Synthesis with H2S04 and CaCO3/CaO?

[ponellibro]

Hi there,
i saw many synthesis methods here and they all seem a bit complicated to me.
My situation is: i got 1l of the yellow oil (i guess its BMK?) and the person, who gave it to me, didn't have a proper instruction for me.
I just got the info, that i need to put the oil in a big dish made out of thick glass and drop H2S04 slowly into the oil.
The other info i got, is that i need some additional ingredient like chalk - but i don't even know if its CaCO3 or CaO.

1. Can somebody please tell me, if this method can work?
2. How much of the sulfuric acid would be needed?
3. Do i need CaCO3 or CaO in addition?
4. When do i need to add the chalk?

Thank you guys!

 

[HerrHaber]

If the acid is all you need to add you most probably got A oil (amphetamine freebase), in this case you need to form the sulfate salt. CaCO3 is an inert insoluble white powder that can be used to cut the product but I advise to use it moderately for this purpose since insoluble means people will have CaCO3 in their noses that won't dissolve. Now, my advice is to dilute part of your oil with at least same volume of acetone and then make a solution of H2SO4 in acetone 5mL acetone per mL acid (the amount of acid needed is dictated by the quantity of A oil) the acid must be added drop by drop with thorough stirring, you will observe it go milky at first and then thicken as you add the acid. The point is not to add too much acid (solution will start to dissolve the precipitate) case in which you add a little bit more A oil. Then you filter the whole thing and wash it with acetone on the filter.

 

[ponellibro]

Thank you!!!
How can i do the filtering process? Are ordinary coffee filters suitable?

 

[bybys_siurblys]

Yes, coffee filters will do, but vacuum filtration is better for filtering crystals, because it sucks off more of the solvent and its faster.

 

[HerrHaber]

ordinary coffee filters will do as well as vacuum filtration as mentioned above which is encouraged but if you simply don't have the vac system then a coffee filter holder (reusable plastic fine sieve with the shape of the coffee filter open that you can place in a palstic funnel large enough to cover at least 2\3 of the thing and it makes gravitational filtration with the coffee filter much faster.

 

[HerrHaber]

Please do yourself a favour and try this with max 25mL oil and 50mL dry acetone to which you only have to prepare like 1mL H2SO4 conc. in 10mL dry acetone (the entire acid solution may not be needed unless you keep adding oil to reach pH not lower than 6) and remember to throw the acid in acetone solution away since it can't be kept. I advise this in case you have BMK oil, which you will know from the first few drops of acid in case no turbidity appears in a minute or two of dropping case in which not that much harm is done just dump in some mild base like sodium carbonate NaCO3, known as washing soda or pH+ (raiser) from the pool supplies you need like half or teaspoon or less then decant it. Remember BMK is one step away from either amphetamine or methamphetamine but you should write back for the process you need to make is different and even if a bit more complicated still doable and well worth it.

 

[ponellibro]

Thanks a lot! One last question:
The H2SO4 has a concentration of 15%. I also found 33% HCl at home. Is it also possible or is it even better to do it with HCl - because of the higher concentration?

 

[UWe9o12jkied91d]

I assume you mean 15% in water, if yes then it is not suitable, especially for that quantity.Each gram of water will eat a gram of product.Ideally you want it as high conc. as possible and as pure as possible.Dirtier and less conc. acid can be used to a point, if this is the case it is highly recommended to freeze your solution for 24h and ideally dillute with more acetone than regular.
Sulphuric acid yields sulphate, HCl yields hydrochlorides. Amphetamine hydrochloride is hygroscopic and not suitable.

 

[ponellibro]

Do I need dry Acetone? Not the fluid?

 

[UWe9o12jkied91d]

Dry =/= solid
By dry acetone it is meant that it needs to contain as little water as possible, since they are miscible with one another.
If it is not available anhydrous it can be dried with drying agent such as MgSO4, CaO, NaSO4 if the water content is low, if it is high or there is other solvents in the mix it's gonna need to be distilled, possibly twice.

 

[ponellibro]

"it is highly recommended to freeze your solution for 24h" you mean the 15% solution of H2SO4 right? And then? The water freezes and i can remove it from the top? and it really needs 24h?

 

[UWe9o12jkied91d]

Not, I told you 15% is not suitable.If you want maximum yield then yes.

 

[ponellibro]

i only have the fluid, but it is pure acetone not a product containing acetone like nail p. rem.
just to be sure i make it the right way:

1. prepare higher concentrated H2SO4 (freeze it in a dish, where the water can easily be removed)
---next day
2. dry the freebase with MgSO4 and wait for 30mins
3. prepare the drop solution:
-dry the acetone with MgSO4 (WHAT AMOUNT?)
-mix the prepared H2SO4 (out of the freezer, water removed) with the acetone/MgSO4 solution like 1:5 or more 1:10
4. drip the acid solution slowly into the base and stir all the time
???
I hope I'm on the right track now

 

[UWe9o12jkied91d]

You can’t freeze the water in sulphuric acid.
Try to get at least 38%

 

[UWe9o12jkied91d]

DOESN’T MATTER

Also, you put the crystalized product after acidification in the freezer, so it’s clear.Dosen’t hurt to put the acetone in aswell and use it cold

 

[ponellibro]

Sorry I don't understand. Can I freeze the 15% H2SO4 and remove the water (on top) to make it higher concentrated and suitable?
"If you want maximum yield then yes" you mean for 24h or what?

 

[UWe9o12jkied91d]

Again, no, you cannot freeze the water in sulphuric acid sol.

 

[ponellibro]

unfortunately this is not possible in the country where i live.
15% is all i can get so i need to work with this somehow

 

[UWe9o12jkied91d]

You can try, but don’t say i didn’t warn you

 

[ponellibro]

OK so now i have this last problem. my H2SO4 has only 15%...
So what can I do?
Can I boil the water away if i can't freeze it away?
Can I do smth else to get a higher concentration?
Or can i substitute the sulfuric acid with other acids? Citric acid f.e. is avaliable in high concentrations fluid or anhydrous...
Ordering higher concentrated H2SO4 is the last option!
Please help, I'm stuck

 

[broken_sharded]

Go to the hardware store and by drain cleaner like rooto liquid drain cleaner, it is 93% sulfuric acid.