TY - JOUR A1 - Kanngießer, B. A1 - Mantouvalou, I. A1 - Malzer, W. A1 - Wolff, Timo A1 - Hahn, Oliver T1 - Non-destructive, depth resolved investigation of corrosion layers of historical glass objects by 3D Micro X-ray fluorescence analysis JF - Journal of analytical atomic spectrometry N2 - 3D Micro X-ray fluorescence analysis was used for the investigation of reverse-glass paintings. The material-specific combination used in reverse-glass paintings leads to damage phenomena reinforced by glass corrosion. To elucidate the mechanism of corrosion processes taking place in the glass object depth profiles of mobile elements are of interest. In order to obtain elemental depth profiles of such kind of fragile objects the method of choice should be non-destructive. Our first results demonstrate the usefulness of the 3D Micro-XRF measurements for this kind of investigations. The assumption that certain binding media may initiate corrosion processes beginning at the interface glass/binding material could be confirmed. KW - Cultural heritage KW - 3D-micro XRF KW - Glass corrosion KW - Quantification PY - 2008 DO - https://doi.org/10.1039/b717286a SN - 0267-9477 SN - 1364-5544 VL - 23 SP - 814 EP - 819 PB - Royal Society of Chemistry CY - London AN - OPUS4-17544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Oliver A1 - Wilke, M. A1 - Wolff, Timo T1 - Influence of aqueous calcium phytate/calcium hydrogen carbo-nate treatment on the chemical composition of iron gall inks JF - Restaurator : international journal for the preservation of library and archival material KW - Archaeometry KW - Restoration KW - Conservation KW - Cultural heritage KW - Iron gall inks PY - 2008 SN - 0034-5806 SN - 1865-8431 VL - 29 SP - 155 EP - 162 PB - Saur CY - München AN - OPUS4-18573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bjeoumikhov, A. A1 - Erko, M. A1 - Bjeoumikhova, Zemfira A1 - Erko, A. A1 - Snigireva, I. A1 - Snigirev, A. A1 - Wolff, Timo A1 - Mantouvalou, I. A1 - Malzer, W. A1 - Kanngießer, B. T1 - Capillary µFocus X-ray lenses with parabolic and elliptic profile JF - Nuclear instruments and methods in physics research A KW - Synchrotron radiation KW - Capillary optics KW - Beamline optics PY - 2008 DO - https://doi.org/10.1016/j.nima.2008.01.087 SN - 0168-9002 SN - 0167-5087 VL - 587 IS - 2-3 SP - 458 EP - 463 PB - North-Holland CY - Amsterdam AN - OPUS4-18922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolff, Timo A1 - Mantouvalou, I. A1 - Malzer, W. A1 - Nissen, J. A1 - Berger, D. A1 - Zizak, I. A1 - Sokaras, D. A1 - Karydas, A. A1 - Grlj, N. A1 - Pelicon, P. A1 - Schütz, R. A1 - Zitniki, M. A1 - Kanngießer, B. T1 - Performance of a polycapillary halflens as focussing and collecting optic - a comparison JF - Journal of analytical atomic spectrometry N2 - Polycapillary halflenses are widely used to focus X-ray radiation onto a small spot. Additionally they can reduce the field of view of a semiconductor detector when placed in front of one. In 3D micro X-ray fluorescence spectroscopy (3D Micro-XRF) with synchrotron radiation, two polycapillary halflenses are used in a confocal geometry. Up until now, characterization measurements in the focal plane have only been performed in the case of the lens focusing parallel radiation. Assumptions have been made, that in the other case, when isotropic radiation from a spot source is transported to a detector, the acceptance distribution in the focal plane is also Gaussian. We performed measurements with an electron beam as well as a proton beam which confirm this assumption. In addition, a comparison between measurements in collecting and focusing mode show differences in spot size and transmission. These differences exemplify the fact that there is not one global spot size or transmission function of a polycapillary halflens. Illumination and divergence effects can alter both characteristic lens parameters. PY - 2009 DO - https://doi.org/10.1039/b817828c SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 669 EP - 675 PB - Royal Society of Chemistry CY - London AN - OPUS4-19415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mantouvalou, I. A1 - Lange, K. A1 - Wolff, Timo A1 - Grötzsch, D. A1 - Lühl, Lars A1 - Haschke, M. A1 - Hahn, Oliver A1 - Kanngießer, B. T1 - A compact 3D micro X-ray fluorescence spectrometer with X-ray tube excitation for archaeometric applications JF - Journal of analytical atomic spectrometry N2 - In this work, the applicability of a new 3D micro X-ray fluorescence (3D Micro-XRF) laboratory spectrometer for the investigation of historical glass objects is demonstrated. The non-destructiveness of the technique and the possibility to measure three-dimensionally resolved fluorescence renders this technique into a suitable tool for the analysis of cultural heritage objects. Although absorption and resolution effects complicate qualitative analysis of the data, layered structures can be distinguished from homogeneous samples without the need for full quantification. Different manufacturing techniques were studied in this work with the help of hand-made reference samples. With the gained knowledge it could be shown for the investigated historical glass object, that black enamel as a stained glass contour colour was used in a cold painting. The object was not fired after the application of the black enamel, but instead the adhesion of the paint was solely provided through organic binding agents and the backing with metal foils. Thus, for the manufacturing of the object, a mixture of cold painting technique with a stained glass color was used. Quantitative measurements with a 3D Micro-XRF setup at the Berlin synchrotron BESSY II confirm the assumptions drawn on the basis of the qualitative investigation with the 3D Micro-XRF spectrometer with X-ray tube excitation. KW - 3D micro XRF KW - Archaeometry KW - Non-destructive testing KW - Cultural heritage PY - 2010 DO - https://doi.org/10.1039/b915912f SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 554 EP - 561 PB - Royal Society of Chemistry CY - London AN - OPUS4-20878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - TY - JOUR A1 - Dietz, G. A1 - Ketelsen, T. A1 - Hoss, M. A1 - Simon, O. A1 - Wintermann, C. A1 - Wolff, Timo A1 - Rabin, Ira A1 - Hahn, Oliver T1 - The Egmont master phenomenon: X-ray fluorescence spectrometric and paper studies for art history research JF - Analytical and bioanalytical chemistry N2 - The aim of the research project 'Typology of Dutch Drawing' was to establish an interdisciplinary approach for investigating heterogeneous drawing collections. To define a type common to a group of drawings, we determine elements that are common to them based on style and the use of identical materials. To that end, we investigated about 750 Dutch drawings from the sixteenth century at the Dresden Kupferstich-Kabinett using art historical and scientific methods. In this work, we present a detailed analysis of 30 drawings ascribed to the Egmont Master. KW - Archeometry KW - Fine arts KW - Nondestructive testing KW - Paper analysis KW - X-ray fluorescence spectrometry (XRF) KW - Reference materials PY - 2012 DO - https://doi.org/10.1007/s00216-011-5309-4 SN - 1618-2642 SN - 1618-2650 VL - 402 IS - 4 SP - 1505 EP - 1515 PB - Springer CY - Berlin AN - OPUS4-25510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolff, Timo A1 - Rabin, Ira A1 - Montouvalou, I. A1 - Kanngießer, B. A1 - Malzer, W. A1 - Kindzorra, Emanuel A1 - Hahn, Oliver T1 - Provenance studies on Dead Sea scrolls parchment by means of quantitative micro-XRF JF - Analytical and bioanalytical chemistry N2 - In this study, we address the question of the provenance and origin of the Dead Sea Scrolls manuscripts. A characteristic low ratio of chlorine to bromine, corresponding to that of the Dead Sea water, may serve as an indicator for local production. For this aim we developed a non-destructive procedure to determine the Cl/Br ratio in the parchment of these manuscripts. Micro-X-ray fluorescence (µ-XRF) measurements of a large number of parchment and leather fragments from the Dead Sea Scrolls were analyzed with a routine we developed based on fundamental parameter quantification. This routine takes into account the absorption of the collagen matrix and the influence of the different sample thicknesses. To calculate the representative Cl/Br ratio for each fragment, we investigated the lateral homogeneity and determined the total mass deposition using the intensity of the inelastically scattered, characteristic tube radiation. The distribution of the Cl/Br ratios thus obtained from the µ-XRF measurements make it possible to distinguish fragments whose origin lies within the Dead Sea region from those produced in other locations. KW - Fundamental parameter quantification KW - Samples of intermediated thickness KW - Chlorine to bromine ratio KW - Scatter peak evaluation KW - Dark matrix KW - Inorganic traces KW - Archaeometry KW - Fine arts KW - Inorganic compounds KW - Trace elements KW - X-ray spectroscopy PY - 2012 DO - https://doi.org/10.1007/s00216-011-5270-2 SN - 1618-2642 SN - 1618-2650 VL - 402 IS - 4 SP - 1493 EP - 1503 PB - Springer CY - Berlin AN - OPUS4-25511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -