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IPA/Acetone Really Produce Big Crystals?
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| Author | Topic: Does IPA/Acetone Really Produce Big Crystals? |
| Quennie Junior Member |
posted 12-23-1999 10:09 AM
A friend of mine wanted to crystallize meth as big and clear crystals. He tried Hematite's suggestion of IPA/Acetone ten times already but what he always got were fine and fluffy crystals and not the big and rock-like ones. He even tried creating the upper acetone layer very slowly using a syringe but still to no avail. So how do we make big ( 1/2 to 1 inch) meth crystals a la Epsom salt? Please help. |
| LaBTop Member |
posted 12-23-1999 10:52 AM
Do'nt worry, your not the only one who is wondering if anybody here REALLY knows how to make them, I'm still waiting for a tested procedure, not one which only recide in the mind of the poster. LT/ ------------------ |
| K.C.
Nicolaou Member |
posted 12-23-1999 12:41 PM
A trick used for getting high-purity(and usually larger) crystals that is used often by non-underground chemists for purposes of obtaining samples of high-purity for x-ray diffraction or elemental combustion analysis is to take whatever solid you want to recrystalize(this would be the small crystals you already made by some other method, not freebase), place it in a flask with a very small amount of solvent(IPA would be good), attach a condensor to the flask, and place the flask in an large oil bath that is several degrees hotter than the bp of the solvent. Wait for the solvent to start refluxing(you should add less than the amount that dissolves the solid when boiling) and slowly(keeping the solvent refluxing) add small portions of additional solvent through the condensor, stopping when all of the solid dissolves. When all of the solid is in solution, stop heating the oil bath, but do not remove the flask. As the bath/flask slowly cools, large, very pure crystals will slowly form. The slower that the bath cools, the larger and purer your cystals will be. It is also important that the solution is not stirrer/agitated at all during the cooling process. I believe Osmium already mentioned this, so I kindly remind you to thouroughly research such topics using the search engine, as you may find the answers to your questions without having to post. |
| Hematite Member |
posted 12-23-1999 12:49 PM
I have posted two methods for crystallising using these two solvent as dry as is possible. One simply for cleansing crystal of impurities rapidly, and the other for an extended crystallisation overnight of a very pure product, and yes/large crystals, needlelike. ------------------ |
| Hematite Member |
posted 12-23-1999 12:49 PM
I have posted two methods for crystallising using these two solvent as dry as is possible, heaps of times over the last couple of years. One simply for cleansing crystal of impurities rapidly, and the other for an extended crystallisation overnight of a very pure product, and yes/large crystals, needlelike. ------------------ |
| Hematite Member |
posted 12-23-1999 12:54 PM
Sorry, didn't read carefully enough obviously. The slower this proceeds, the nicer the crystal formed. You are correct though, always they are needle like with acetone for me. I believe it is an MeOH involvement that heads to what your after, but I'm only trying to cover up for posting three times like a doink! ------------------ |
| just_iced Member |
posted 12-24-1999 11:23 AM
if you use a very good starting product, then u should be able to use denatured alcohol to get what u are looking for. things to remember: 1. simmer 2. NEVER BOIL 3. repetition 4. evaporation 5. patience 6. dry crystals completely ***the impatient cook is meth's worst enemy** you never want to smoke crystals wet with methanol!!!!! its all in your technique, ice |
| dextram Member |
posted 12-24-1999 03:32 PM
why could not final crystalizaion be done from water of course it takes forever and a day to crystalize it from water but ya get a huge chunk of ice looking mass shortly after a smaller crop of pretty looking needle like clusters, I have never done anthing illegal but rystalization is a fun thing, I like to mine them from the ground amethyst is my favorite. Anyways the method looks sound to me if done in water there seems almost certainly the crystals seperate even further than any hurried method, often see them trying to climb from the crystalization container, I like either to cover this is a good idea, such like a drinking cooler, this keeps flies and bugs, dirst out I do like a tiny amout of ambient light as well as ussual tempature flucuations to occure when recrystalizing acids, the gunk seperating out looks very much like lithium stuff to me, salt lake has alot of lithium in their salt stuff it seems, anyways the slime um the bottom being slightly convex the sludge seems to seperate of along the outside forming a ring with big pretty purish crystals, um the needle like shards are allways the cleanest but each time the sludge stuff is lessened, I think they are different the wal crystals and the main aggreation they are fluffy the wall XYLS and partly yellow where as the ring is brownish and the middle is clear shards with some intermixed vein looking sludge, they can be crushed and washed with fresh water and process repeated as many times as sees fit, the resultant removal of sludge seems to restore the acid to usefull regent |
| Android Member |
posted 12-24-1999 03:48 PM
If you're referring to Meth. First of all it helps if it IS Meth and not bunk. Then simply saturate your powder with Heet(dry CH2(OCH3)2) and let it dry in normal atmosphere. 
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| Quennie Junior Member |
posted 12-25-1999 03:15 AM
Thank you bees for those great answers. I'll tell my friend about your suggestions. We'll post results soon. |
| Quennie Junior Member |
posted 12-25-1999 03:36 AM
Labtop : Sir, I can discern from your posting that you are a bee with big wings. I and my friend have a very high regard for you. My friend also tried the recrystallization procedure in your one pot d,l -ice method and what my friend got was a very hard mass but it was always brown. My friend used glass instead of alu flat bottom and he also recrystallized his d,l meth three times even four times but it was always brown. So what caused the brown, is it the impurity or the the overheating by the glass? KC Nicolaou: THanks a lot for that very detailed procedure. Hematite: Sir, I am thrilled to get a response from you. WHen I posted this query, what I prayed was that I be able to get a response from you because your post about IPA/acetone was what initiated this. I do understand that the crystals will be bigger the slower the crystallization rate is. What I was wondering was: How did you make the process as slow as possible? Sorry for the ignorance Sir... |
| Xaja Member |
posted 12-25-1999 06:23 AM
Use K.C. Nicolaou's procedure. It is called recrystallization and it is what organic chemists do to purify compounds. And big crystals are the result. |
| mnm Member |
posted 12-25-1999 08:57 PM
Android is absolutely correct from what i've been told it will work best w/ large amount of product when solvent product mixture is allowed to evap. undisturbed. Or you could always try the method used to make those big ass sugar rock candy chunks seen in the candy store. -mnm |
| fix-it-chick Junior Member |
posted 12-26-1999 04:31 AM
k.c., et al: 1.prefer an auto-controlled temp pot like a crock-pot in which to place oil/flask, or thermometers in both flask and pot? 2.through the condensor: prefer ipa or denature? what % ipa? is icewater not an option? 3.condensor construction: prefer glass, stainless steel, something else? and finally, can this be done with product that never fully reached xtal state? much obliged....and merry christmas! |
| Quennie Junior Member |
posted 01-04-2000 05:42 AM
Thanks for the replies/suggestions and Happy Millenium to all bees. |
| LaBTop Member |
posted 01-05-2000 01:09 PM
Quennie, when you make d,l-meth ice, you must use a thin pan and that pan must stand in an oil bath on 3 little triangular stones, so that the heat from the bottom of your oil bath can not form hotspots at the bottom of the crystallization pan.(A holdfast would be better). And a magnetic stirrer in the oilbath is better to prevent hotspots. So a small pan in a big pan on a magnetic stirrer/hotplate is ideal. These hotspots will very fast colour your product brown. The whole procedure is sensible for overheating, patience is the winner. But still there will be a slight colour in the crystal mass.(which has no bad effect at all at the effectiveness of the product, but we want GLAS like product, aint it?) The more I think about it, the more I start believing that what dextram
(good olle Fman) says about water, could be the obvious solution for this
problem. Then it should give you a crystalclear lookingglass like BIG
crystalmass at the end. ------------------ |
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