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Results of HPLC and SEM-EDX analysis

Results of HPLC and SEM-EDX analysis. - Dyed textiles - Dye bath - Organic pigments. Maarten van Bommel. Report of HPLC analysis (ICN). ICN report usually exist of: - Summary - Introduction, aim of the research - General description of the work done - Results and discussion

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Results of HPLC and SEM-EDX analysis

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  1. Results of HPLC and SEM-EDX analysis - Dyed textiles - Dye bath - Organic pigments Maarten van Bommel

  2. Report of HPLC analysis (ICN) ICN report usually exist of: - Summary - Introduction, aim of the research - General description of the work done - Results and discussion - Conclusion - References and additional information - Analytical reports - Microscopy - FTIR - XRF - GC-MS - HPLC-PDA - SEM-EDX

  3. Report of HPLC analysis (ICN) Analytical report (HPLC): - Information about the sample and object - Short description of the procedure used - Graph at wavelength were most components of interest shows VIS absorption - Spectra of the components found - Discussion of the results

  4. 0.35 0.30 0.25 0.20 0.15 0.10 0.05 0.00 HPLC-PDA Chromatogram 16.683 Absoption at 350nm (AU) 15.469 20.812 17.985 22.069 5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 50.00 Retention time (min)

  5. UV-VIS spectra Luteolin-3’,7- diglucoside Apigenin glucoside? Luteolin Apigenin Luteolin-7- glucoside

  6. Results and Discussion • Description of the components identified • Explanation which dye source is identified • Explanation about unknown components • Explanation about un-assigned peaks Conclusion -Usually a short description of the dye source identified

  7. 0.35 0.30 0.25 20.906 0.20 0.15 22.165 0.10 0.05 0.00 HPLC-PDA Chromatogram Absoption at 350nm (AU) 5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 50.00 Retention time (min)

  8. HPLC-PDA Chromatogram

  9. Results Textile samples • -Luteolin and Apigenin found (99,5%) • Other flavonoids at low concentration • Ratio luteolin and apigenin calculated at 350 nm • Just to compare the samples Wool, weld and potash (quadruple) Ratio luteolin:apigenin 90:10 Rsd area luteolin and apigenin 9% Rsd ratio luteolin:apigenin 2% Wool, weld only (duplo) 10% more dyestuff Ratio luteolin:apigenin 88:12

  10. Results Textile samples Silk, weld and potash -Amount dyestuff compare to wool 30% -Ratio luteolin:apigenin 95:5 Silk, weld only -Amount dyestuff compared to wool the same -Ratio luteolin:apigenin 86:13

  11. Results Textile samples Wool was also extracted with formic acid -Only 35% dyestuff extracted (compared to HCL) -Luteolin is main component -Luteolin 3’,7-diglucoside found -Luteolin 7 glucodide found Wool was also extracted with EDTA -Only 25% dyestuff extracted (compared to HCL) -Luteolin is main component -Luteolin 3’,7-diglucoside found -Luteolin 7 glucodide found

  12. Results pigment samples -Luteolin and Apigenin main components -Two other flavonoids were found as well (unidentified) -Amount organic colorant in pigment pigment 1>pigment3.2>pigment2>pigment 3

  13. Results pigment samples Ratio Luteolin: apigenin: unknowns P1 87% 11% 2% P2 67% 10% 23% P3.1 76% 19% 4% P3.2 84% 12% 4%

  14. Results SEM-EDX Elements found in wool -Sulphur (from the protein) -Traces of aluminium (mordant) -Traces of calcium (also in untreated wool) Elements found in silk -No mordant was found! Elements found in the pigments P1 – not analysed P2 – Calcium and trace aluminium P3 – Aluminium and trace of calcium

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