【引用本文】 杨理勤, 陈占生, 谢璐, 等. 卡林型金矿金砷成分分析标准物质研制[J]. 岩矿测试, 2018, 37(2): 209-216. doi: 10.15898/j.cnki.11-2131/td.201711210183
YANG Li-qin, CHEN Zhan-sheng, XIE Lu, et al. Preparation of Gold and Arsenic Certified Reference Materials for Chemical Composition Analysis in Carlin-type Gold Deposits[J]. Rock and Mineral Analysis, 2018, 37(2): 209-216. doi: 10.15898/j.cnki.11-2131/td.201711210183

卡林型金矿金砷成分分析标准物质研制

武警黄金地质研究所, 河北 廊坊 065000

收稿日期: 2017-11-21  修回日期: 2018-02-01  接受日期: 2018-03-21

基金项目: 国家黄金专项业务费资助项目(HKY2012-05)

作者简介: 杨理勤, 高级工程师, 主要从事金及多金属分析技术和质量控制研究。E-mail:ylqgold@163.com

Preparation of Gold and Arsenic Certified Reference Materials for Chemical Composition Analysis in Carlin-type Gold Deposits

Gold Geology Institute of Chinese People's Armed Police Force, Langfang 065000, China

Received Date: 2017-11-21
Revised Date: 2018-02-01
Accepted Date: 2018-03-21

摘要:卡林型金矿因其含砷影响金的分析和选冶回收率而备受关注,需要研制相应的标准物质支撑应用研究。本文依托近年来探明的超大型卡林型金矿——阳山金矿采集候选物,按照国家一级标准物质技术规范研制了4种卡林型金矿标准物质GBW07854~GBW07857。共有20家实验室联合定值,金主要分析方法为原子吸收光谱法和火试金法,湿法分析采用梯度焙烧-活性炭吸附金而分离砷等干扰组分;砷分析主要采用电感耦合等离子体发射光谱法和分光光度法。引用金量分析相对偏差允许限界定组内离群值,弥补了Dixon法和Grubbs法剔除离群值不够完全的缺陷。均匀性检验指标F < F0.05(29,30)=1.84,表明组内和组间均无明显差异;在22个月内进行了5次检验,稳定性良好。4种标准物质金和砷的定值结果准确度均优于同量级的国家一级金矿石标准物质和国外含砷多金属矿石标准物质。该系列标准物质可用作卡林型金矿金和砷分析与研究等工作的量值标准。

关键词: 卡林型金矿, , 成分分析, 标准物质, 标准值

要点

(1) 卡林型金矿在国内外是重要的金矿类型,分布较广且金资源量较大,矿石中金砷共存并且砷影响金的分析准确度和选冶回收率。

(2) 金的定值方法主要采用梯度焙烧-活性炭吸附-原子吸收分光光度法,砷定值方法主要采用王水溶样-电感耦合等离子体发射光谱法。

(3) 定值数据处理中应用了DZ/T0130—2006中YGYC为判据剔除Au和As组内数据中的离群值,后续用Grubbs法和Dixon法检验并剔除组间数据中的离群值。

(4) 参加金定值的协作单位中包括1个国际检测机构。

Preparation of Gold and Arsenic Certified Reference Materials for Chemical Composition Analysis in Carlin-type Gold Deposits

ABSTRACT

BACKGROUND:

Carlin-type gold deposits have attracted much attention because of the influence of As on the analysis and recovery of gold. It is necessary to develop the specific reference materials (RM) to support application research.

OBJECTIVE:

Study samples were collected from the super large Carlin-type gold deposit in the Yangshan gold mine, discovered in recent years. Four kinds of reference materials GBW07854-GBW07857 for Carlin-type gold ore were developed according to country-level standard technical specification.

METHODS:

A total of 20 laboratories simultaneously determined element values. The main gold analysis methods included Atomic Absorption Spectrometry and Fire Assay. Wet analysis uses gradient roasting-activated carbon adsorption of gold to separate arsenic and other interference components. Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) and Spectrophotometry were mainly used to analyze arsenic. Citation analysis relative deviation permissible limit to define within-group outliers makes up for the incompleteness of the Dixon and Grubbs methods to eliminate outliers.

RESULTS:

The homogeneity test index F < F0.05(29, 30)=1.84, indicated that there were no significant differences between the groups and within the group. No statistically significant changes were observed in 5 analyses during 22 months. The certified values of gold and arsenic in this series of certified reference materials (CRMs) were superior to those of the same level country-level gold ore RM and foreign arsenic-bearing polymetallic ore RM.

CONCLUSIONS:

This series of CRMs can be used as standards for the analysis and study of gold and arsenic in Carlin-type gold deposits.

KEY WORDS: Carlin-type gold deposit, arsenic, chemical composition analysis, reference material, certified value

HIGHLIGHTS

(1) Carlin type gold deposit is important type of gold mine because of wide distribution and large amount of gold resources. For this type of ore, gold and arsenic are coexisted, and arsenic affects accuracy of gold analysis and recovery rate of minerals processing.

(2) Au was determined by Gradient Roasting-Activated Carbon Adsorption-Atomic Absorption Spectrometry, Inductively Coupled Plasma-Optical Emission Spectrometry were mainly used for As analysis.

(3) In the data processing, the fixed value YG and YC in DZ/T0130—2006 were applied to eliminate the outliers in the data of the Au and As groups, respectively. Then the outliers in the group data were examined by Grubbs and Dixon method.

(4) The coordination unit in the gold determination included an international testing agency.

本文参考文献

[1]

宋丽华, 郝原芳, 杨柳, 等. 地质标准物质的研制方法[J]. 地质与资源, 2013, 22(5): 419-421.

Song L H, Hao Y F, Yang L, et al. Preparation method of geochemical reference materials[J]. Geology and Resources, 2013, 22(5): 419-421.

[2]

贺志红. 使用标准物质进行质量控制的必要性探讨[J]. 广州化工, 2014, 42(5): 189-191.

He Z H. Discussion of the need for quality control laboratory using standard material[J]. Guangzhou Chemical Industry, 2014, 42(5): 189-191.

[3]

刘源, 侯中建, 李定武, 等. 我国卡林型金矿研究现状[J]. 四川地质学报, 2013, 33(2): 132-136.

Liu Y, Hou Z J, Li D W, et al. Present situation of research into Carlin-type gold deposits in China[J]. Acta Geologica Sichuan, 2013, 33(2): 132-136.

[4]

闫凤增,齐金忠,郭俊华. 甘肃省阳山金矿地质与勘查[M] . 北京: 地质出版社, 2010: 1-54.

Yan F Z,Qi J Z,Guo J H. Geology and Exploration of Yangshan Gold Deposit in Gansu Province[M] . Beijing: Geological Publishing House, 2010: 1-54.
[5]

喻光明, 郭华. 川陕甘地区卡林型金矿对比研究[J]. 地质学报, 2010, 32(2): 163-169.

Yu G M, Guo H. Comparison of geological and geochemical features of Carlin-type Au deposits in the Sichuan-Shannxi-Gansu border region[J]. Acta Geologica Sinica, 2010, 32(2): 163-169.

[6]

于连涛, 孟德铭, 代淑娟, 等. 某含砷金矿选矿实验研究[J]. 中国矿业, 2014, (5): 130-133.

Yu L T, Meng D M, Dai S J, et al. The flotation experiment on a certain arsenic gold ore[J]. China Mining Magazine, 2014, (5): 130-133.

[7]

中华人民共和国标准物质目录[M]. 北京: 中国质检出版社, 2013.

Reference Material General and Statistical Principles for Certification[M]. Beijing: China Jiliang Publishing House, 2013.

[8]

徐书荣, 王毅民, 潘静, 等. 关注地质分析文献, 了解分析技术发展-地质分析技术应用类评述论文评介[J]. 地质通报, 2012, 31(6): 994-1016.

Xu S R, Wang Y M, Pan J, et al. Paying attention to the literature of geoanalysis and gaining knowledge of the development of analytical techniques-Assessment of commentary papers on geoanalysis application[J]. Geological Bulletin of China, 2012, 31(6): 994-1016.

[9]

卢晓华, 汪斌, 郭敬, 等. 2015-2016国家有证标准物质资源发展分析[J]. 中国计量, 2017, (3): 82-85.

Lu X H, Wang B, Guo J, et al. Analysis on the development of certified reference materials in 2015-2016 country[J]. China Measurement, 2017, (3): 82-85.

[10]

王毅民, 王晓红, 高玉淑, 等. 中国地质标准物质制备技术与方法研究进展[J]. 地质通报, 2010, 29(7): 1090-1104.

Wang Y M, Wang X H, Gao Y S, et al. Advances in preparing techniques for geochemical materials in China[J]. Geological Bulletin of China, 2010, 29(7): 1090-1104.

[11]

刘妹, 顾铁新, 鄢卫东, 等. 高品位矿石金标准物质的研制与应用[J]. 黄金, 2017, 38(1): 80-83. doi: 10.11792/hj20170119

Liu M, Gu T X, Yan W D, et al. Preparation and application of geochemical reference material for sulfide gold concentrate[J].Gold, 2017, 38(1): 80-83. doi: 10.11792/hj20170119

[12]

芦新根, 陈永红, 洪博, 等. 金矿石和金精矿国家标准物质的研制[J]. 黄金, 2016, 37(2): 75-79.

Lu X G, Chen Y H, Hong B, et al. Development of national standard substance of gold ores and gold concentrates[J]. Gold, 2016, 37(2): 75-79.

[13]

杨理勤, 宋艳合, 李文良, 等. 金标样定值中全金量的湿法分析[J]. 岩矿测试, 2004, 23(1): 75-76.

Yang L Q, Song Y H, Li W L, et al. Application of combined sample digestion method to determination of gold in certification of standard reference gold material[J]. Rock and Mineral Analysis, 2004, 23(1): 75-76.

[14]

马新荣, 马生凤, 王蕾, 等. 王水溶矿-等离子体光谱法测定砷矿石和锑矿石中砷锑硫铜铅锌[J]. 岩矿测试, 2011, 30(2): 190-194.

Ma X R, Ma S F, Wang L, et al. Determination of As, Sb, S, Cu, Pb, Zn in arsenic ore and stibium ore by ICP-AES with aqua regia digestion[J]. Rock and Mineral Analysis, 2011, 30(2): 190-194.

[15]

陈永红, 孟宪伟, 苏广东, 等. 2011-2012年中国金分析测定的进展[J]. 黄金, 2013, 34(12): 72-78.

Chen Y H, Meng X W, Su G D, et al. Progress of gold determination and analysis technology in China during 2011-2012[J]. Gold, 2013, 34(12): 72-78.

[16]

陈永红, 孟宪伟, 苏广东, 等. 2013-2014年中国金分析测定的进展[J]. 黄金, 2016, 37(1): 79-85. doi: 10.11792/hj201601019

Chen Y H, Meng X W, Su G D, et al. Progress of gold determination and analysis technology in China during 2013-2014[J].Gold, 2016, 37(1): 79-85. doi: 10.11792/hj201601019

[17]

罗立强,吴晓军. 现代地质分析研究与应用[M] . 北京: 科学出版社, 2017: 369-372.

Luo L Q,Wu X J. Research and Application of Modern Geoanalysis[M] . Beijing: Science Press, 2017: 369-372.
[18]

岩石矿物分析编委会. 岩石矿物分析(第四版)[M] . 北京: 地质出版社, 2011: 616-637.

The Editorial Committee of Rock and Mineral Analysis . Rock and Mineral Analysis (The Fourth Edition)[M] . Beijing: Geological Publishing House, 2011: 616-637.
[19]

李玄辉, 杨理勤. 断续流动-氢化物发生原子荧光光谱法测定矿石中高含量砷[J]. 黄金, 2013, 34(6): 75-77.

Li X H, Yang L Q. Application of intermittent flow-hydride generation atomic fluorescence spectrometry to determine high level of arsenic ores[J]. Gold, 2013, 34(6): 75-77.

[20]

魏灵巧, 付胜波, 罗磊, 等. 电感耦合等离子体发射光谱法多向观测同时测定锑矿石中锑砷铜铅锌[J]. 岩矿测试, 2012, 31(6): 967-970.

Wei L Q, Fu S B, Luo L, et al. Simultaneous determination of Sb, As, Cu, Pb and Zn in anatimony ores by inductively coupled plasma-atomic emission spectrometry with a multi-directional observation mode[J]. Rock and Mineral Analysis, 2012, 31(6): 967-970.

相似文献(共20条)

[1]

王昌燧, 毛振伟, 朱铁权, 何伟, 贾兴和, 张茂林, 黄宇营. 斯里兰卡曼泰遗址出土青花瓷的化学成分分析及产地初探. 岩矿测试, 2008, 27(1): 37-40.

[2]

秦颍, 董亚巍, 魏国锋, 韩楚文, 曲毅, 王昌燧. 大冶李德贵冶炼遗址矿冶遗物分析. 岩矿测试, 2008, 27(2): 99-102.

[3]

林立, 周谙非, 张曼玲, 田艳玲, 杨彦丽. 微波消解-电感耦合等离子体发射光谱法分析食品中的总硼. 岩矿测试, 2008, 27(1): 21-24.

[4]

余宇, 刘江斌, 党亮, 陈月源, 曹成东, 谈建安, 赵峰. X射线荧光光谱法同时测定石灰石中主次痕量组分. 岩矿测试, 2008, 27(2): 149-150.

[5]

黄仁忠. 硫脲介质-石墨炉原子吸收光谱法测定化探样品中微量银. 岩矿测试, 2008, 27(3): 237-238.

[6]

李曼, 王连和. 区域地球化学样品分析质量管理计算机控制. 岩矿测试, 2008, 27(3): 219-222.

[7]

许春雪, 王亚平, 张旭, 董波, 孙德忠, 安子怡. 矽线石成分分析标准物质研制. 岩矿测试, 2017, 36(4): 396-404. doi: 10.15898/j.cnki.11-2131/td.201608190123

[8]

李刚, 苏文峰. 焙烧分离-氢化物发生-原子荧光光谱法测定土壤样品中微量硒. 岩矿测试, 2008, 27(2): 120-122.

[9]

林光西. 氢化物发生-原子荧光光谱法直接测定地球化学样品中痕量碲. 岩矿测试, 2008, 27(2): 151-152.

[10]

徐婷婷, 夏宁, 张波. 熔片制样-X射线荧光光谱法测定海洋沉积物样品中主次量组分. 岩矿测试, 2008, 27(1): 74-76.

[11]

李刚, 曹小燕. 电感耦合等离子体质谱法测定地质样品中锗和镉的干扰及校正. 岩矿测试, 2008, 27(3): 197-200.

[12]

蔡玉曼. 硅钼蓝分光光度法测定钛铁矿中二氧化硅不确定度评定. 岩矿测试, 2008, 27(2): 123-126.

[13]

曾美云, 刘金, 邵鑫, 邹棣华. 磷矿石化学成分分析标准物质研制. 岩矿测试, 2017, 36(6): 633-640. doi: 10.15898/j.cnki.11-2131/td.201705170082

[14]

卜维, 刘妹, 鄢明才, 鄢卫东, 史长义, 顾铁新. 生物成分系列标准物质的研制. 岩矿测试, 2006, 25(2): 159-172.

[15]

袁建, 王亚平, 许春雪, 代阿芳, 王苏明, 安子怡. 地下水中砷形态标准物质研制. 岩矿测试, 2012, 31(2): 331-337.

[16]

冯静, 王瑞敏, 张激光. 重晶石矿石成分分析标准物质研制. 岩矿测试, 2010, 29(2): 175-178.

[17]

赵晓亮, 李志伟, 王烨, 王君玉, 仲伟路, 陈砚. 铌钽精矿标准物质研制. 岩矿测试, 2018, 37(6): 687-694. doi: 10.15898/j.cnki.11-2131/td.201711230185

[18]

李冰, , 史世云. 电感耦合等离子体质谱法同时测定地质样品中痕量碘溴硒砷的研究:Ⅱ.土壤及沉积物标准物质分析. 岩矿测试, 2001, (4): 241-246.

[19]

顾勇冰, 张春牛, 郑云法. 1-偶氮苯-3-(5-氯-2-吡啶)-三氮烯的合成及其与镍的显色反应. 岩矿测试, 2005, (2): 112-114.

[20]

程志中, 刘妹, 张勤, 顾铁新, 黄宏库. 水系沉积物标准物质研制. 岩矿测试, 2011, 30(6): 714-722.

计量
  • PDF下载量(24)
  • 文章访问量(435)
  • HTML全文浏览量(104)
  • 被引次数(0)
目录

Figures And Tables

卡林型金矿金砷成分分析标准物质研制

杨理勤, 陈占生, 谢璐, 李玄辉, 冯亮, 艾晓军, 汤宇磊