recrystallization help and questions

[karma1485]

I thought that since recrystallization is praised highly on this site that we should have a thread dedicated to it. This can be a place for people to ask questions about recrystallization and for those more experienced to leave some guidance. on that note: Swim is attempting her first recrystallization and is looking for some guidance. Swim followed nomans suggestions for recrystallization, 1 gram of washed (but noticeably dirty very dark yellow) spice heated as suggested, warm naptha added, let cool to room temp, put in fridge (let it sit in fridge over night) and transfered it to the freezer in the morning. Is swim on the right track? And can someone please explain what it means to filter from here? What should be disgarded from the shot glass and what should be kept? What is the best way to remove the crystals from the shot glass?

 

[kosmos]

Some thoughts on re-crystallization. The fridge freezer cycle may only be useful in an attempt to grow larger crystals - if the purpose is simply to clean up, then proceed straight to the freezer. Crystals may be small and powdery, but it's not a beauty contest at this stage. Without getting into a A/B vs STB discussion, the STB would appear to render yellower crystals. A friend has consistently had good yields with STB, but reports that even with 3 -4 re-crystallizations using either fridge freezer cycling, fast freezing or week long room temp evaporation, which grows attractive large crystals, a considerable degree of yellow remains - it almost seems to be locked into the matrix of the crystals themselves. The yellow may not matter in practice of course. My acquaintance has come to the conclusion that Coschi's BAB may be a sensible procedure. Simplicity and high yield of STB, followed by an 'acid wash'. Not yet tried though. Activated carbon washes were tried and removed all the yellow, but also a considerable amount of spice (like half).

 

[MrM]

I recommend reading these; http://www.dmt-nexus.me/phpBB2/viewtopic.php?t=229 http://www.dmt-nexus.me/phpBB2/viewtopic.php?t=691 Also my friend's goldfish had these observations to make; [b:95587b73d9][size=18:95587b73d9]My Friend's Goldfish's Guide to Recrystallisation[/size:95587b73d9][/b:95587b73d9] [size=18:95587b73d9]Items required;[/size:95587b73d9] 1 gram of DMT extract is a good quantity to start with, though as little as 500mg would work fine. 30ml of warm naptha for every gram of DMT. 1 Funnel 1 Cotton wool ball 1 tall and thin glass container that can hold 40ml of liquid. A double shot glass works well. 2 wider glass containers for the crystals to grow in. 1 Saucepan or similar container for hot water with flat bottom. 1 Glass jar with lid Cling film (plastic wrap) [size=18:95587b73d9]Steps[/size:95587b73d9] First boil some water in a kettle and empty this out into the large container with the flat bottom to make a hot water bath. Put the double shot glass into the hot water so that the glass heats up but upright so that the inside stays dry. If condensation forms dry the inside of the glass with a paper towel before adding any naptha to prevent water getting mixed up with the naptha and DMT. Fill the glass jar full of naptha and put it into the hot water to heat that up as well. Once the shot glass is hot remove it from the water and put the gram of DMT inside. The DMT might start to melt in contact with the glass, this is fine. Add about 30ml of hot naptha to the shot glass containing the gram of DMT and swill the liquid gently. Most of the material should go into solution quickly. You can put the shot glass back into the hot water for 5 minutes to make sure if you wish. You should now prepare the funnel by tearing off a small piece of the cotton wool ball and stuffing the narrow end of the funnel to produce a fine filter. The less cotton wool used the better as this will soak up and waste some of the naptha which contains DMT during the filtration process. Pour the DMT/Naptha solution out of the shot glass through the funnel and filter and into the second glass container. If there is a scummy residue at the bottom of the shot glass try not to pour that bit away but hopefully the filter will catch this if you do. This will help get rid of any obvious impurities like bits of plant or fluff. Now comes the important bit if you want extra pure crystals. The filtered naptha with the DMT in solution should ideally be completely clear. This will ensure clear DMT crystals form. Most likely it wont be, it will be a yellow or milky white or somewhere in between. In order the clear up the solution allow it to cool to room temperature slowly. You can leave it sitting in the water so that it cools at the slower rate rather than leaving it out but this may make no difference. Some DMT will probably start to crystallise out, but more importantly most of the yellow colour should fall out of solution and collect at the bottom. Hopefully the solution should go clear after a few hours. If the solution does not go clear after a few hours of being at room temperature then it may be that even though all the yellow has fallen out there are small crystals of DMT that have formed in suspension that are making the liquid appear cloudy. If this is the case then the liquid may appear more milky and less yellow than before. To fix this warm up some more water (not as hot as before) and use the hot water bath to warm the solution back up. The stuff in suspension should redissolve almost straight away and the solution will go clear so don't take your eyes off it. As soon as this happens remove the liquid from the warm water or it will continue to heat up and the yellow stuff might start to redissolve from the bottom. When you have the DMT containing naptha clear, pour it into the second identical glass container for crystallisation (leaving the yellow stuff stuck to the bottom of the previous container) and cover with cling film. The cling film prevents condensation forming and getting water mixed up with the naptha. It also stops all the naptha evaporating away. Leave the cling film covered glass container of DMT containing naptha at room temperature for a few hours then stick it in the fridge. Leave it in the fridge for 12 hours or so then move to the freezer. After it has been in the freezer for 12 hours or so you can remove the cling film and pour the naptha out into a separate container (keep this as it probably has some DMT left in it – reuse it next time for minimal losses). Recover with the glass with cling film and allow it to warm slowly to room temperature. Once at room temperature remove the cling film and let the DMT crystals completely dry (it may take a day or so for all the naptha to evaporate). Scrape the glass with a spoon or whatever and collect your perfectly white crystals. If you do this right you will lose maybe 10% or 20% of your weight of DMT you started with, but it is worth it. This technique relies on both physically filtering the naptha/DMT solution and on the fact that the 'yellow' colour (whatever that is) falls out of solution at a warmer temperature than most of the DMT. When you have finished this process you will have some scummy yellow stuff stuck to the bottom of the tall shot glass and also the glass container used to get the yellow stuff out. Don't throw this away as it probably contains some DMT – redissolve the DMT using more hot naptha and just add it to your next crystallisation attempt so as not to waste it. Using this technique my friend's goldfish can get perfectly white pure looking crystals from 1 recrystalisation. This method doesn't produce the largest of crystals though - for that you need to either cool the naptha down more slowly or else evaporate the naptha slowly once it is clear.

 

[MrM]

[quote:f0ce4daa4d="karma1485"]on that note: Swim is attempting her first recrystallization and is looking for some guidance. Swim followed nomans suggestions for recrystallization, 1 gram of washed (but noticeably dirty very dark yellow) spice heated as suggested, warm naptha added, let cool to room temp, put in fridge (let it sit in fridge over night) and transfered it to the freezer in the morning. Is swim on the right track? And can someone please explain what it means to filter from here? What should be disgarded from the shot glass and what should be kept? What is the best way to remove the crystals from the shot glass?[/quote:f0ce4daa4d] Unless i'm reading you wrong all you've done is dissolve the DMT in Naptha, warm it up and cool it down. You need to actually filter it somehow or else you'll just end up with exactly what you started with. The filtration stage happens before you cool below room temperature (or at least it does the way my friend's goldfish does it). I've written my friend's goldfish's technique above. If you have any questions just ask.

 

[Noman]

The filtration mentioned in my tek is simply to catch any loose crystals when the solvent is poured off. Most of them should be stuck to the sides of the glass on top of a pellet of yellow slag. Pour off the solvent (it can be reused) and warm the glass in your hands so that moisture doesn't condense and then scrape the whole mess out onto a piece of heavy paper. Stir the crystals around (carefully) until they're completely dry and then separate them from the slag. BTW - heptane is well worth seeking out for recrystalization. It works a [i:4ec17b1c6d]lot[/i:4ec17b1c6d] better than naptha.

 

[MrM]

Poor choice of words on my part there; when i said 'filteration' i ment whatever process used to filter out the larger bits of 'stuff' that isn't DMT, rather than the specific part of the process where filter paper is used in the tech given by Noman. 'filtration' as I used it might just be pouring one from one container into another leaving behind the scumy bits at the bottom. I would imagine most recrystalisation techniques involve some kind of 'filtration' process to get the bits out and the yellow stuff. Otherwise there wouldn't be much point. My Friend's Goldfish's tech doesn't include a filter paper stage, unlike the tech you give Noman, simply because the goldfish in question has always found the DMT all sticks to the inside of the glass and thus simply pouring off the DMT is enough to seperate the two.

 

[gimpy]

currently thru first attempt of noman's tek, the recryst stage is just around the corner. just wondering what temperature is good to work at (if following noman's process). ie, wouldn't want the magic stuff to vaporise from shotglass. also wondering if it would be easier or harder to vapourise from crystal form or from solution? qt's tek has got chemical data - melting at 45deg, but it's a bit hazey for the boiling temp. aim for 50-55 i suppose

 

[gimpy]

scrap that last question, i have another: 1st pull, crystals from freezer were filtered and dried, no ammonium was used. the dried crystals were white and fluffy. job's a goodun? would there be any need to recrystallise? also, how much lye is going to be left in those crystals if it doesn't dissolve in the naptha, surely none? and if swim can't get hold of ammonia, chilled dh2o will have to do. the dmt won't dissolve in it at all, will it? just worried about washing the magiv stuff down the sink!

 

[Garulfo]

Gimpy, If your spice is quite white, why wanting to recrystallize ? Lye is not soluble in naphta. Ammonia washes are useless.

 

[gimpy]

[quote:ca5ef80dae="Garulfo"]Gimpy, If your spice is quite white, why wanting to recrystallize ? Lye is not soluble in naphta. Ammonia washes are useless.[/quote:ca5ef80dae] Errr... i don't know... Just seemed like something that had to be done. Although in the end i didn't bother. It was my first batch ever and i didn't feel like having to wait to try the stuff. Those crystals certainly did the trick! And that's what i thought. But (following noman's tek) it says a proportion of the filtrate will wash away with it, so it sounded important.

 

[Noman]

Shit man, if I could eradicate anything from that tek, it would be the ammonia wash. At least the way its worded. I really doubt that any lye comes over and even if it did, it doesnt vaporize at the low temps of DMT. But it does wash something away. Do an ammonia wash. Dry the ammonia down. Smell the residue. Taste it. Wanna smoke it? Be my guest. But if one has gone that far they should be recrystalizing anyway.