TY - JOUR A1 - Mantouvalou, I. A1 - Wolff, Timo A1 - Hahn, Oliver A1 - Rabin, Ira A1 - Lühl, Lars A1 - Pagels, M. A1 - Malzer, W. A1 - Kanngiesser, B. T1 - 3D Micro-XRF for cultural heritage objects: new analysis strategies for the investigation of the Dead Sea scrolls JF - Analytical chemistry N2 - A combination of 3D micro X-ray fluorescence spectroscopy (3D micro-XRF) and micro-XRF was utilized for the investigation of a small collection of highly heterogeneous, partly degraded Dead Sea Scroll parchment samples from known excavation sites. The quantitative combination of the two techniques proves to be suitable for the identification of reliable marker elements which may be used for classification and provenance studies. With 3D micro-XRF, the three-dimensional nature, i.e. the depth-resolved elemental composition as well as density variations, of the samples was investigated and bromine could be identified as a suitable marker element. It is shown through a comparison of quantitative and semiquantitative values for the bromine content derived using both techniques that, for elements which are homogeneously distributed in the sample matrix, quantification with micro-XRF using a one-layer model is feasible. Thus, the possibility for routine provenance studies using portable micro-XRF instrumentation on a vast amount of samples, even on site, is obtained through this work. KW - Archaeometry KW - 3D X-ray spectroscopy PY - 2011 DO - https://doi.org/10.1021/ac2011262 SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 16 SP - 6308 EP - 6315 PB - American Chemical Society CY - Washington, DC AN - OPUS4-25209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolff, Timo A1 - Malzer, W. A1 - Mantouvalou, I. A1 - Hahn, Oliver A1 - Kanngießer, B. T1 - A new fundamental parameter based calibration procedure for micro X-ray fluorescence spectrometers JF - Spectrochimica acta B N2 - Fundamental parameter based quantification of X-ray fluorescence (XRF) measurement data requires an accurate knowledge of the spectrometer parameters, including the spectral distribution of the excitation radiation. In case of micro-XRF where a polycapillary optic is utilized in the excitation channel this distribution is changed due to the transmission properties of the lens. A new calibration procedure, based on fluorescence data of thin standard samples, was developed to determine the excitation spectrum, i.e., the product of the X-ray tube spectrum and the transmission of the used X-ray optic of a micro-XRF setup. The calibration result was validated by the quantitative analyses of certified multi-element reference standards and shows uncertainties in the order of 2% for main components, 10% for minor elements and 25% for trace elements. The influence of secondary order effects like Coster–Kronig transitions and cascade effects is analyzed and the accuracy of fundamental parameters in common databases is discussed. KW - Polycapillary optic KW - Transmission KW - Micro-XRF calibration KW - Reference free quantification PY - 2011 DO - https://doi.org/10.1016/j.sab.2011.01.009 SN - 0584-8547 SN - 0038-6987 VL - 66 IS - 2 SP - 170 EP - 178 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-24213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -