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Question regarding pulls during Q21Q21's The Fluffy White Funfest Options
 
Lemonade
#1 Posted : 11/6/2015 4:18:45 AM
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Hi, a friend of a friend of my next door neighbour that moved last year, left a note on my front porch asking me to post this for him...

He hopes everyone is doing well! Big grin

Quote:

I have a couple of quick questions regarding Q21Q21’s Tek – The Fluffy White Funfest

This is my first time extracting spice and there definitely was a “learning curve” but so far it’s been going pretty good. The tek is awesome, but I think there were some mistakes made along the way. Currently my 2nd pull is drying and 3rd pull is precipitating away in the freezer.

I’m doing this at a buddy’s house and am limited to being there about 2 - 3 hours at a time, so every pull is 24 hours apart.

Anyways Smile Here are my newbie questions:

1. When doing pulls, am I losing potential spice if I filter the naphtha through a coffee filter before putting it in the freezer? (I was concerned that I might get traces of the basified mix – MHRB/Bark/Lime into the solvent, so I've been filtering it through a coffee filter (Pull 1) and the next day tried filtering it through a cotton ball in a funnel (Pull 2)

2. Also, would it be helpful to add another spoonful of lime to the mixture now and then wait 24 hours before doing a 4th or 5th pull?

The results of my first pull were bittersweet. It measured about .120 grams (from 100 grams of bark). I was kind of shocked that it worked at all Big grin but must admit to have hoped for more. I didn’t mix the solvent very hard (because I was scared of emulsions) but the 2nd pull that’s drying, I mixed the **** out of....so I’m hoping for a better yield.

To any kind soul who has read so far, thank-you for your time and help!
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
daspaismusflo
#2 Posted : 11/6/2015 6:18:47 AM

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Filtering naphtha through coffee filter is pointless, because the basic water will still seep through as it is water. You will also leave a littlebit of naphtha on the coffee filter which might make you lose like 50mg or something small like that.

What I do if I have a contamination is use multiple bowls and slowly pour the naphtha in to another bowl so that you can see the black water sludge sitting at the bottom of the bowl while the naphtha is poured in to fresh bowl. Make sure bowls are dry.

This doesn't make sense:

Quote:
MHRB/Bark/Lime into the solvent, so I've been filtering it through a coffee filter (Pull 1) and the next day tried filtering it through a cotton ball in a funnel (Pull 2)


You were talking of basic mixes now your talking about bark and lime and filtering that with naphtha??? Maybe u just refering to filtering your excess bark sludge before you basify with lye which is fine. best to do filtering with a t-shirt and if ur picky u can do coffee filters or cotton ball and funnel.

Add another spoonful of acid (lime) on the last pulls won't matter really, as long as you already have added acid and have a ph of 2-3 you are ok either way. leaving for 24 hours isn't as good as heating it up and boiling it for 30mins-2hrs... a few ppl suggest that leaving for days on end with lime water is the same as boiling for an hour caus the heat lyses the plant cells.

You can stir the naphtha in really hard and see how emulsion goes, if there no emulsion after that you can even roll the jars and see what u can get away with... ur leaving it days at a time which will make emulsions settle anyway after like 10-20 hours. All that depends on how much you filtered before hand and how much lye you used though
 
Talkswithtrees
#3 Posted : 11/6/2015 3:51:59 PM
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daspaismusflo wrote:


What I do if I have a contamination is use multiple bowls and slowly pour the naphtha in to another bowl so that you can see the black water sludge sitting at the bottom of the bowl while the naphtha is poured in to fresh bowl. Make sure bowls are dry.


^ This.
When your solvent is supersaturated it can be hard to see to the bottom so make sure you do the above steps in glass containers so you can see all the basic gunk sink to the bottom. If your pulls are *HOT* base particles can get suspended in the solvent so I would let your solvent sit out of the hot bath for ~10 minutes after pulling it off your bark and lime sludge so all the suspended particles can sink and then decant the solvent. If all else fails do a sodium carbonate wash or -in extreme cases- back salt with vinegar evap add an excess of sodium carbonate add water dropwise to make a paste then dry it out and pull 3x with dry acetone or dry ipa.

To answer your questions:
1 yes you will slightly waste some
2 the only time I add more lime (which is a base not an acid) is if my solvent wont separate from my bark sludge. But you dont want it too dry or itll float in your solvent (and then you really will have to filter and/or decant)!

Also when I do q21 I find it easiest to hold the lid to the jar (I use jars and a crockpot instead of bowl like in the tek -makes pouring easier)slightly offset and pour it like that into a wide mouth glass container and then decant from there in case any sludge falls out with the solvent.
 
Lemonade
#4 Posted : 11/6/2015 11:21:46 PM
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Thank you both for your help!

Yes, using a lid and then decanting into smaller jars makes a lot of sense and I will definitely heed your advice! And that is great to know if/when to add extra lime, because I was planning on adding more tomorrow. (I will definitely skip on that!)

I have to say, I feel a little sick thinking about potential crystals that may have become trapped in the filters, but at least for my next extractions I’ll know better.

Thanks again!
 
Talkswithtrees
#5 Posted : 11/8/2015 4:24:25 PM
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Lemonade wrote:
Thank you both for your help!

Yes, using a lid and then decanting into smaller jars makes a lot of sense and I will definitely heed your advice! And that is great to know if/when to add extra lime, because I was planning on adding more tomorrow. (I will definitely skip on that!)

I have to say, I feel a little sick thinking about potential crystals that may have become trapped in the filters, but at least for my next extractions I’ll know better.

Thanks again!

Do you have the filters still? Run some warm vinegar through them evap it and do a mini ab on the goo if you like.


I actually dont think filtering is completely pointless just a little time consuming. Itd just be better to decant but if the particles dont settle (not really a problem w naphtha ime) then maybe filter.

And no problem. Smile
 
stitch
#6 Posted : 11/9/2015 9:14:43 AM

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Hello there fellow forumers. It has been quite a while since I last visited this internet heaven Razz. I wanted to use the topic to ask a few quesitons myself .that my dog was asking me the other day.

1. My dog's end product is goo-like. It use q21's tek. Freeze then thaw the roots , then add 6 % vinegar , then comes the lime he says. My dog's solvent is petroleum ether. I get the feeling that its problem is due to the heat bath. My dog Charlie heats the solvent a bit and then throws it inside the mush which is in a mason jar that is under heat bath aswell. Charlie stirs the solvent to get in contact with all the mix. After that he said he has done it 2 ways:

1. Either heat the baking which has the solvent in it ( heat it from distance, not straight on the cooker). While it is being heated from the bottom, Charlie channels his cold blow-dryer from the top. First time he did that it resulted in the solvent evapping ( DUUUH) and getting more milky, then straight jam it in the freezer. The other 2 times it did not happen like this for him. The solvent simply evapped into nothing. It did not get any milky. Which means it did not pull anything at all ? The end results were somewhat potent goo but judging by previous results it was a bit shitty.

2. The other way is when Charlie straight puts the solvent in the freezer, waits a few hours, pours off the naphta and puts back the dish inside the freezer for another 10+ hours.


Charlie has several opinions on the fails.
1. The solvent gets too heated up and gets a lot of plant fats?
2.Since it does not turn milky there is no goodies inside so prob is from mix ?
3. Is it really effective to heat from below and fan it from above ? Will the intensity of the blow-dryer matter ?

Thank you and sorry if it was a bit rude to pop in like that.
And to give my opinion aswell towards your problems - the coffee filter is a nono for my dog Charlie. He uses some metal filtering ( tea-like) , since particles are not that small. Mixture is dry and crumbly ?! Still if something stays inside, in the end when Charlie takes out dish from freezer he can easily spot where there is some brown spots left of it which i clean with some paper and make sure it is all gone? ( correct me if this is something really stupid)
The path is endless and fascinating, but those who know why they follow it, are never late.
 
Talkswithtrees
#7 Posted : 11/9/2015 11:24:44 PM
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How thorough was the acid step? If your dog *JUST* added the vinegar (no heat) that could be a problem... how hot were your pulls? Ime too hot and you pull plant junk (oils and base but usually pulling base is not much of a problem w this tek) not hot enough and you get no dmt... What plant are you extracting? If you got at least one decent pull I wouldnt worry about the acid step just yet. Ime w this tek its more likely your basic mush wasnt hot enough. Ive actually had the same thing happen and the bark was the same tree Ive extracted for years.

Regarding goo.
Goo isnt as pretty but its definitely nothing to look down at. Its *EXTREMELY* common to have your extract come out as goo. Theres really nothing wrong with it. Did this goo come out of this same extraction or was this another time of extracting?

To answer your questions...
1 yes but... what heat does here is twofold: it makes your solvent pull more actives, and it makes your solvent pull more fats and oils. Heating pulls is a double edged sword you sacrifice purity of product for quantity of product. Too hot and you get plant gunk too cold you get no actives. Especially for the 10 minute pulls this tek suggests.
2 sounds like a saturation issue actually.. it could be your bark is weak but imo it sounds like you fumbled something doing pulls... how long were your pulls? Did you let the mix heat up for awhile before adding solvent? Ime warming your solvent before adding it is ineffective if the base mix isnt warm too. The solvent will simply be cooled down by the base mud. The ffefctive way for me is to leave it in a heat bath for a while add solvent, mix, then pull after 10 minutes.
3 if you mean while doing pulls I highly doubt it. If you mean while evapping then yes thats perfect. However Ive read dmt oxide can form this way. But Im not sure how long it takes or anything along those lines.
4 I wouldnt recommend cleaning spice like that... bc a) youll lose some and b) if you have base in your dmt it wont necessarily be just where you can see it...
I would reccommend a mini a\b, a sodium carbonate wash, or multiple recrystallizations and a ph test at the end to make sure you arent inhaling base particles.


And as a sidenote read the attitude section swearing is prohibited on the forums. Not trying to make waves just want to give you a heads up Smile you said its been a while maybe the rules have changed since then?
 
Hiyo Quicksilver
#8 Posted : 11/10/2015 2:49:41 AM

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Q21Q21's tek does have a slightly higher chance of leaving contaminants, but they're all fairly easy to see. If you're doing the tek properly, you should not have any aqueous solution in your solvent; The aqueous phase should be thick and sludgy, with only enough water to keep the fibrous bark from absorbing your naptha. It should be the consistency of thin oatmeal, not watery.

Unless you can see solid contaminants or a liquid layer, you should be fine. Lye/Lime/KOH loves water, and will not migrate into your solvent unless you accidentally pour a huge gob of bark mash into your solvent collection vessel while pulling. Even then, this can be easily remedied by filtration. There is no need to filter your solvent each time if it looks clear and has no sediment, and this will not help reduce contaminants.

Yes, it is a good idea to add a little bit of lime between pulls! Naptha will effectively lower the pH of the mixture and additional lime assures that your pH is sufficiently high enough to keep the alkaloids soluble in your NPS.

I suggest you review the tek again. If your chemicals are the correct ones, then your yield is suffering because there is too much water in your mixture. Leaving it to evap in dry air with no heat or fan pressure can correct this. Your yield for 100g of bark should at least be many times what you got, if you sourced good quality bark.

Note: DO NOT USE AN ALUMINUM BAKING DISH FOR THIS. I've done this in the past to thicken a bark mash for this tek, and ended up spoiling the whole batch because your base may interact with the aluminum of the dish. This will cause the mash to heat up, and produces hydrogen bubbles which will cause the starchy mass to rise like a cake or souffle. This also produces toxic chemical by-products which are soluble in your solvent, meaning that you've turned your very safe MHRB or ACRB in a useless, toxic mess.

Good luck, be safe, and Happy Trails! Smile
 
Talkswithtrees
#9 Posted : 11/10/2015 6:34:09 AM
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Hiyo Quicksilver how quickly does the naphtha lower ph of the bark mud? Ime if I have too much water or the ph is too low the naphtha (with correct proportions used ie not a twice as much) will simply refuse to separate from the mash until it dries some or I add lime. Is this a good indication of correct ph? Next time I do this tek Ill measure ph between pulls so that we have data on it if you arent sure. Smile Thank you for your input.

Also I know it shouldnt be soluble but if I get heated pulls to hot with liquid ab extractions the naphtha does indeed retain a small portion of lye. How can this be? I know it shouldnt be soluble but it comes out in the freezer and has burned my lips when vaped. I have no analytical equipment to test if its lye or not just my ph papers and my own meandering experience.
 
Hiyo Quicksilver
#10 Posted : 11/10/2015 10:37:48 PM

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If you want definite answers, you'll probably want to ask somebody with far moar chemistry experience than I..

q21q21's tek has notes on the ideal consistency for pulls, and I've found that if it is followed correctly, the MHRB+base mash hardly absorbs any solvent at all. If not followed correctly, it can quickly become hard to manage because the mash becomes too thin and impossible to separate from the solvent. It then must indeed be dried and tried again at that point, probably resulting in a bit of oxidation and a lower yield because of it. I've noticed that DMT obtained this way tends to be markedly more yellow and less potent than DMT obtained from a "perfect" execution of the tek.

I'm not sure of the numbers, but I think I learned of the problem of pH lowering between pulls from a post by Benzyme. You'd likely be able to find it by spending some time with the search function.

 
Talkswithtrees
#11 Posted : 11/10/2015 11:58:46 PM
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Im actually familiar with the correct consistency and I agree. If you have too much water the nps wont separate. Too dry and it will need to be filtered. You want it the consistency of moist dirt.

Ive looked around for the lye being slightly miscible and havent really found anything out I didnt know...
But Im not trying to derail this thread so I guess Ill leave it at that..
 
Hiyo Quicksilver
#12 Posted : 11/11/2015 1:52:06 AM

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I should mention that this tek is written for use with lime, not lye or KOH. Lime is significantly easier to work with in this scenario using the quantities listed, and can be added dry. Also, the chosen solvent has a lot to do with absorption. Hexane, naptha and xylene will all absorb differently, and trial-and-error will indicate what works best in your situation.

One variation I always make to q21q21: I use a bit less vinegar in the acid stage and then use a solution of KOH (or lye) to raise the pH. This ensures that there is no extra base added which might leave residual solids which could be rinsed off into the collected solvent and and settle on the bottom of the jar a midst your precipitating alkaloids.

Likewise, an over-saturated KOH solvent may have tiny crystals of solid KOH floating in it, which can settle out. These can be easily seen in the light, as they are conspicuously sparkly. Once can simply add a splash of warm, distilled water and let it sit for a few hours, and these extra bits will disappear.

If you use the quantities listed in the tek, you should have no problem... But if your bark mash is too dry and you're not adding the base in the form of a solution, you're very likely to leave undissolved base in the mix which can simply be physically rinsed off by your solvent.
The quantities listed in the tek are there for a reason, and should only be adjusted unless your plant matter or solvent choice requires it (or unless you choose to use a KOH or lye solution). I believe that the tek lists the optimal consistency as able to flow, but not so thin that it can splash and slop when tilted around in a dish.
 
Talkswithtrees
#13 Posted : 11/11/2015 3:20:34 AM
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Talkswithtrees wrote:


Also I know it shouldnt be soluble but if I get heated pulls to hot with liquid ab extractions the naphtha does indeed retain a small portion of lye.

I know, I was talking about liquid:liquid acid base extractions. Not dryteks.
And reallt the only reason I mentioned it is bc Ive had floaters in my nps from this tek a couple of times. But rarely.
 
stitch
#14 Posted : 11/11/2015 4:22:41 PM

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Thank you both for your answers. Really appreciate the way you described things in-depth talkswithtrees. I think the problem was with the temperature of the vinegar when it was added. Thank you so much for clearing the missing puzzle parts for me !

As for the base in the pulls... usually the thing that falls are really small crumbly parts that can be spotted after and yes it is inevitable this way to loose a bit of spice.

I know goo is ok I even prefer it. It is just that my dog's goo had really low consistency of dmt and mostly other alkaloids. He usually make the pulls with slightly heated solvent and keep the mason jar with the mix inside a hot(more like warm) bath when the pulls are being done.

And as a sidenote : yeah you are right about the cursing. I did not mean to type it in such manner. I am aware of the rules it is just that every once in a while something slips of my mouth/fingers?! sorry if that would affect forumers in a negative way Smile .

Cheers guys! Wish you love and neverending positivity !
The path is endless and fascinating, but those who know why they follow it, are never late.
 
Hiyo Quicksilver
#15 Posted : 11/11/2015 8:01:59 PM

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I think that you're losing DMT mostly due to not fully understanding the tek. It's not usually smart to go mixing elements of different teks until you understand at least one tek completely. Both your contamination problems and your low yield are, it seems, caused by poor execution of the tek and poor choice in tools/materials. I suggest you re-read the tek in its entirety, including the introduction and background information, and then assemble the materials required to complete the tek.


-I find that it seems to work best with warm vinegar, but in reality.. The temperature of the vinegar when added makes negligible difference in your end result, if you're following the tek as written. If you're not allowing sufficient time between steps for the pH to even out, then it's important to use more vinegar and hotter water. I prefer to use a pre-mixed 2:1 solution of water to vinegar, and add until it reaches the consistency described in the tek.


-Once the base is added, there's no place for a mason jar during the non-polar wash (unless it's simply used to collect your solvent after the non-polar wash). I suggest using a low-sided glass or ceramic baking dish or something similar, and a glass stir rod for stirring. The dish can simply be tilted, causing the solvent to run off to one side where it can be poured off or removed with a glass baster.
The same dish can be used for precipitation, after collecting all of the pulls and evaporating to the point of saturation (no more, as this causes secondary alkaloids and contaminants to precipitate as well). This provides optimal surface area for the formation of crystals and speeds the process.
This is usually my go-to vessel. They come in a variety of sizes, to suit your chosen quantities. Great for extractions and casseroles alike.


-Warm solvent is fine for the first pull or two, but room-temperature solvent seems best for the later pulls because it will pull less of the oils and secondary alkaloids. This results in more DMT, and less goo.
Once nearly all of the DMT has been pulled into a clear, nearly colorless collection of naptha, you can then freeze precipitate that DMT from it to collect nice crystals and then evaporate it to collect a waxy, dense form of DMT that is still very potent.

Then, don't bother screwing around with naptha any more.. Let the naptha dry from your basified MHRB and then repeat the non-polar wash phase with Methanol or Xylene to collect the "goo". This stuff is hard to handle but great for changa because it is less potent and is more gentle, energetic and physically grounded. Naptha-extracted DMT can also be added back into the "goo" to increase its psychedelic effects in a synergistic way. More information on this substance and how to extract it can be found in this post by director of sound.
 
Talkswithtrees
#16 Posted : 11/11/2015 11:55:05 PM
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Hiyo how do you keep that container warm during pulls? If that works better maybe I should change up my vessel. Smile
Ive had no problem with jars thus far but then again I dont do huge extractions either. If you did I could see surface area w nps contact being an issue. Would you care to elaborate on that or does surface area pretty much cover it?
Also how long do you let the later pulls sit?
 
Hiyo Quicksilver
#17 Posted : 11/12/2015 1:12:02 AM

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Talkswithtrees wrote:
Hiyo how do you keep that container warm during pulls? If that works better maybe I should change up my vessel. Smile

With an electric slow-cooker, usually. I place the solvent in a mason jar with the lid on upside-down (certain solvents may dissolve the rubber seal or paint on the lid), and place that in a slow-cooker half full of water heated to about 50C (do NOT do this with dichloromethane).
I then place a small towel over the slow-cooker, and put the MHRB mash on top of that to warm. This speeds up pulls, because you need not wait for the naptha to warm as described in the tek as written.

Talkswithtrees wrote:
Ive had no problem with jars thus far but then again I dont do huge extractions either. If you did I could see surface area w nps contact being an issue. Would you care to elaborate on that or does surface area pretty much cover it?

Mason jars are actually great for precipitating crystals.. You can do that in just about any glass jar. I personally don't like scraping crystals out of a mason jar, but by all means use whatever you like best.

When it comes to the vessel used for performing the non-polar wash, a mason jar will not do. There is very little surface area over which the solvent can move, and much of the DMT is trapped under a fair amount of water-saturated bark through which the solvent prefers not to penetrate.
A vessel similar to a baking dish (as described in the tek) is preferable because it allows the bark to be spread in a thin layer, and is more easily stirred (gently) while allowing the warm solvent to move over the top of it. You need not shake it or stir it vigorously, as this encourages the bark to encapsulate the solvent in small bubbles, eventually forming an emulsion... Simply allow the solvent to directly contact as much of the basified, aqueous bark as possible, and chemical attraction does the rest of the job for you.

Gentleness is key here, as solvent trapped in the bark mash will still absorb a lot of DMT, but be nearly impossible to fully recover... The only solution then is to let the solvent evaporate from the mix fully, and try again. This leads to more oxidation and is less than ideal.

Talkswithtrees wrote:
Also how long do you let the later pulls sit?

If the bark mash and the solvent are pre-heated, I let the later pulls sit in contact with the MHRB for no more than ten minutes. I stir it gently and slowly with a rod during this time.
I've actually noticed yield drop noticeably when giving it more time, all else being equal. 8-10 minutes is my limit.

I usually give my first two pulls only 4-6 minutes and precipitate those separately, which gives a separate portion of very pure, lovely white crystals when done properly.
 
Talkswithtrees
#18 Posted : 11/12/2015 3:42:59 AM
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Hiyo Quicksilver wrote:

With an electric slow-cooker, usually. I place the solvent in a mason jar with the lid on upside-down (certain solvents may dissolve the rubber seal or paint on the lid), and place that in a slow-cooker half full of water heated to about 50C (do NOT do this with dichloromethane).
I then place a small towel over the slow-cooker, and put the MHRB mash on top of that to warm. This speeds up pulls, because you need not wait for the naptha to warm as described in the tek as written.


Doesnt the heat from the nps just diffuse with the mash mix? Wut?
It seems like the pyrex dish wouldnt get warm enough...
Ill have to try this. Smile Seems like a good idea regarding surface area.
One more question and I promise Ill leave you alone. You mentioned room temp pulls how long do you let those sit. Not warm just room temp. Ive had very little success at room temp pulls with this tek. Sad


 
Hiyo Quicksilver
#19 Posted : 11/15/2015 6:53:56 PM

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Talkswithtrees wrote:
Doesnt the heat from the nps just diffuse with the mash mix? Wut?
It seems like the pyrex dish wouldnt get warm enough...

Nope, the solvent should be just a bit warmer than the mash if heated as I described.

Again... Put the solvent in a vented jar, nearly submerged in ~50C water. Place a towel over the slow cooker and place the bark mash in your pyrex dish on top of the towel. Then wrap the towel like a cozy around the dish. The mash is always left to sit on the slow cooker between pulls, which warms it to extracting temp without endangering the alkaloids.

The desired temperature is between 40-60C and depends on your chosen solvent. Naptha, Acetone, methanol and hexane may boil in this range and care should be taken to keep the temperature of the water below the boiling point of your solvent at your present air pressure. Xylene and toulene boil at a much higher temperature and are thus easier to handle.
Dichloromethane, while being a very good solvent for full-spectrum extraction, boils at a temperature barely above room temperature, and should not be heated at all. Furthermore, care should be taken during the non-polar wash as it does not float in water.

Heavier naptha will boil at a higher temperature... VM&P Naptha may boil as low as 40C, where as Ronsonol may be warmed to 70-80C before boiling depending on the batch and air pressure.

Pressure matters a lot with solvents; a few thousand feet in elevation can mean a big difference in boiling point and solubility.

To clarify: This is to be done with an electric slow cooker with adjustable temperature, or laboratory hot plate with the proper vessel attached. Do not use a kitchen hot plate or stove. Please use all appropriate safety precautions when handling chemicals and/or sources of heat or flame.

Warming non-polar solvent generally results in a large amount of toxic vapors. Please do this only with adequate protection and in a ventilated space, away from other people, animals and especially children.

Talkswithtrees wrote:
One more question and I promise Ill leave you alone. You mentioned room temp pulls how long do you let those sit. Not warm just room temp. Ive had very little success at room temp pulls with this tek. Sad

For the first two pulls, I use solvent that is just over room temperature. This is to decrease the amount of oils in those pulls, because I prefer to precipitate these separately to collect a separate quantity of more pure DMT for sentimentality and special occasions.

The mash is warmed in the manner described above. The only difference in the aforementioned procedure when doing room-temp pulls is that the solvent is not placed into the slow-cooker while the mash is warming up. If the bark and the solvent are both at room temp, you won't be pulling much.
 
Talkswithtrees
#20 Posted : 11/17/2015 2:28:41 PM
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I truly apologize if I got on your nerves Hiyo.
You cleared up my question though. The reason I cant pull at room temp w naphtha is bc both the solvent and mash werent warm at all.
I get the that too hot isnt good bc you pull plant crud thats not active.
At any rate I hope your day goes well and again sorry if I frustrated you that was not my intention.
 
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