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freeze precip vs room temp recrystallization

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travinski

travinski

Rising Star
i left a saturated heptane recrystallization at room temp and had huge ...well bigger than my normal crystals with freeze precip. you can tell which is which in the pics but the pic doesnt do these crystals justice they shine like a mf!!. has anyone else tryed this? there seems to be very little loss of product. i added the cold heptane to the crystals and then used a hot water bath but made sure the crystals couldnt be dissolved in the amount of cold heptane. then added slowly enough to barely dissolve them after it warmed. then let it sit out covered to cool
 

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Yep, room temperature definitely grows larger crystals (top picture), but freeze-precipitation is just so quick and easy (bottom pic).

My nose fills with that flowery/plastic smell just looking at the pics :lol:
 
when you recrystal at room temp,does that compromise the purity of the end product by causing dmt n-oxide,won' it oxidize?
 
you can see slight yellow spots on the top pic from reused heptane but all of these crystals are clear, would they be more pure than the freeze precip? the freeze precip seems to glue the yellow oily stuff to the sides but at room temp it seems to stay in the solvent and away from the crystals. im trying another batch with clean heptane and a new shot glass....will post more pics
oh ya the room temp recrystal only took a few hours extra
 
I know others that use the same method of recrystalizing and i have wanted to try it myself because i hear you get such nice,pretty crystals.....like the one's in your pic......but the only thing that concerns me is any n-oxide,which i'd prefer to avoid.

I always copy/paste any info that might be useful (and theres tons of it!!)but here is one i save about growing big crystals without forming n-oxide.I believe this post came from 69Ron.

QUOTE***QUOTE


The yellow discoloring is most likely DMT n-oxide. This is the main problem with growing the crystals slowly when exposed to oxygen in the air.

Growing Large Cyrstals Without Forming DMT N-Oxide

What you do is you have two containers, one that fits inside the other. You put a little zinc dust on the bottom of the larger container to absorb oxygen, and you put anhydrous magnesium sulfate to absorb any moisture build up. Or even better, use a tiny canning mason jar. You put your freeze precipitation solvent mix in a smaller container that fits inside the larger container. You place that on top of the zinc dust and magnesium sulfate, and then you close the lid of the larger container so that it’s air tight. Both containers should be Pyrex glass and the lid must be freezer safe and flexible enough to account for the pressure changes cause by the change in temperature.

Once in the container you do one of the following methods.

Cheap Kitchen Method

You let it sit for 2 days at room temperature. Then 2 days in the refrigerator. Then 2 days in the freezer. This produces an effect similar to slow evaporation except that there is no fresh oxygen or moisture present to degrade the DMT because the lid is closed and you have zinc dust and anhydrous magnesium sulfate taking care of what was in the container when the lid was closed. When you’re done you open the container, take out your DMT container, pour off the haptane and dry the crystals in a vacuum or open air at room temperature (without a fan!).

Lab Method

What works even better is to put the closed container on a digital hotplate that can reduce it’s hotplate surface temperature. These are available but cost quite a lot. This is done like above except it’s kept on the hotplate most of the time. You start by putting the container on a hotplate set to 40 C. Everyday you reduce the temperature by 10 C. On the 5th day you are at 0 C (or 5 C, because many hotplates only go down to 5 C). On day 6 you place it in the freezer set at the coldest setting (usually -15 C or below). When you’re done you open the container, take out your DMT container, pour off the haptane and dry the crystals in a vacuum or open air at room temperature (without a fan!).

Long Term Storage

Place the DMT inside a small glass container that has a screw on cap with whole drilled into it. Put a good quality flexible glass micro fiber filter paper on top of the container and close the lid so that the filter paper is held firmly in place by the lid. This filter is there to prevent dust from getting inside the container while allowing the oxygen in the container to flow out of the container. In a larger container place a small amount of zinc dust and anhydrous magnesium sulfate just like before. Place your DMT container in the larger container. Close the lid of the larger container using a flexible air tight lid that is freezer safe. Because the DMT is protected by a filter paper, if the larger container is ever accidentally shaken, the DMT will not get contaminated with the powder in the larger container. Also, the filter paper allows the zinc dust to absorb all the oxygen present in the DMT container.

Manufacturers and sellers (such as Sigma-Aldrich) recommended that 5-MeO-DMT be stored at 2 - 8 C and NOT KEPT FROZEN. So this probably applies to DMT as well. Actually this applies to the majority of drugs. It might be a good idea to buy a small freezer adjusted to 5 C just for this purpose. Topic: Pure DMT Fumarate from freebase DMT
 
I would think that larger crystals would oxidize much slower than very small crystals. Surface area!

I personally enjoy growing large crystals... I melt most of it down afterwards for storage and potency, but I just like looking at a nice crystal formation.
 
travinski said:
i left a saturated heptane recrystallization at room temp and had huge ...well bigger than my normal crystals with freeze precip. you can tell which is which in the pics but the pic doesnt do these crystals justice they shine like a mf!!. has anyone else tryed this? there seems to be very little loss of product. i added the cold heptane to the crystals and then used a hot water bath but made sure the crystals couldnt be dissolved in the amount of cold heptane. then added slowly enough to barely dissolve them after it warmed. then let it sit out covered to cool
Click to expand...

Looks great, and would you be willing to write up a short simple tek?
 
ya i guess so but this is the first time ive done it maybe one of the more experienced members here knows how to do it better...oh and i just posted them new pics above and figured out how to work the camera ...lol
 
My buddy has done over ten extractions and he has since to get the beauty of crystals that he did on his first try just plain evaping. but freeze precipitating altho not such nice crystals is amazing for purity! Freeze precip all the way less ur trying to make big crystals!
 
dunno bout the purity yet coz i havent smoked the big crystals yet, but the way i did it theres no evapping and this seems to take about the same amount of time give or take an hour or 2. when i freeze precip the yellow oils seem to get glued to the sides and top along with the crystals, when i do it this way you can see that there is minimal yellow, its stays dissolved ....(poor lighting in the pics, sorry)and the crystals are as clear/ white as a mutha fucka
 
SWIM's FOAF never really understood why people like to get ultra-pure white spice. Some specks of yellow N-oxide is absolutely fine, no harsher to smoke and no less enjoyable than ultra pure white.

He reckons it is nice to do it just for the fun of it, that he respects a lot. The same goes for growing big crystals! But after the enthusiasm and the OCD-feeling of his very first extractions, he eventually stopped bothering about that. He's now mostly concerned about total alkaloid yields and quality of experience from those different alkaloids.

And of course, there is always the dreadful inverse relationship between purity and yield.
 
travinsky,
Did swiy leave the container completeley open or did he put the heptane saturated solution inside aanother container to avoid any possible dust or other air contaminates?

How long did it take for it to evap and get those crystals?

swim is in the middle of an extraction and is going to try an room temp evap. (he always does freeze precip) but swiy has inspired swim to try the room temp. evap., due to those magnificent crystals?

Also..... Do you know the amount of bark/spice yield ratio? what type of yield did swiy get?
 
DWHITTY !!!!I DIDNT EVAP ANYTHING TO GET THE CRYSTALS lol



i did a freeze precip first and got yellow crystals, did a recrystal on those with freeze precip in a shot glass to get the yellow out then did another recrystal with heptane (2 total recrystallizations -1 freeze precip in the shotglass and 1 room temp ). the last recrystall i did the saturation i added 10 ml heptane or so to the crystals in a clean shot glass and then put it in a hot water bath (almost boiling, not full boiling) uncovered and stirred it around till they dissolved adding more solvent if needed. just start with a little bit of solvent and dont put alot of crystal in the glass i think i may have put about .5 or less. after it dissolves take it out of the water bath and cover with cellophane and a small hair elastic. if the solvent doesnt go cloudy after about 45 min you have too much solvent just uncover it and let some evap until crystals start to form or heat again to evap a bit off. you should see crystals forming after about 1.5 hours
and like everyone says save everything the solvent you pour off probably has a fair bit of dmt in it still just keep it in a jar and evap the down later for further recystallization
 
i was reading some problems in the extraction help thread about peoples crystals turning into goo after hitting room temp. i was thinking that the crystals made from a room temp recrystal could solve this. if the crystals from a freeze precip are forming at freezing temps and are trapping impuritys that make them dissolve at room temp, wouldnt it be a better idea to perfect a room tempurature method for recystallization? if the crystals are formed at room temp they would most likely stay this way, and one would think that they would be more pure. anyone here pickin up what im puttin down?lol
 
travinski said:
i was reading some problems in the extraction help thread about peoples crystals turning into goo after hitting room temp. i was thinking that the crystals made from a room temp recrystal could solve this. if the crystals from a freeze precip are forming at freezing temps and are trapping impuritys that make them dissolve at room temp, wouldnt it be a better idea to perfect a room tempurature method for recystallization? if the crystals are formed at room temp they would most likely stay this way, and one would think that they would be more pure. anyone here pickin up what im puttin down?lol
Click to expand...

yeah, SWIM saw that they really turn to goo at room temp, maybe because of some solvent that they still have, and then with the raise of the temperature, it starts to dissolve spice, but with just some minutes (too few for get as impurities as room temp recrystallization) the solvent evapores and the clumps get dry, so you just have to break them to let the little solvent they hold inside evaporate.

First time i saw them turning to goo i became desperate, but then it was ok :)
 
I evap down almost everything slowly when I recrystalize. I find that 4:1 Heptane:VM&P Naphtha works very well for large xtal growth (I've been messing aroud with ratio's recently).

I will use a mason jar and 1/2 cover it with a lid, or use a piece of paper towl and screw it on using just the lid screw cap thingy. Let it sit for 2-3 days max in a cool, dark, still (no vibrations!) place. Pour off the remaining solvent and stick it in the freezer....keep losses to a minimum!
 
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