【引用本文】 杨榕, 尹伟刚, 张菊霞, 等. 痕量金及金矿石标准物质复制[J]. 岩矿测试, 2021, 40(5): 751-762. doi: 10.15898/j.cnki.11-2131/td.202106110005
YANG Rong, YIN Wei-Gang, ZHANG Ju-xia, et al. Preparation of Trace Gold and Gold Ore Reference Materials[J]. Rock and Mineral Analysis, 2021, 40(5): 751-762. doi: 10.15898/j.cnki.11-2131/td.202106110005

痕量金及金矿石标准物质复制

1. 

中国地质科学院地球物理地球化学勘查研究所, 河北 廊坊 065000

2. 

河北地质职工大学, 河北 石家庄 050000

收稿日期: 2021-06-11  修回日期: 2021-07-20  接受日期: 2021-08-28

基金项目: 中国地质科学院基本科研业务费项目"南极玄武岩、锂辉石及黝铜矿等36种地质分析标准物质研制"(YYWF201622)

作者简介: 杨榕, 硕士研究生, 工程师, 地球化学专业。E-mail: yangrong0516@163.com

通信作者: 尹伟刚, 高级工程师, 地质勘查专业。E-mail: 1004989957@qq.com

Preparation of Trace Gold and Gold Ore Reference Materials

1. 

Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Science, Langfang 065000, China

2. 

Hebei Geological Workers University, Shijiazhuang 050000, China

Corresponding author: YIN Wei-Gang, 1004989957@qq.com

Received Date: 2021-06-11
Revised Date: 2021-07-20
Accepted Date: 2021-08-28

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。

关键词: 标准物质, 痕量金, 金矿石, 复制, 电感耦合等离子体质谱法, 原子吸收光谱法

要点

(1) 复制7个痕量金及3个矿石金地球化学标准物质,定值成分的RSD均小于6%,标准值及不确定度良好。

(2) 标准值的不确定度由均匀性、稳定性和定值三部分引起的不确定度合成。

(3) 该系列金标准物质定值数据的标准偏差小于原批次的标准偏差,定值水平优于原批次,符合标准物质复制的要求。

(4) 该系列金标准物质含量范围广(0.87ng/g~51.8μg/g),可有效监控金矿勘探开发各阶段样品分析全过程。

Preparation of Trace Gold and Gold Ore Reference Materials

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.

KEY WORDS: certified reference materials, trace gold, gold ore, replication, inductively coupled plasma-mass spectrometry, atomic absorption spectrometry

HIGHLIGHTS

(1) Seven trace gold and three ore gold geochemical reference materials were copied, and the RSD of the fixed components was less than 6%, with good standard value and uncertainty.

(2) The uncertainty of the standard value was composed of uniformity, stability and fixed value.

(3) The standard deviation of this series of gold reference materials was smaller than that of the original batch, and the fixed value level was better than that of the original batch, which met the requirements of reference material replication.

(4) This series of gold standard materials covered a wide content range (0.87ng/g-51.8μg/g), which can effectively monitor the whole process of sample analysis in each stage of gold exploration and development.

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痕量金及金矿石标准物质复制

杨榕, 尹伟刚, 张菊霞, 潘含江