Example of isomer separation for Meth

[hunter12]

Please help, after mixing amd leaving it overnight it turned out pink.

 

[btcboss2022]

Please help, after mixing amd leaving it overnight it turned out pink.

hunter12Pink color normally means too acid but not in 100% of cases also could be impurities from your freebase, check the PH should be around 4 anyway I dont see any precipitate in your pic.

 

[hunter12]

Is there some thick material appearing on the walls of the beaker during stirring?
If there is. Use a glass rod to scratch the side of the beaker. Will help with crystallization.

qwe111This is how it gets during stirring but no precipitate after

 

[hunter12]

Try 150ml h2O+80gr tartaric once dissolved add the freebase with heavy stirring until solid mass formed could take some minutes.

btcboss2022Ok thanks il try that, il come back with results

 

[btcboss2022]

This is how it gets during stirring but no precipitate after

hunter12On my experience I think it needs more time stirring it's getting thick and finally solid.

 

[hunter12]

I just added a very bit of sodium hydroxide solution about 5 grams and its showing crystals. I dont know if i did the right thing by adding sodium hydroxide.

 

[btcboss2022]

I just added a very bit of sodium hydroxide solution about 5 grams and its showing crystals. I dont know if i did the right thing by adding sodium hydroxide.

hunter12You simply increased the PH, check the PH now to have an idea if you are in the right way.
Honestly I never had this color in that process and I did it hundreds of times in different ways, amounts, routes...but maybe is right you will see it.

 

[hunter12]

You simply increased the PH, check the PH now to have an idea if you are in the right way.
Honestly I never had this color in that process and I did it hundreds of times in different ways, amounts, routes...but maybe is right you will see it.

btcboss2022The PH is at 5

 

[btcboss2022]

The PH is at 5

hunter12Could work, update us when you finish the process thanks.

 

[hunter12]

Could work, update us when you finish the process thanks.

btcboss2022Hi i manged to finish the process. I basifid both layers(d and l) after separation. The total freebase i used was 300 grams. And got 90 grams from the aqueous layer around 170 grams from solid layer. Then i crystallised with hcl. The crystals from the aqueous layer (d insomer) was just powder even when i try to recrystalize and the other layer (l-insomer) has more small glassy crystals with powder.

 

[qwe111]

Hi i manged to finish the process. I basifid both layers(d and l) after separation. The total freebase i used was 300 grams. And got 90 grams from the aqueous layer around 170 grams from solid layer. Then i crystallised with hcl. The crystals from the aqueous layer (d insomer) was just powder even when i try to recrystalize and the other layer (l-insomer) has more small glassy crystals with powder.

hunter12Hai brother,
Can you share how you accomplished this?
pH value?
I also completed this process successfully, but my yield was very low,
From 100ml free base I get 20ml d. I couldn't get any more.
What did you do right?

 

[hunter12]

Hai brother,
Can you share how you accomplished this?
pH value?
I also completed this process successfully, but my yield was very low,
From 100ml free base I get 20ml d. I couldn't get any more.
What did you do right?

qwe111I dont think i did the right way bro. Since my crystals are still racemic. I will try it once again

 

[qwe111]

I dont think i did the right way bro. Since my crystals are still racemic. I will try it once again

hunter12good brother
I’m waiting for you to share the right things!

Losing 300ml of free base is really a sad story!

I also did something stupid yesterday. I steam distilled P2P and then used DCM to extract P2P. I then fell asleep while the DCM was evaporating. And the heating jacket temperature is above 200°.
After I woke up, p2p had been evaporated!
Lost about 500ml

 

[chef learner]

May I ask what is the reason why when I add tartaric acid, it does not dissolve and does not crystallize? Is it the wrong methamphetamine free base? Or is the pH incorrect?
Already stored for 24H

What is the correct pH of methamphetamine free base?

 

[hunter12]

May I ask what is the reason why when I add tartaric acid, it does not dissolve and does not crystallize? Is it the wrong methamphetamine free base? Or is the pH incorrect?
Already stored for 24H

What is the correct pH of methamphetamine free base?

chef learnerWhat is your current PH? And what was your freebase Ph before adding the tartaric acid?

 

[Sjeik]

It has to be like this..

 

[hunter12]

It has to be like this..

View attachment 40157 View attachment 40157

SjeikNice, you used the same method?

 

[Sjeik]

Nice, you used the same method?

hunter12Yes, ph of freebase should be around 11

 

[qwe111]

Yes, ph of freebase should be around 11

SjeikThe initial free base pH is 11?
What is the pH value after mixing?

How many D methyl groups do you get after separation?

 

[qwe111]

I had like 700ml racemic fb, And after sepration got around 320ml d-fb.

SjeikHey man, this yields great!
Did you clean the L-fb and L-tartaric acid mixture inside the funnel during vacuum filtration? If so, what cleaning do you use? Then how to detach D-fb

 

[Sjeik]

Hey man, this yields great!
Did you clean the L-fb and L-tartaric acid mixture inside the funnel during vacuum filtration? If so, what cleaning do you use? Then how to detach D-fb

qwe111No, i use an centrifuge

 

[Fringg]

Hello, I greet you all. I want to share with you my experience with the separation of isomers using L-wine. I did three tests. 2x using methanol when I changed the ratio of free base methanol and tartaric acid in both tests. Both tests turned out basically the same, after combining the ingredients and mixing, a solid mass precipitated, which I filtered after 24 hours. As for the appearance of the product and the overall split isomers, perhaps there was a little more products in one test than in the other test. From 30ml of free base I got about 9 grams of d-meth. During evaporation, when the crystals started to appear, it looked good at first, small needles were formed here and there, but the drier it got, the more it resembled a racemate (ugly amorphous substance). When it dried completely, in terms of appearance, I could not tell the difference between the racemate and this divided product. When it was put on foil and warmed up a little, it was obvious that the crystals crystallize a little faster after dissolution than when it is done with the racemate. From this I concluded that some division took place, but not enough. I note that I did not wash the tartrate powder during filtering. It was not written in the procedure, so I preferred not to do it. Well, now we come to the third test, which I did with the help of water according to the btcboss procedure. After combining all the ingredients and mixing vigorously, after a while I got a thick, really thick mass resembling some kind of cream. It had a consistency basically like the photo that was added by the user Sjeik a couple of posts above mine. I closed the container and let it sit for 24 hours, then I put this substance in the filter and spread it over the vacuum filter and turned on the suction. This thick cream-like substance was really difficult to filter, also in the procedure there was nothing written about washing the tartrate in the filter, so I didn't do it. I only got 11 grams of product from 60ml of free base. But the crystals that arrived were transparent and beautiful. I tried melting them on tin foil to see how fast they solidify and it was really fast like pseudoephedrine meth. So I think that the Split izomer was successful except for the mass tragedy of only 11 grams. The problem was probably mainly that I had a bit of a problem during filtration with the fact that the funnel on the suction flask did not seal well and it might also help to wash off the tartrate salt during filtration, but please advise me how much water I can use for this so as not to disturb the solubility of the tartrate in water and thus did not get L isomers into the product. Well thank you

 

[Acab1312]

Hello, I greet you all. I want to share with you my experience with the separation of isomers using L-wine. I did three tests. 2x using methanol when I changed the ratio of free base methanol and tartaric acid in both tests. Both tests turned out basically the same, after combining the ingredients and mixing, a solid mass precipitated, which I filtered after 24 hours. As for the appearance of the product and the overall split isomers, perhaps there was a little more products in one test than in the other test. From 30ml of free base I got about 9 grams of d-meth. During evaporation, when the crystals started to appear, it looked good at first, small needles were formed here and there, but the drier it got, the more it resembled a racemate (ugly amorphous substance). When it dried completely, in terms of appearance, I could not tell the difference between the racemate and this divided product. When it was put on foil and warmed up a little, it was obvious that the crystals crystallize a little faster after dissolution than when it is done with the racemate. From this I concluded that some division took place, but not enough. I note that I did not wash the tartrate powder during filtering. It was not written in the procedure, so I preferred not to do it. Well, now we come to the third test, which I did with the help of water according to the btcboss procedure. After combining all the ingredients and mixing vigorously, after a while I got a thick, really thick mass resembling some kind of cream. It had a consistency basically like the photo that was added by the user Sjeik a couple of posts above mine. I closed the container and let it sit for 24 hours, then I put this substance in the filter and spread it over the vacuum filter and turned on the suction. This thick cream-like substance was really difficult to filter, also in the procedure there was nothing written about washing the tartrate in the filter, so I didn't do it. I only got 11 grams of product from 60ml of free base. But the crystals that arrived were transparent and beautiful. I tried melting them on tin foil to see how fast they solidify and it was really fast like pseudoephedrine meth. So I think that the Split izomer was successful except for the mass tragedy of only 11 grams. The problem was probably mainly that I had a bit of a problem during filtration with the fact that the funnel on the suction flask did not seal well and it might also help to wash off the tartrate salt during filtration, but please advise me how much water I can use for this so as not to disturb the solubility of the tartrate in water and thus did not get L isomers into the product. Well thank you

FringgRepeat the isomeric separation for a higher yield.

Freebase the failed salt and repeat process

- Wash it with cold anhydrous methanol, the L-meth/tartaric acid mixture is not soluble in methanol.

 

[qwe111]

Repeat the isomeric separation for a higher yield.

Freebase the failed salt and repeat process

- Wash it with cold anhydrous methanol, the L-meth/tartaric acid mixture is not soluble in methanol.

Acab1312Sir, after cleaning the mixture with methanol, the methanol is mixed into the mixture of D methyl and water.
Is D methyl soluble in methanol?

If D and methanol are mixed, do we just need to add sodium hydroxide solution to separate them?