田口方法用于地质样品中痕量超痕量金三种分析方法的对比

陈爱平; 孙自军; 李振

田口方法用于地质样品中痕量超痕量金三种分析方法的对比

1.
国土资源部郑州矿产资源监督检测中心，河南郑州 450012

2.
国土资源部贵金属分析与勘查技术重点实验室，河南郑州 450012

详细信息

作者简介: 陈爱平，高级工程师，主要从事岩石矿物测试工作。E-mail: chenaipingyx@163.com

中图分类号: O614.123; O657.31; O657.63

收稿日期: 2012-05-18

录用日期: 2013-11-06

Application of Taguchi Methods for Comparing Three Analytical Methods of Trace and Ultra-trace Gold in Geological Samples

1.
Zhengzhou Supervision and Analysis Center for Mineral Resources， Ministry of Land and Resources, Zhengzhou 450012, China

2.
Key Laboratory of Ministry of Land and Resources Analysis and Exploration of Precious Metals, Zhengzhou 450012, China

Received Date: 18 May 2012

Accepted Date: 06 November 2013

摘要

摘要: 目前测定地质样品痕量、超痕量金常用的三种方法是活性炭吸附富集-发射光谱法、泡塑吸附富集-石墨炉原子吸收光谱法、活性炭吸附富集-电感耦合等离子体质谱法，这三种方法的检出限在0.1~0.3 ng/g之间，由于矿石矿物的组成非常复杂，因此在有效富集和分离的基础上，采用合适的分析手段，能够对地质样品提供满意的分析结果。为保证试样要求的灵敏度和准确性，分析方法的选择需求应根据具体试样情况和实验室条件而定。根据田口玄一博士在测量工程学中提出的信噪比(S/N)能测量系统抗干扰能力，评价测量系统的稳健性和可靠性这一观点，本文利用田口测量质量控制理论，评价地质样品中痕量、超痕量金常用的上述三种分析测试方法，对这三种分析方法三个金标准物质的测试数据进行分类处理，计算S/N值和相对标准不确定度，通过比较三者的S/N值和相对标准不确定度值，确定更为可靠的测试体系。分析结果表明，对于地质样品中痕量金(含量大于1 ng/g)的测试，三种分析方法均能够满足要求；对于超痕量金(含量小于1 ng/g)的测试，活性炭吸附富集-电感耦合等离子体质谱法是较好的测试方案。
- 田口方法 /
- 地质样品 /
- 痕量金 /
- 超痕量金 /
- 活性炭吸附富集-发射光谱法 /
- /
- /
Abstract: There are currently three principle methods to measure trace and ultra-trace gold in geological samples， including activated carbon enrichment-Emission Spectrometry, foam enrichment-Graphite Furnace Atomic Absorption Spectrometry (GFAAS), and activated carbon enrichment-Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Of these, the Emission Spectrometry uses domestic equipment, with low cost and a lengthy process; the GFAAS is easy to operate but is costly as it employs an imported graphite tube. The ICP-MS method has a low detection limit but demands higher environmental conditions with high cost. The detection limits of these three methods are from 0.1 to 0.3 ng/g. As the composition of the ore mineral is very complicated, satisfactory results for the analysis of geological samples are provided by adopting a suitable analysis method based on the effective enrichment and separation. To ensure sensitivity and accuracy of sample requirements, selection of the analysis method should follow the specific sample and laboratory conditions. According to the signal-to-noise ratio (S/N) concept proposed by Doctor Genichi Taguchi in measurement engineering, the S/N is equal to the magnitude of the mean of the process compared to its variation. The bigger the S/N, the greater the anti-interference ability, the higher sensitivity, the better the linearity, the safer, and the more reliable is the measuring system. In this paper, a description of how the Taguchi measurement quality control method was conducted to evaluate three common analysis methods for trace and ultra-trace gold measurement in geological samples for the first time is given. The measurement data obtained by the three common methods for three national standard materials were processed to calculate the S/N values and the relative standard uncertainties, respectively. By comparing the three S/N values and the relative standard uncertainties, a more stable method was selected. The experimental results show that all three analytical methods met the requirements of the trace gold measurement in geological samples, whose Au content is greater than 1 ng/g, however, the activated carbon enrichment-ICP-MS is more suited for the ultra-trace gold in samples whose Au content is less than 1 ng/g.

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表 1 GAu-2a样品测试结果

Table 1. Analytical results of Au in GAu-2a sample

测量次数	w(Au)/(ng·g^-1)
测量次数	A法	B法	C法
1	1.01	0.71	0.87
2	0.74	0.83	0.86
3	1.25	0.59	0.88
4	0.80	0.82	0.89
5	0.83	0.89	0.73
6	0.83	0.94	0.70
7	0.87	1.04	0.70
8	0.81	0.71	0.90
9	0.86	0.89	0.77
10	0.83	1.27	0.72
11	0.83	1.07	0.78
12	0.82	0.58	0.81
13	0.88	0.88	0.68
14	0.83	0.80	0.75
15	0.85	0.73	0.79

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表 2 GAu-9a样品测试结果

Table 2. Analytical results of Au in GAu-9a sample

测量次数	w(Au)/(ng·g^-1)
测量次数	A法	B法	C法
1	1.59	1.65	1.72
2	1.43	1.38	1.73
3	0.92	1.41	1.60
4	1.04	1.38	1.88
5	1.55	1.61	1.47
6	1.51	1.46	1.31
7	1.57	1.60	1.69
8	1.61	2.00	1.54
9	1.65	1.42	1.72
10	1.48	1.54	1.65
11	1.59	1.54	1.41
12	1.54	1.36	1.69
13	1.28	1.17	1.50
14	1.42	2.08	1.61
15	1.44	2.18	1.64

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表 3 GAu-10a样品测试结果

Table 3. Analytical results of Au in GAu-10a sample

测量次数	w(Au)/(ng·g^-1)
测量次数	A法	B法	C法
1	5.22	4.98	5.91
2	5.44	5.31	5.78
3	5.27	5.69	5.51
4	5.30	5.13	4.68
5	5.11	4.77	4.85
6	5.47	5.09	5.23
7	5.18	4.99	4.76
8	5.14	4.76	5.00
9	5.11	5.54	5.99
10	5.02	5.38	5.54
11	5.03	4.62	4.96
12	5.05	5.60	4.86
13	5.11	6.71	5.96
14	7.37	5.69	6.13
15	5.09	4.66	4.78

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表 4 痕量金三种分析方法的测量数据处理结果

Table 4. Data processing results of trace gold using three analytical methods

金标准物质	分析方法	S_m	V_e	$ \widehat \eta $	η/dB	γ	极限值
GAu-2a	A法	11.336	0.014	52.700	17.220	0.138	11.20
	B法	10.838	0.034	21.410	13.310	0.216	7.29
	C法	9.330	0.006	107.740	20.324	0.096	14.30
GAu-9a	A法	31.162	0.044	46.850	16.710	0.146	10.69
	B法	37.699	0.083	30.250	14.810	0.182	8.79
	C法	38.914	0.021	123.680	20.920	0.090	14.90
GAu-10a	A法	425.729	0.339	83.580	19.220	0.109	13.20
	B法	415.224	0.296	93.540	19.710	0.103	13.69
	C法	426.027	0.275	103.350	20.140	0.098	14.12

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田口方法用于地质样品中痕量超痕量金三种分析方法的对比

1. 国土资源部郑州矿产资源监督检测中心， 河南 郑州 450012 2. 国土资源部贵金属分析与勘查技术重点实验室， 河南 郑州 450012

作者简介: 陈爱平，高级工程师，主要从事岩石矿物测试工作。E-mail: chenaipingyx@163.com

Application of Taguchi Methods for Comparing Three Analytical Methods of Trace and Ultra-trace Gold in Geological Samples

1. Zhengzhou Supervision and Analysis Center for Mineral Resources， Ministry of Land and Resources, Zhengzhou 450012, China 2. Key Laboratory of Ministry of Land and Resources Analysis and Exploration of Precious Metals, Zhengzhou 450012, China

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1.
国土资源部郑州矿产资源监督检测中心，河南郑州 450012

2.
国土资源部贵金属分析与勘查技术重点实验室，河南郑州 450012

1.
Zhengzhou Supervision and Analysis Center for Mineral Resources， Ministry of Land and Resources, Zhengzhou 450012, China

2.
Key Laboratory of Ministry of Land and Resources Analysis and Exploration of Precious Metals, Zhengzhou 450012, China