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soxhlet exctracter Options
 
Dwhitty76
#21 Posted : 8/1/2008 4:26:59 AM
That sucks,what happend? i think most of swims pieces arrived in the mail today ( i know the dig.hotplate did) but i'll find out tommorrow.Swim went a little nuts w/ the $ and purchased a bunch of helpful lab equp.You said that swiy uses a fish tank for the water? what size tank does he use ans what size water pump? swim is probably gonna do a mhrb extraction to sart and i read to use 91% API (Isopropyl Alcohol).What has swiy found to be effective?I was also was looking around the web for info on using a soxhlet on cannabus and others can you point me in a direction?
" Freedom from the desire for an answer is essential to the understanding of a problem." - jiddu Krishnamurti
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#22 Posted : 8/1/2008 5:39:42 AM
swim uses a large glass mixer bowl, and a small aquarium water pump. uses tygon tubing

IPA should work fine for MHRB, even EtOH (ethanol) would work well. swim would actually use ethanol (everclear).
ethanol is also good for extracting cannabinoids.

some people actually use butane to get 'honey oil' from cannabis. obviously couldn't get butane to cycle through a soxhlet, but hexane or heptane would.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Dwhitty76
#23 Posted : 8/1/2008 6:14:59 AM
swim bought a 500ml soxlhet w/condenser,flat bottom boil flask an a Cimarec® Digital Hot Plate 7.25 x 7.25 .Once swim gets it together it seems pretty basic and i likes the idea of using cotton balls as appose to a thimble.One question,though. Swim is used to a/b extractions (marsfold specifcally).That tek cals for 3/1 water vineger for the polar extraction (which the soxhlet does more efficiently for you).Why is it best to use IPA or EVERCLEAR as appose to what some of the other teks use,for instance; Vovins polar is distilled h20 and hydrochloric acid.why does api and eveclear seem to work better w/ soxlet the some of the other solvents?
" Freedom from the desire for an answer is essential to the understanding of a problem." - jiddu Krishnamurti
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#24 Posted : 8/1/2008 2:04:52 PM
mentioned this before: alcohols are lower-boiling solvents.
keep in mind, soxhlets make use of low boiling solvents to cycle through material, concentrating it in the flask at the bottom. pure simplicity, and done in a few hours.
much cooler than putting it in vinegar in a crock pot, and letting it simmer overnight.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
D_Juggz
#25 Posted : 8/1/2008 3:11:15 PM
Why not just use a stovetop? saves a bit of money.
Swims busy using the stove, but the flask is in a hot water bath. Hes a bit scared of it shattering from the heat, bust since its proper lab glass, it shouldn't right?

Swims sick of all the water vapours going everywhere all the time, think hes vapored away about 10L today.

Also what solvents do you guys use?
SWIMs trying it with naptha tonight, because hes so excited about getting his new soxhlet from the US. (not the big 1000ml yet though),

Swim actually bought 4 soxhlet bodies off e-bay just because they were so cheap. He'll have to sell them again, so if there are any aussies looking to get into it, message me.
The hardest thing of all is to find a black cat in a dark room, especially if there is no cat.
-Confucius

"Under the skin of our lives; somewhere deep and early, forgotten, we all share the same dreams"
 
Dwhitty76
#26 Posted : 8/1/2008 5:18:45 PM
i believe it was you benzyme that said if swim was doing 500g mhrb extractions that a 500ml soxhlet would be sufficient.Obviously the most organic material swim can extract would be how much he can fit into the soxhlet,or should there be xtra room left,How much generally (at max) root bark can you fit into 500ml.Also what about minimum amounts of material.With 500ml, would it make a difference if say you only wanted to do a 50-100g extraction,does that change anything?
" Freedom from the desire for an answer is essential to the understanding of a problem." - jiddu Krishnamurti
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#27 Posted : 8/1/2008 5:33:37 PM
no, it wouldn't matter if you used 50g or 250.

and I'm not sure you could fit all 500g in a 500ml extractor, which is roughly 500cc's. to fit, that would mean MHRB would need to have a density similar to water.. ~ 1g/mL.
however, a 500mL soxhlet should easily be able to extract from half a pound (227g) of powdered material at a time.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
69ron
#28 Posted : 8/1/2008 9:02:31 PM
The only thing that matters is that you have enough solvent to fill the Soxhlet completely or it will never siphon.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
Dwhitty76
#29 Posted : 8/1/2008 10:01:14 PM
Can swim buy IPA or EVERCLEAR at most harware stores?he's never used it before. Also 69ron you mentioned that when swim is done w/ the polar extraction,using the soxhlet he can continue to follow whatever tek he chooses,is that correct?
" Freedom from the desire for an answer is essential to the understanding of a problem." - jiddu Krishnamurti
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#30 Posted : 8/1/2008 10:09:02 PM
69ron wrote:
The only thing that matters is that you have enough solvent to fill the Soxhlet completely or it will never siphon.


it just needs to fill to the level of the top of the inner siphon, which (depending on the extractor) may be well below the top of the outer siphon
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#31 Posted : 8/1/2008 10:10:26 PM
Dwhitty76 wrote:
Can swim buy IPA or EVERCLEAR at most harware stores?he's never used it before. Also 69ron you mentioned that when swim is done w/ the polar extraction,using the soxhlet he can continue to follow whatever tek he chooses,is that correct?


IPA can be obtained at a pharmacy. denatured alcohol can be obtained at a hardware store. everclear is found at liquor stores
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Dwhitty76
#32 Posted : 8/1/2008 11:47:54 PM
swim just walked into his house and has about five packages waiting to be opened!!!Very happy
" Freedom from the desire for an answer is essential to the understanding of a problem." - jiddu Krishnamurti
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#33 Posted : 8/1/2008 11:56:17 PM
ahh, it's a great feeling getting packages of equipment in the mail.
swim is getting a vacuum desiccator in the mail soon
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
69ron
#34 Posted : 8/2/2008 1:42:23 AM
benzyme wrote:
69ron wrote:
The only thing that matters is that you have enough solvent to fill the Soxhlet completely or it will never siphon.


it just needs to fill to the level of the top of the inner siphon, which (depending on the extractor) may be well below the top of the outer siphon


Exactly...and the amount varies according to how dense the plant material is. Actually I was a little incorrect in my statement. The general rule is like this:

Before starting the system, fill Soxhlet with cotton balls, add plant matter, cover with cotton balls. Add enough solvent to cause the Soxhlet to siphon once into the boiling flask. Then add solvent to fill the Soxhlet 1/2 way to the siphon point. For example, if it took 300 ml to cause a siphon, then add 150 ml more. That's the general rule anyway. It varies a little according to the solvent used. DCM, for example usually requires more solvent than IPA, or it won't siphon properly. If at any time it fails to siphon while the system is running, adding a little more solvent usually solves the problem.

There are cases when it won't siphon at all for many hours even after adding more solvent. This is usually because the drainage is inadequate (if the plant is too finely powdered and DE wasn’t added) and so it will just drip endlessly down from the Soxhlet’s siphon arm (the small tube) into the boiling flask. If this happens and the solvent level stays at the siphon arm, don’t worry, it is still extracting. It doesn’t actually need to siphon. As long as it is dripping back down, it is extracting.

But, if at any time the solvent level in the Soxhlet starts to reach the distillation arm (the larger tube) then you’re in trouble. This means the system is clogged. You should turn it off. Remove the plant material, replace any cotton with new cotton, and add DE to the material to prevent it from clogging again. Then put it back in the Soxhlet. This is almost never a problem if the plant material is coarsely ground, and often a problem if the plant material is very fine powder.

Remember if you are using very fine plant powder then add DE to it. This works really well to prevent clogging.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
D_Juggz
#35 Posted : 8/2/2008 3:03:53 AM
Can someone please tell me if its possible to use Naptha or Ethanol for extraction? Or are you better off finding Methanol?
The hardest thing of all is to find a black cat in a dark room, especially if there is no cat.
-Confucius

"Under the skin of our lives; somewhere deep and early, forgotten, we all share the same dreams"
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#36 Posted : 8/2/2008 3:08:01 AM
D_Juggz wrote:
Can someone please tell me if its possible to use Naptha or Ethanol for extraction? Or are you better off finding Methanol?


depends on the procedure you want to use.

if you want to do a relatively quick pre-extraction like this thread addresses, you'd use hot ethanol, methanol, or isopropanol.
if you wish to soak or simmer the material with acidic water, you'd basify that, then add naptha.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
D_Juggz
#37 Posted : 8/2/2008 3:19:40 AM
Swim tried the acidic water, but couldn't get it to boil in my hot water bath, Tried it with naptha also, and it did seem to turn yellow after about 4-6 hours, but there is a little bit of water at the bottom that must have came from the plants, its also turned dark, is it possible that there is DMT trapped in that water? Should it be siphoned off before continuing?

So you say 95% Ethanol (what Swim has available) would work better than naptha? Wouldn't it be worse because its polar instead of the nonpolar methanol?
The hardest thing of all is to find a black cat in a dark room, especially if there is no cat.
-Confucius

"Under the skin of our lives; somewhere deep and early, forgotten, we all share the same dreams"
 
benzyme
Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert
#38 Posted : 8/2/2008 3:35:22 AM
D_Juggz wrote:
Swim tried the acidic water, but couldn't get it to boil in my hot water bath, Tried it with naptha also, and it did seem to turn yellow after about 4-6 hours, but there is a little bit of water at the bottom that must have came from the plants, its also turned dark, is it possible that there is DMT trapped in that water? Should it be siphoned off before continuing?

So you say 95% Ethanol (what Swim has available) would work better than naptha?


you don't want it to boil, just use low heat. DMT is quite soluble in acidic water, heat increases the solubility. but boiling can break down the alkaloids. gentle heat for a few hours or even overnight is more than enough.
likewise with alcohols, though even shorter timeframe. DMT is quite soluble in short-chained aliphatic alcohols, which require even less heat. and yes..DMT, straight from the root bark, is more soluble in ethanol than naptha.

you don't use naptha (unless you want to defat..which is optional, not really necessary) until after you basify the acidic solution.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
D_Juggz
#39 Posted : 8/2/2008 3:47:44 AM
Thanks, swim will start over Smile
The hardest thing of all is to find a black cat in a dark room, especially if there is no cat.
-Confucius

"Under the skin of our lives; somewhere deep and early, forgotten, we all share the same dreams"
 
D_Juggz
#40 Posted : 8/2/2008 4:37:24 AM
Would u say DCM would work better than ethanol?
The hardest thing of all is to find a black cat in a dark room, especially if there is no cat.
-Confucius

"Under the skin of our lives; somewhere deep and early, forgotten, we all share the same dreams"
 
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