4mmc brown crystals. How to fix it ?

[Zabka]

Hi everyone.
I had a problem with color of my 4mmc crystals. Crystals become BROWN color.
Does anyone have a solution of this problem ?

 

[$!$]

Wash with acetone.
What way u use to made it?

 

[Zabka]

Made in DCM
Washed with acetone. After wash, the powder was white.

I am interested how to fix it

 

[Berlin777]

how you crystallized? Have you picked cleaner crystals before full evaporation of solvents?

 

[Zabka]

Yes, exactly. I think that’s the problem. Crystals were white at the beginning of crystallization, and in the end become brown.

 

[Dr. MMX]

wash in minus celcius temp acetone
i believe you did somem isatkes when crystalizing, like you crystalized that including impurities. if liquid with mmc was dark colors you should removethem before all of the luqid crystalized - I believe.

 

[Dr. MMX]

remember to make them almost solid to make good purufication, if you dont do that you will waste a lot of acetone,1-3 rinses will dp its job but if you wont push them into surface it will take a lot

 

[Dr. MMX]

if you have not good quality acetone - you should distill it 1st, but if you have access to buy clean or better - possess it and use it

 

[Dr. MMX]

as well please tell us what exactly you do to "crystalize" it, i think we can improve that as well

 

[Zabka]

I make a solution of water / IPA (70/30), warning it up and add 4mmc powder, in proportion ( 1g 4mmc / 2,5ml water/ipa )
After complete dissolution I pour it into a container for evaporation and put it in dark place.

 

[Dr. MMX]

what was color of solution?

 

[$!$]

And on big scale u will wait weeks and temp need room minimum 25°

 

[$!$]

The same can do in 1 day

1:50 sec the same made meth

 

[Dr. MMX]

^ yes
proper crystalization would be that you disolve product with as less as you can of hot boiling solvent, then you get crystals in 1h

 

[$!$]

Made video and show is better for other people to see

 

[Zabka]

Light enough (lemon color) for the volume that I did.

 

[Dr. MMX]

Zabka, you just left your solution to evaporate all of it, instead of that you should leave impurities and take crystals when they were clean

 

[MocnykutasMomIsHot!]

Yes please made video because is better for "OTHER" people to see. Not for mine son though cause he already made 10 years.

 

[ifeelsorry]

@MMX right now I'm in evaporation process of 60g of meph powder in 30:70 water: alcohol solution, If i heat it will it crystalize faster? How much heat should i use ? And how to heat it? Like direct heat for hot plate or hot water bath? What is difference between organic evaporation, and heating it?

 

[$!$]

If like it then is pure

 

[Zabka]

It’s hard to say, my solution volume was 10L, but I think my solution was darker a little bit

 

[Dr. MMX]

yes it was beacsue the impurities were in less volume, cuz of cryatlls appeareed. but your mistake was that you let evaporate solution with impurities that made one solid mass with previously purified crystals.