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Spectroscopic Techniques for in situ non invasive Study of Natural Dyestuffs

Centre of Excellence SMAArt University of Perugia, Italy. CNR – ISTM (Institute of Molecular Sciences and Technologies). Spectroscopic Techniques for in situ non invasive Study of Natural Dyestuffs. Costanza Miliani. Catia Clementi, PhD student Brenda Doherty, PhD student

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Spectroscopic Techniques for in situ non invasive Study of Natural Dyestuffs

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  1. Centre of Excellence SMAArt University of Perugia, Italy CNR – ISTM (Institute of Molecular Sciences and Technologies) Spectroscopic Techniques for in situ non invasive Study of Natural Dyestuffs Costanza Miliani

  2. Catia Clementi, PhD student Brenda Doherty, PhD student Alessandro Sassolini, fellowship

  3. How to study in situ natural dyestuffs ? • XRF : elemental analysis of mordents and chelation ions • FTIR : molecular analysis of mordents and chelant • UV-vis abs : color characterization • UV-vis fluo : dye characterization MOLAB equipments and lab spectrofluorimeter (Varian)

  4. I. Non invasive portable equipments: x-ray fluorescence The X-ray fluorescence portable equipment for in situ measurements, ismade up by: 1. open beam X-ray generator (W target, excitation energy Lb=9.671 keV); 2. non-cryogenic silicon drift detector SDD having resolution of 130 eV at 5.9 keV.

  5. Remspec mid-IR fiber optic sampling probe: 19 chalcogenide glass fibers spectral range: 900-4000 cm-1  best S/N from 900 to 2000 cm–1 abs of Se-H between 2050 and 2250 cm-1 I. Non invasive portable equipments:fiber optic mid-FTIR portable JASCO VIR 9500 spectophotometer: Midac Illuminator IR radiation source Michelson interferometer liquid nitrogen cooled MCT it is easily portable: weight ~35 Kg volume 50x50x50 cm3 optical layout: 0°/0° geometry probe surface distance 2-5 mm

  6. I. Non invasive portable equipments: UV-vis fluorescence A. Exciting light source: 175 W Xenon lamp, 240-650 nm emission. B. H-10 Jobin Yvon UV monochromator for selecting the excitation wavelength. C. Quartz fibre-optic Y cable D.CCD spectrometer Avantes AvaSpec-2048 pixels (200-1100 nm) of high sensitivity (86 photons/counting). E. Optical filters (interference and cut-on filter) are used to cut-off 2nd order scatter and stray light.

  7. 1. weld lakes

  8. XRF: the mordant W1: Ca, W2: Ca, W3: Ca & K

  9. mid FTIR: the mordant

  10. mid FTIR: the mordant

  11. mid FTIR: the mordant OH comb. band 5160

  12. UV-vis absorption: the colour

  13. UV-vis fluorescence: the lake Normalized emission spectra of weld lakes (lexc:366 nm)

  14. 3D UV-vis fluorescence: the lake Exc. 250-400 nm

  15. 550 weld1 weld2 525 weld3 3D UV-vis fluorescence: the lake

  16. UV-vis fluorescence: the lake

  17. Summary Complex luteolin:Al lmax fluo = 540 nm Complex apigenin:Al lmax fluo = 523 nm Complex luteolin:Mg lmax fluo = 520 nm O.S. Wolfbeis et al. Z. Naturforsc 39b, 231-237, 1983

  18. 1. textiles

  19. XRF: the mordant

  20. XRF: the mordant

  21. mid FTIR: the textile

  22. UV-vis absorption: the colour

  23. UV-vis absorption: the colour

  24. UV-vis fluorescence: wavelenght effect (bath 4)

  25. UV-vis fluorescence: dyed Silk bath effect

  26. 3D UV-vis fluorescence: dyed Silk Bath 3 Bath 4

  27. UV-vis fluorescence: dyed wool bath 1

  28. dyed wool Bath 1 Exc. 250-390 Exc. 450-560

  29. UV-vis fluorescence: dyed wool bath 2

  30. dyed wool bath 2 Exc. 250-390 Exc. 450-560

  31. Summary

  32. UV-vis fluorescence: the lake

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