13C DNP Juice with TEMPOL at 50mM Sample : 6/2/2 DMSO-d6/H2O/D2O + 3M Sodium Acetate and 50mM TEMPOL Topspin folder : 20240205_13C_Acetate and 20240122_13C_HYPSO_2 (for CP build up) Data folder path : Direct 13C DNP : 301 MW 28,17 GHz w freq mod without echo is 300 CP-DNP : without flipback 205 (8NS) @ 28,15 GHz —> E = comp to 209 Direct 13C DNP T build up : 305 using satrec under DNP until 50 s 12 s at 28,22 GHz w freq mod from -2800 ppm. to -3050 ppm General model: val(t) = a*(1-exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 12.18 (10.43, 13.94) a = 1.083 (1.02, 1.147) d = -0.04458 (-0.07104, -0.01813) T1 13C : 211 delay incremented after CP delay from until 50 s at 28,22 GHz w freq mod From 5880 to 5620 ppm General model: val(t) = a*(exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 12.03 (10.3, 13.76) a = 1.399 (1.318, 1.481) d = -0.284 (-0.3274, -0.2406) CP DNP build up : 202 (wit DNP juice !! wrong title. But wrong sample positioning this day) MW 28,16 GHz w freq mod from -8660 to -8900 ppm General model: val(t) = a*(1-exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 0.6656 (0.6019, 0.7294) a = 0.9957 (0.962, 1.029) d = -0.01011 (-0.03077, 0.01056)

Spectroscopic Data DNP 1T 77K 1H DNP Juice with TEMPOL at 50mM Sample : 6/2/2 DMSO-d6/H2O/D2O 200µL Topspin Folder : 20231102_HDNPjuice_50mM_CB Note : no phc1 in the data processing not to affect the integral as we have a broad signal TE : 100 / 200 / 300 substraction of the 100 TE and 1000 BG with Topspin —> exp 1 For 200 w BG1000 —> exp 2 proc 999 For 300 w BG1000 —> exp 3 proc 999 DNP : 105 / 205 / 305 MW 28,16 GHz ± 20 MHz @ 60 kHz E 105 (comp to 2) : 110 E 205 (comp to 3) : 97 E 305 (comp to 4) : 95 T build up with satrec : 206 28,18 GHz no fmod General model: val(t) = a*(1-exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 0.5164 (0.4523, 0.5805) a = 0.7312 (0.6996, 0.7628) d = 0.3518 (0.3163, 0.3873) T1 : 207 satrec experiment at TE General model: val(t) = a*(1-exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 0.5067 (0.4584, 0.555) a = 0.7826 (0.7567, 0.8085) d = 0.2713 (0.2458, 0.2967)

13C HYPSO NL-104A at 43 µmol/cm3 of TEMPOL Sample : 8/2 D2O/H2O + 3.00M acetate 42 µL impregnated in 66.6 mg of HYPSO Topspin Folder : 20240205_13C_Acetate CP-DNP : without flipback 405 at 28,35 GHz T CP build up : General model: val(t) = a*(1-exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 0.8274 (0.7077, 0.9471) a = 0.9999 (0.9465, 1.053) d = -0.004187 (-0.03447, 0.0261) with 403 MW 28,32 GHz w freq mod with satrec, flipback and echo from -2280 to -2550 ppm 13C DNP buildup / T1 : 408 delay incremented after CP delay from until 60 s at 28,35 GHz w freq mod From 6592 to 6360 ppm General model: val(t) = a*(exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 18.26 (16.55, 19.98) a = 1.008 (0.9698, 1.046) d = -0.01884 (-0.05639, 0.0187)

1H HYPSO NL-104A at 43 µmol/cm3 of TEMPOL Sample : 8/2 D2O/H2O 46,4µL impregnated in 73,7 mg HYPSO Topspin Folder : 20231116_1H_HYPSO_43 TE : 10 for quantification (proc 997 of exp1) : subtracted from background 1000 (with lb 1000Hz) for plot 10 (proc 998 exp 1 phased 0) DNP : 105 MW 28,17 GHz ± 20 MHz with frequency modulation @ 60kHz E = 62 (comp to proc 997 and with lb 1000 Hz) T build up with satrec : 106 T1 : 107 satrec experiment at TE General model: val(t) = a*(1-exp(-(t)/T)+d) Coefficients (with 95% confidence bounds): T = 0.8797 (0.6137, 1.146) ± 0,27 a = 0.828 (0.7287, 0.9273) d = 0.208 (0.1427, 0.2732)