"MY" MDMA freebase crystallization

[crocodile]

great post, quick question though.
what color does the mdma come out if you use a 10 to 1 acetone ratio? I imagine it would be white mdma. What ratio of acetone would you recommend for champagne color mdma?

 

[Sig]

We do 2.5 liter aceton on 1 liter base and then we put the ph on 5.5 with with hcl 37% and than freeze 4 days

 

[btcboss2022]

Of course you can mix the freebase with solvent before adding the HCL but later you Will need more time to put the mixture at 130C due this solvent will be evaporated, with the HCL from freezer, the freebase cold too and avoiding high temperatures during the addition wont be any problem ;-)

 

[Hank Schrader]

Do you know that MDMA cannot be heated with acids to high temperatures? The product breaks down and is no longer pure MDMA.

 

[btcboss2022]

Agree not pure it turns ultrapure!

Lab report

 

[Mr Good Cat]

Nice. Who provides such precise lab test? As I know, usually the error is 5%.

 

[btcboss2022]

In that case is a German company but there is many of them Energy control...

 

[Mr Good Cat]

As I have read, MDMA freebase boiling point under regular AP is about 300C. Why do you believe it might be spoiled if heated?

 

[Davidrobinson]

It should be ok because you crashed ot out in acetone. More acid just makes more impurities.
Did you get big crystals from pouring the hot acidified freebase into cold acetone?

 

[btcboss2022]

When I did It in past at 120C yes I got Big crystals now at 130C I get shiny powder

Thanks.

 

[viking1111]

Fucking true...

 

[Doubleboil]

@btcboss2022 @Unreacted Freebase
I did the cold acetone. Left in freezer. precipitated and settled on bottom. Separated the solids. Left out drying but still very mushy. Does this look right ? Thanks.

 

[kharpa177]

did you heat up your ph 3 acidified freebase and drop it in ice cold acetone..? was it ok after it dried?

 

[Unreacted Freebase]

Dry it and wash it. I would agree with btcboss. Better to go for lower PH and make sure all freebase is neutralized. then have unreacted freebase in product Use roughly 430ml 37% HCL per liter of distilled freebase.

 

[Mr Good Cat]

Sorry, pal. I was talking about meth today, so wrong molecular weight was used. You are totally right!

1L of FB = 900 gr (roughly)
900 gr = 4.66 mole

 

[kharpa177]

how many ml of hcl 37% would be used to acidify 1 liter of mdma freebase

 

[Mr Good Cat]

@Unreacted Freebase suggests to add HCl in proportions 1:1.1 (FB:HCl).
Me personally would go little less: 1:1.05

Let's study how to calculate. It is very simple:

First, you need to calculate how many moles are in 1L
Molar weight of MDMA FB is 193.25 gr.
FB density is 0.9gr/ml, that means 1L of FB is 900gr
1L of FB contains 900/193.25=4.66 moles.

Then you calculate necessary moles of HCL
4.66*1.05=4.89 moles of HCl.

Then you may find in internet a table that shows molarity (molar volume concentration) for different percentages, and 37% among them.
In your case it is 12.08 mol/L.

4.89/12.08=0.405ml

@Unreacted Freebase suggests little more - 430ml

 

[Mr Good Cat]

fuck... shit...
not 0.405 ml, 405 ml of course!

 

[Mr Good Cat]

2. Heat the mixture gradually while stirring until 130C
3. Has ready a bucket, with 10 times the volume of initial freebase, of freezed acetone that has been at least 48 hours in freezer
4. When mixture is at 130C stop heating and pour It fast in the acetone bucket with vigorously stirring.

"pour It fast" and "vigorously stirring" are relative. May you specify if my understanding is adequate, please? I consider to use it for medium batches, corresponding to 5-10L of acetone.

I consider acetone canister PEHD as a bucket. Then I put inside a steel spiral that used for protein shakers.

Then, as chloride is ready, I pour it inside. Considering the density of chloride and diameter of cap it will take around 10-20 sec to do it. Then I close the cap and start shaking vigorously for a while.

Will it work, or it is too slow and not enough vigorous?

 

[Mr Good Cat]

I really love this re-crystallization method for its simplicity, but not 100% satisfied with color.



This is the best result I was able to get with this method at point 107C. It is not bad, but still not perfectly white transparent.

This time I checked the weight of water I drained.. It was 2 gr per 50 gr of salt. Rest of water evaporated naturally.

I applied Raoult to this data and got the result below. I shall consider atmospheric pressure as well. As for the sea level water boiling point is 100C, but for 700m altitude it is 98C.
So the shift for sea level is 7C, for 700m - 9C while heated till 107C.

mw = 0.52 * ms * 1000 / (dT * 229.7)

mw (sea level) = 0.52 * 50 * 1000 / (7 * 229.7) = 16.2 gr.

What if I try to add some side solvent, with more high than water boiling point and less than water solubility? The target is to run crystallization in bigger volume of sovlen to slow crystallization down and decrease nucleation. Hopefully, more liquid can trap more impurities with bigger size and purity crystals in result?

Glycerol for example dissolves the salt half much as water and has boiling point at 290C.

If I stop crystallization with the same volume of water, then there will be 5 * 1.26 / 16.2 = 38.8% glycerol water solution with boiling point 117C without salt.

Then, when salt added, Raoult increases boiling point as well with another 8-10C - I need to know ebullioscopic constant of such mixture to calculate it precisely, but probably it shall be more than 0.52 and less than 1.5.

So, probably I shall heat chloride solution till 125-127C with resulting 50 gr of salt in 16 ml of water + 5 ml glycerol solution for better result?

 

[btcboss2022]

Washing these crystals with freeze clean acetone they will be transparent another option is to leave them inside clean acetone in the freezer during 4-5 hours moving it time to time.

 

[Mr Good Cat]

I've just finished leftovers recovery and want to share my experience.

Main batch was 71 gr of pure white mdma hydrochloride in powder after base extraction. Final yeld was 56 gr, that means 15 gr, 21% of initial weight are in water leftovers.



There are a few ways to recover it, but I'm not aiming to recover all, I'm aiming to recover more or less PURE. So I do recovery in two steps.

1. I move crystallizator with water leftovers to average refrigerator under temperature 4c and keep it for a while. Small crystals appear soon in size about 4x2x1mm. They were taken out and weight checked - 7.0 gr.

2. Rest of leftovers were left at RT for some time till dry weight. Weight checked, and it was exactly 6.95 gr. That looks more or less reasonable, considering some product was evaporated or damaged while heated.



This powder was dissolved in water - acetone solution, prepared in volume proportions 1:10. I add this solution by weight 20 gr of this solution per 10 gr of salt.
I use a hot plate to dissolve it: put a stir bar, and set plate temperature 50c.



All salt dissolves easy and fast. Then it moved to refrigerator. After a while it is taken out and filtered with vacuum.. Yeld is 3.5 gr.



Final yeld of recovery is 10.5 gr of 15.0, or 70%, that me personally consider as very good result, and pretty pure, fits for my own needs - at least it will not spoil next batch with its presence.

Water-acetone leftover still keep around 3.5 gr and can be proceeded in the future, but obviously will be more dirty than mentioned above.



I wouldn't work with it without base extraction, but street vendors in Poland might be more than happy with it. Yeaaahhhh!!

 

[Mr Good Cat]

I did apply your method in this part for recrystallization of ready product.
I.e. ready crystals were dissolved, then heated up to 130C, then thrown to the frozen acetone. Works very well.

 

[davethedead]

Anyone have any tips for a situation where there was to much water in freebase/added acid , and now alot product is trapped in acetone?
Has anyone had this situation, would adding more actone or IPA to solution get rid of excess water and release the salt?

 

[WillD]

You can add alcohol or acetone (so that the solution with water does not freeze) and put in the freezer, if you do not want to evaporate. In some cases, it helps.

 

[jamesdavies]

Does anyone know if this method will still work effectively when you change acetone for IPA,ethanol or methanol ?

 

[Mr Good Cat]

Depends what you want.
Probably this crystallization in water is the best to get big crystals. I really love, many thanks to author. But you will not get your crystals to much pure as there is no a lot of solvent. It is not for purification, it is to get final product.

Some people report they obtained big crystals in IPA, but not me. I tried IPA a few times. Even I tried very slow crystallization in IPA on water bath with decreasing temperature from 56C to RT during 20 hours, all I got a heap of small crystals around 1.5 mm size. But, what is more important, IPA removes black compound very well, the best solvent I guess. Very good for purification.

Methanol and ethanol - i don't know. May be @btcboss2022 may give more information, he is more experienced.

 

[jamesdavies]

Its not for big crystals but the part for cleaning . I am referring to the the point where I heat the super saturated solution of acidified freebase and pour it into acetone. Can I change acetone for alcohol.
Acetone is highly watched in my country since 10days ago/

 

[Mr Good Cat]

Ah, sorry, got your problem. A bit of theory if so, bro.

Acetone has a unique property: it solves a lot of mdma hcl at 50C (1 gr of mdma hcl per 2.5 gr of acetone i guess) and almost zero if acetone is frozen. This property is related with "vacuum permittivity". Vacuum permittivity of acetone at 50C = 17.7 and at 0C = 1.0

So you need to find a solvent with similar vacuum permittivity, not more than 2.0. It is benzene, petroleum ether, hexane.

I don't think IPA is good for this purpose, as it solves a lot of mdma hcl even in the freezer, around 30%. And even if you evaporate it the leftovers will be more dirty than they were at the beginning.