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摘要:
1986年至2007年期间，中国先后研制了适用于区域地球化学调查、矿产勘查与评价、采矿与选冶等不同工作需求的背景、异常、中等、高含量以及矿化、边界品位、精矿等不同品级的痕量金和矿石金系列标准物质。经过多年使用尤其是近年来使用量的递增，这些标准物质中多数样品已经或已近耗尽，急需研制替代的标准物质。2016—2018年，本文严格按照国家一级标准物质研制的相关规范，开展了7个痕量金（GBW07805、GBW07806、GBW07243~GBW07247）和3个矿石金[GBW（E）070012、GBW07807、GBW07299]地球化学标准物质的复制工作。在全国范围内选采了矿床和介质类型具有代表性的候选物，经粗碎、烘干、组合配置、细碎、过筛、混匀等步骤制备而成。经粒度检查，样品粒径达到0.74μm的累计含量达到99%以上，符合规范要求。本系列标准物质采用电感耦合等离子体质谱法（ICP-MS）、火焰原子吸收光谱法（FAAS）及石墨炉原子吸收光谱法（GFAAS）等经典可靠的分析方法测定金含量，每个样品随机抽取25瓶子样进行均匀性检验测试，相对标准偏差（RSD）均都小于10%，方差检验的F值均小于单尾临界值F0.05（24，25）=1.98，表明样品均匀性良好。在一年的考察期内，定值成分未发现统计学意义上的明显变化，证明样品的稳定性良好。由中国5家具有金测试经验、技术力量强的实验室，采用经典可靠的多种测试方法共提供了292组分析数据完成定值测试。原始数据经统计检验并剔除可疑值后符合正态分布，以算术平均值作为标准值，并按照最新规范详细评定了不确定度。复制的标准物质量值准确可靠，不确定度合理。与原批次相比，两个批次的认定值基本一致，定值数据的标准偏差呈缩小趋势，符合标准物质复制的要求。本系列金标准物质含量范围广，适用于不同含量级次的量值比对和分析监控，可以满足地质矿产研究、区域地球化学调查、金矿勘查与评价的需要。
Abstract:BACKGROUND From 1986 to 2007, different grades of trace gold certified reference materials (background grade, anomaly grade, medium grade and high grade) and mineral gold certified reference materials (mineralization grade, cutoff grade and concentrate grade) had been developed by IGGE and used for regional geochemical survey, mineral exploration and evaluation, mining and smelting. With the increase of the service life period and the consumption of recent years, most of the gold certified reference materials has been used up or almost used up. New gold standard materials need to be developed urgently.
OBJECTIVES To develop a new gold certified reference material and compare it with the original gold certified reference material.
METHODS The trace gold certified reference materials in 7 levels and mineral gold certified reference materials in 3 levels were prepared in strict accordance with relevant specifications. The collected candidates were sampled from different types of deposits and different matrices. The collected candidates were prepared through coarse crushing, drying, composite configuration, fine crushing, sieving, blending and other steps. After the particle size inspection, the cumulative content of the sample with a particle size of 0.74μm reached more than 99%, which met the requirements of the specifications. 25 bottle samples of each grade were randomly selected. Homogeneity testing was carried out by ICP-MS, FAAS and GFAAS.
RESULTS The relative standard deviation (RSD) was less than 10%, and the F values of the variance test were less than the one-tailed critical value F0.05(24, 25) of 1.98, indicating that the sample uniformity was good. During the one-year investigation period, no significant changes in statistical significance were found in the fixed value components, which proved that the stability of the sample was good. Five highly experienced and skilled laboratories in geology gold samples testing in CHN were invited to evaluate the gold certified reference materials by classically reliable analytical methods. The original data conformed to the normal distribution after statistical inspection and the suspicious values were eliminated. The arithmetic mean was used as the standard value, and the uncertainty was evaluated in detail, in accordance with the latest specifications. The certified value of the copied standard material was accurate and reliable, and the uncertainty was reasonable. It was approved as a national first-level standard material in 2019. Compared with the original batch, the certified values of the two batches were basically the same, and the standard deviation of the fixed value data showed a shrinking trend, which met the requirements for copying standard materials.
CONCLUSIONS This series of gold standard materials has a wide content range, and meets the value comparison and analysis monitoring of different content levels. Moreover, it has good applicability, and meets the needs of geological and mineral research, regional geochemical investigation, gold mine exploration and evaluation.
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表 1 金地球化学标准物质组合制备方案
Table 1. Combined preparation for gold reference materials
标准物质名称 样品编号 预设量值 样品质量 基体 加入已知金标准物质的用量 GBW07805a (GAu-2b) 0.85ng/g 3000kg 黄土 黄土原样 GBW07806a (GAu-7b) 1.5ng/g 4500kg 黄土 5.4kg GBW07807(1.1μg/g) GBW07243b (GAu-9b) 3.1ng/g 5000kg 黄土: 坡积土=2:1 10.4kg GBW07807(1.1μg/g) 痕量金分析标准物质 GBW07244b (GAu-10b) 5.1ng/g 4500kg 黄土: 坡积土=1:1 17.6kg GBW07807(1.1μg/g) GBW07245b (GAu-11b) 10.5ng/g 5000kg 黄土: 坡积土=1:2 13.7kg GBW07808(3.2μg/g) GBW07246a (GAu-12a) 21ng/g 2500kg 坡积土 15.67kg GBW07808(3.2μg/g) GBW07247a (GAu-13a) 50ng/g 3000kg 黄土: 坡积土=3:1 11.6kg GBW07809(10.6μg/g) GBW(E)070012a (GAu-15a) 0.30μg/g 5000kg 坡积土 140kg GBW07809(10.6μg/g) 矿石金分析标准物质 GBW07807a (GAu-16b) 1.1μg/g 4500kg 花岗岩风化物 472kg GBW07809(10.6μg/g) GBW07299a (GAu-21a) 52μg/g 2000kg 建昌金矿石 金矿石原样 
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表 2 候选物均匀性检验结果
Table 2. Homogeneity test results of the candidates
参数 GBW07805a
(ng/g)GBW07806a
(ng/g)GBW07243b
(ng/g)GBW07244b
(ng/g)GBW07245b
(ng/g)X 0.87 3.1 1.5 5.2 10.4 RSD(%) 8.69 4.86 6.77 4.52 4.43 F 1.44 1.10 0.98 1.26 1.37 ubb 0.032 0.034 0.039 0.079 0.18 参数 GBW07246a
(ng/g)GBW07247a
(ng/g)GBW(E)
070012a
(μg/g)GBW07807a
(μg/g)GBW07299a
(μg/g)X 21.3 50.1 0.32 1.10 51.8 RSD(%) 3.96 1.91 4.96 2.58 1.18 F 1.15 1.04 1.24 1.32 1.18 ubb 0.22 0.13 0.005 0.011 0.18 注：X为测定平均值，RSD为相对标准偏差, ubb为均匀性引入的不确定度。
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表 3 候选物稳定性检验结果
Table 3. Stability test results of the candidates
稳定性检验时间 GBW07805a
(GAu-2b)GBW07806a
(GAu-7b)GBW07243b
(GAu-9b)GBW07244b
(GAu-10b)GBW07245b
(GAu-11b)第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值2018年4月
2018年6月
2018年9月
2019年1月
2019年5月$\begin{array}{ll} 0.87 & 0.83 \\ 0.81 & 0.86 \\ 0.90 & 0.85 \\ 0.86 & 0.81 \\ 0.89 & 0.84 \end{array}$ $\begin{array}{ll} 3.06 & 3.12 \\ 3.10 & 3.05 \\ 3.04 & 3.11 \\ 3.06 & 3.14 \\ 3.10 & 3.03 \end{array}$ $\begin{array}{ll} 1.53 & 1.49 \\ 1.52 & 1.55 \\ 1.47 & 1.56 \\ 1.42 & 1.58 \\ 1.49 & 1.54 \end{array}$ $\begin{array}{ll} 5.08 & 5.13 \\ 4.94 & 5.22 \\ 5.24 & 5.01 \\ 5.22 & 5.08 \\ 5.07 & 5.12 \end{array}$ $\begin{array}{ll} 10.43 & 10.54 \\ 10.76 & 9.87 \\ 10.13 & 10.80 \\ 10.57 & 10.22 \\ 10.14 & 10.75 \end{array}$ 平均值(ng/g)
RSD(%)
β1
t0.05·s(β1)
s(β1)
us(ng/g)0.85
2.10
0.001
0.006
0.002
0.023.08
0.45
-0.001
0.005
0.002
0.021.52
0.84
-0.001
0.005
0.001
0.025.11
0.53
0.001
0.010
0.003
0.0410.42
0.65
0.002
0.026
0.008
0.10稳定性检验时间 GBW07246a
(GAu-12b)GBW07247a
(GAu-13b)GBW(E)070012a
(GAu-15b)GBW07807a
(GAu-16b)GBW07299a
(GAu-21a)第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值第1次 第2次
测定值 测定值2018年4月
2018年6月
2018年9月
2019年1月
2019年5月$\begin{array}{ll} 20.72 & 22.09 \\ 21.83 & 20.91 \\ 21.41 & 20.76 \\ 20.98 & 21.50 \\ 22.02 & 20.67 \end{array}$ $\begin{array}{ll} 50.15 & 50.32 \\ 49.96 & 50.34 \\ 50.03 & 50.46 \\ 50.09 & 50.25 \\ 50.93 & 49.57 \end{array}$ $\begin{array}{ll} 0.316 & 0.324 \\ 0.319 & 0.329 \\ 0.323 & 0.318 \\ 0.321 & 0.307 \\ 0.311 & 0.322 \end{array}$ $\begin{array}{ll} 1.092 & 1.083 \\ 1.106 & 1.121 \\ 1.069 & 1.128 \\ 1.117 & 1.102 \\ 1.087 & 1.101 \end{array}$ $\begin{array}{ll} 52.54 & 51.47 \\ 51.42 & 52.03 \\ 52.40 & 51.60 \\ 51.75 & 51.68 \\ 51.44 & 52.27 \end{array}$ 平均值(ng/g)
RSD(%)
β1
t0.05·s(β1)
s(β1)
us(ng/g)21.29
0.61
-0.002
0.049
0.009
0.1150.21
0.09
0.003
0.017
0.005
0.060.32
1.21
-0.001
0.001
0.0003
0.0041.10
0.98
-0.0002
0.004
0.001
0.0151.86
0.27
-0.007
0.052
0.008
0.10注：RSD为相对标准偏差；β1为直线的斜率; t0.05·s(β1)为自由度95%的学生分布列表值; us为稳定性引入的不确定度分量。
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表 4 痕量金及金矿石标准物质定值数据汇总
Table 4. Summary of test data of trace gold and gold ore reference materials
标准物质编号 实验室代码 分析方法 痕量金系列(ng/g) 平均值
(ng/g)标准偏差
s(ng/g)A类不确定度(UA) 测定值1 测定值2 测定值3 测定值4 组平均值 GBW07805a
(GAu-2b)1 DA-P-GFAAS 0.85 0.92 0.81 0.87 0.86 0.87 0.01 0.004 1 DA-C-ICPMS 0.88 0.88 0.83 0.86 0.86 2 DA-P-GFAAS 0.89 0.83 0.90 0.93 0.89 3 DA-P-ICPMS 0.80 0.91 0.78 0.94 0.86 3 FA-ICPMS 0.81 0.90 0.85 0.93 0.87 4 DA-C-ICPMS 0.95 0.94 0.83 0.81 0.88 5 DA-F-ICPMS 0.91 0.88 0.84 0.86 0.87 GBW07806a
(GAu-7b)1 DA-P-GFAAS 3.05 3.08 3.00 3.42 3.14 3.1 0.07 0.03 1 DA-C-ICPMS 3.14 3.14 3.11 3.15 3.14 2 DA-P-GFAAS 3.18 3.30 3.30 2.97 3.19 3 DA-P-ICPMS 3.20 3.10 3.10 3.00 3.10 3 FA-ICPMS 3.13 3.06 3.09 3.15 3.11 4 DA-C-ICPMS 2.88 3.00 3.04 2.94 2.97 5 DA-F-ICPMS 3.49 3.05 2.99 3.16 3.17 GBW07243b
(GAu-9b)1 DA-P-GFAAS 1.53 1.47 1.62 1.37 1.50 1.5 0.06 0.02 1 DA-C-ICPMS 1.35 1.35 1.41 1.48 1.40 2 DA-P-GFAAS 1.53 1.50 1.66 1.43 1.53 3 DA-P-ICPMS 1.50 1.60 1.60 1.50 1.55 3 FA-ICPMS 1.53 1.51 1.55 1.52 1.53 4 DA-C-ICPMS 1.62 1.50 1.55 1.66 1.58 5 DA-F-ICPMS 1.45 1.42 1.55 1.60 1.51 GBW07244b
(GAu-10b)1 DA-P-GFAAS 5.06 4.78 5.24 4.81 4.97 5.1 0.10 0.04 1 DA-C-ICPMS 5.25 5.25 5.55* 5.26 5.33 2 DA-P-GFAAS 4.97 5.19 5.28 5.17 5.15 3 DA-P-ICPMS 5.00 5.30 5.20 5.00 5.13 3 FA-ICPMS 5.12 5.06 5.08 5.14 5.10 4 DA-C-ICPMS 5.00 5.00 4.87* 5.00 4.97 5 DA-F-ICPMS 4.92 5.06 5.79* 5.05 5.20 GBW07245b
(GAu-11b)1 DA-P-GFAAS 9.97 9.93 11.17 10.71 10.45 10.4 0.23 0.08 1 DA-C-ICPMS 10.23 10.23 11.38 10.65 10.62 2 DA-P-GFAAS 10.13 10.68 10.13 10.05 10.25 3 DA-P-ICPMS 10.30 10.60 10.30 10.60 10.45 3 FA-ICPMS 10.46 10.53 10.70 10.30 10.50 4 DA-C-ICPMS 10.10 10.50 9.79 10.00 10.10 4 FA-ICPMS 10.80 10.20 10.60 9.80 10.35 5 DA-F-ICPMS 10.55 11.09 11.75 9.99 10.85 GBW07246a
(GAu-12b)1 DA-P-GFAAS 21.23 22.29 21.57 20.14 21.31 21.3 1.02 0.36 1 DA-C-ICPMS 22.95 22.95 21.91 21.98 22.45 2 DA-P-GFAAS 19.28 19.98 18.37 19.36 19.25 3 DA-P-ICPMS 20.80 21.50 21.20 21.30 21.20 3 FA-ICPMS 21.12 21.08 21.40 21.10 21.18 4 DA-C-ICPMS 20.30 22.00 21.40 20.70 21.10 4 FA-ICPMS 23.20 22.30 22.10 22.60 22.55 5 DA-F-ICPMS 21.36 21.87 18.95 21.91 21.02 GBW07247a
(GAu-13b)1 DA-P-GFAAS 49.55 49.47 49.07 56.02 51.03 50.1 0.53 0.19 1 DA-C-ICPMS 52.28 52.28 50.10 49.43 51.02 2 DA-P-GFAAS 51.79 49.23 48.87 50.56 50.11 3 DA-P-ICPMS 49.60 50.40 50.60 49.80 50.10 3 FA-ICPMS 50.26 50.18 50.50 50.10 50.26 4 DA-C-ICPMS 50.20 49.50 49.30 50.00 49.75 4 FA-ICPMS 51.70 49.80 47.30 53.10 50.48 5 DA-F-ICPMS 48.19 48.80 51.72 49.52 49.56 标准物质编号 实验室代码 分析方法 矿石金系列(μg/g) 平均值
(μg/g)标准偏差
(s)A类不确
定度(UA)1-1 1-2 2-1 2-2 组平均值 GBW(E)070012a
(GAu-15a)1 DA-C-AAS 0.31 0.31 0.31 0.30 0.31 0.32 0.02 0.007 1 FA-AAS 0.31 0.31 0.32 0.30 0.31 2 DA-C-AAS 0.31 0.32 0.31 0.33 0.32 5 DA-P-AAS 0.34 0.36 0.40 0.32 0.36 4 FA-AAS 0.30 0.28 0.30 0.32 0.30 4 DA-C-VOL 0.30 0.30 0.30 0.30 0.30 4 FA-VOL 0.30 0.35 0.30 0.30 0.31 GBW07807a
(GAu-16b)1 DA-C-AAS 1.07* 1.12 1.12 1.13* 1.11 1.10 0.04 0.015 1 FA-AAS 1.16 1.21 1.15 1.06 1.15 2 DA-C-AAS 1.14 1.10 1.09 1.16 1.12 5 DA-P-AAS 1.02 1.05 1.38* 1.26* 1.04 4 FA-AAS 1.15 1.09 1.06 1.01 1.08 4 DA-C-VOL 1.11* 1.06 1.06 1.06 1.07 4 FA-VOL 1.11 1.16* 1.11 1.11 1.12 GBW07299a
(GAu-21a)1 DA-C-AAS 52.60 51.73 51.91 52.32 52.14 51.8 0.65 0.25 1 FA-AAS 52.13 52.05 52.21 51.62 52.00 2 DA-C-AAS 52.06 52.71 51.02 51.69 51.87 5 DA-P-AAS 51.70 48.70* 53.90* 49.90 51.05 4 FA-AAS 52.30 53.50 52.00 52.80 52.65 4 DA-C-VOL 51.40 51.20 51.00 50.80 51.10 4 FA-VOL 52.40 52.00 52.50 51.90 52.20 注：实验室代码1—黑龙江省第一地质勘查院；2—内蒙古第三地质矿产勘查开发院实验室；3—青海省岩矿测试应用研究所；4—中国地质科学院矿产综合利用研究所；5—中国地质科学院地球物理地球化学勘查研究所。右上角带“*”为剔除数据。分解和富集方法DA—王水分解；P—泡沫塑料富集；C—活性炭富集；FA—铅试金富集。测定方法GFAAS—石墨炉原子吸收光谱法；ICP-MS—电感耦合等离子体质谱法；AAS—火焰原子吸收光谱法；VOL—容量法。
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表 5 金标准物质的标准值及扩展不确定度
Table 5. Certified values and expanded uncertainty of gold reference materials
标准物质类型 标准物质编号 n X
(ng/g)uchar
(ng/g)ubb
(ng/g)us
(ng/g)U
(ng/g)结果表达
(ng/g)痕量金分析标准物质 GBW07805a (GAu-2b) 7 0.87 0.006 0.032 0.022 0.08 0.87±0.08 GBW07806a (GAu-7b) 7 3.11 0.03 0.03 0.02 0.1 3.1±0.1 GBW07243b (GAu-9b) 7 1.51 0.02 0.04 0.02 0.1 1.5±0.1 GBW07244b (GAu-10b) 7 5.09 0.05 0.08 0.04 0.2 5.1±0.2 GBW07245b (GAu-11b) 8 10.4 0.10 0.18 0.10 0.5 10.4±0.5 GBW07246a (GAu-12a) 8 21.3 0.37 0.22 0.11 0.9 21.3±0.9 GBW07247a (GAu-13a) 8 50.1 0.31 0.13 0.06 0.7 50.1±0.7 标准物质类型 标准物质编号 n X
(μg/g)uchar
(μg/g)ubb
(μg/g)us
(μg/g)U
(μg/g)结果表达
(μg/g)矿石金分析标准物质 GBW(E)070012a (GAu-15a) 7 0.32 0.007 0.005 0.004 0.02 0.32±0.02 GBW07807a (GAu-16b) 7 1.10 0.015 0.011 0.007 0.04 1.10±0.04 GBW07299a (GAu-21a) 7 51.8 0.34 0.18 0.10 0.8 51.8±0.8 注：n—数据组数; ubb—均匀性引入的不确定度; us—稳定性引入的不确定度; uchar—定值过程引入的不确定度; U—扩展不确定度。
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表 6 本次复制标准物质与原批次标准物质数据对比
Table 6. Comparison of certified values of this study with original gold reference materials
标准物质编号 单位 本次金成分分析标准物质 原批次金成分分析标准物质 标准值 标准偏差 不确定度 标准值 标准偏差 GBW07805a(GAu-2b) ng/g 0.87 0.01 0.08 0.85 0.05 GBW07806a(GAu-7b) ng/g 3.1 0.07 0.1 3.1 0.2 GBW07243b(GAu-9b) ng/g 1.5 0.06 0.1 1.6 0.1 GBW07244b(GAu-10b) ng/g 5.1 0.10 0.2 5.1 0.2 GBW07245b(GAu-11b) ng/g 10.4 0.23 0.5 10.5 0.5 GBW07246a(GAu-12a) ng/g 21.3 1.02 0.9 21.5 1.1 GBW07247a(GAu-13a) ng/g 50.1 0.53 0.7 50 2 GBW(E)070012a(GAu-15a) μg/g 0.32 0.02 0.02 0.3 0.01 GBW07807a(GAu-16b) μg/g 1.10 0.04 0.04 1.1 0.03 GBW07299a(GAu-21a) μg/g 51.8 0.65 0.8 53 2.4
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