EY/Cu mediated photo-ATRP of OEOMA500 with varying degrees of polymerizationa.
No. | [OEOMA500]/[HOBiB]/[EYH2]/[CuBr2]/[TPMA] | [HOBiB] (mM) | Conv.b (%) | M n,th | M n,abs c | M n,app d | Đ d |
---|---|---|---|---|---|---|---|
1 | 50/1/0.0025/0.05/0.15 | 6.0 | 74 | 18 500 | 16 500 | 17 000 | 1.22 |
2 | 100/1/0.005/0.1/0.3 | 3.0 | 81 | 40 500 | 38 000 | 34 000 | 1.16 |
3 | 200/1/0.01/0.2/0.6 | 1.5 | 84 | 84 000 | 79 500 | 62 000 | 1.15 |
4 | 400/1/0.02/0.4/1.2 | 0.75 | 79 | 158 000 | 179 000 | 121 000 | 1.16 |
5 | 600/1/0.03/0.6/1.8 | 0.5 | 73 | 219 000 | 305 000 | 188 000 | 1.16 |
6 | 800/1/0.04/0.8/2.4 | 0.325 | 68 | 272 000 | 483 000 | 275 000 | 1.15 |
7 | 1000/1/0.05/1.0/3.0 | 0.3 | 69 | 345 000 | 607 000 | 332 000 | 1.15 |
Reaction conditions [OEOMA500] = 300 mM, [HOBiB] = 6.0–0.3 mM, [EYH2] = 15 μM, [CuBr2] = 0.3 mM, [TPMA] = 0.9 mM in PBS with DMSO (10% v/v), irradiated for 30 min under green LEDs (520 nm, 9.0 mW cm−2) in an open vial with stirring at 500 rpm.
Monomer conversion was determined by using 1H NMR spectroscopy.
Molecular weight (Mn,abs) was determined by Mark–Houwink calibration (see ESI).
Apparent molecular weight (Mn,app) and dispersity (Đ) were determined by GPC analysis (DMF as eluent) calibrated to poly(methyl methacrylate) standards.