When acidifying 15 ml MDMA free base in cold aceton with concentrated hydrochloric acid (SWIM is not fond of gassing ) the first "crystals" that are formed are fine white particles. Then after standing for 4 hours at -18 C SWIM filtrated the mixture to separate the crystals, SWIM washed them thrice with cold acetone and finally obtained 8 gram of dry fine white powder. SWIM recombined the original aceton fraction, which has an amber colour, with the slightly yellow acetone from the washings and placed this in the freezer for another 24 hours. After 1 hour SWIM observed another type of crystals beeing formed. They are more transparant and have a structure that resembles quartz. They seem to stick to the wall of my glass container. After 24 hours SWIM filtrated the mixture and obtained 6.4 grams of this more glass-like material. Upon grinding an off-white powder was obtained.
Now SWIM is really curious what causes this difference in crystallisation? Is it due to the concentration of free base, the acidity or is there another explanation? Maybe there are (more) impurities in the last material?
SWIM will measure melting points tonight to see if there is a significant difference.
Since this person doesnt really have good method of insuring that the two crystal types arnt contaminated with eachother the melting point might not be as effective as one would think, but its a good idea. SWIMs feeling is that its all good stuff, its just crystalizing at different rates and the color is due to impurities. This person might take extra effort washing the solvents and the resulting crystals should certainly be recrystalized in clean dry acetone.
If this person can get some capilary tubes (fine lengths of hollow glass tubing once used for taking blood samples) one can create a micro test tube by heating the center over a flame and pulling apart. This micro test tube can be loaded with a crystal fragment and placed into a water or oil solution along with a thermometer for the melting point test.
Also remember the longer the crystal has to develop the larger and more pronounced it will apear - which may seem to be different in characteristics from the micro shards that appear right away.
SWIM has determined the melting points of the two types of material: white powder from crystals that appeard immediately and didnīt grow upon standing in a freezer for 4 hours, and an off-white powder, made from transparant, slightly yellow glass-like material recystallised from the original solution of MDMA free base in aceton (after crystallization and filtration).
The white precipitate showed a melting point of 147,5 C.
The larger crystals melted at a slightly higher temperature: 148 C
Just like PolyAlchemia already sugested: the melting points are not very different suggesting that the composition of both materials is more or less the same. Maybe SWIM will run some GC/MS to identify low amounts of impurities. If so, results will be posted.
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) the first "crystals" that are formed are fine white particles. Then after standing for 4 hours at -18 C SWIM filtrated the mixture to separate the crystals, SWIM washed them thrice with cold acetone and finally obtained 8 gram of dry fine white powder. SWIM recombined the original aceton fraction, which has an amber colour, with the slightly yellow acetone from the washings and placed this in the freezer for another 24 hours. After 1 hour SWIM observed another type of crystals beeing formed. They are more transparant and have a structure that resembles quartz. They seem to stick to the wall of my glass container. After 24 hours SWIM filtrated the mixture and obtained 6.4 grams of this more glass-like material. Upon grinding an off-white powder was obtained.
