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Need help, sucked up some brown layer into naptha, marsofold ten Options
 
Jellyfox
#1 Posted : 3/11/2013 9:24:24 PM

were off to see the jelly fox, he'll give us what we need.


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hello fellow travelers of spice space. Ive been wanting to make a profile here for a while and this is my first post!

now to cut the topic, i recently performed my first extraction of MHRB using marsofolds tek. I followed the tech precisely using only sanctioned ingredients. my only problem is i did something dumb. whilst sucking up the clear layer of naptha to be put into a jar to be freeze precip'd i noticed i accidently caught a little bit of reddish brown layer from the bottom into the jar. i got greedy and was trying to get as much of the clear layer as possible. anyways, i wasnt thinking and put the jar in the freezer anyway hoping it would only be root bark or something. so my question to you more expireinced extracters is what to do about it. since this is my first extraction i did not want to try a recrystalization although it seems i will have to now. is there a way to wash it that will leave me with a clean product. i dont care about loss of yield just as long as i get the purest product possible. Also to clarify it was only a tiny bit of red and brown that got into the clear naptha, and i realize now i should have not put it in the freezer and let it seperate , then suck off the clear layer and freeze it. its been in the freezer 2 days now. So yes now i come to you guys asking is recrystallization the only method available to get a pure product at this point or can a wash take care of it?
 

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mrnice
#2 Posted : 3/11/2013 9:53:19 PM
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Well, I'm not an expert, but I think if it precipitated out of the naphta because you froze it, the dmt should be in the brown layer. I think if you put everything back into the extraction container, warm it up a little and separate, it should yield the clean alkaloids in the naphta.

Thumbs up
 
d*l*b
#3 Posted : 3/11/2013 11:59:53 PM

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No need to put it back into the main solution you were extracting from.

Get the basic solution and naphtha you put in the freezer and return to room temperature (keep sealed until at room temp). Make a warm water bath and put the collection vessel (if it is a size that makes sense for this, otherwise decant into a suitable glass container that has a lid) in there and warm through. Give a bit of a roll about for a few miutes 2 or 3 times. Separate naphtha from the basic solution and put into a new vessel to freeze precipate again, put the basic solution back in with the rest of it.

A good trick to avoid your issue in future is to put the pulled naphtha into a intermediate vessel before you put into the one you will precipate in. You may have basic solution in there whether it is very visible or not. After a few minutes anything that is there will settle to the bottom and you can decant/pull out the naphtha easily.

I do one more step before freeze precipating, and give the naphtha a wash with sodium carbonate/water solution myself.
D × V × F > R
 
Jellyfox
#4 Posted : 3/12/2013 3:16:33 AM

were off to see the jelly fox, he'll give us what we need.


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thanks for replying so quickly, the thing is its been 2 days and theres some pretty large crystals already, if i keep sealed and return to room tempature will the crystals dissolve? or can i put the whole jar in the bath?.

also i only have gas stoves, so i can make a warm bath in my crockpot right?
 
anonenium
#5 Posted : 3/12/2013 6:07:02 PM
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ok jelly listen, another option

grab another bottle.

get the jar you have now .

carefully pour the liquid from jar a to b

take a spoon.

carefully scrape the sides for crystals and put them in jar b,

now add about half of the layer of naphtha you had before into the jar (you want enough to catch any lose crystals, so adjust as needed) with the brown and spin that baby round and round, a big glob should form in the center.

now open the jar and put it next to a fan, come back in twenty minutes or when it has lost about 20% of its naphtha volume, 99% of the crud will have fallen out of suspension, decant as much of the solvent into jar b and pour the rest back into the big jar.

im presuming your going to recrystallize it again later, otherwise disregard what i said, but this is a fast way to clean it and prepare for when the big rexing comes, then you can do a washing all at once and save time.

goof luck
 
d*l*b
#6 Posted : 3/12/2013 7:37:45 PM

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Jellyfox wrote:
thanks for replying so quickly, the thing is its been 2 days and theres some pretty large crystals already, if i keep sealed and return to room tempature will the crystals dissolve? or can i put the whole jar in the bath?.

Some of the crystals may dissolve, but larger ones probably not. Hard for me to say without seeing. The reason I say return to room temp is if you go from cold to hot too fast the glass will shatter. The reason I say keep the jar sealed until at room temp is if you don't water will condense in the jar.

Jellyfox wrote:
also i only have gas stoves, so i can make a warm bath in my crockpot right?

You don't need a constant heat source, you can just use hot water from the tap or the kettle. Replace the water in once it cools. I would not use boiling water unless using glass made for this purpose as you may watch it shatter.
D × V × F > R
 
Jellyfox
#7 Posted : 3/12/2013 9:48:16 PM

were off to see the jelly fox, he'll give us what we need.


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thanks a bunch db. just to clarify tho, when you say put the basic solution back in with the rest of it, you mean put it into the gallon wine jug full of redish brown crap? and if so is there any more use to the liquid in the wine jug, i thought it was useless to me now.
 
anonenium
#8 Posted : 3/13/2013 3:50:53 PM
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jelly how many extractions have you performed on your red brown carp?

yes you can put the brown stuff back in to swim with the other fishes.
 
*oneironaut*
#9 Posted : 3/13/2013 4:25:58 PM

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Jellyfox wrote:
thanks a bunch db. just to clarify tho, when you say put the basic solution back in with the rest of it, you mean put it into the gallon wine jug full of redish brown crap? and if so is there any more use to the liquid in the wine jug, i thought it was useless to me now.


DON'T throw it away... it's not useless until it's useless, and I'm betting you probably still have goodies in there. IF you have already done multiple pulls (3-5) then you could try adding salt to your brown soup (ice cream salt/rock salt) not iodized salt. Add about half the grams of salt as you had bark to a bit of water and disolve, then add that to your soup. Then heat up some naphtha using a water heat bath as mentioned and do a couple more pulls. You will probably get more out.
You can't do anything about yesterday, but you can do everything with tomorrow.

Everything I write on this forum is pure gibberish and fanciful nonsense!
 
d*l*b
#10 Posted : 3/14/2013 2:13:00 AM

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If it was me I would pull out the DMT-laden naphtha, once this is separate I would add a little water to the basic solution at the bottom of the vessel, swirl and add back to the solution you are extracting from.
D × V × F > R
 
Jellyfox
#11 Posted : 3/14/2013 8:17:56 AM

were off to see the jelly fox, he'll give us what we need.


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awesome thanks so much for your responses guys. i bathed my naptha so that the bad stuff sank to the bottom and i carfefully siphoned the clean layer into another jar without getting any of the crap this time. now it is freeze precip'n so i guess ill just have to wait 3 more days, o well tho better to wait and have it be more pure.

thanks a lot everyone!
 
 
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