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soxhlet exctracter

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So, now that swim has evrything he needs for using a soxhlet for his polar extaction,he is debating on how to carry out the rest of his extraction (he hasnt started yet).The Tek that swim has seen written (that uses a soxhlet) also requires distillation and a liquid/liquid extractor for the defatting.Swim is thinking of using a hybrid of vovins tek but using a soxlet for the initial extraction and will be using isp for the solvent.Swim has never defatted before or never recrystalized (he's excited by recrystallization).His first couple extractions were very basic a/b ext (marsfold).Wanted to see if anyone w/ experience w/ soxhlet has any input on whats worked best for them after the polar, or does it even matter?
 
swim honestly hasn't gone the soxhlet route for MHRB (he has with psilocybin from mushroom sclerotia), but will in a couple of weeks. he will run an initial polar extraction in the soxhlet with denatured ethanol, and is debating going STB; extract with DCM. this will ensure better yields than before.
no need to really defat, as MHRB isn't as fatty as say, phalaris grass
 
Finally swim is about to attempt to do his first mhrb extraction using a soxhlet extractor.The solvent of choice is ISP and it was said earlier in this thread that the solvent must be filled to the top of the inner siphon in order for it to siphon properly.It appears as if, in order for swim to fill the flask and have the solvent reach the TOP of the inner siphon (the little tube that reaches all the way to the bottom of the soxhlet joint)it will surpass the level of where the bypass tube starts and he just wants to make sure thats o.k.Swim will post a pic pointing a blade at the level he understads the solvent to reach.Most of the pictures swim has looked at the solvent doesnt even reach the top of the flask,which is why he's asking this question.Also it was never mentioned at what temperature should the hotplate be set at. Swim know's that the boiling point for ISP is 88 celcius (190 F) but swim is dealing with a HIGHLY flammable substance and doesnt want to burn his house down.Swim would appreciate the feedback.I know he's asking a lot of questions and really does appreciate the patience and generosity of those more knowledgeable than he.He just doesnt want to fuck up.
 

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impressive setup. the top end of that inner siphon is where the solvent will peak (half-way up the extractor body), and flush back down into the bottom flask. the large outer siphon is where the solvent boils over and condenses onto the material.
SWIY would just fill the bottom flask about 2/3 full of solvent, put the material in some coffee filters or stuff a cotton ball as 69ron suggested (make sure the material is lower than the top of the outer siphon, obviously), into the extractor body. once it's all assembled, get the water flowing through the condenser (water goes in through the bottom, out through the top), and turn the heat on. it'll take care of the rest of the work.

looks like the same size extractor body SWIM has, looks like it's suitable for ~ 100-200g material at a time.

no need to worry about IPA's flammability, if SWIY isn't working near an open flame.
 
yeah, its actually 500ml soxhlet. If swim does 100g extraction he'd probably be better off using his 500ml flask rather than 1000ml,what does swiy think?Does swiy have any idea of the temp on the hotplate?Does swim bring it to it's boiling point 0f 88c (which is not an option because it goes in 5c increments it would have to be 85c or 90c) does it need to reach boiling point in order to cause siphoning?Swim is glad he has another 2kg's of mhrb,so if anything goes wrong its not a big deal.He still doesnt know if he's gonna do an stb or a/b.
 
Moment of truth! Swim has packed in 100g mhrb ontop of a couple cotton calls,filled the flask w/ sovent and has plugged everything in and its been going for about 10min.As soon as he turned on the power strip w/ the hotplate and water pump are plugged into,he saw the water start to fill up in the condenser.The only thing was it stopped at a cetain point and didnt immediately start flowing out of the outlet.Is that normal?Does it take a while for the water level to build up to where it flows back out of the condenser.The other thing is that swim was suprised for a 500ml soxhlet it seemed like a little bit of a tight squeeze to fit 100g of mhrb.No DE was used the powder wasnt as fine as he thought it would be and the hotplate is set at 85c.Posting a couple pics.
 

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An hr has gone by and nothing is happening.The water level hasent gone up in the condenser nor any siphoning.Should swim be more patient or add more solvent.The boiling point for ISP is 88 c,swim has the hotplate on 85.mabey he should increase it up to 90c.Any suggestions?
 
3 hrs. in and nothing.:( I added more solvent, increased the temp to 90c.Although the water is now flowing through back out the output but no siphoning at all.
 
swim is fucking pissed.Dont know what he did wrong and it's not like anyone in his circle of friends that has any experience w/ a soxhlet that can help.Obviously swim did something wrong and he thought he followed the directions that were given to a tee.I think using a 6 qt crockpot is an easier route to go.Swim is just frustrated and doesnt know what he did wrong. 7 hrs and no siphoning :x
 
Bad luck man, hopefully benzyme or 69ron can identify what went wrong. Was the ISP not boiling/condensing down onto the MHRB powder at all?

Very informative thread by the way.

Not wanting to interrupt your porblem but I just wanted to ask what the steps would be for extracting DMT from the IPA once its extracted everything from the MHRB. Would you just do a few naphta pulls on the IPA or would you need to basify it & then pull with naphta?
 
Dwhitty76 said:
swim is fucking pissed.Dont know what he did wrong and it's not like anyone in his circle of friends that has any experience w/ a soxhlet that can help.Obviously swim did something wrong and he thought he followed the directions that were given to a tee.I think using a 6 qt crockpot is an easier route to go.Swim is just frustrated and doesnt know what he did wrong. 7 hrs and no siphoning :x
Click to expand...

I was looking at the pics above that you posted. The condenser doesn’t look right. The water in the condenser should be all the way up to the top water outlet, but it’s not. Where is the water entering? The inlet at the bottom or the outlet at the top?

If you’re using water to extract, you’ll need a really high temperature on the hotplate. The water should be vigorously boiling, if not, turn up the hotplate. SWIM would use 540 C on the hotplate whenever using water as the solvent.

Also, sometimes siphoning just doesn’t happen. This is the case if drainage inside the Soxhlet isn’t good. If the solvent is dripping out of the siphon tube (the thin tube) of the Soxhlet back into the beaker, then it’s extracting. It doesn’t actually need to siphon to extract.

Make sure you solvent is vigorously boiling. One thing, the Soxhlet is packed a little too high. It’s hard to see if any solvent is dripping down into the Soxhlet that way. Even so, if solvent is dripping out of the siphon arm then you are ok, otherwise the hotplate is set too low, or the Soxhlet is clogged. If the Soxhlet is clogged it’s obvious because the thing fills to the top with solvent.

Getting the hang of using a Soxhlet is a little tricky at first, but once you do, it's easy to use. The problems you're having should have a very simple solution. It's just a matter of finding what you did wrong and correcting it. If I was there, I’m sure I could find the problem in a second, but I'm not there, and it's hard to debug remotely.

Using a Soxhlet can be like staying in a hotel overseas...you know it must be simple to turn on the water in the shower, but you spent 10 minutes trying to turn the damn water on and still can't get the water on! So you call the front desk and are a little embarrassed to tell her your problem, and she says politely, "you just pull the known towards you and turn it to the right", which is the one thing you never thought to try. Sure enough it works. With a Soxhlet, there are a few basic things to it, but if any of them are done wrong, it won’t work.

REASONS FOR NOT SIPHONING:

PROBLEM: Solvent is not entering the Soxhlet or condenser.
SOLUTION: Turn up the hotplate to cause solvent to boil more rapidly until drops of solvent can be seen in the bottom of the condenser.

PROBLEM: Solvent can be smelled at the top of the condenser, siphon tube either slowly drips out solvent or no solvent drips out at all.
SOLUTION: The condenser is not condensing and solvent is escaping the condenser. This means the condenser is set up wrong (water inlet is used as a water outlet) or the coolant in the solvent is not cold enough, or the hotplate is turned up too high so that the condenser cannot cool the solvent well. Make sure the water in entering the bottom inlet of the condenser, not the top outlet. Make sure the coolant liquid is cold. Make sure the hotplate is not set too high.

PROBLEM: Solvent is entering the Soxhlet slowly, siphon tube just drips solvent and never siphons.
SOLUTION: Turn up the hotplate to cause solvent to boil more rapidly.

PROBLEM: Solvent is entering the Soxhlet rapidly, siphon tube just endlessly pours out solvent and never siphons.
SOLUTION: This is fine, the Soxhlet is extracting. It doesn’t need to siphon to extract. This means the material in the Soxhlet is not draining well. You can stop and remove the contents and add more celite to improve drainage, or just continue extracting.

CONDENSER PROBLEMS:

PROBLEM: I smell solvent coming from the top of the condenser.
SOLUTION: The condenser is not condensing and solvent is escaping the condenser. This means the condenser is set up wrong (water inlet is used as a water outlet) or the coolant in the solvent is not cold enough, or the hotplate is turned up too high so that the condenser cannot cool the solvent well. Make sure the water in entering the bottom inlet of the condenser, not the top outlet. Make sure the coolant liquid is cold. Make sure the hotplate is not set too high.

PROBLEM: The condenser is not filling up all the way with coolant.
SOLUTION: The condenser is set up backwards or there is no coolant flowing into it. Make sure the coolant (usually cold water) is entering the bottom inlet and not the top outlet. Make sure the coolant is flowing into the Soxhlet.

PROBLEM: Drops of solvent are forming above the lower half of the condenser.
SOLUTION: The condenser is not condensing well enough. Increase condenser coolant flow or turn down the heat on the hotplate. Also make sure condenser is setup properly. The coolant should enter the bottom inlet and not the top outlet of the condenser and the coolant should be cold.

PROBLEM: The condenser coolant tubing keeps coming off and spilling coolant (water) all over even though they are put on tightly.
SOLUTION: The coolant pressure is too high causing the tubing to come lose. Turn down the pressure of the coolant entering the condenser. The coolant should be flowing slowing into the condenser, but no so slow that it drips. It should form a slow stream of water.
 
I'm glad swiy responded. Swim fixed water level situaion (and the bottom line is the input).The aquarium pump wasnt pushing enough pressure through,so swim elevated the bucket of water to make it easier for the pump and eventually the water did reach the top and circulated back out. Swim couldnt get the solvent to even drip down thru the soxhlet.He used ISP 91% (boiling point 88 c) and he had the hotplate turned up to 90 c,he figured that would be the right temp to get it to boil but it never looked like it was boiling,like water does when it's bubbling.Mabey swim was wrong about the boiling point of isp but he looked it up on the web.Swim used cotton balls like swiy said and he put 2 at the bottom and packed in 100 of mhrb then a couple cotton balls at the top and was suprised on how full it got, and that swim had to pack it tighter so it wouldnt come up so high,it should stay well below the top end of the bypass tube,right?Swim was under the impression that 500 ml soxhlets could handle 250g of mhrb but it doesnt look like it could being that it was so full w/ 100g.Swim had also bought DE because he was dealing with pre powdered bark but when he opened the jugs w/ the bark,he saw that it wasnt as finely powdered as it usually is but it was more coarse and srtringy (he used a new vendor from mexico),so he didnt think there would be any draining issues so he didnt add any DE.The issue was that the solvent wasnt even making it up into the soxhlet.I've seen other post's from swiy and swiy has used ISP w/ MHRB in a soxhlet.So do you think it was simply a temperature issue?What does swiy set his hotplate to when using ISP? Swim is pretty busy during the work week but will probably make a second attempt next weekend.Swim would be complteley lost without hte help of you and benzyme,thanx again.
 
all very good info.

yes, make sure the condenser is cycling, and perhaps try a lower boiling solvent. denatured ethanol (hardware store) should be suitable.

IPA boils about 4C higher than ethanol, it would probably be slightly more efficient to use DE.
don't sweat it, Dwhitty. these things take a bit of practice. know that swiy invested good money in equipment that is tried and true in labs everywhere.

I got bent out of shape the first time I tried to get a stirplate working, it was a bit tricky.
 
yeah, mabey swim should give denatured ethanol a go,if its has a lower boiling point and more efficient.Whatever solvent is used,if it reaches it's boiling point it should look like its boiling,right? just like bubbling water,because i think thats the problem swim was having even though his hotplate was set above isp's supposed boiling point,it didnt look like it was boiling. Swim will give another crack at it next weekend.Looking back at this whole thread w/ swiy's walking swim through this whole process is very good info for all and i hope some other folks get some use out of this really helpful information.
 
The boiling point of IPA is about 82 C.

You need to set the temperature on the hotplate many times higher than the boiling point of the solvent. For example, for IPA, SWIM sets the hotplate to about 400-500 C for a 1000 ml flask filled with 600 ml of IPA. For water he uses 540 C. His hotplate is accurate within +-2.5 C. Remember that the temperature reading on the hotplate is for the center of the surface of the hotplate only. The temperature of the liquid above it in the flask will be many times lower.

Don’t pay too much attention to the temperature reading on the hotplate. It has little to do with the temperature of the liquid in the flask. Just make sure the solvent is vigorously boiling as if you were boiling eggs in a pot. Once you reach to proper boiling level where solvent is entering the Soxhlet but not too hot that solvent in escaping the condenser, then make note of the temperature reading on the hotplate so that the next time you use that hotplate with that flask and that amount of that solvent, then you’ll know exactly what temperature to set the hotplate to to repeat the results.

The temperature on the hotplate is helpful in the future after you’ve determined the right temperature of Y to boil solvent X of Z amount. For example, if 450 C can bring 600 ml of IPA to a boil in a 1000 ml flask, then now you know exactly what temperature to set the hotplate at for future reference. The value to set the hotplate at depends on many factors: size of boiling flask, amount of solvent, type of solvent, model of hotplate, size of hotplate surface, distance from boiling flask to Soxhlet, etc.

Remember, only a hotplate with a probe that can be placed inside the boiling flask gives a reading of the temperature of the solvent. The other hotplates only give the surface temperature of the center of the hotplate. If you’re using a tiny 10 ml beaker filled with solvent, and you set the hotplate to 100 C, the beaker will probably get to about 95 C. If you use a 100 ml beaker filled with solvent, then it might get to about 80 C, etc. The larger the quantity of solvent, and the larger the boiling flask is, the less it heats up. A 1000 ml flask filled with solvent will maybe reach 30 C or so if endlessly sitting on a hotplate set to 100 C.
 
Thats obviously the issue swim was running into.He simply looked up the boiling point of the solvent and set the hotplate to the closest setting,not taking into consideration the volume of solvent. :idea: Swim was using a 500ml flask for 100g he also has 1k ml flask at his disposal.Swims train of thought is that the less solvent used the more saturated the solvent will become w/ alkaloids and so it would be better to use 500 ml than th 1k flask,is swims thinking correct? Also,69ron if swiy is using a 1k ml flask w/ 600ml of solvent and is running his hotplate at about 400-500c,i'm assuming that if swim (given he is still using IPA) is using a 500 ml flask w/ say..300ml of solvent, he's probably looking at a ballpark of 200c -300c.Does that sound about right? Man swim was WAY off at 90c :lol:
 
Dwhitty76 said:
Looking back at this whole thread w/ swiy's walking SWIM through this whole process is very good info for all and i hope some other folks get some use out of this really helpful information.
Click to expand...

I've gotten plenty of useful information out of it already, just wanted to ask a few questions, one follows on from your last post of volumes of solventfor volume of MHRB powder. I wanted to ask what the appropriate (best) volume of IPA to use for a given quantity of MHRB, say 100g? My thinking is that it'd be best to use the lowest volume of solvent that'll fill a flask (eg 250ml) simply as you'd have less liquid to work with, but I'm wondering if you're using a 500ml Soxhlet (even if it holds only 100g) then you should always be using 500ml (or just below it).

I'm not too clear from what's been said before on the volume of IPA (or ethanol, etc) to use. There's been a lot said about fill it up to the level of the inner siphon arm (small tube above bigger tube) but I think I must've missed something as surely can't you only fill it up to the max level of the boiling flask or surely you'd have problems dismantling it?

Also I wanted to ask about the type of Ethanol which could be used in a soxhlet. Here in the UK you can only buy without a licence 'Completely Denatured Alcohol' (defined as "Completely denatured alcohol must be made in accordance with the following formulation: with every 90 parts by volume of alcohol mix 9.5 parts by volume of wood naphtha or a substitute for wood naphtha and 0.5 parts by volume of crude pyridine, and to the resulting mixture add mineral naphtha (petroleum oil) in the proportion of 3.75 litres to every 1000 litres of the mixture and synthetic organic dyestuff (methyl violet) in the proportion of 1.5 grams to every 1000 litres of the mixture." - see wikipedia) or Methylated Spirits - which I'm very wary of using. Would these substitute well for 'pure' Ethanol & be used without any safety concerns.

One last question
Attention All Shipping said:
I just wanted to ask what the steps would be for extracting DMT from the IPA once its extracted everything from the MHRB. Would you just do a few naphta pulls on the IPA or would you need to basify it & then pull with naphta?
Click to expand...

Thanks
 
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