mescaline is freely soluble in alcohol; denatured ethanol or everclear would be suitable
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soxhlet exctracter
- Thread starter Dwhitty76
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Attention All Shipping
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Anyone?Attention All Shipping said:
that denatured ethanol is fine, even with the adulterants they add (pyridine? ugh)
what swiy would do is an a/b or STB extraction on the reduced volume of alcohol (boil down the alcohol to a managable amount, 100mL or less).
what swiy would do is an a/b or STB extraction on the reduced volume of alcohol (boil down the alcohol to a managable amount, 100mL or less).
Attention All Shipping
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Thanks Benzyme,
So the IPA/ethanol would need to be treated just as MHRB juice after going through the soxhlet, got it.
What about the appropriate volume of IPA/ethanol for, say 100g of MHRB, any idea what would be the suitable volume to use?
As you say denatured ethanol would be fine I assume that the same would be true of methylated spirits?
So the IPA/ethanol would need to be treated just as MHRB juice after going through the soxhlet, got it.
What about the appropriate volume of IPA/ethanol for, say 100g of MHRB, any idea what would be the suitable volume to use?
As you say denatured ethanol would be fine I assume that the same would be true of methylated spirits?
yes
about 200-250mL alcohol should do it, or as much alcohol as it takes to fill the extractor for cycling
about 200-250mL alcohol should do it, or as much alcohol as it takes to fill the extractor for cycling
ChemicalEudaemonia
Rising Star
One time when SWIM was using a sox, much of the solvent was absorbed by the plant matter, and with the combination of inadequate drainage he ended up burning the entire 1/2 pound worth of collected extract. SWIM's home still smells of burnt DMT and mimosa... Now he makes sure the plant matter is always somewhat saturated and the flask filled at least 80% full. Also, he employs a drain mesh to ensure that the liquid always siphons (This is just a piece of screen that has been wrapped around a pen to form into a cylinder. It should span about the length of the soxhlet body. The plant matter simply surrounds the screen after insertion into the body, but be careful not to dump any into it).
SWIM's treatment for excess solvent is to empty the soxhlet body of the plant matter (after all extraction is complete), then run it as normal. Once the solvent distills over and collects just below the siphon U-bend he quickly removes the body and empties it into a container. (Isopropanol is usually SWIM's solvent of choice and the collection is extremely pure and reuseable for future extractions). When the volume of the boiling flask is significantly reduced, he dilutes it with a bit of water and further fractions off the rest of the alcohol.
SWIM usually does a basification on this extract and pulls with DCM or naptha as standard procedure. If you're working with a small volume, or alcohol is still present, it helps to dilute with about 1/2 - 1 liter of water to aid viscosity. In the case your extract is in alcohol, it is always necessary to dilute this with water otherwise your solvent of choice will mix and refrain from separating.
SWIM's treatment for excess solvent is to empty the soxhlet body of the plant matter (after all extraction is complete), then run it as normal. Once the solvent distills over and collects just below the siphon U-bend he quickly removes the body and empties it into a container. (Isopropanol is usually SWIM's solvent of choice and the collection is extremely pure and reuseable for future extractions). When the volume of the boiling flask is significantly reduced, he dilutes it with a bit of water and further fractions off the rest of the alcohol.
SWIM usually does a basification on this extract and pulls with DCM or naptha as standard procedure. If you're working with a small volume, or alcohol is still present, it helps to dilute with about 1/2 - 1 liter of water to aid viscosity. In the case your extract is in alcohol, it is always necessary to dilute this with water otherwise your solvent of choice will mix and refrain from separating.
Attention All Shipping
Rising Star
I know this thread has been inactive for a while but I thought it better to include my question here rather than start a new thread.
I've just splashed out on a Soxhlet and I'm now ensuring I've got everything set up ok to run it. I've got 8mm id tubing (11mm od) which fits the condenser but I'm having trouble finding something to allow me to attach this diameter tubing to the water tap on the sink (I don't want to buy an aquarium pump inless I have to & don't have access to a shop to make sure I'd get the right one/right size connection anyway) so can someone point me in the right direction for a tap attachment/s so I can fit the condensor tubing directly to the tap?
Thanks
I've just splashed out on a Soxhlet and I'm now ensuring I've got everything set up ok to run it. I've got 8mm id tubing (11mm od) which fits the condenser but I'm having trouble finding something to allow me to attach this diameter tubing to the water tap on the sink (I don't want to buy an aquarium pump inless I have to & don't have access to a shop to make sure I'd get the right one/right size connection anyway) so can someone point me in the right direction for a tap attachment/s so I can fit the condensor tubing directly to the tap?
Thanks
Eagerfish
Rising Star
Well the low budget way is to use a simple funnel. Connect the tubing to the small side of the funnel, use some iron wire to connect the funnel to the tap. You don't really need a lot of water, just a small amount will do. That's why the funnel won't be overloaded.
This method was tested and approved by SWIM
This method was tested and approved by SWIM
Attention All Shipping
Rising Star
I hadn't considered that, its certainly low-tech. I've got a little funnel that fits the tubing and I'll test it out with the condenser attached. Only problem seems to be keeping the funnel attached at the right angle to the tap. I'll need to drill some holes round the top of the funnel to wire it onto the tap but it could work if I can get it attached right. Thanks.
Eagerfish
Rising Star
SWIM thinks he made a terrible mistake: he didn't boil down the denatured alcohol, but he did add some NOAH to basify the solution and he added naptha (@60 degrees celcius). Afterwards SWIM shuffled the solution vigourously with way too much enthousiasm (oops....). The solution was then placed in a hot water bath. After 10 minutes or so, SWIM took a look and all he found was a terrible sticky brown emulsion that reminded him of some brown gelatin pudding
The stuff isn't even liquid anymore! The former solution consisted of circa 600 ml denatured alcohol plus some NOAH and naptha. Is there any way this can be fixed? Should SWIM add water, if yes, how much?
Attention All Shipping
Rising Star
Just wondering if instead of using ethanol as the liquid in a soxhlet 99% Benzyl Alcohol would work just as well, or for that matter Methanol?
69ron
Rising Star
Methanol is a great Soxhlet solvent. Benzyl Alcohol has a really high boiling point (205 C). It would work, but you’d need a really powerful hotplate to boil it, and it would take a long time. Something like methanol is much better with a boiling point of 64.7 C.
Any solvent will work, it’s just that the high boiling point solvents require a really powerful hotplate and tend to destroy more active compounds, take longer to boil, and therefore longer to extract. The lower boiling solvents tend to work much faster and don’t harm as many alkaloids. Solvents that boil at a temperature below water are preferred. Many alkaloids are safe at temperatures just bellowing boiling water (100 C).
Which solvent is best also depends on the alkaloid being extracted. For example, pure methanol and ethanol both can extract the natural mescaline salt present in Peruvian Torch pretty well, but pure isopropanol has a hard time extracting it.
In some cases you need to use water because other solvents might react with the alkalkoids.
Just think of a Soxhlet as a fancy coffee machine. Water works as the solvent, and pretty much any other solvent also works in it.
Any solvent will work, it’s just that the high boiling point solvents require a really powerful hotplate and tend to destroy more active compounds, take longer to boil, and therefore longer to extract. The lower boiling solvents tend to work much faster and don’t harm as many alkaloids. Solvents that boil at a temperature below water are preferred. Many alkaloids are safe at temperatures just bellowing boiling water (100 C).
Which solvent is best also depends on the alkaloid being extracted. For example, pure methanol and ethanol both can extract the natural mescaline salt present in Peruvian Torch pretty well, but pure isopropanol has a hard time extracting it.
In some cases you need to use water because other solvents might react with the alkalkoids.
Just think of a Soxhlet as a fancy coffee machine. Water works as the solvent, and pretty much any other solvent also works in it.
Attention All Shipping
Rising Star
I've finally got everything set up and I ran my soxhlet for the first time today, actually its still running. I'm just not sure its running correctly so I wanted to ask your advice.
I can't post a pic at present as my camera battery is charging but I've observed that the level of IPA in the siphon arm (little inner tube) hasn't changed or moved at all in the 3 hrs its been running, there are drips coming out the bottom of it but I'm concerned that this might just be IPA thats evaporated up the siphon arm and condensed out again.
It hasn't siphoned at all, though I realise this doesn't imply anything.
I'm a little concerned that IPA may be going up the distillation arm (larger outer tube) condensing in the condenser and then dropping back into the distillation arm. I'm not sure if my eyes are playing tricks on me through the curved glass but I think that I've seen some going down the dist arm, not too sure though as it isn't too easy to tell.
I'm not seeing any condensate in the condenser other than drops from the bottom of the lower condenser bulb - though these drops are clear and haven't stained the cottonwool at the top of the soxhlet at all.
The IPA in the flask is dark in colour, though this may be because of a wee mistake in the beginning when before turning on I saturated the MHRB, to aid flow of IPA, by pouring some IPA in the top of the soxhlet to let it flow down. I didn't think of the distillation arm & a lot of IPA & MHRB went down there. I removed stray MHRB from flask & arm but the IPA had picked up enough to change colour. Hard to tell but I think in the past 3 hrs it has gotten darker though.
I realise you may not be able to tell me much from this and I'll post a pic as soon as I can take one but I'd appreciate your thougts on whether I'm worrying over nothing or whether soxhlet may be clogged.
Thanks
I can't post a pic at present as my camera battery is charging but I've observed that the level of IPA in the siphon arm (little inner tube) hasn't changed or moved at all in the 3 hrs its been running, there are drips coming out the bottom of it but I'm concerned that this might just be IPA thats evaporated up the siphon arm and condensed out again.
It hasn't siphoned at all, though I realise this doesn't imply anything.
I'm a little concerned that IPA may be going up the distillation arm (larger outer tube) condensing in the condenser and then dropping back into the distillation arm. I'm not sure if my eyes are playing tricks on me through the curved glass but I think that I've seen some going down the dist arm, not too sure though as it isn't too easy to tell.
I'm not seeing any condensate in the condenser other than drops from the bottom of the lower condenser bulb - though these drops are clear and haven't stained the cottonwool at the top of the soxhlet at all.
The IPA in the flask is dark in colour, though this may be because of a wee mistake in the beginning when before turning on I saturated the MHRB, to aid flow of IPA, by pouring some IPA in the top of the soxhlet to let it flow down. I didn't think of the distillation arm & a lot of IPA & MHRB went down there. I removed stray MHRB from flask & arm but the IPA had picked up enough to change colour. Hard to tell but I think in the past 3 hrs it has gotten darker though.
I realise you may not be able to tell me much from this and I'll post a pic as soon as I can take one but I'd appreciate your thougts on whether I'm worrying over nothing or whether soxhlet may be clogged.
Thanks
69ron
Rising Star
Sounds fine to me. The Soxhlet doesn’t always siphon. Sometimes the siphon arm endlessly drips into the boiling flask below.
As long as the liquid level in the Soxhlet isn’t at the level of the distilling arm (the larger outer arm) and is at or lower than the level of the siphon arm, then everything is fine. Don’t worry about it. This can be caused by slow draining in the Soxhlet. Maybe it’s packed a little too tightly. This often happens with DCM no matter how loose you pack the Soxhlet.
Another thing that can lead to this situation is inadequate solvent amount. Try adding about 25 ml of solvent through the top condenser using a funnel. Pour it in as fast as you can. That should force a siphon.
Remember that siphoning isn’t needed for extraction to work. As long as solvent is dripping down the siphon arm, extraction is happening.
As long as the liquid level in the Soxhlet isn’t at the level of the distilling arm (the larger outer arm) and is at or lower than the level of the siphon arm, then everything is fine. Don’t worry about it. This can be caused by slow draining in the Soxhlet. Maybe it’s packed a little too tightly. This often happens with DCM no matter how loose you pack the Soxhlet.
Another thing that can lead to this situation is inadequate solvent amount. Try adding about 25 ml of solvent through the top condenser using a funnel. Pour it in as fast as you can. That should force a siphon.
Remember that siphoning isn’t needed for extraction to work. As long as solvent is dripping down the siphon arm, extraction is happening.
also, the amount of solvent in your RBF to start with should exceed the volume the extractor can hold up to the top of the siphon..very important. otherwise, it will never cycle
69ron
Rising Star
The general rule is:
1 - fill Soxhlet (with herbs in it) until it siphons once.
2 - add 1/2 the amount of solvent used to cause the first siphon.
That works in most cases. But with DCM, it still often doesn't siphon even if the maximum amount of solvent is used.
The boiling flask should never be too low on solvent, and it should NEVER GO DRY EVER! If the Soxhlet is filled to the siphon arm, there should still be enough solvent in the boiling flask to fill the Soxhlet 1/2 over again.
The condenser should only show drops of condensation near the bottom. If drops appear near the lower center or higher, you’re condenser isn’t condensing properly and some solvent may be escaping. You’ll either need to speed up the water cooling it, or turn down the hotplate.
1 - fill Soxhlet (with herbs in it) until it siphons once.
2 - add 1/2 the amount of solvent used to cause the first siphon.
That works in most cases. But with DCM, it still often doesn't siphon even if the maximum amount of solvent is used.
The boiling flask should never be too low on solvent, and it should NEVER GO DRY EVER! If the Soxhlet is filled to the siphon arm, there should still be enough solvent in the boiling flask to fill the Soxhlet 1/2 over again.
The condenser should only show drops of condensation near the bottom. If drops appear near the lower center or higher, you’re condenser isn’t condensing properly and some solvent may be escaping. You’ll either need to speed up the water cooling it, or turn down the hotplate.
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Thanks guys, you've set my mind at ease, I've shut the soxhlet off now & I'll basify & do heptane pulls tommorrow - the amount of recovered DMT will be a final confirmation that everything went ok.
I think that I have filled the soxhlet too densely, though I was surprised how little fit in it, I had weighed out 100g but I could only get 60g in it. I think next time I'll get ahold of some diatomaceous earth or a hollow mesh cylinder to aid draining.
As far as the liquid level in the soxhlet goes it's very hard to tell - probably because its packed too tight. It did look though that it was above the level of the siphon arm so it may not've worked too well. In any event I'll retain the MHRB until after I've recovered crystals & if yield is low I'll reuse it bearing in mind your advice.
69Ron, you say "Try adding about 25 ml of solvent through the top condenser using a funnel. Pour it in as fast as you can. That should force a siphon." I think we must have different types of condenser as that's not possible for me, the only hole in the condenser while at the top is on the side & the outlet pipe comes out from the top. I'd post a pic but I've now found out that my cameras broken.
One final thing, I still have IPA stuck in the siphon arm - from just after where it leaves the soxhlet body to just after the bend where the arm turns downwards. How do I get this out and back into the flask?
Thanks again.
I think that I have filled the soxhlet too densely, though I was surprised how little fit in it, I had weighed out 100g but I could only get 60g in it. I think next time I'll get ahold of some diatomaceous earth or a hollow mesh cylinder to aid draining.
As far as the liquid level in the soxhlet goes it's very hard to tell - probably because its packed too tight. It did look though that it was above the level of the siphon arm so it may not've worked too well. In any event I'll retain the MHRB until after I've recovered crystals & if yield is low I'll reuse it bearing in mind your advice.
69Ron, you say "Try adding about 25 ml of solvent through the top condenser using a funnel. Pour it in as fast as you can. That should force a siphon." I think we must have different types of condenser as that's not possible for me, the only hole in the condenser while at the top is on the side & the outlet pipe comes out from the top. I'd post a pic but I've now found out that my cameras broken.
One final thing, I still have IPA stuck in the siphon arm - from just after where it leaves the soxhlet body to just after the bend where the arm turns downwards. How do I get this out and back into the flask?
Thanks again.
Attention All Shipping
Rising Star
Help, something's gone terribly wrong.
I may be better putting this in the extractions forum but as it relates to soxhlet and 69Ron & Benzyme are familiar with this & use of IPA I thought I'd continue in this thread.
Having a quantity of IPA (~200ml) that's been through the soxhlet I started the next step to get the DMT out, stupidly I went ahead and added Heptane (~30ml) without remembering to basify first. Its a big mistake I know but I'm not sure if what happened next stemmed from that or not. When I added the heptane it didn't really seperate out into 2 distinct layers as it does when added to basified MHRB water. It was then I realised I hadn't added the Sodium Hydroxide (Lye). Not too sure if that was the reason or if the non-seperation is peculiar to IPA but I then added ~25g of Lye. When added this turned the reddish IPA a dull browny grey colour and even after agitating I could see that at the bottom of the flask there is still a lot of undissolved Lye. This doesn't reduce or disappear no atter how much I agitate the flask.
By now a distinct layer of Heptane has emerged.
Have you ever experieced anything like this? Is the greying of the IPA normal? Have I added too much Lye? Did I mess it all up by adding the Heptane first?
And most importantly how can I recover and fix it?
I may be better putting this in the extractions forum but as it relates to soxhlet and 69Ron & Benzyme are familiar with this & use of IPA I thought I'd continue in this thread.
Having a quantity of IPA (~200ml) that's been through the soxhlet I started the next step to get the DMT out, stupidly I went ahead and added Heptane (~30ml) without remembering to basify first. Its a big mistake I know but I'm not sure if what happened next stemmed from that or not. When I added the heptane it didn't really seperate out into 2 distinct layers as it does when added to basified MHRB water. It was then I realised I hadn't added the Sodium Hydroxide (Lye). Not too sure if that was the reason or if the non-seperation is peculiar to IPA but I then added ~25g of Lye. When added this turned the reddish IPA a dull browny grey colour and even after agitating I could see that at the bottom of the flask there is still a lot of undissolved Lye. This doesn't reduce or disappear no atter how much I agitate the flask.
By now a distinct layer of Heptane has emerged.
Have you ever experieced anything like this? Is the greying of the IPA normal? Have I added too much Lye? Did I mess it all up by adding the Heptane first?
And most importantly how can I recover and fix it?
Dwhitty76
Rising Star
Definately keep it in this thread.
Thats strange, I'm not sure of the reaction between heptane and IPA but even if SWIY did'nt basify first....i would think they would still seperate...as if swiy is doing a defat first.
Whenever swim defats he adds the solvent to the aqueous solution before basification to pull any unwanted fats out....based on 69rons & Benzymes explanation... of moving on foward to your normal A/b extion after siphoning through the soxhlet....even if you didn't basify first, i would think they would seperate.
Obvious question : Did you agitate?
This is definately something that 69ron and Benzyme would be more equiped to help you with but i still think it's strange that they didn't seperate.
Swim ran into some trials and tribulations on his first soxhlet extracton....i've come to the conclusion that it is better for extracting from different plant sources,such as phalaris, although i might be wrong.
Thats strange, I'm not sure of the reaction between heptane and IPA but even if SWIY did'nt basify first....i would think they would still seperate...as if swiy is doing a defat first.
Whenever swim defats he adds the solvent to the aqueous solution before basification to pull any unwanted fats out....based on 69rons & Benzymes explanation... of moving on foward to your normal A/b extion after siphoning through the soxhlet....even if you didn't basify first, i would think they would seperate.
Obvious question : Did you agitate?
This is definately something that 69ron and Benzyme would be more equiped to help you with but i still think it's strange that they didn't seperate.
Swim ran into some trials and tribulations on his first soxhlet extracton....i've come to the conclusion that it is better for extracting from different plant sources,such as phalaris, although i might be wrong.
Attention All Shipping
Rising Star
After I added the Lye it seperated out, so it may've just been a matter of not giving it enough time, though going by past experience of water extractions I thought it had sufficient time to seperate. I did agitate it after adding the heptane & after adding the lye.
After a while I put it all into a coffee filter in a funnel draining into a sep funnel. I still had a lot of lye left in the flask along with some mixed in MHRB/IPA juice so I added watter to it to dissolve the lye. The liquid I poured into the coffee filter is interesting in that no reddish MHRB/IPA drained through the coffee filter, only reddish heptane. Though an awfl lot of it, I think more than I'd put in, so it may not all be heptane, then later more yellowy heptane which I kept in a seperate jar.
The red MHRB/IPA in the coffee filter became more sludgey and much less liquid. Eventually I added the water lye mix to it and emptied the cofee filter so it all drained into the sep funnel. I poured the initial reddish (suspect) heptane back into the sep funnel with it and at present its all seperating out into 2 layers. Actually looking a it now it looks more like 3 - red layer at the bottom, a more irregular greyey red layer then clearer heptane. I wish I had a working camera to show you.
I think I'm going to leave it overnight and see how it continues to seperate.
Regardless of anything else I'm sure I added too much lye, I was just following the noman tek quantities but evidently its not suitable for soxhleted solutions of IPA.
After a while I put it all into a coffee filter in a funnel draining into a sep funnel. I still had a lot of lye left in the flask along with some mixed in MHRB/IPA juice so I added watter to it to dissolve the lye. The liquid I poured into the coffee filter is interesting in that no reddish MHRB/IPA drained through the coffee filter, only reddish heptane. Though an awfl lot of it, I think more than I'd put in, so it may not all be heptane, then later more yellowy heptane which I kept in a seperate jar.
The red MHRB/IPA in the coffee filter became more sludgey and much less liquid. Eventually I added the water lye mix to it and emptied the cofee filter so it all drained into the sep funnel. I poured the initial reddish (suspect) heptane back into the sep funnel with it and at present its all seperating out into 2 layers. Actually looking a it now it looks more like 3 - red layer at the bottom, a more irregular greyey red layer then clearer heptane. I wish I had a working camera to show you.
I think I'm going to leave it overnight and see how it continues to seperate.
Regardless of anything else I'm sure I added too much lye, I was just following the noman tek quantities but evidently its not suitable for soxhleted solutions of IPA.