摘要
目前巴西、英国、日本、南非等国研制有一些石英岩类标准物质,Si O2含量均在96%以上,含量范围较窄,定值元素较少。我国尚无石英岩类的标准物质,无法满足石英岩勘查和实际应用的需要。本文研制了3个石英岩化学成分分析标准物质,样品采自我国具有代表性的安徽省凤阳县大庙镇老青山、青海省大通县景阳镇和湖北省蕲春县灵虬山3个石英矿区,利用流化床式气流粉碎机将样品细碎至-45μm,解决了纯度较高的石英岩粉碎加工易受污染的难题。因石英岩样品难以压制成型,均匀性检验未采用压片制样X射线荧光光谱法,而是采用以电感耦合等离子体发射光谱法和电感耦合等离子体质谱法为主的检验方法。结果表明,方差检验的F值均小于临界值,证明其均匀性符合要求。为期两年的长期稳定性8次检验中未发现统计学意义上的明显变化,在颠震和极端温度条件下所检验的短期稳定性良好。经我国10家实验室使用多种分析方法联合定值,同时探索采用类似元素比较法获取未进行均匀性和稳定性检验的成分的相应不确定度分量,给出了36个成分的认定值（或参考值）和相应的不确定度。3个标准物质现已被批准为国家一级标准物质（编号GBW 07835、GBW 07836、GBW 07837）,其主要成分Si O2的含量相应为92.93%、95.97%、99.18%,呈梯度分布。此系列标准物质具有样品粒度均匀、粒度分布范围窄（D25-D75在4-16μm之间）,定值元素种类多,Si O2含量分布广泛的特点,可以满足石英岩样品化学成分分析质量监控的需要。
At present,quartzitic reference materials are prepared by Brazil,England,Japan,and South Africa but are not in series. The Si O2 contents in these reference materials are generally above 96% and accurate concentration values are determined for only small number of elements. To date,no quartzitic reference material has been prepared in China,which cannot meet the demand of quartzite exploration and practical applications. In this study,three quartzitic reference materials were developed with samples from representative quartz mining areas,namely Damiao Town, Fengyang County, Anhui Province; Jingyang Town, Datong County, Qinghai Province; and Lingqiu mountain,Qichun County,Hubei Province. The samples were finely crushed to- 45 μm with a fluidized bed-type airflow crusher to prevent sample contamination. Homogeneity and stability testing was conducted chiefly by Inductively Coupled Plasma-Atomic Emission Spectrometry and Inductively Coupled PlasmaMass Spectrometry rather than X-ray Fluorescence Spectrometry with tablet sample preparation,which results in the quartzite material being difficult to mould. F values for the variance test were less than the threshold,which indicated a good homogeneity. No significant statistical changes were observed in eight two-year stability tests. The short-term stability analysis in the condition of extreme temperatures and vibration were also consistent. Determined values were certified by 10 laboratories in China with multiple methods. For components without homogeneity and stability tests,values and relative uncertainty of 36 components were obtained by comparing similar elements. The three quartzitic reference materials have been approved as national standard reference materials（ GBW 07835,GBW 07836 and GBW 07837）,with 92. 93%,95. 97% and 99. 18% of Si O2,respectively,as a gradient distributed series. The series of reference materials has the characteristics of uniform grading,narrow diameter distribution（ D25- D75 ranged between 4- 16 μm）, multiple value determined ele
出处
《岩矿测试》
CAS
CSCD
北大核心
2014年第6期849-856,共8页
Rock and Mineral Analysis
基金
国土资源公益性行业科研专项(200911044-05)
关键词
石英岩
标准物质
均匀性
稳定性
电感耦合等离子体发射光谱法
电感耦合等离子体质谱法
quartzite
standard reference material
homogeneity
stability
Inductively Coupled Plasma-Atomic Emission Spectrometry
Inductively Coupled Plasma-Atomic Emission Spectrometry-Mass Spectrometry
