Need help with recristalisation (N.N. Demethyl Chloride???)

[Dee Em Tea]

SWIM has been attempting his first recistalisation, for this he's aquired some alcaholbased stuff, called N.N. Demethyl Chloride. SWIM loves the name for one, but do any of you guy's know if this is a good thing to use A friend of his, brought some from his work, where it's been used as a break cleaner. SWIM Has evaporated some, and it disapeard in seconds, and left no residu. Yesterday SWIMM has desolved 1 gram of the yellow spice in it, and let it evap. until it whent milky. After that he's put it in the freezer, to recristalize. This morning SWIM can see the yellow layer at the bottem, but doesn't see any cristals. :? Can anyone tell my how to go about this. Your help wil be greatly appreciated. Greetzzz from Holland, Dee Em Tea

 

[DZ-015]

When you dissolved the spice in the solvent did you heat it? As far as the solvent goes, i've heard of methylene chloride (AKA Dichloromethane), but never used it myself. I couldn't find much information on dimethyl chloride so there's really only one way to find out. Be safe.

 

[fourthripley]

Hello De Em Tee Firstly I'm guessing what you have [i:cd23170d88]is[/i:cd23170d88] DCM or a chlorinated solvent of that family.I think you're confusing freeze precip and recrystalisation; freeze precip is crashing your goodies out by lowering the temperature whereas recrystaling is seperating the crap from the goodies in hot solvent,Both depend on using a [i:cd23170d88]saturated[/i:cd23170d88] hydrocarbon such as naptha/hexane/heptane; both processes rely on the fact that saturated's aren't particuarly good solvents unless nice and hot.With recrys the idea is that the goodness will solubise in the saturated solvent before the horrid fats do, then you seperate the clear solvent from the junk in the bottom.Aromatic solvents like toluene and xylene and chlorinated ones- like I believe you are using- are rather good solvents and will solubize(is that a word?) the goodies [i:cd23170d88]and[/i:cd23170d88] all the fats and oils.Assume- if you can't get anything better, ie. pure hexane/heptane - you can get fuel for Zippo type lighters in Holland? thats the stuff you want, but I reckon the solvent you [i:cd23170d88]do[/i:cd23170d88] have could prove pretty useful for moregeneral work

 

[Dee Em Tea]

Thank for the reply's guy's. So SWIM attempted a recristallisation with this stuff a view days ago. Although he didn't quite understand that you had to separate the solvent from the sludge. SWIMM made the solvent as hot as possible and dissolved one gram of the yellow spice, as the spice dissolved the solvent went milky straight away .SWIMM cooled this down to room temperature, and put it in the freezer. The next morning most of the spice recristalized , but as he didn’t separate he thought his experiment has failed. SWIMM has evaporated the solvent, and got all the spice back, so all was not lost. At this moment he’s trying it just with the turpentine he’s been using from his initial pulls. Now I hear a lot of you (people) talking about that toluene is a good solvent for recristalisation . Now SWIM has been doing some resurge of what kind of solvent holds this ingredient, and found that in the ordinary paint thinner here in Holland holds toluene. http://www.progold.nl/media/images/progold_thinner.pdf Could this be a good solvent for recristalisation? Your help is most welcome. Dee Em Tea

 

[DZ-015]

I wouldn't use toluene. You can't find any kind of lighter fluid like is used in refillable cigarette lighters?

 

[Dee Em Tea]

@DZ-015, Yeah you can find lighter fluid here, but only the wan from Zippo, of witch I read everywhere that it is far from pure and leaves loads of residue. So I found that Thinner that holds toluene. He’ll go and get some today, and give it a try. I have to say though; his second attempt with the turpentine wasn’t unsuccessful either, even though the spice is still a bit yellow, it looks a lot better as that what he started out with. He’s learning as he goes. Dee Em Tea