Hello all,
This would be my third extraction to date. My first try was a STB tek, second was a variation of an A/B extraction as far as I can remember. This write up is in the middle of an A/B extraction following a combo of Cyb's MAX ION tek and "Art of Liquid-Liquid ext. The Basics" by Dozuki. The plan is/was as follows.
1. 100g of MHRB powdered are added to 400ml of RO water and brought to 50C on a hotplate with overhead stirring for 2 hours.
2. Mixture is allowed to cool to room temp and 3 freeze/thaw cycles are performed.
3. Solution is acidified using hardware HCl to a pH of 2-4. 1)
4. Solution is brought to 60C on a hotplate with overhead stirring for 2.5h.
5. After allowing it to settle, the top (approx. 300ml) is decanted to a beaker.
6. Vacuum filter using a Buchner funnel with a paper filter. 2)
-repeat steps 3-6 with a new addition of 2-4pH HCl solution -
7. Defat using NPS. (I have heptane but i'm stingy with it. I attempted to defat using old NPS that was used for freebase pulls and separated using separatory funnel) 3)
WE ARE HERE
8. Salt using 80g of NaCl
9. Basify to ~6-7 pH and reduce then continue to basify to pH 13 using NaOH or just straight basify to pH13. 4)
10. Add solution to 1L separatory funnel , add NPS (heptane) and do pulls with that. 5)
A few issues arose and I have a few questions regarding them and in general would appreciate tips:
1) Hardware HCl is stated to be 33%. With that information I asked chatgpt to do some math in order to create 0.1M solution. That ended up being 0.03-4 ish judging by pH measurements taken with a cheap digital pH meter. I played around a bit creating different strength solution however I ran into an inconsistency. My digital pH meter would show say a pH of 2.43 , I'll try to double check it with some indicator paper and it wouldn't have any reaction. If i test it directly with a the (supposedly) 33% acid I see a reaction with the test paper.
-Which should I trust - digital pH meter or some pH indicator paper I've found in my stuff?
When making my solution in step 3. i erred of it being too acidic ( around 2) because my indicator paper wasn't reacting. Can that be a problem?
2) Straight vacuum filtration from the decanted liquid proved impossible. I was originally using FAST 90mm filtration paper that got clogged almost immediately. There was also a lot of foaming. I then switched to a piece of cotton t-shirt in the Buchner funnel which proved to work. A lot of foaming again. After filtering it twice i attempted to use a proper filter paper again. Immediately clogged.
-Is there a smarter way to do the filtration? Has anyone used any type of flocculant/clarifying agent at this stage?
I have left my 'acidic pulls' to settle out and i'll try to decant in 12-18 hours and see if that can be vacuum filtered.
3) After the t-shirt filtration I decided to see if the solution isn't clear enough to use my separatory funnel. It seemed like it was. I tried to defat using spent NPS from years ago. 80ml was added and shaken/swirled. Foaming again and quite a bit of an emulsion. That was left to settle which more or less happened. Lower phase was separated with a small emulsion remaining and a clear-ish NPS. I didn't notice a noticable change in the colour of the NPS.
Can I use xylene n-butyl acetate as a solvent for the defat stage as i'm stingy with my heptane? I'll try to get pure xylene but we'll see when that happens.
Am I crazy for being so anal about defatting MHRB?
4) Any suggestions on what I should do here? From 3 acid pulls I'll end up with over a liter of acidic solution. My sep funnel is 1L.
5) How long should I swirl/agitate the NPS during the final pull of the freebase? Should I do it all in the sep funnel or should I do it in a beaker with magstirring for a while then move to sep funnel for the final phase separation?
6) I have read here that there's big problems with emulsions when the acidic/basified solution isn't filtered well.
How clear is clear enough?
Any advice on filtering?
Will emulsions be such a problem even with salting?
Thank you
This would be my third extraction to date. My first try was a STB tek, second was a variation of an A/B extraction as far as I can remember. This write up is in the middle of an A/B extraction following a combo of Cyb's MAX ION tek and "Art of Liquid-Liquid ext. The Basics" by Dozuki. The plan is/was as follows.
1. 100g of MHRB powdered are added to 400ml of RO water and brought to 50C on a hotplate with overhead stirring for 2 hours.
2. Mixture is allowed to cool to room temp and 3 freeze/thaw cycles are performed.
3. Solution is acidified using hardware HCl to a pH of 2-4. 1)
4. Solution is brought to 60C on a hotplate with overhead stirring for 2.5h.
5. After allowing it to settle, the top (approx. 300ml) is decanted to a beaker.
6. Vacuum filter using a Buchner funnel with a paper filter. 2)
-repeat steps 3-6 with a new addition of 2-4pH HCl solution -
7. Defat using NPS. (I have heptane but i'm stingy with it. I attempted to defat using old NPS that was used for freebase pulls and separated using separatory funnel) 3)
WE ARE HERE
8. Salt using 80g of NaCl
9. Basify to ~6-7 pH and reduce then continue to basify to pH 13 using NaOH or just straight basify to pH13. 4)
10. Add solution to 1L separatory funnel , add NPS (heptane) and do pulls with that. 5)
A few issues arose and I have a few questions regarding them and in general would appreciate tips:
1) Hardware HCl is stated to be 33%. With that information I asked chatgpt to do some math in order to create 0.1M solution. That ended up being 0.03-4 ish judging by pH measurements taken with a cheap digital pH meter. I played around a bit creating different strength solution however I ran into an inconsistency. My digital pH meter would show say a pH of 2.43 , I'll try to double check it with some indicator paper and it wouldn't have any reaction. If i test it directly with a the (supposedly) 33% acid I see a reaction with the test paper.
-Which should I trust - digital pH meter or some pH indicator paper I've found in my stuff?
When making my solution in step 3. i erred of it being too acidic ( around 2) because my indicator paper wasn't reacting. Can that be a problem?
2) Straight vacuum filtration from the decanted liquid proved impossible. I was originally using FAST 90mm filtration paper that got clogged almost immediately. There was also a lot of foaming. I then switched to a piece of cotton t-shirt in the Buchner funnel which proved to work. A lot of foaming again. After filtering it twice i attempted to use a proper filter paper again. Immediately clogged.
-Is there a smarter way to do the filtration? Has anyone used any type of flocculant/clarifying agent at this stage?
I have left my 'acidic pulls' to settle out and i'll try to decant in 12-18 hours and see if that can be vacuum filtered.
3) After the t-shirt filtration I decided to see if the solution isn't clear enough to use my separatory funnel. It seemed like it was. I tried to defat using spent NPS from years ago. 80ml was added and shaken/swirled. Foaming again and quite a bit of an emulsion. That was left to settle which more or less happened. Lower phase was separated with a small emulsion remaining and a clear-ish NPS. I didn't notice a noticable change in the colour of the NPS.
Can I use xylene n-butyl acetate as a solvent for the defat stage as i'm stingy with my heptane? I'll try to get pure xylene but we'll see when that happens.
Am I crazy for being so anal about defatting MHRB?
4) Any suggestions on what I should do here? From 3 acid pulls I'll end up with over a liter of acidic solution. My sep funnel is 1L.
5) How long should I swirl/agitate the NPS during the final pull of the freebase? Should I do it all in the sep funnel or should I do it in a beaker with magstirring for a while then move to sep funnel for the final phase separation?
6) I have read here that there's big problems with emulsions when the acidic/basified solution isn't filtered well.
How clear is clear enough?
Any advice on filtering?
Will emulsions be such a problem even with salting?
Thank you