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When freeze precip, does it matter how saturated the naptha is? Options
 
InnerDarkness
#1 Posted : 6/2/2010 10:13:46 AM
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Say for instance we take a pint mason jar

Usually I only fill them up about 1/3 full of naptha after doing a pull. But this time around I used a little more naptha than usual & now my pint mason jars are like 3/4 of the way full.

Is this going to affect the spice dropping out during a freeze precip because there is a lot of naptha this time around?

Does it matter how saturated the naptha is?

Will all of the spice still freeze precip properly & all fall out?
 

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endlessness
#2 Posted : 6/2/2010 10:44:36 AM

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Yes sure it matters how saturated. The whole point is that naphtha should be as saturated as possible so that once the temperature goes down, naphtha will hold even less DMT so most will precipitate. If there's too much naphtha, even at freeze temperatures it might still hold most of your DMT.

As an imaginary example (not real numbers, just to illustrate the point), lets say 50ml naphtha holds 1g dmt at room temperature, and at freeze temperature 50ml of naphtha only holds 100mg DMT. So if you had 50 ml saturated naphtha and you put it in the freezer, 90% of your DMT will precipitate. Now if you instead had that 1g of dmt dissolved in, say, 200ml naphtha, when you put it in the freezer, even in those temperatures, if we take these numbers im using, then at least 400mg of dmt wont crash out, meaning 40% of your dmt is not crashing out.

So yes, as saturated as possible is better. There's two things you can do now: 1- pre-evap a significant amount of the naphtha before sticking in the freezer
or 2- Stick it in the freezer as-is, and after a day or so of precipitation, retrieve any crystals that might have precipitated and reuse the naphtha for more pulls (meaning the unprecipitated dmt wont be lost, it will be there for next pull), or if its your last pull, evap it till the end to retrieve the rest of your dmt.
 
L_Star
#3 Posted : 6/2/2010 5:10:10 PM

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What endlessness says Razz

In short: YES

remeber the points 1 - 2 in that v. important

A good way to test your stauration is to blow on the naptha and to see if cloud forms, if so then carry on to precip otherwise let it evap
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acolon_5
#4 Posted : 6/2/2010 7:11:45 PM

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As the others have said, YES!!!

Personally, I use very small amounts of solvent for each pull. On a kilo of bark I will only add 100-200mL per pull, granted I need more pulls to get everything out, but I can also stick that 200mL into the freezer and have it snow spice for 2 hours and have clear naphtha to reuse on the next pull. More work, but I believe higher yields and a LOT less waste. Evaping 500ml because you used too much takes a LOT more time, has obvious eco harm, and is just wasteful.

Go with small amounts of naphtha each pull, keep one in the freezer and another in the jug (100-200mL solvent that is) switch every 2-4 hours. As the mimosa jug nears becoming devoid of spice you may need longer times in the freezer.

A Toluene pull at the end will recover quite a bit of spice as well, but you should purify before using.
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HyperD
#5 Posted : 6/6/2010 5:38:33 PM

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I would say its not wrong to use quit much hepthan but evaporate it to from ex 200ml to 50ml before freezer and it will be good




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fractal rider
#6 Posted : 6/22/2010 4:15:30 AM

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what to best way too pre evap , the extraction i used a fan but i think thats why i got yello spice
om namah shivaya
 
Ice House
#7 Posted : 6/22/2010 4:33:58 AM

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fractal rider wrote:
what to best way too pre evap , the extraction i used a fan but i think thats why i got yello spice



and, whats wrong with yellow spice?

I'd love, some time, to do a blind test on some of the most experienced voyagers out there.


Side by side, yellow and white, In a blind test, 50mg vaped. Me says, you wont be able to tell the difference.

No Way.

You could guess and you have a 50% chance. I dont believe there are very many that can realy tell for sure.

I've compared em. When propery vaped I have no clue.

Any experts out there.
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fractal rider
#8 Posted : 6/22/2010 6:15:21 AM

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nothing wrong with yellow spice butilike the looks of white spice thats all
om namah shivaya
 
sleeper
#9 Posted : 6/22/2010 7:25:51 AM
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I disagree with most of the posts in this thread.

I have found negligible difference in yield between 150ml naphtha and ~500ml naphtha (for extraction of 250g of bark). In fact, the amount of naphtha used, as long as its "enough" is one of the least affecting parts of the recipe to worry about.

HOWEVER (big however), the more naphtha you use, the longer it will take to crystalize, and the colder you must make the jar of solution! So in a way, using more solvent and freezing for the same period of time will yield less spice...kinda. Haha.
 
69ron
#10 Posted : 6/22/2010 10:58:07 AM

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Sleeper is making an important point here.

If you want fast crystallization by freezing the naphtha, or heptane, or whatever solvent you’re using, the faster it freezes, and the less solvent to DMT you have, the quicker the crystals fall out, and the smaller and more abundant they are.

If you use more solvent, and freeze it more slowly, the DMT crystals take much longer to form, but are usually far more pure and many times larger.

The largest DMT crystals are formed by slow crystallization. A week will give very nice crystals.

It can take weeks for crystals to grow if there’s way too much solvent. There is a point at which too much solvent will prevent DMT crystallization, but it’s a lot.

So the key things to remember are:

LESS SOLVENT = FASTER CRYSTALLIZATION
MORE SOLVENT = SLOWER CRYSTALLIZATION
TOO MUCH SOLVENT = NO CRYSTALLIZATION

SLOW FREEZING = SLOWER CRYSTALLIZATION
FAST FREEZING = FASTER CRYSTALLIZATION

FAST CRYSTALLIZATION = SMALL CRYSTALS
SLOW CRYSTALLIZATION = LARGE CRYSTALS
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slayed
#11 Posted : 6/22/2010 3:01:53 PM

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How do you do SLOW FREEZING? Is this what people are talking about with the fridge first?
 
Gir
#12 Posted : 6/22/2010 3:11:33 PM

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slow freezing: fridge, room temp, fridge room temp, fridge room temp, fridge, freezer, fridge, freezer, freezer freezer, done. takes about a day
Lets go extract something together Smile

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sleeper
#13 Posted : 6/22/2010 6:35:59 PM
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Gir wrote:
slow freezing: fridge, room temp, fridge room temp, fridge room temp, fridge, freezer, fridge, freezer, freezer freezer, done. takes about a day


...or just put in the freezer at a medium temp setting, and forget about it for 3-4 days Wink

Any crystals forming *completely* in 24 hours would be suspect to really high concentrations of dmt in your solution. This would make me want to wait another 24hours to see what else would precipitate out!
 
sleeper
#14 Posted : 6/22/2010 6:43:06 PM
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I have found the best quality/quantity results from slow-freezing initially, then melting and fast freezing.

Put your mason jars in the freezer for 48 hours. Remove, pour out naphtha back into MHRB basic solution jugs, and leave in front of a hair dryer (hot/slow setting). When melted into a puddle, splash in some fresh naphtha, and put the resealed jars in a glass dish filled with ice and a splash of water and freeze for 18-24 hours. The entire bottom of your jar will become one giant fluffy crystal forest.

My last extraction I got 3.07g of powdered white bliss on the first freeze precip of 250g bark!
 
StrangeLoop
#15 Posted : 6/23/2010 12:09:29 AM

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We just did a rextalization experiment in my lab class today and I learned why people often have their crystals turn into oily goo after removing the naphtha and setting to dry. You do NOT want to drastically alter the temperature of your solvent when crystallizing. In lab we took solvent off a hotplate, cooled to room temperature, added seed crystals, put it in a cold water bath, then finally an ice bath. This keeps your solvent from getting caught inside the crystals as they form. An ice bath would probably be preferable to a freezer but fairly annoying to do at home. So I say SLOW FREEZING going back and forth between the fridge and the kitchen a few times before sticking it in the freezer is the way to go. I've done that on my most recent pull and it forms some beautiful shards. Very happy
 
Dreamwalker79
#16 Posted : 10/25/2017 9:50:24 AM
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Swim has been having problems with freeze precipitation. He thinks maybe evap some of the naptha before trying again. Swim can blow on the naptha and see the good stuff but nothing forms. He used 80ml of naptha per 50gr of mhrb. Swim thinks this thread was very educational and thanks all the more experienced members for their help.
 
saphdmt
#17 Posted : 10/26/2017 6:46:45 AM

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Just a thought- what is the temperature of your freezer? I know some freezers, espc those combined with cheap fridges, arent very cold.

On a related note: is backsalting an effective way to extract a small amount of actives from a large amount of naptha? Or would one still want to evaporate a lot of it first to get it closer to saturated?
 
mrczyk
#18 Posted : 1/1/2018 3:25:41 AM

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just a note about freezers,
They usually work by dumping the heat from the refrigerator section, and there are a few things you can do to make them as cold as possible. One is to fill the freezer. If it's not completely filled you can add water bottles, which take a long time to warm up. Also make sure the rubber seals are cleaned of dirt and that the fit is good and tight. Then add some Vaseline jelly directly to the seals. And of course make sure the thermostat is on the coldest setting. My old fridge gets to minus 12 degrees F.
Also when your solvent is in the freezer don't let anyone slam the doors on the fridge. The lack of movement is also important for crystal formation.
 
HOVA
#19 Posted : 9/29/2018 10:50:28 PM
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If I am already around 18 hours deep into a freeze precipitation is there any way to possibly take it out and air evaporate some of the naphtha or possibly take the crystals that have already formed and then just evaporate the naphtha left slightly and then freeze again?

Sorry if this sounds stupid, I just usually allow my naphtha to air evaporate for 8-10 hours at least before sticking it in the freezer to precipitate. However this time I was in a hurry and didn’t have time to do this before and have already noticed a difference between the extraction I did this with and the one I did not which are both currently still in the freezer
 
downwardsfromzero
#20 Posted : 9/30/2018 12:45:33 AM

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HOVA wrote:
If I am already around 18 hours deep into a freeze precipitation is there any way to possibly take it out and air evaporate some of the naphtha or possibly take the crystals that have already formed and then just evaporate the naphtha left slightly and then freeze again?

Sorry if this sounds stupid, I just usually allow my naphtha to air evaporate for 8-10 hours at least before sticking it in the freezer to precipitate. However this time I was in a hurry and didn’t have time to do this before and have already noticed a difference between the extraction I did this with and the one I did not which are both currently still in the freezer

You will actually get purer crystals from a less concentrated naphtha solution, assuming your freezer is cold enough. There are ways to recover all of the DMT from your naphtha without having to evaporate it.
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