DMT-Nexus member
Posts: 121 Joined: 05-May-2008 Last visit: 30-May-2024 Location: 2nd star to the right
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I've been having a lot of success with small extractions using sodium carb as my base and sunflower oil as the NPS. I decided to try a 500g extraction of ACRB following the same methods I've used on the smaller ones: acid boiling / decanting with citric acid and vinegar till significant color change reduce to minimum volume base with sodium carb and add salt pull with sunflower oil wash with sodium carb salt out with vinegar Things started going wrong as soon I tried basing the reduced liquid. It was a thick red syrup. Upon adding sodium it expanded and kept expanding. I tried to add slowly but clearly not slowly enough. I added around 200g of sodium carb by the end. Eventually it turned into a big spongy mess. So I added more water and this help it to become a thick paste. Usually I do a 'dry' extraction on such a mixture, but this had become too moist, so i added more water and attempted to do a wet extraction. But alas, even after filling 2 1 litre jars over half way it was still not liquid enough. When adding the oil to one jar to test if it would work it just combined in a big sludge. So i transferred to a bigger vessel and added more water. The oil separated but now there is a horrible emulsion in the oil which won't budge. I've added over 300g of salt without any effect. I probably have around 3 litres of fluid in the vessel. I tried sucking off the messy oil and washing with sodium carb which is having some success but even here I am getting more emulsions that won't go away. Too much sodium carb? Any bright ideas where to go from here? intosamadhi attached the following image(s): 20150209_073336.jpg (36kb) downloaded 322 time(s). 20150213_182313.jpg (42kb) downloaded 322 time(s). 20150213_182319.jpg (48kb) downloaded 323 time(s). 20150213_182332.jpg (34kb) downloaded 326 time(s).
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DMT-Nexus member
Posts: 1893 Joined: 18-Jan-2008 Last visit: 26-Sep-2023
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Looks like the dreaded soap Im afraid. For the emulsion you can separate it and reacidify it then heat it on the stove, separate the layer of oil again, allow it to cool then freeze it. Pour off the remaining oil then rebasify steadily and pull again. The main jars dont have enough water in anyway, 500ml per 250g of sludge is not adequate for a wet extraction you would need at least 1l , considering the saponification you could need way more, say 1.5-2l/250g sludge.
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DMT-Nexus member
Posts: 121 Joined: 05-May-2008 Last visit: 30-May-2024 Location: 2nd star to the right
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Hey DreamTripper, you're always the fastest to come to my aid ;-)
The large vessel has around 3 litres of water in it now. I don't think this is saponification because I've seen that before and it looks different. This is mostly a foamy layer which is getting trapped in the oil. When i agitate the water very quickly it bubbles.
Re-acidifying at this point is going to be hell i think considering how much sodium carb I've used and how much liquid there is. Also, after re-acidifying I will be back to square 1 and am still not sure on how to proceed since this is the method Iโve used for smaller batches without problems.
What i am considering is pulling with the oil regardless of the mess and trying to clean it up as best I can. Then salting out from the mess. It will produce a dirty product but it should still be usable for oral dosing. What do you think?
There is still enough room for me to add more water in that container. But my concern there is that the more water I add the less efficient the pulling will be.
I am determined to win here though ;-)
Any thoughts on what to do with the other jar? I've added a bunch of salt which has now pushed the volume up to almost 1 litre of sludge (no oil in there, just basic mix). I could just throw that in with the rest and try to pull it all. I can't think of any other way to dry the mix so that i could do a dry pull from it.
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DMT-Nexus member
Posts: 121 Joined: 05-May-2008 Last visit: 30-May-2024 Location: 2nd star to the right
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DreaMTripper wrote:Looks like the dreaded soap Im afraid. For the emulsion you can separate it and reacidify it then heat it on the stove, separate the layer of oil again, allow it to cool then freeze it. Pour off the remaining oil then rebasify steadily and pull again.
Ah i misread this. Thought you were implying to re-acidify the whole mix. I don't really understand why this happened. My previous liquid extraction worked really well. No emulsions and very fast separation. So I am a bit lost. I didn't use so much citric acid during the acidification phase last time, and I used more decanting and less boiling. So maybe that has something to do with it. I noticed quite a lot of foam during the acid cooks but this disappeared once it was reduced enough. Perhaps all the boiling has pulled more fats from the bark?
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DMT-Nexus member
Posts: 121 Joined: 05-May-2008 Last visit: 30-May-2024 Location: 2nd star to the right
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I think i know whats going on now. I believe i have pulled a lot of plant fats from the bark, because of all the acid boiling (usually i decant). This has never been an issue with smaller batches but because I am working with 5x my normal amount it has become an issue.
I've also always had problems with my oil developing emulsions during the salting phase. I used to think that this was just because the oil and vinegar combine to make a soapy layer by default. Now i suspect that it is also because of the plant fats. What I've noticed is that the first 1 or 2 pulls are usually emulsion free but after that more and more emulsions develop as more fats are pulled with the oil.
So my strategy for future extractions will be to do a defat step before basing.
Right now I am having success with washing the dirty oil i am pulling, so its not completely futile, just very messy. ;-)
1 pull down, another 8 to go
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DMT-Nexus member
Posts: 995 Joined: 08-Dec-2013 Last visit: 24-Apr-2022
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Looks like an awful lot of work just to be food safe , is that the reason you choose this Tek Intosamadhi ?
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DMT-Nexus member
Posts: 121 Joined: 05-May-2008 Last visit: 30-May-2024 Location: 2nd star to the right
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Partly, but it's mostly because these are the most accessible items at my disposal. I live on a tropical island and its not easy to come by other reagents here. If i could get high quality ethanol i would use that, but I haven't managed to find any yet from the chemical supply companies around here. I've used limonene and lime before, but those I had to order online and have a friend bring over for me.
The idea of getting the whole job done with simple ingredients like vinegar, oil and sodium carb appeals to me. So i am going to keep at it until i figure out a way to make the process as quick and easy as possible. It would be great if it could all be done in 1 jar like with cyb's salt tek, but this doesn't work well with oil because its so thick.
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DMT-Nexus member
Posts: 1893 Joined: 18-Jan-2008 Last visit: 26-Sep-2023
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intosamadhi wrote:DreaMTripper wrote:Looks like the dreaded soap Im afraid. For the emulsion you can separate it and reacidify it then heat it on the stove, separate the layer of oil again, allow it to cool then freeze it. Pour off the remaining oil then rebasify steadily and pull again.
Ah i misread this. Thought you were implying to re-acidify the whole mix. I don't really understand why this happened. My previous liquid extraction worked really well. No emulsions and very fast separation. So I am a bit lost. I didn't use so much citric acid during the acidification phase last time, and I used more decanting and less boiling. So maybe that has something to do with it. I noticed quite a lot of foam during the acid cooks but this disappeared once it was reduced enough. Perhaps all the boiling has pulled more fats from the bark? Yeah I wouldnt be surprised. Hard boiling will break down the whole material rather than tease the alks out gently I think those types of teks require finesse and patience. You seem to be on the right track now its all a learning process.
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DMT-Nexus member
Posts: 1311 Joined: 29-Feb-2012 Last visit: 18-Jul-2023
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intosamadhi wrote:Partly, but it's mostly because these are the most accessible items at my disposal. I live on a tropical island and its not easy to come by other reagents here. If i could get high quality ethanol i would use that, but I haven't managed to find any yet from the chemical supply companies around here. I've used limonene and lime before, but those I had to order online and have a friend bring over for me.
The idea of getting the whole job done with simple ingredients like vinegar, oil and sodium carb appeals to me. So i am going to keep at it until i figure out a way to make the process as quick and easy as possible. It would be great if it could all be done in 1 jar like with cyb's salt tek, but this doesn't work well with oil because its so thick. I'd like to see all the kinks in this process worked out & a tek written up Food safe & easily available, more discreet materials used in extraction is a major plus.
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