Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis
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1 Supporting Information Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis * frederik.vanmeert@uantwerpen.be Table of Contents RESULTS AND DISCUSSION... S-2 PDF codes... S-2 Quantitative information Diffractograms of the lead white regions... S-3 Quantitative information Lead white in bottom cartouches... S-4 Quantitative information Diffractograms in the scrollwork... S-5 Depth-selective information Different experimental configurations... S-6 Depth-selective information Vegetal and floral decorations... S-7 REFERENCES... S-8 S-1
2 RESULTS AND DISCUSSION PDF codes Table S-1 Overview of reference diffraction files Compound Formula AMCSD code a Azurite 2CuCO 3.Cu(OH) Malachite CuCO 3.Cu(OH) Quartz SiO Barite BaSO Gold Au Cinnabar HgS Calcite CaCO Gypsum CaSO 4.2H 2 O Lead Tin Yellow Pb 2 SnO 4 Gavarri (1981) 1 Massicot o-pbo Hydrocerussite 2PbCO 3.Pb(OH) Cerussite PbCO a American Mineralogist Crystal structure database 2 S-2
3 Quantitative information Diffractograms of the lead white regions Figure S-1 X-ray diffractograms and diffraction images of single data points located in (A) a pink corolla, (B) a grey-white highlight and (C) in a green leaf (respectively from the red, blue and green regions in the lead white false color image, Figure 2E in main text). S-3
4 Quantitative information Lead white in bottom cartouches Figure S-2 Photographs of the bottom cartouche depicted (A) on the front side and (B) on the back side (mirrored) of the parchment. Detail region of the compound-specific distribution images obtained for (C) hydrocerussite and (D) cerussite (step size: mm 2 ; dwell time: 0.2 s). Whiter tones indicate a higher scaling parameter. The green and red dashed lines are added to highlight the different pictorial features visible in (A) and (B). (E) False color image of the lead white distribution using the color scheme shown in the histogram (scale bar = 5 mm). (F) Histogram of the HC/(HC+C) ratios. A threshold based on the hydrocerussite scaling parameter was employed to remove data points in which lead white was not detected. The histogram was constructed from 1523 individual XRPD patterns. S-4
5 Quantitative information Diffractograms in the scrollwork Figure S-3 X-ray diffractograms and diffraction images of single data points located in the blue and golden scrollwork from the (A) green and (B) red regions in the azurite false color image (see Figure 3 in main text). S-5
6 Depth-selective information Different experimental configurations Figure S-4 (A) Angular shift in function of the momentum transfer Q calculated for different primary energies (d = 100 µm; z = 75 mm). The inset covers the entire Q-range for the different energies up to 90 2θ. (B) Angular shift of the LaB 6 (110) reflection in function of the sample-detector distance (z) calculated for different energies (d = 100 µm; Q = nm - 1 ). (C) Angular shift in function of the momentum transfer Q calculated for different configurations (d = 100 µm). The inset covers the entire Q-range for the different configurations up to 90 2θ. (D) The displacement resulting from a peak shift of the LaB 6 (110) reflection that equals the angular resolution of each configuration. A description of the different configurations is given in the companion paper 3 (this study: configuration 9). All calculations were performed based on Eq. 1 given in the main paper. S-6
7 Depth-selective information Vegetal and floral decorations Figure S-5 False color images of the (A) cinnabar, (B) lead tin yellow, (C) malachite, (D) massicot, (E) hydrocerussite and (F) cerussite distributions (scale bar = 10 mm). The histograms of the displacements for (G) cinnabar, (H) lead tin yellow, (I) malachite, (J) massicot, (K) hydrocerussite and (L) cerussite show the color schemes that were used. A threshold based on the scaling parameter was employed to remove data points in which the compounds are not present. S-7
8 REFERENCES (1) Gavarri, J. R.; Vigouroux, J. P.; Calvarin, G.; Hewat, A. W. J. Solid State Chem. 1981, 36, (2) Downs, R. T.; Hall-Wallace, M. Am. Mineral. 2003, 88, (3) Vanmeert, F.; De Nolf, W.; De Meyer, S.; Dik, J.; Janssens, K.; Anal. Chem S-8
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