Raman spectroscopy for real-time and in situ monitoring of mechanochemical milling reactions

Extended Data Fig. 1

ATR-IR of reactants na, sal and resulting na:sal cocrystal.

Extended Data Fig. 2 Rietveld refinement of PXRD pattern (X-ray source: CuKα) of the resulting na:sal cocrystal after 60 min milling.

CSD code of the used structural model: SODDOF. Color scheme: blue—experimental PXRD pattern, red—refinement, gray—difference.

Extended Data Fig. 3 Selected Raman spectra from the monitoring experiment.

Lines indicate the Raman bands of interest for qualitative monitoring of the reaction progress.

Extended Data Fig. 4

The plot of in situ collected Raman spectra stored in variable SpectraAll before spike corrections.

Extended Data Fig. 5

The plot of in situ collected Raman spectra stored in variable SpectraAll after spike corrections.

Extended Data Fig. 6

The plot of in situ collected Raman spectra stored in variable Spectra after the subtraction of the PMMA contribution.

Extended Data Fig. 7 The plot of in situ collected Raman spectra stored in variable sp after defining spectral and temporal range.

Note that spectral range is now in the range from first_wnmb up to last_wnmb .

Extended Data Fig. 8

a , b , Examples of the baseline correction of selected in situ Raman spectra at 1 min ( a ) and 50 min ( b ) into milling experiment. Color code: blue—experimental Raman spectrum, orange—baseline estimation.

Extended Data Fig. 9

The plot of in situ collected Raman spectra stored in variable Nsp after the baseline correction.

Extended Data Fig. 10 The plot of in situ collected Raman spectra stored in variable N1sp after normalization.

Note the different scale on y -axis when compared with the nonnormalized spectra in Extended Data Fig. 9 .

Supplementary Information

Supplementary Figs. 1–3.

Reporting Summary

Supplementary Data 1

Experimental Raman spectra and GNU Octave scripts.