.0020	0.0048	0.0037	0.0030	0.0008	0.0047	0.0048

样品编号	项目	组分含量(μg/g)
样品编号	项目	LOI	Ba	Be	Cu	Pb	Zn	Co	Ni	Cd	U	Th
Y-1	平均值	3.20	489	3.07	47.9	18.4	112	15.7	23.2	0.11	3.45	24.5
	RSD(%)	2.00	3.40	3.38	3.64	4.53	4.42	2.70	3.94	4.35	6.63	4.93
	F实测值	1.28	1.07	0.85	2.87	1.04	0.79	1.55	0.47	0.65	0.47	1.56
	u_bb	0.0224	2.9939	0.0406	1.2169	0.1230	1.9670	0.1980	0.4000	0.0020	0.1000	0.5670
Y-2	平均值	6.01	224	1.73	32	16.5	92	10.9	11.2	0.035	4.76	26.7
	RSD(%)	1.33	3.80	3.75	3.91	3.93	5.48	3.30	5.09	5.38	3.83	5.75
	F实测值	1.20	1.06	0.95	0.78	0.94	0.70	0.92	0.75	0.73	1.01	0.87
	u_bb	0.0239	1.4935	0.0246	0.4980	0.2475	2.0550	0.1376	0.2280	0.0010	0.0129	0.5970
J-1	平均值	1.45	78.6	2.97	12.2	3.34	38.88	3.68	5.41	0.039	2.61	18.7
	RSD(%)	2.35	4.20	3.20	4.09	5.00	2.27	3.86	6.48	8.08	5.15	2.51
	F实测值	0.79	1.19	2.31	0.53	0.45	1.03	0.88	1.26	0.82	1.95	1.07
	u_bb	0.0135	0.9879	0.0601	0.2133	0.0734	0.1131	0.0551	0.1196	0.0012	0.0765	0.0842
注：LOI(烧失量)的单位为%。

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表 3 稳定性检验结果

Table 3. Analytical results of the stability tests

样品编号	项目	组分含量(%)
样品编号	项目	TAl₂O₃	SAl₂O₃	Na₂O	MgO	SiO₂	P₂O₅	K₂O	CaO	TiO₂	MnO	TFe₂O₃	FeO
Y-1	平均值	25.83	14.08	0.448	0.94	56.23	0.103	2.49	0.25	1.26	0.085	9.41	4.66
	b₁	0.0008	0.0039	0.00004	-0.00157	0.0051	0.000340	0.0009	-0.00145	-0.00093	-0.00026	0.00058	0.0021
	t_0.05·s(b₁)	0.0061	0.0611	0.00142	0.00741	0.0401	0.000678	0.0154	0.00295	0.003183	0.0011	0.02281	0.01062
	u_s	0.020	0.032	0.005	0.024	0.13	0.0022	0.050	0.0096	0.010	0.0036	0.074	0.035
Y-2	平均值	28.43	11.91	0.070	1.21	46.96	0.127	1.84	0.25	1.52	0.065	13.30	6.77
	b₁	0.0068	0.01007	-0.00013	-0.0022	-0.00060	-0.00001	-0.00023	-0.00178	-0.00378	-0.00033	-0.00332	-0.00153
	t_0.05·s(b₁)	0.0071	0.02499	0.00097	0.0135	0.01258	0.00191	0.00235	0.00377	0.00779	0.00098	0.01673	0.00427
	u_s	0.023	0.081	0.003	0.044	0.041	0.0062	0.0076	0.012	0.025	0.003	0.054	0.014
J-1	平均值	54.96	48.33	0.057	0.13	40.83	0.121	0.37	0.121	0.15	0.012	1.27	0.18
	b₁	-0.0103	-0.01868	-0.00030	0.00049	-0.00823	-0.00077	0.00121	0.00009	0.00077	0.00002	-0.00075	0.00066
	t_0.05·s(b₁)	0.0338	0.02243	0.00079	0.00151	0.03021	0.00167	0.00318	0.00253	0.00230	0.00007	0.00538	0.00382
	u_s	0.11	0.073	0.0026	0.0049	0.098	0.0054	0.010	0.0082	0.0075	0.0002	0.018	0.012

样品编号	项目	组分含量(μg/g)
样品编号	项目	LOI	Ba	Be	Cu	Pb	Zn	Co	Ni	Cd	U	Th
Y-1	平均值	3.18	480	3.05	45.95	18.61	109	15.34	22.71	0.108	25.16	3.43
	b₁	0.0055	-0.607	-0.00169	0.01870	-0.03523	0.14161	0.0183	-0.01024	-0.0002	-0.01412	0.00335
	t_0.05·s(b₁)	0.02199	2.2715	0.03395	0.20763	0.41792	0.39956	0.1294	0.22949	0.002443	0.06156	0.01428
	u_s	0.072	7.40	0.111	0.68	1.36	1.30	0.42	0.75	0.008	0.20	0.046
Y-2	平均值	6.12	231	1.67	33.05	16.46	85.6	10.89	10.74	0.037	4.57	28.06
	b₁	0.00471	-0.8571	0.00490	0.07183	-0.07171	0.23142	0.00259	-0.03455	0.00006	-0.01295	-0.09094
	t_0.05·s(b₁)	0.01114	1.8597	0.00499	0.61560	0.14865	1.26567	0.10693	0.13887	0.00057	0.03160	0.4175
	u_s	0.036	6.05	0.016	2.00	0.48	4.12	0.35	0.45	0.0018	0.10	1.36
J-1	平均值	1.45	83.2	2.08	11.46	2.60	36.1	3.60	4.68	0.038	2.62	18.52
	b₁	0.00338	0.30359	0.0069	-0.02718	0.01265	-0.00720	-0.01439	0.00085	-0.00019	-0.00127	-0.0059
	t_0.05·s(b₁)	0.00842	1.62143	0.0226	0.39033	0.04560	0.25997	0.02649	0.02171	0.00054	0.01501	0.04122
	u_s	0.027	5.28	0.074	1.27	0.15	0.85	0.086	0.071	0.0018	0.049	0.13
注：LOI(烧失量)的单位为%。

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表 4 矽线石标准物质各定值指标的分析方法

Table 4. Analytical methods used for the elements determination in sillimanite reference materials

定值指标	定值方法
全铝(TAl₂O₃)	VOL，XRF，ICP-OES
硅铝(SAl₂O₃)	VOL
SiO₂	ICP-OES，XRF，GR
Na₂O	ICP-OES，XRF，AAS
K₂O	ICP-OES，XRF，AAS
CaO	ICP-OES，XRF，AAS
MgO	ICP-OES，XRF，AAS
TFe₂O₃	ICP-OES，XRF，COL，VOL
FeO	VOL
LOI	GR
MnO	ICP-MS，ICP-OES
P₂O₅	ICP-OES，XRF，COL
TiO₂	ICP-OES，XRF，COL
CO₂	VOL
C	VOL，IR
S	VOL，IR
Ba	ICP-MS，ICP-OES
Be	ICP-MS，ICP-OES
Cd	ICP-MS，AAS
Ce	ICP-MS，ICP-OES
Co	ICP-MS，ICP-OES
Cr	ICP-MS，ICP-OES，COL
Cu	ICP-MS，ICP-OES
F	ISE
Ga	ICP-MS
La	ICP-MS，ICP-OES
Li	ICP-MS，ICP-OES
Mo	ICP-MS，POL
Nb	ICP-MS
Ni	ICP-MS，ICP-OES
Pb	ICP-MS
Rb	ICP-MS，AAS
Sr	ICP-MS，ICP-OES
Th	ICP-MS
U	ICP-MS
V	ICP-MS，ICP-OES
Y	ICP-MS
Zn	ICP-MS，ICP-OES
Zr	ICP-MS
注：VOL—容量法；XRF—X射线荧光光谱法；ICP-OES—电感耦合等离子体发射光谱法；GR—重量法；AAS—原子吸收光谱法；COL—比色法；ICP-MS—电感耦合等离子体质谱法；IR—红外光谱法；ISE—离子选择电极法；POL—示波极谱法。

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表 5 矽线石标准物质认定值及扩展不确定度

Table 5. Certified values and expanded uncertainty of sillimanite reference materials

定值指标	数据单位	认定值与扩展不确定度
定值指标	数据单位	GBW07843 (Y-1)	GBW07844 (Y-2)	GBW07845 (J-1)
TAl₂O₃	%	25.85±0.19	28.16±0.22	55.06 0.34
SAl₂O₃	%	13.86±0.26	12.16±0.64	46.20±1.43
SiO₂	%	55.90±0.38	47.15±0.28	40.82±0.28
Na₂O	%	0.46±0.03	0.069±0.010	0.061±0.008
K₂O	%	2.45±0.11	1.73±0.04	0.35±0.03
CaO	%	0.27±0.03	0.29±0.04	0.14±0.03
MgO	%	0.94±0.06	1.02±0.10	0.13±0.02
TFe₂O₃	%	9.43±0.19	13.57±0.22	1.30±0.10
FeO	%	4.69±0.12	6.77±0.07	0.20±0.04
LOI	%	(3.01)	(5.81)	(1.34)
MnO	%	0.086±0.010	0.057±0.004	0.011±0.003
P₂O₅	%	0.097±0.011	0.11±0.01	0.096±0.018
TiO₂	%	1.23±0.04	1.56±0.04	0.15±0.02
CO₂	%	(0.14)	(0.23)	(0.20)
C	%	0.087±0.026	0.38±0.01	0.14±0.02
S	%	0.050±0.004	0.15±0.01	0.019±0.004
Ba	μg/g	485±19	222±17	78.8±11.1
Be	μg/g	3.5±0.4	2.1±0.3	3.0±0.4
Cd	μg/g	0.08±0.02	0.04±0.01	0.035±0.007
Ce	μg/g	161±6	176±4	112±19
Co	μg/g	15.9±1.2	11.2±0.9	3.7±0.3
Cr	μg/g	105±11	135±10	186±28
Cu	μg/g	48.2±3.0	31.3±4.4	12.0±2.7
F	μg/g	397±9	562±20	107±14
Ga	μg/g	28.4±3.8	30.8±4.8	51.0±9.1
La	μg/g	79.1±5.4	85.9±9.0	56.1±10.5
Li	μg/g	51.4±0.5	55.3±0.9	22.9±0.5
Mo	μg/g	2.1±0.2	1.60±0.11	0.85±0.08
Nb	μg/g	24.5±2.6	30.2±3.3	3.5±0.4
Ni	μg/g	23.5±1.9	10.7±1.1	5.1±0.5
Pb	μg/g	17.5±2.8	15.2±1.3	3.3±0.5
Rb	μg/g	102±7	81.8±8.8	14.5±0.8
Sr	μg/g	73.0±1.6	28.9±1.6	12.6±1.2
Th	μg/g	25.3±1.3	(24.8)	17.8±1.3
U	μg/g	3.4±0.5	4.4±0.4	2.6±0.3
V	μg/g	180±17	252±17	340±47
Y	μg/g	47.6±8.2	73±11	14.7±3.3
Zn	μg/g	118±7	90.3±9.9	41.7±4.1
Zr	μg/g	(259)	(286)	(639)

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