Author Topic: help crystallization  (Read 207 times)

mdhard

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help crystallization
« on: August 08, 2012, 01:46:27 AM »
is a pleasure to know this forum ... a friend invited me to come in here ..

I would like to take a doubt with algem, please

I have ...

mdp2p via NaBH4

ammonium acetate --- "mda"

methylamine --- "mdma"


example:

MDA has 100ml freebase (pure, distilled)

what better way to crystallize? (Gas hcl 37% --- or go hcl dosing dropwise 37%)

.................................................. ...................................

I tried this way .. crystals and not get ... someone could give me a light to do?


1) 100ml freebase. + 100 ml 99% IPA
2) dripping 37% HCl solution until the pH to be 6.
3) evaporating the ipa alert vacuum.

Finally it was left ...
http://img140.imageshack.us/img140/1396/20120806045.jpg

crystal is not ...

using hcl dropwise a solution of 37% freebase, would get 100% crystal? or only 37%?

two questions, please


100gr 100gr of freebase crystals are? or have a loss?

someone could help me the best method to crystallize freebase?
including solvents, IPA or acetone?

thankss
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POSEIDON

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Re: help crystallization
« Reply #1 on: August 08, 2012, 03:31:49 AM »
The best book about MDMA & MDA , Total Synthesis II by Strike, read and learn

http://filecloud.io/qj8gabc
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim

mdhard

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Re: help crystallization
« Reply #2 on: August 08, 2012, 04:20:31 AM »
I can not see the file ...

I am very difficult to crystallize the freebase oil ...

I'd like a good method please ..

and I have a doubt ..

if I have 100gr of freebase mda (distilled and clean)

100g of freebase would make 100g crystals at the end of crystallization?
or is there a loss?
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carl_nnabis

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Re: help crystallization
« Reply #3 on: August 08, 2012, 05:15:23 AM »
why should there bee a loss? you add something to your freebase, a molecule HCl, you dont remove anything.
if anything there should bee more and not less at the end...
"It's like the drug trip I saw when I was on that drug trip!"

mdhard

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Re: help crystallization
« Reply #4 on: August 08, 2012, 06:44:02 AM »
I do not understand what you said, sorry

My first doubt is the crystallization ..
....................

example ... I have 100gr of freebase mda, which the income can I expect after this crystallized freebase? or by any kind of crystallization ..

example ..
(1gr - freebase mda) = 1gr - mda crystals?

(100gr - freebase mda)  100g = mda crystals?

and so on? understand?

I would like to know the income, so I know what I expect in my future freebase


so after I choose a method for crystallization ... and I know I can get crystal mda, starting from the freebase solution ...

thank you
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Sneak

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Re: help crystallization
« Reply #5 on: August 08, 2012, 07:15:14 AM »
You will get back from 100g free base oil 100g+ mda/mdma, As you are adding a molecule of HCl to the mda. Same as MDMA.

If you gas or titrated you will achieve 100% crystallisation so long as it's done correctly and no water is present in solvent.

Do not think that because the HCl acid is 37% that it only removes this amount of end product. That is incorrect.

At least it seems you have a fair amount to play around with. Post some more images if possible.
« Last Edit: August 08, 2012, 07:16:51 AM by Sneak »
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

carl_nnabis

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Re: help crystallization
« Reply #6 on: August 08, 2012, 07:22:06 AM »
I dont understand what your problem is really? Just add enough hcl to neutralise your freebase, add a dash acetone then let it stand at room temperatur two or three days or such, you will end up with big fat crystals.
"It's like the drug trip I saw when I was on that drug trip!"

mdhard

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Re: help crystallization
« Reply #7 on: August 08, 2012, 07:48:50 AM »
I understand ..

then is it so? see if it is correct, please


1) I have 100gr of freebase mda ...
2) dropwise hcl 37% correct? (Which until ph level should be?) Ph 6?
3) add acetone in freebase + HCl solution (those ml of acetone to 100g of freebase mda?)

4) Dump everything in a bowl and let acetone evaporate at room temperature?

is just that?

doubts ...

1) so all my 100gr of freebase mda will be crystallized? 100g freebase = 100% of crystallization?

2) with this form of free base 100gr crystallization would become mda mda 100gr of crystal?

3) My biggest doubt is really how I can get crystal mda ... understand?

(Freebase 1gr MDA) is equal to 1gr mda crystal (after being crystallized?)

(1kg freebase mda) would equal (1kg mda crystal (crystallized)

understand my doubts?
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carl_nnabis

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Re: help crystallization
« Reply #8 on: August 08, 2012, 08:42:14 AM »
actually every gram of freebase gets more than 100mg of HCl added to it   ::)
so go calculate yourself how much you get  ;)
"It's like the drug trip I saw when I was on that drug trip!"

mdhard

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Re: help crystallization
« Reply #9 on: August 08, 2012, 09:57:49 AM »
hi friend ..

you're talking to dose hcl 100mg of the freebase?

My doubt is still ..

100g of freebase was crystallized ... I'll see at the end have the same weight (100g) in crystals?

you understand?

independent so that the crystallization was conducted .. in the end I'll get 100% of the weight of my freebase crystals?
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Shake

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Re: help crystallization
« Reply #10 on: August 08, 2012, 10:30:55 AM »
carl canibus is on the right track with what he is saying.. let me tell you, it takes a super small amount of HCL to prononate the goods.. the exess does NOT have a real effect on yields unless you use a tonne of HCL when we only really need 5 or so drops for the qty we are dealing with here.

for your crystalization, the dual solvent system will always work, when you combine acetone, tiny bit of ipa and toluene, dissove your freebase in that and you get some nice big crystals, IF you leave the mix i the freezer for a couple days.. but those crystals are not ideal, you will get more potent goods if you  mix your freebase with some ipa, drop in a few drops of HCL put on a low heat and stir till everything turns to crystals.. you can use acetone to wash if you like but you will only destroy goods so dont wash it

POSEIDON

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Re: help crystallization
« Reply #11 on: August 08, 2012, 02:19:24 PM »
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim

mdhard

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Re: help crystallization
« Reply #12 on: August 08, 2012, 04:51:22 PM »
carl canibus is on the right track with what he is saying.. let me tell you, it takes a super small amount of HCL to prononate the goods.. the exess does NOT have a real effect on yields unless you use a tonne of HCL when we only really need 5 or so drops for the qty we are dealing with here.

for your crystalization, the dual solvent system will always work, when you combine acetone, tiny bit of ipa and toluene, dissove your freebase in that and you get some nice big crystals, IF you leave the mix i the freezer for a couple days.. but those crystals are not ideal, you will get more potent goods if you  mix your freebase with some ipa, drop in a few drops of HCL put on a low heat and stir till everything turns to crystals.. you can use acetone to wash if you like but you will only destroy goods so dont wash it


mda the freebase already been crystallized only with ipa hcl and dropwise 37% ... up to PH6

and evaporate ipa ...

but no crystals were formed ... so I have a white goo, that has a picture on the front page ..

this mode of crystallization is not right for me ...

and I still do not know how many grams of crystals will collect from 100gr freebase ...
I  do  not  mind  being  negative!

Shake

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Re: help crystallization
« Reply #13 on: August 08, 2012, 05:52:50 PM »
mix the goo with ipa add a drop or 2 of hcl put it over a hot plate and you wont get goo..

or stop being impatient, use acidic water to extract the goods from the freebase, then evaporate the water.


this is how you get full yield

stop asking questions like a tard


mdhard

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Re: help crystallization
« Reply #14 on: August 08, 2012, 06:25:55 PM »
ok my friend ..

I'm sorry for the many questions ..

I lost all my freebase trying to crystallize with ipa ... is only a white goo ..

100gr of freebase lost ... and not got no crystal 1gr = [

try again in the next synthesis crystallize with more success
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carl_nnabis

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Re: help crystallization
« Reply #15 on: August 08, 2012, 06:59:13 PM »
Well... UTFSE before you open a new thread...
http://127.0.0.1/talk/index.php/topic,1021.0.html
and you must be kidding, have you really tossed away more than 100g mda?
"It's like the drug trip I saw when I was on that drug trip!"

bubble

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Re: help crystallization
« Reply #16 on: August 08, 2012, 07:24:01 PM »
dude filter your white goo, wash it with some acetone and then recrystallize it in some water, which you heat until you dissolve everything. then you cool it slowly down. Big crystals will form which you can filter off. then you add some acetone which will precipitate the rest of the mda/mdma. You will get out of 100g mda free base nearly 120g mda hydrochloride in crystal form.

mdhard

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Re: help crystallization
« Reply #17 on: August 08, 2012, 08:28:28 PM »
dude filter your white goo, wash it with some acetone and then recrystallize it in some water, which you heat until you dissolve everything. then you cool it slowly down. Big crystals will form which you can filter off. then you add some acetone which will precipitate the rest of the mda/mdma. You will get out of 100g mda free base nearly 120g mda hydrochloride in crystal form.

thank you .... I was expecting a response like this ..

but I've got no freebase, hehe ... I lost everything in tests to crystallize = [

soon I'll try again ...

I can get at least 100g hydrochloride mda .. from 100 grams of freebase mda?

because I do not know how the final yield was ... because I could not even 1gr hydrochloride mda ... then my income was 0%

the conversion of freebase is 1x1 in relation to weight the yield will be very good
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POSEIDON

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Re: help crystallization
« Reply #18 on: August 09, 2012, 01:07:41 AM »
and I still do not know how many grams of crystals will collect from 100gr freebase ...

read this pdf and look for a basic chemistry book (Mass Relations in Chemistry; Stoichiometry)
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim

mdhard

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Re: help crystallization
« Reply #19 on: August 09, 2012, 02:52:18 AM »
and I still do not know how many grams of crystals will collect from 100gr freebase ...

read this pdf and look for a basic chemistry book (Mass Relations in Chemistry; Stoichiometry)

thanks for your help my friend ... I read the article
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