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 ?

 

[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?

 

[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

 

[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?

 

[TheVacuumGuy]

I think your problem lies in the previous step (eg. Filtering precipitate. It may be white, but off-white often also appears white).
For crystallization you could use 2 beakers. In 1 you add water and boil it. In 2 you add dry powder (and/or) a stirbar. Then you slowly pour the some water from 1 to into 2, and place 2 on the heater as well. You keep pouring tiny bits of 1 into 2, until 2 is fully dissolved. You end up having a saturated solution, with minimal of water (1g on 1ml avg). This way, impurities are spotted more easily.

Pour into container and leave for couple hours.

 

[RegulierTier]

You should wash it with cold acetone first.
Then disolve your product in hot isoprop and place it in a freezer (over night) until it recrystallized, suck the isoprop up under vakuum and wash it again with cold acetone.

then start to make crystals...