钡矿化学成分标准物质研制
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摘要
我国目前没有毒重石类钡矿化学成分标准物质,重晶石类钡矿标准物质有几个,但定值的组分较少。本文研制了4个毒重石类钡矿化学成分标准物质。标准物质候选物采自重庆市城口县巴山钡矿,将样品粉碎至粒度小于0.074 mm,混合均匀后进行均匀性检验和稳定性检验,代表性元素的分析结果表明方差检验的F值小于临界值,样品均匀性良好;经1年5次抽样检测,检测数据均未发现统计学意义的明显变化,样品的长期稳定性良好。选择6家具有资质的试验室,采取经典分析方法与现代仪器分析技术相结合的方式对标准物质进行联合定值,依照ISO导则35和国家一级标准物质技术规范,4个钡矿标准物质给出了18项组分(包括主含量、伴生含量、工业利用有益有害组分、微量元素、物相成分)的标准值和不确定度。钡矿标准物质中主成分BaCO3含量分别为18.37%、35.32%、53.43%、83.05%,形成一个从边界品位、工业品位、富矿品位到精矿品位较为完整的含量系列,能够满足钡矿勘查、评价和综合开发利用的需求。
TAt present, there are no witherite chemical composition certified reference materials, the closest being of Barite composition. But the accurate concentration values are determined for only small number of elements. Four certified chemical composition reference materials of witherite barium ore were prepared by first collecting samples from Bashan barium mine in Chengkou county, Chongqing city. The samples were crushed until the particles were less than 0.074 mm, and then loaded in a coulter-mixing machine for thorough mixing. Inductively Coupled Plasma-Mass Spectrometry(ICP-MS) and Inductively Coupled Plasma-Atomic Emission Spectrometry(ICP-AES) were conducted for homogeneity and stability testing, For the homogeneity test, the variance test F value was less than the threshold, indicating a good homogeneity. According to JJF 1343—2012 and standard material specifications, 6 qualified laboratories were selected to give certified values and uncertainties of 18 elements, including major, associated, trace elements, by using the combination of classical methods and modern instrumental technologies. The content range of BaCO3 was 18.37%, 35.32%, 53.43%, 83.05%. These reference materials meet the requirements of ilmenite exploration, evaluation and development demand.
TAt present, there are no witherite chemical composition certified reference materials, the closest being of Barite composition. But the accurate concentration values are determined for only small number of elements. Four certified chemical composition reference materials of witherite barium ore were prepared by first collecting samples from Bashan barium mine in Chengkou county, Chongqing city. The samples were crushed until the particles were less than 0.074 mm, and then loaded in a coulter-mixing machine for thorough mixing. Inductively Coupled Plasma-Mass Spectrometry(ICP-MS) and Inductively Coupled Plasma-Atomic Emission Spectrometry(ICP-AES) were conducted for homogeneity and stability testing, For the homogeneity test, the variance test F value was less than the threshold, indicating a good homogeneity. According to JJF 1343—2012 and standard material specifications, 6 qualified laboratories were selected to give certified values and uncertainties of 18 elements, including major, associated, trace elements, by using the combination of classical methods and modern instrumental technologies. The content range of BaCO3 was 18.37%, 35.32%, 53.43%, 83.05%. These reference materials meet the requirements of ilmenite exploration, evaluation and development demand.
引文
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[24]左全周,范琼发,来宏,等.重庆市城口县钡矿资源调查评价[R].重庆市地质矿产勘查开发总公司川东南地质大队,2006.12.
[25]左全周,来宏.重庆市城口县巴山钡矿普查报告[R]重庆市地质矿产勘查开发总公司川东南地质大队,2005.12.
[26]高玉淑.中国地质标准物质的研究和应用[J].地球学报,1996,12(4):249-252.
[27]全国标准物质管理委员会编著.标准物质定值原则和统计学原理[M].北京:中国质检出版社,2011.
[28]冯静,王瑞敏,张激光.重晶石矿石成分分析标准物质研制[J].岩矿测试,2010(2):175-178.
[29]全国标准物质管理委员会.标准物质定值原则和统计学原理[M].北京:中国计量出版社,2011.31-107.
[2]颜茂弘,鲍琪儿,王祖荫,等.岩石标准物质均匀性的XRF检验法[J].岩矿测试,1988,7(1):61-64.
[3]李国会,樊守忠.X射线荧光光谱法在标准物质均匀性检验中的应用[J].地质试验室,1995,11(1):40-43.
[4]李国会.均匀性检验中用X计数与含量计算F值的比较[J].地质试验室,1996,12(4):249-252.
[5]全浩,韩永志.标准物质及其应用技术[M].北京:中国标准出版社,2003,45-126.
[6]岩石矿物分析编委会.岩石矿物分析(第四版第一分册)[M].北京:地质出版社,2011.44-200.427-446.
[7]全国标准物质管理委员会.标准物质的研制管理与应用[M].北京:中国计量出版社,2010:39-110.
[8]《矿产资源工业要求手册》编委会.矿产资源工业要求手册(2014年修订本)[M].北京:地质出版社,2014,491-496.
[9]柯瑞华.化学测量不确定度的估计和表示[J].冶金标准化与质量,2004,24(1):63-68.
[10]韩永志.化学测量不确定度的估计和表示[J].冶金标准化与质量,2009,47(2):35-40.
[11]鄢明才.地球化学标准物质标准值不确定度估算探讨[J].岩矿测试,2001,20(4):287-293.
[12]ISOGuide35:2006,Certificationof Reference MaterialsGeneral and Statistical Principles(3rd Edition)[S].
[13]Kane J S,Potts P J,Wiedenbeck M,Carignan J,Wilson S.International Association of Geoanalysts,protocol for the certification of geochemical and environmental reference material[J].Geostandards and GeoanalyticalResearal,2003,27:227-244.
[14]王璞,潘兆橹,翁玲宝.系统矿物学(上册)[M].北京:地质出版社,1982.315-318.
[15]卢静文,彭晓蕾.金属矿物显微鉴定手册[M].北京:地质出版社,2010.136-147.
[16]C larka SHB,Poole F G,W ang Z C.Comparison of som e sed-iment-hos ted,stratiform barite deposits in China,the United States,and India[J].Ore G eology Review s,2004,24r
[17]M aynard J B,Ok ita P M.Bedded barite deposits in th e United States,Canada,Germany,and China:two m ajortypes based ontectonic setting[J].Economic Geology,1991
[18]Whitford D J,KorschM J,SolomonM.Strontium isotope stud iesof barites:imp lications for the origin of base m etalmineralization in T asm an ia[J].Economic Geology,1992
[19]Habicht K S,Can field D E.Su lfu r isotop e fractionat ion during bacterial sulfate reduction in organ ic-rich sediments[J]Geochimica et CosmochimicaActa,1997.
[20]重庆市地勘局川东南地质大队.重庆市钡矿资源远景调查[R]重庆,1998.
[21]左全周.重庆市成矿区带和矿床成矿系列初步划分[J]重庆地质矿产,2010,2
[22]杨弘忠,左全周.重庆市城口县后裕~左岚地区毒重石矿普查报告[R].重庆市地质矿产勘查开发总公司川东南地质大队,2002.12.
[23]左全周,范琼发,来宏,等.重庆市矿产资源潜力评价毒重石矿资源潜力评价成果报告[R].重庆市地质矿产勘查开发局川东南地质大队,2010.12.
[24]左全周,范琼发,来宏,等.重庆市城口县钡矿资源调查评价[R].重庆市地质矿产勘查开发总公司川东南地质大队,2006.12.
[25]左全周,来宏.重庆市城口县巴山钡矿普查报告[R]重庆市地质矿产勘查开发总公司川东南地质大队,2005.12.
[26]高玉淑.中国地质标准物质的研究和应用[J].地球学报,1996,12(4):249-252.
[27]全国标准物质管理委员会编著.标准物质定值原则和统计学原理[M].北京:中国质检出版社,2011.
[28]冯静,王瑞敏,张激光.重晶石矿石成分分析标准物质研制[J].岩矿测试,2010(2):175-178.
[29]全国标准物质管理委员会.标准物质定值原则和统计学原理[M].北京:中国计量出版社,2011.31-107.