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Filtering Trouble
- Thread starter onward33
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@Sakkadelic @Memberberries
So I made one mistake, which is when working through the a/b steps I forgot to add vinegar one time, then the solution became overbased when I based it, and I had to compensate with more vinegar to get the harmalas dissolve before salting to crash back out. I think I sorted back out by adding enough vinegar, and I resumed the process and it seems to have gone ok, but Im wondering if this could have caused any issues with my final product (im assuming not, I didn't introduce any new products or anything)? The last few a/b rounds went smooth, so I assume Im back on track and what Im looking at is good product, but I don't want to consume anything Im not sure about. So my questions are now as follows:
What color should my final product be? It's almost pure white at the moment with clear water above when the solution settled. Im currently doing water washes (final step), should the PH of the solution go down with each wash? It's still pretty high after 1-2 washes (like 11ish using test papers). I used lye for each a/b step except the final one, in the last base I used sodium carbonate solution (again, just want to make sure safe to consume)
The final couple rounds of salting during the a/b process created pretty small, powdery needles, not long needles as shown in many pictures. Is this an indication that I went wrong somewhere or is that fine?
Here's a pic of my current situation, keep in mind I just washed and stirred like 20 minutes ago so it's still settling. The water above the freebase is basically clear once settled.
So I made one mistake, which is when working through the a/b steps I forgot to add vinegar one time, then the solution became overbased when I based it, and I had to compensate with more vinegar to get the harmalas dissolve before salting to crash back out. I think I sorted back out by adding enough vinegar, and I resumed the process and it seems to have gone ok, but Im wondering if this could have caused any issues with my final product (im assuming not, I didn't introduce any new products or anything)? The last few a/b rounds went smooth, so I assume Im back on track and what Im looking at is good product, but I don't want to consume anything Im not sure about. So my questions are now as follows:
What color should my final product be? It's almost pure white at the moment with clear water above when the solution settled. Im currently doing water washes (final step), should the PH of the solution go down with each wash? It's still pretty high after 1-2 washes (like 11ish using test papers). I used lye for each a/b step except the final one, in the last base I used sodium carbonate solution (again, just want to make sure safe to consume)
The final couple rounds of salting during the a/b process created pretty small, powdery needles, not long needles as shown in many pictures. Is this an indication that I went wrong somewhere or is that fine?
Here's a pic of my current situation, keep in mind I just washed and stirred like 20 minutes ago so it's still settling. The water above the freebase is basically clear once settled.
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I am not sure I understood the mistake but the product is looking pretty clean, good job! Over basing or over acidifing is not an issue as long as you do it properly in the last step. Yes it seems you still need 1 or 2 more water washes. How are you measuring PH? if PH paper that's good but meter can have problems. One way to test is to rub a drop of the liquid between your fingers, if it feels slippery it is still too basic and you need more water wash, and of course wash you hands well after. Once it feels and tastes like water you're good to go. If you're not using distilled water for the washes, you can add a small pinch of soda carb to make sure you're not losing product.
Powdery crystals from manske happen if you cool it too fast, and possiblly other factors too. To get long needles bring it to a boil and put it in a bowl of hot water and leave it 12 hrs undisturbed.
Powdery crystals from manske happen if you cool it too fast, and possiblly other factors too. To get long needles bring it to a boil and put it in a bowl of hot water and leave it 12 hrs undisturbed.
Yes, using PH paper. Thanks!
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What was your yield?
You've done really well, that last pic you shared looks super clean and a good amount too
You've done really well, that last pic you shared looks super clean and a good amount too
Still evaporating, Ill let you know!
Seems like my yield was a bit low actually, about 1.7g for 86g rue seeds, about 2%. Im not surprised, I wasn't super careful decanting at the end and I think I went through quite a few more wash cycles than probably needed since I oversaturated with base/sodium carbonate. It's fine by me, it's more than what I need and i learned the process.
That's nice, 1.7g of extra pure freebase harmalas!
I think it's more likely the major losses happened during the previous steps. How did you do the manske steps? It maybe what you described with fine powder rather than needles that you needed to wait longer for more xtals to precipitate out, or needed more salt. Also how many manske steps did you do? Each manske step you can expect >5% losses.
Typically you only need to do 1 manske step and another if you wish to collect the harmala HCl. For the A/B cycles, you acidify, filter and base again, no need for manske each A/B cycle
I think it's more likely the major losses happened during the previous steps. How did you do the manske steps? It maybe what you described with fine powder rather than needles that you needed to wait longer for more xtals to precipitate out, or needed more salt. Also how many manske steps did you do? Each manske step you can expect >5% losses.
Typically you only need to do 1 manske step and another if you wish to collect the harmala HCl. For the A/B cycles, you acidify, filter and base again, no need for manske each A/B cycle
Yah I def did too many manskes, I was trying to be thorough but overdid that part. Im satisfied overall and am happy to know that for next time i'll be able to keep it simpler. I do appreciate the advice and help.
