dealing with south-of-the-border's technique to stretch their inventory is a bear.
a friend of mine has now performed several tasks to remove MSM (and whatever else) including heating to MSM melting point (which does significantly reduce volume), acetone washes, and single and dual solvent recrystallization.
it's still getting through. well, the dual solvent recrystallization may not have been performed entirely properly. but still.
in single solvent recrystallization, after heat treatment and wash, the initial crystal formations are very thin needles which dry to an opaque white. they display the melting characteristics of MSM: flash melting to a watery clear rapidly turning brown, with the billowing clouds of powdery smoke, the tendency to boil and flash ignite at a much lower temperature than otherwise expected.
question: is the above description of the crystals consistent with MSM? how is it that after being subject to 255degF heat for 45mins, then washed in acetone, that recrystallization would yield an enormous quantity of said crystals, with virtually no other crystal formation?
leaving out the heating, the result is almost identical.
in terms of dual solvent recrystallization, the addition of acetone to the near-boiling alcohol at or beyond the point of saturation seems to cause no effect overall, except to delay the formation of crystals.
is there a ratio or acetone to alcohol that is required? is there an issue with timing?is filtration required? what is not being done?
Help! Thanks!
a friend of mine has now performed several tasks to remove MSM (and whatever else) including heating to MSM melting point (which does significantly reduce volume), acetone washes, and single and dual solvent recrystallization.
it's still getting through. well, the dual solvent recrystallization may not have been performed entirely properly. but still.
in single solvent recrystallization, after heat treatment and wash, the initial crystal formations are very thin needles which dry to an opaque white. they display the melting characteristics of MSM: flash melting to a watery clear rapidly turning brown, with the billowing clouds of powdery smoke, the tendency to boil and flash ignite at a much lower temperature than otherwise expected.
question: is the above description of the crystals consistent with MSM? how is it that after being subject to 255degF heat for 45mins, then washed in acetone, that recrystallization would yield an enormous quantity of said crystals, with virtually no other crystal formation?
leaving out the heating, the result is almost identical.
in terms of dual solvent recrystallization, the addition of acetone to the near-boiling alcohol at or beyond the point of saturation seems to cause no effect overall, except to delay the formation of crystals.
is there a ratio or acetone to alcohol that is required? is there an issue with timing?is filtration required? what is not being done?
Help! Thanks!