Harmala CWE experiment

[Ambrosaure]

@Ambrosaure another base that is convenient in availability and in not having any risks of having excess base in the end result is ammonia.


What helps break down the fibers is the process of freezing and thawing, so they don't need to remain frozen for any particular time. Once they're completely frozen you can thaw them already (although there's no harm in leaving them frozen for longer).

thanks! finally I found soda pretty easily so I took that, but I note ammnoiac for next time (but it's more expansive than soda)

Also, I'm not sure if I understood right this part of the recipe so in case:

• In the morning I decanted as much as possible of the liquid, acidified with vinegar until color change is observed and the solution becomes fluorescent again, I add a bit more acid for good measure but a lot of stuff won't dissolve so one should not keep adding acid. I let the solution rest for some hours for the impurities to settle, then pour the solution slowly through a coffee filter leaving the impurities till the end so they won't clog the filter early on.
• I then based again using as little base as I could, let settle, decanted and did 2-3 water washes with at least 10x the volume each (I used mineral water with 7.9 pH). Finally I moved it to a narrow cup and let it settle in the fridge, poured off the water, and put it a wide dish to dry on the roof in the shade.

What I understand is:
- basify the harmalas liquid will decant it (make visible separation between the tannin and harmalas) (and also what should the liquid color look like at this point?)
- wait until it's the most decant it can get
- put back vinegar (we don't took anything before that from the yellow liquids right?)
- filter to get off impurities
- base again, decant, wait
- and now we can get the harmala white powder? not sure if i'm right. So we filter the potion to get that, wash it with water (I don't understand "10x volume each", if we have like 1g of powder thats mean 10g of water?)
- and then dry it

I'm gonna basify for the first time in my life, I hope it's gonna work

 

[Transform]

super cheap sodium carbonate at the store so I'm just gonna buy that

While that is absolutely OK, it's still worth noting that the SC produced from baking soda would technically be closer to food grade than the stuff (presumably Heitmann brand, if I'm inferring your region correctly?) which is sold as a cleaning agent (and there's also the stuff sold as "aktiv Natron" which is essential the cleaning-grade form of sodium bicarbonate).

visible separation between the tannin and harmalas

While I wouldn't necessarily call the base-soluble components of rue 'tannins', the rest of your procedure looks about right. Patience is key - you're gonna get a lot of practice with decanting, and bear in mind that if you keep your supernatant and washings, you'll be able to rescue some of the fine solids that sometimes escape. Have a plentiful supply of large jars ready, and best of luck!

 

[Ambrosaure]

While that is absolutely OK, it's still worth noting that the SC produced from baking soda would technically be closer to food grade than the stuff (presumably Heitmann brand, if I'm inferring your region correctly?) which is sold as a cleaning agent (and there's also the stuff sold as "aktiv Natron" which is essential the cleaning-grade form of sodium bicarbonate).

Oh okay I understand! I will know for next time and I'm not german, I'm french aha (why did you think I was German haha?) , I bought this one excatly

While I wouldn't necessarily call the base-soluble components of rue 'tannins', the rest of your procedure looks about right. Patience is key - you're gonna get a lot of practice with decanting, and bear in mind that if you keep your supernatant and washings, you'll be able to rescue some of the fine solids that sometimes escape. Have a plentiful supply of large jars ready, and best of luck!

Ok thanks! Here for the record is the first pull after his first decant, and the second pull just before being decanted (I just poured the soda right in and stirred it with a metal spoon so I wouldn't have to add any more liquid)
I took the rue and put it the freezer to get more from the third pull
I use 30g of rue

 

[Ambrosaure]

acidify the harmalas with a minimal amount of acid so that they redissolve and pour through a coffee filter into a collection vessel, getting rid of undissolved stuff.

just a rapid question because I'm doing this step now, it is normal that I had to put a LOT of white vinegar to get a ph 6? Maybe I put too much soda and that's why but I even had to find a bigger jar

 

[blig-blug]

just a rapid question because I'm doing this step now, it is normal that I had to put a LOT of white vinegar to get a ph 6? Maybe I put too much soda and that's why but I even had to find a bigger jar

If you needed to use a very large amount yes, it probably means you had an excess of sodium carbonate that hadn't dissolved, together with your harmalas. I personally like to dissolve the base (when it's sodium carbonate or sodium hydroxide) before adding it, making a saturated solution that I then add as needed to the acidic part. That way it's less likely you have undissolved base in your harmalas.

It's important to make sure that your final product doesn't have sodium carbonate. For that, you can put the harmala freebase in water and stir (it won't dissolve), and then check pH. If the pH is high, you can do washes adding water, decanting, and repeating the cycle until the pH is close to 7. The larger the volume of water you use for this, the less cycles you'll need.

 

[Transform]

why did you think I was German haha?

oops, sorry must be the "saure" (="sour") bit of your name, and it's resemblance to "Säure" = "acid". But, hey, only one country off, eh? One of the other French Nexians is close to the border and… European history, etc.

Regarding the addition, of a solid base - if you imagine what happens when a particle of SC enters the harmala solution, the harmala freebase forms instantaneously, right at the surface of the particle as the SC begins dissolving. The resulting crust of insoluble freebase effectively stops any more of the SC from going into solution and, well, you now know the result.

I do feel like my explanation of converting baking soda may have contributed to your decision, and I did omit to emphasise that use of SC solution, and not solid, was actually necessary to help avoid this minor inconvenience. Please accept my apologies - but I hope you also learned something.

The liquid volume you hoped to save with that method has now been more than made up for by the additional vinegar you've had to use, as vinegar is typically far more dilute than the sodium carbonate solution you'd want to be using. A possible silver lining here is that your next base precipitation should come done nice and clean.

A couple of quick questions - what water did you use? And, now that I know my assumption was wrong, did you use anhydrous soda or the hydrated form?

super cheap sodium carbonate at the store

 

[Ambrosaure]

oops, sorry must be the "saure" (="sour") bit of your name, and it's resemblance to "Säure" = "acid". But, hey, only one country off, eh? One of the other French Nexians is close to the border and… European history, etc.

Regarding the addition, of a solid base - if you imagine what happens when a particle of SC enters the harmala solution, the harmala freebase forms instantaneously, right at the surface of the particle as the SC begins dissolving. The resulting crust of insoluble freebase effectively stops any more of the SC from going into solution and, well, you now know the result.

I do feel like my explanation of converting baking soda may have contributed to your decision, and I did omit to emphasise that use of SC solution, and not solid, was actually necessary to help avoid this minor inconvenience. Please accept my apologies - but I hope you also learned something.

The liquid volume you hoped to save with that method has now been more than made up for by the additional vinegar you've had to use, as vinegar is typically far more dilute than the sodium carbonate solution you'd want to be using. A possible silver lining here is that your next base precipitation should come done nice and clean.

A couple of quick questions - what water did you use? And, now that I know my assumption was wrong, did you use anhydrous soda or the hydrated form?

saure comme from "dinosaure" actually haha (I was a lot into dinosaur as a kid )

No problem at all, I learned something so no worries. I expected to have difficulty doing this recipe anyway. And btw I remember I have acid citric so I could have use that instead of 1L of white vinagar and I did a second mistake, I through we needed to put the ph back to 11 so I put a ton of soda lol (for changing ). And after rereading I saw it only needed to be base Well, I can only do better for the next two pull aha

I used demineralised water And I used anhydrous soda But blig blue explained just above why I shouldn't do that so I'm not gonna do that for the 3th pull

So your message made me have a new question, for the last step, when we wait for the harmalas to decant again do we need to wait a lot of time or should it be instant? If it's instant can I filter it now and retrieve the freebase?

 

[Transform]

for the last step, when we wait for the harmalas to decant again do we need to wait a lot of time or should it be instant? If it's instant can I filter it now and retrieve the freebase?

Waiting a while for the fine solids to settle helps to improve yields a little, as well as letting the 'cake' of precipitate to consolidate somewhat, so that losses are reduced during decanting.

If you can put it in the fridge for this part, the gentle vibrations help with the settling process while the lower temperature keeps the solubility of the freebase to a minimum.

If it's more convenient for you to proceed as soon as the solution has visibly cleared of turbidity, that's fine but it may be worth keeping the decanted liquid to check whether anything more settles out.

 

[doubledog]

Oh okay I understand! I will know for next time and I'm not german, I'm french aha (why did you think I was German haha?) , I bought this one excatly

Ok thanks! Here for the record is the first pull after his first decant, and the second pull just before being decanted (I just poured the soda right in and stirred it with a metal spoon so I wouldn't have to add any more liquid)
I took the rue and put it the freezer to get more from the third pull
I use 30g of rue
View attachment 108866

It does not seem right, there is no visible sediment in your jars.