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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.
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.