CAJ | 학술논문

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，SiO2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SiO2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，SiO2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。
목전파서、영국、일본、남비등국연제유일사석영암류표준물질，SiO2함량균재96％이상，함량범위교착，정치원소교소。아국상무석영암류적표준물질，무법만족석영암감사화실제응용적수요。본문연제료3개석영암화학성분분석표준물질，양품채자아국구유대표성적안휘성봉양현대묘진로청산、청해성대통현경양진화호북성기춘현령규산3개석영광구，이용류화상식기류분쇄궤장양품세쇄지－45μm，해결료순도교고적석영암분쇄가공역수오염적난제。인석영암양품난이압제성형，균균성검험미채용압편제양X사선형광광보법，이시채용이전감우합등리자체발사광보법화전감우합등리자체질보법위주적검험방법。결과표명，방차검험적F치균소우림계치，증명기균균성부합요구。위기량년적장기은정성8차검험중미발현통계학의의상적명현변화，재전진화겁단온도조건하소검험적단기은정성량호。경아국10가실험실사용다충분석방법연합정치，동시탐색채용유사원소비교법획취미진행균균성화은정성검험적성분적상응불학정도분량，급출료36개성분적인정치（혹삼고치）화상응적불학정도。3개표준물질현이피비준위국가일급표준물질（편호GBW 07835、GBW 07836、GBW 07837），기주요성분SiO2적함량상응위92．93％、95．97％、99．18％，정제도분포。차계렬표준물질구유양품립도균균、립도분포범위착（D25～D75재4～16μm지간），정치원소충류다，SiO2함량분포엄범적특점，가이만족석영암양품화학성분분석질량감공적수요。
At present,quartzitic reference materials are prepared by Brazil,England,Japan,and South Africa but are not in series. The SiO2 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 Plasma-Mass 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 1 0 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 , GBW07836 and GBW 07837),with 92.93%,95.97% and 99.18% of SiO2,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 -1 6 μm ), multiple value determined elements, and wide-range distribution of SiO2 content,which should meet the monitoring requirements of chemical composition analysis of quartzite samples.