If SWIM obtains glycol/epoxide from the Oxone reaction, exactly as posted on Rhodium's site, and proceeds to hydrolize with 15% H2SO4, the result is probably glycol. Freezing the glycol/epoxide immediately after the Oxone reaction (before hydrolisis) would make it almost solid or very thich and slow moving (depending on buffered or non-buffered reaction--glycol or epoxide). However, after the hydrolisis it would still be slow moving. I believe that the hydrolisis failed. Previous attempts of distilling post-hydrolisis product would yield some MDP2P and mostly glycol or epoxide.
What would cause the hydrolisis to fail? Different brands of Oxone were tried, buffered, unbuffered, and varying the ammount of buffer, still problems. Hydrolisis ran at 3 hours. Might the H2SO4 be bad? It is suryupy and has good density (to the best that it can be measured). Is the quality (water content, etc) of H2SO4 very important? All distilled water used. Reflux rate on hydrolisis (with methanol) is 1-1.5 drops per sec. Is the heat too low? Stirring does not stay stable at high speed, but is set to the highest possible (when it stirs and the stirrer is turned off, tiny droplets can be seen forming at the bottom (leading to the belief that the stirring is sufficient to mix all of the reactants). Are there any other variables that may have been overlooked? How viscous is post-hydrolisis ketone when in a freezer? Any suggestions?