Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis
Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis
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DOI：
10.1016/j.sab.2004.09.001
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发表时间：
2004-12
期刊：
影响因子：
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通讯作者：
D. Papadopoulou;G. Zachariadis;A. Anthemidis;N. Tsirliganis;J. Stratis
中科院分区：
文献类型：
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作者：
D. Papadopoulou;G. Zachariadis;A. Anthemidis;N. Tsirliganis;J. Stratis
采用两种多元仪器分析方法--微X射线荧光光谱仪(Micro-XRF)和电感耦合等离子体原子发射光谱仪(ICP-AES)对公元前7世纪和公元前5世纪的古陶瓷碎片进行了分析，以评价这两种方法的优劣，并评价了目前紧凑、便携的微型XRF仪器用于古陶瓷原位分析的可能性。令人感兴趣的区别因素是，微型XRF光谱分析提供了非破坏性分析的可能性，这是文物成分分析中最重要的一个方面。首先直接对陶瓷碎片进行微XRF测量，除表面清洗(对碎片进行微XRF)外，不进行任何特殊的预处理；然后对为每个陶瓷碎片制备的压制颗粒盘(对颗粒进行微XRF)进行测量。对于元素的电感耦合等离子体原子发射光谱分析，样品溶液是在封闭的高压PFA容器中应用微波消解程序制备的。同时，将标准物质SARM69用于微型XRF仪器的效率校准，并用两种方法对其进行了分析。为了验证定标结果，对标准物质NCS DC 73332和SRM620以及标准物质AWI-1和PRI-1进行了微区X射线荧光分析。用三种分析方法(电感耦合等离子体原子发射光谱分析、碎片微X射线荧光分析和小球微X射线荧光分析)测定的元素浓度经相关分析和学生t检验(95%可信水平)进行统计学处理。
Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level).