光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
4期
1118-1123
,共6页
不确定度%地质样品%偏振能量色散X射线荧光光谱仪
不確定度%地質樣品%偏振能量色散X射線熒光光譜儀
불학정도%지질양품%편진능량색산X사선형광광보의
Uncertainty%Geological samples%P-EDXRF
建立了一种X射线荧光光谱分析方法分析结果不确定度的评估模式。以大量有可靠值的硅酸盐类地质样品的偏振能量色散X射线荧光光谱的分析结果为研究对象,对27个组分分别采用浓度分段,分别评估不同浓度段内各个组分分析方法精密度引入的相对不确定度(n=6,一个浓度段内各水平相对标准偏差的平均值)和准确度引入的相对不确定度(一个浓度段内各个水平的相对偏差的相对标准偏差),依据误差传递理论,合成精密度和准确度分别引入的相对不确定度得到总的相对不确定度。这种基本模式可以解决一定浓度范围内常规大量类似基体未知地质样品不确定度评估难的问题,不必对每个未知样品的分析结果都进行不确定度的评估,可以从这种模式统计的结果中给出不确定度的值。这种评估模式是一种基本的具有实际应用价值的统计模式,可以为后续的不确定度评估的函数模式的建立提供有力的基础。但是该不确定度评估模式涉及的有可靠值的样品数量较多,难以简单应用到其他基体样品分析结果的不确定度评估。争取以本研究为基础尽快建立一种合理的数理统计函数模式以适用于不同类型样品X射线荧光光谱分析结果不确定度的评估。
建立瞭一種X射線熒光光譜分析方法分析結果不確定度的評估模式。以大量有可靠值的硅痠鹽類地質樣品的偏振能量色散X射線熒光光譜的分析結果為研究對象,對27箇組分分彆採用濃度分段,分彆評估不同濃度段內各箇組分分析方法精密度引入的相對不確定度(n=6,一箇濃度段內各水平相對標準偏差的平均值)和準確度引入的相對不確定度(一箇濃度段內各箇水平的相對偏差的相對標準偏差),依據誤差傳遞理論,閤成精密度和準確度分彆引入的相對不確定度得到總的相對不確定度。這種基本模式可以解決一定濃度範圍內常規大量類似基體未知地質樣品不確定度評估難的問題,不必對每箇未知樣品的分析結果都進行不確定度的評估,可以從這種模式統計的結果中給齣不確定度的值。這種評估模式是一種基本的具有實際應用價值的統計模式,可以為後續的不確定度評估的函數模式的建立提供有力的基礎。但是該不確定度評估模式涉及的有可靠值的樣品數量較多,難以簡單應用到其他基體樣品分析結果的不確定度評估。爭取以本研究為基礎儘快建立一種閤理的數理統計函數模式以適用于不同類型樣品X射線熒光光譜分析結果不確定度的評估。
건립료일충X사선형광광보분석방법분석결과불학정도적평고모식。이대량유가고치적규산염류지질양품적편진능량색산X사선형광광보적분석결과위연구대상,대27개조분분별채용농도분단,분별평고불동농도단내각개조분분석방법정밀도인입적상대불학정도(n=6,일개농도단내각수평상대표준편차적평균치)화준학도인입적상대불학정도(일개농도단내각개수평적상대편차적상대표준편차),의거오차전체이론,합성정밀도화준학도분별인입적상대불학정도득도총적상대불학정도。저충기본모식가이해결일정농도범위내상규대량유사기체미지지질양품불학정도평고난적문제,불필대매개미지양품적분석결과도진행불학정도적평고,가이종저충모식통계적결과중급출불학정도적치。저충평고모식시일충기본적구유실제응용개치적통계모식,가이위후속적불학정도평고적함수모식적건립제공유력적기출。단시해불학정도평고모식섭급적유가고치적양품수량교다,난이간단응용도기타기체양품분석결과적불학정도평고。쟁취이본연구위기출진쾌건립일충합리적수리통계함수모식이괄용우불동류형양품X사선형광광보분석결과불학정도적평고。
Evaluating uncertainty of analytical results with 165 geological samples by polarized dispersive X-ray fluorescence spectrometry (P-EDXRF) has been reported according to the internationally accepted guidelines .One hundred sixty five pressed pellets of similar matrix geological samples with reliable values were analyzed by P-EDXRF .These samples were divided into several different concentration sections in the concentration ranges of every component .T he relative uncertainties caused by pre-cision and accuracy of 27 components were evaluated respectively .For one element in one concentration ,the relative uncertainty caused by precision can be calculated according to the average value of relative standard deviation with different concentration lev -el in one concentration section ,n=6 stands for the 6 results of one concentration level .The relative uncertainty caused by accu-racy in one concentration section can be evaluated by the relative standard deviation of relative deviation with different concentra-tion level in one concentration section .According to the error propagation theory ,combining the precision uncertainty and the accuracy uncertainty into a global uncertainty ,this global uncertainty acted as method uncertainty .This model of evaluating un-certainty can solve a series of difficult questions in the process of evaluating uncertainty ,such as uncertainties caused by complex matrix of geological samples ,calibration procedure ,standard samples ,unknown samples ,matrix correction ,overlap correction , sample preparation ,instrument condition and mathematics model .The uncertainty of analytical results in this method can act as the uncertainty of the results of the similar matrix unknown sample in one concentration section .This evaluation model is a basic statistical method owning the practical application value ,which can provide a strong base for the building of model of the follow-ing uncertainty evaluation function .However ,this model used a lot of samples which cannot simply be applied to other types of samples with different matrix samples .The number of samples is too large to adapt to other type's samples .We will strive for u-sing this study as a basis to establish a reasonable basis of mathematical statistics function mode to be applied to different types of samples .