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Boiling small amounts of IPA with a normal water-boiler (Outside) = Safe? Options
 
Levanah
#1 Posted : 9/11/2016 7:51:45 PM

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Hello fellow travelers,

i'm curious about cleaning my (second pull) fumarates from a Q21Q21 - BLAB Hybrid (Dry Lime-Limoene + FASI) Tek with hot IPA.

I did 3x cold IPA washes with the yield of my first pull:

Yield before cold IPA wash: 0,81g fumarate
Yield after IPA wash (removing excess limonene and fumaric acid): 0,71 fumarate
(the IPA washes did not remove any of the DMT -> collected IPA was put in a freezer thereafter without precipitation)

My end product from the first pull (SLOW freebasing with water and saturated soda carbonat solution) is waxy and I haven't reached my expected 530mg freebase out of 710mg fumarate yet (yielded 250mg so far, but will surely safe more from the evap dish and glass jar).

But that's not my problem - Actually, I have no problem at all, I'm very very happy about my first yield of very nice spice. My thanks goes to this forum which has educated me perfectly. "[Question] site:www.dmt-nexus.me" @ Google is the friend for all newcommers.

Pic 1: Fumarate Yield
Pic 2: Freebase Yield (still has limonene smell - hope it'll vaporize good in my volcano vaporizer)

Both pics show the yield from the first pull. The fumarates from my second pull are a bit more orange and waxy.

My question is:

I know boiling solvents is very dangerous.

My simple idea is that I use a simple stainless steel water boiler with a small amout of IPA in it - and do it OUTSIDE in the garden and just move far away from it - if the IPA is hot enough and boils the water boiler turns off automatically and my fumarates will be dissolved quickly then... Then I'll put the IPA in a glass jar into the freezer and will get very clean fumarate crystals.

Would this be safe? Or do you have any objections?

Thanks for advice! Smile



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Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Levanah
#2 Posted : 9/11/2016 8:03:54 PM

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Another thing to mention about the waxy consistency of the freebase from the first pull as seen above.

When I did the fumarates conversion (with water as described in BLAB) I expected cleaner crystals.

Here is another photo BEFORE the crystals got WAXY.

They turned watery-oily-waxy when I took them out of the glass jar after decanting the water.

I think my mistake was that I removed them immediately from the jar (to dry them on a wider dish) instead of drying them in the glass over night without touching them.

The crystals looked whiter before ... Did'nt they? Smile



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endlessness
#3 Posted : 9/11/2016 8:17:40 PM

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Safer alternative: Boil some water, turn off the heat source, put your IPA in a container and put the IPA container inside the freshly boiled and still very hot water (obviously not letting the water get in the IPA container).
 
1ce
#4 Posted : 9/12/2016 12:33:56 AM

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Exactly as endlessness said.

There are advantages in doing it this way. Obviously, no open flames. Also, water has an uper temperature limit of ~100C. Thays god because you cant overheat your desirabe compounds.

Open a window though, unless you want a free nosebleed. XD
 
Chaska
#5 Posted : 9/12/2016 4:26:36 AM

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id do a double boiler with an electric heater
grow plants, make tea, love life
 
Levanah
#6 Posted : 9/12/2016 7:40:03 PM

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endlessness wrote:
Safer alternative: Boil some water, turn off the heat source, put your IPA in a container and put the IPA container inside the freshly boiled and still very hot water (obviously not letting the water get in the IPA container).


Thanks for that! Worked great Smile

Reading through some posts of this forum I thought it would be difficult to dissolve fumarates in hot IPA - thought it must be boiling.

Hot / very warm IPA was really enough to dissolve the 780mg fumarates. Did a short cold IPA wash before.

Added pictures:
Pic1: 780mg unclean fumarates from limonene-fasi Tek
Pic2: My setup and dissolved fumarates (glass jar was closed when it was put in the hot water container)
Pic3: +2 hours in the freezer. Milky and cloudy.
Pic4: +10 hours in the freezer. I can see crystals precipitating. Yeah Thumbs up

Will tell you the cleaned fumarate yield when it's done.
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Levanah
#7 Posted : 9/14/2016 3:11:01 PM

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... Shocked

What looked so nice like white crystals while in the freezer now looks like a failure?

Picture 1 shows the white washed fumarates which were washed with hot ipa and precipitated for two days in the freezer and then put out on the evap dish, to evap the rest of the ipa

But then ... After a short time ... Everything turned to Picture 2 ...

No solids anymore at all.

Why do I have something like a fumarate oil now?

What would you suggest me to do now? My aim is freebase.

Scrape this consistency together, mix with sodium carb, dry, and pull with IPA?
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endlessness
#8 Posted : 9/15/2016 8:28:26 AM

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My guess is residual water dissolving it. Keep scraping/rescraping and it should harden up.

But yes if you want in freebase, you can mix with sodium carb and then pull with IPA

Whatever you do just remember never throw anything away before you're totally finished, that way if something goes wrong you can always go back and recover your DMT.

Good luck and let us know how it goes!
 
Levanah
#9 Posted : 9/15/2016 1:48:52 PM

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Thanks Wink The fumarates are slowly recrystalizing and buidling white flat snow flake patterns. It's beatiful.

Will let it sit some more and then scrap it together and measure the yield. Then freebase.

In my next extraction with 100g MHRB, I'll try the more easy and fast way and go straight to base from a cold ipa wash and mix with sodium carb + pull with IPA. And compare the yields of the two 100g MHRB extractons. I think it's less prone to errors / yield loss.










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Levanah
#10 Posted : 9/15/2016 10:15:23 PM

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Finally scraped the fumarates up!

Started with 780mg unclean fumarates.
Ended up with 550mg of clean fumarates (don't smell like limonene anymore)

Total weight loss through hot ipa cleaning: 30%
Compared to total weight loss through 3x cold ipa wash (done with the yield of my first pull): 12%

Picture shows 500mg clean fumarates + the other 50mg brown fums that I safed from the jar which was used for the hot ipa wash (used destilled water to get that stuff and evapped it)

Absolutely don't know why the 50mg from the same wash and evap with distilled water look brown now.

But I'm fine with the end-product and hope that the 30% yield loss were really just impurities and not good spice.

Time to freebase! Thumbs up

Thanks for everything. Smile
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endlessness
#11 Posted : 9/15/2016 11:15:43 PM

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Good job! Enjoy!

(and let us know how the conversion to freebase and the bioassay go Smile )
 
Levanah
#12 Posted : 9/16/2016 4:35:23 PM

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We learn from our mistakes ...

Did make a paste (1:1) with sodium carb and dried it.

Because it dried so fast within hours, I thought that a food dehydrator, heat plate or oven on low setting would be not necessary. From time to time a came across the dried pulver and and broke it into finer and finer pulver.

When it looked very, very fine and dry I pulled with new, dry (99,99%) IPA out of a closed container and pipetted away the liquid from the powder that settled ... Did this 3x BUT:

Got a cloudy, cloudy, and always again cloudy IPA solution.

I expected a more clear IPA solution. So what happened, mhhmm??

It can only be that that my paste was'nt dry completely and due to water contamination I know have again sodium carb contamination.

What ever happened, it can't hold me down Smile. The spice will arise in the end and bring forth Light!
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Levanah
#13 Posted : 9/16/2016 6:45:42 PM

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And just for the record. Maybe someone new to extraction will google this thread one day:

- I used 100g MHRB

- a 180ml DMT saturated limonene solution needed exactly just 7ml FASI to stop clouding and get 800mg (unclean) Fumarates. -> So never ever be confused about the statement "for best results add 10ml FASI every 5 minutes" in BLAB which is meant for much larger quantities than 100g MHRB exctractions.

- My third pull stopped clouding after less then 3ml (around 300ml saturated limonene)

- However I must mention that I re-used the limonene from my first two pulls and unfortunately forgot to wash it with water before to get rid of excess fumaric acid and IPA.

--- Will tell you my freebase yield of the scond pull and bio-assay soon Smile Will let the cloudy IPA evap, dry and re-pull with IPA -> evap -> elfes
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Levanah
#14 Posted : 9/19/2016 2:01:35 PM

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Conversion to freebase went with yield loss.

As stated before started with 780mg fumarates and got 500mg fumarates out of my hot ipa wash.

500mg fumarates (* 0,76) should yield about 380mg freebase.

I only got 233mg freebase.

Pic1: 188mg freebase + 52mg freebase (the 52mg freebase were scraped from the edges of the evap dish and look a bit more white. I'm not sure if this stuff might be sodium carbonate contaminated)

Pic2: This is the (sodium carbonate) residue of the IPA pull. Wherever my lost spice is, this is the only place where it could be.

Question: I'm wondering if the conversion to freebase by making a paste could be done with lime instead of sodium carb?

What I understand is that lime is not very water soluble, so reaction might take a bit longer than with sodium carb. However, the IPA pulls with lime would be safer, because lime will always stay at the bottom.
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