Homemade PaRodinal questions

[Yamato]

Hi there.

I read a very interesting thread (there was a url link here which no longer exists) about a crystal-clear PaRodinal.

After reading each and every message in there, I end up with some doubts, maybe someone around could help me.

I will be creating, PaRodinal (not Rodinal) with the tips that I read in the threat.
First, I'm obtaining pure paracetamol from paracetamol tablets.
Specifically, I need 15 grams of paracetamol, so I'm using 15 tablets of paracetamol 1 gram.
I mixed those 15 tables with methanol. Heating the mixture and gently agitating, I obtained a whiteish-transparet part and a white precipitate that easily gets in suspension with the white-liquid part, if I agitate.

So, after resting for some minutes and carefully using a syringe, I extracted the whiteish foggy liquid part from the precipitate, and stored this into another crystal bottle.
What I want to do now is to evaporate the methanol to obtain the pure paracetamol diluted in it.

So now, in theory this sounds nice and funny, but I have two doubts:

the liquid part, which theoretically should be Paracetamol + Methanol, does look too much transparent, so I'm not sure if it contains the Paracetamol or the whiteish "fog" is just some excipient in suspension that didn't precipitated to the bottom, or even if I need to aggitate much more to dissolve more paracetamol within the methanol, or if the solution requires much more methanol to not get oversaturated.

I know that something must be diluted because the weight of that precippitate is less than the weight of the 15 tables. I can't remember those weights now, but it was quite a noticeable difference, maybe like 15 or 20% less in weight.

Actually, the liquid that I sepparated has been resting for several hours and right now I can look through it. Also, a very thin layer of precipitate has appeared in the bottom of the bottle, that looks exactly like the one before sepparating with the syringe: white, very "light" in weight and easy to get in suspension if I move the bottle.
The liquid looks like a glass full of water where you pour some drops of milk. You can clearly see through it but it is a bit foggy.
Anyone who did this experiement could tell me how much concentrated should it be? The amount of methanol that I used was like 120 or 125 mililiters, so I can't really start evaporating until I really know that this liquid actually has the paracetamol diluted in it.


The second doubt is: should I just evaporate the methanol "as-is", I mean, place the opened bottle to take the sun, or it is better to cool the bottle so crystals may form on the bottle? I'm not sure which method would be better.



Now, as for another story, not really related to Rodinal, but to developers, I have access to tons of Sodium BIcarbonate (NaHCO3), but not to Sodium Carbonate (Na2CO3) at all.
I read somewhere that it is possible to obtain Carbonate from Bicarbonate by "cooking" the Bicarbonate at 200+ ºC. Is this any true or just an urban legend?

I would like to obtain Carbonate for future use, for example, for Caffenol or any other developer that uses Carbonate. If I'm not wrong, washing soda should be Sodium Carbonate with some unwanted additives, so i would say that using pure Carbonate would result in a developer free of nasty impurities.


[EDIT]

I forgot a small question: is there any way to know if the thing that I may obtain after evaporating the alcohol is really paracetamol molecules or something different? So far, I have both the liquid and another bottle with the solid precipitate.

Thanks in advance.

 

[pschwart]

Pure sodium carbonate is commonly available from stores selling pool supplies (Lowe's and Home Depot in the US). The last time I purchased this I recall it was $8 USD for 6 lbs, so very inexpensive.

 

[David A. Goldfarb]

I'm not sure why one should be concerned about having such a pure form of paRodinal. If it has some precipitate, that's fine. It's diluted usually 1:25, 1:50, or 1:100, so it all dissolves in the working solution, and the stock solution seems to last for years, like the original Rodinal.

 

[Gerald C Koch]

If you heat sodium bicarbonate in an oven at around 300F for an hour the bicarbonate will be converted to carbonate. The crystalline bicarbonate will change to a very fluffy powder. You must use a glass baking dish. Do not use an aluminum one. Transfer the powder to a jar that can be well sealed as the anhydrous sodium carbonate will absorb moisture from the air.

 

[Gerald C Koch]

Once you have extracted the paracetamol, also known as acetaminophen from the tablets with methanol you still have a ways to go to make a developer from it. Unless you live in an area where it is difficult to get Rodinal or one the other commercial name variants it is just not worth the bother to make your own. They are cheap and more dependable.

 

[alanrockwood]

Be very careful working with methanol. It is quite toxic.

 

[Yamato]

If you heat sodium bicarbonate in an oven at around 300F for an hour the bicarbonate will be converted to carbonate. The crystalline bicarbonate will change to a very fluffy powder. You must use a glass baking dish. Do not use an aluminum one. Transfer the powder to a jar that can be well sealed as the anhydrous sodium carbonate will absorb moisture from the air.

I will try doing it.

Once you have extracted the paracetamol, also known as acetaminophen from the tablets with methanol you still have a ways to go to make a developer from it. Unless you live in an area where it is difficult to get Rodinal or one the other commercial name variants it is just not worth the bother to make your own. They are cheap and more dependable.

Doing this is not a bother for me, it is a hobby.

Also the money is a reason why I do it. Getting Rodinal costs me like 20 € per 500ml, while doing it myself costs me something like 5 €.

Be very careful working with methanol. It is quite toxic.

Thanks for the tip. But don't worry, I will be far away, drinking a cup of Caffenol while the methanol evaporates.

 

[Alan Johnson]

If you have some potassium bisulfite you can make a clear version from crushed paracetamol tablets without doing the alcohol extraction you describe.
(there was a url link here which no longer exists)
Using the crushed tablets in place of the capsule contents mentioned leaves all the binder and fillers as solids in solution but it will all be removed at the filtration stage.
If you filter ordinary PaRodinal it will remove sodium sulfite preservative crystals but the potassium version has just as much sulfite preservative as ordinary PaRodinal.
Potassium sulfite is much more soluble than sodium sulfite so you can filter it without removing any preservative crystals.

 

[Xuco Martin]

Make a small amount of Parodinal, from crushed paracetamol tablets without doing the alcohol extraction you describe.
No filter, and then draw your own conclusions
https://www.flickr.com/photos/felixucomartin/sets/72157628196915445/

 

[alanrockwood]

Thanks for the tip. But don't worry, I will be far away, drinking a cup of Caffenol while the methanol evaporates.

Avoid getting it on your skin as well.