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soxhlet exctracter

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Dwhitty76

Dwhitty76

Rising Star
swim has been doing some homework on soxhlet extracters and has learned some of the basics but some of the chemistry lingo is beyond my scope..If anyone here has experience w/this type of extraction,i have some questions.Lets say someone were to do a 500g mhrb extraction,what size soxhlet would he want.It was also mentioned by someone else to use 91% IPA, is that rubbing alcohol?and what would be the purpose for using that?Swim is used to acid/base extractions 3/1 water/vinegar.With the water flowing into the soxhlet apparatus,what about the acidity that is needed?I assume you just hook up a hose from "regular tap water"instaed od distilled water and the water that water output on the soxhlet is that just suppose to drain? Is there anyway to use distilled water SWim has heard some impressive things about this method and would love to try it but before he spends the money,he just wants to get his facts straight.Any feedback would be much appreciated.
 
The condender water would stay seperate from the liquid & solids inside the soxhlet, it just runs through the condenser cooling the liquid/gas inside the soxhlet so it condenses & drips down to the bottom again. The ph of the condenser water would therefore be irrelevant.
 
the purpose of a soxhlet is to utilize a low-boiling solvent, in this case, IPA, to extract the alkaloids from the plant material. AAS is correct, pH of the water in the condenser is irrelevant, and IPA is fairly neutral. SWIY has two options: SWIY can cycle the alcohol several times over the ground MHRB, evaporate most of the IPA and crash it out (freeze precipitate), or do an A/B extraction on the reduced volume as you would with str8 bark. the soxhlet just speeds up the process.

a 500mL soxhlet would suffice for the amount specified.

SWIM has a soxhlet, and has used it successfully in psilocybin extractions. everclear is his preferred solvent for extracting tryptamines.
 
thanx guys.It's finally starting to seep in to my fogged brain:).Just trying to figure out if it's worth if for swim to purchase one.Someone said that it not only makes the process earsier but is more efficient at pulling out as much of the alks. as possible and good for other organic extractions,so it might be worth it.Anyway thanx for the clarification.
 
a 500mL soxhlet would suffice for the amount specified.

is that the size of the flask? because i'm looking at different sizes of soxhlets and i see joint sizes that read like 55/50. I'm not seeing actual ml. sizes for the soxhlet.I'm only seeing ml. sizes for the bottom flask.Swim was gonna try and just buy the parts seperately off of ebay but he didnt want to risk getting two pieces that dont fit.So he wants to try and just find a vendor that sells the whole apparatus (sox,condenser,flask).The vendor where he got my other glasswear doesnt sell soxhlets,do know any good vendors w/ reasonable prices?what about the tubing for the water i noticed none of the vendors include tubing for the water,any suggestions?
 
the 'bay would be the place, much cheaper than you'd find anywhere else. the US 'bay site has a store that ships worldwide, for a 500mL extractor (the bottom part is 500mL...comes with allihn condenser) for 90 USD or so, hundreds less than other vendors. use an aquarium water pump in a large glass bowl of tap water, that's how SWIM rolls. a soxhlet extractor is one of the best pieces of glassware one can have, but one should also get a round-bottom-flask, a mantle, and an input (temp) controller for the mantle. this stuff is not cheap, but it's completely legit, and ultimately useful for many many things. SWIM highly recommends it if SWIY is seriously into these sort of things. SWIY would not be disappointed. aside from a distillation apparatus, a soxhlet is one of the most useful glassware setups one can have.

note: 45/50, 55/60, etc. refers to the metric (mm) size of fittings, the end pieces that connect. make sure they all jive, same numbers. SWIY can get reducers/adapters to get pieces to fit.


this is a 125mL soxhlet SWIM used to have, before upgrading to a 250mL


CIMG0217.JPG
 
one should also get a round-bottom-flask, a mantle, and an input (temp) controller for the mantle.

Why not a flat bottom flask and an ccurate hotplate?
 
swim took the first step and bought 500ml Soxhlet Extraction Apparatus with a 4 bulb
Allihn condenser for 85$ usd.Now he needs to decide to whether or not to go w/flat bottom flask and hot plate or round bottom flask and a heat mantle. Benzyme,one question i have is that w/ a mantle it would seem that it would be difficult to change the size of the flask (if needed be) because mantle's seem to have a fixed depth and circumference,Right? Or is there a way to use different sized flasks with a heat mantle? why do you prefer that over hotplate? Damn these gadgets are pricey.
 
Dwhitty76 said:
Benzyme,one question i have is that w/ a mantle it would seem that it would be difficult to change the size of the flask (if needed be) because mantle's seem to have a fixed depth and circumference,Right? Or is there a way to use different sized flasks with a heat mantle? why do you prefer that over hotplate? Damn these gadgets are pricey.
Click to expand...
swim's used a 250mL 3-neck RBF with a 500mL mantle with no problems. a flask larger than 500mL would pose a problem because it would not be making direct contact with the heating element, which is focused in the center of the mantle.
as for the mantle preference, I dunno... just works well with a soxhlet setup using an RBF. obviously a hot plate would work better with a flat-bottom flask. both are superior to bunsen burners, especially when working with volatiles/flammables. 😉
 
swim, might go "the hoplate route",just because its a little cheaper.I found one that seems reasonable i price 200$ usd and its size is 7.25" x 7.25".I'm thinking thats probably big enough to fit either a 250 or 500 ml flask.Do you know if there is anything else swim needs to keep in mind when buying a digital hotplate, other than it size? I'm gonna copy/paste th product info,if you dont mind glancing at it just to make sure swim doesnt waste 200$. I appreciate your help.

PRODUCT DESCRIPTION
• New easy-to-read digital display indicates temperature settings, adjustable in 5°increments, from 5° up to 540°C (41° to 1004°F), depending on model.
• Microprocessor-controlled feedback technology maintains consistent, repeatable temperature settings. Ideal for labs that perform repetitive procedures.
• Hot surface alert safety systems protect from accidental burns. Bright red warning lights signal when heating surface is above 50°C (122°F). Unit display flashes "HOT" - "OFF" when heating is turned off, until heating surface is below a cool 50°C.
• Cimarec's seamless reflective white ceramic top enhances sample visibility and provides an easy-to-clean and alkali/acid resistance surface.
• Flat top and high-wattage heating elements combine to provide superior heating transfer and fast time-to-boil.
• Three sizes offer flexibility from microscale chemistries to larger vessels.
• Integral ring-stand holder accommodates 0.5" (1.3 cm) diameter support rod.
• Rugged low-profile cast aluminum body provides stability and durability.
• Accommodates sample weights to 35 lb. (15.9 kg) on the 10" x 10" models, 25 lb. (11.3 kg) on 7" x 7" models and 15 lb. (6.8 kg) on 4" x 4" models.
• All models supplied with detachable cord. Stirring models include 2" x 3/8" dia. TFE-coated stir bar, (4" x 4" units include 1" stir bar).


Desc Hot plate Amps 8.6 Top plate Surface D 7.25 (18.4 cm) Heating Surface Material Ceramic Top plate surface W 7.25 (18.4 cm) Hertz 50/60 Operating Temp Range C 5 - 540°C Operating Temp Range F 41 - 1004°F Overall Dimensions D 13 (33 cm) Overall Dimensions H 3.8 (9.7 cm) Overall Dimensions W 8.2 (20.8 cm) Product Line Thermolyne Shipping Weight LK 9.2 (4.2 kg) Stirring Speed Range NA Sub Product Group Id 412.0 Volts 120 Watts 1040
 
obviously if the bottom "male" joint of the soxhlet that goes to the flask measures 24/40.Then my guess is that the boiling flask opening also has to be 24/40.If so, i'm having a bitch of a time finding 24/40 flat bottom boiling flask that measures under 1000ml,which is too big right?I've been looking all over.Do you know of any lab companie's that might meet my measurements?Also,what size stoppers do think i need ?
 
hey benzyme,
Since you have experience with soxhlet,if swim has some questions for you when he gets the pieces in the mail,do you mind if he pm's you?
 
Dwhitty76 said:
one should also get a round-bottom-flask, a mantle, and an input (temp) controller for the mantle.

Why not a flat bottom flask and an ccurate hotplate?
Click to expand...

SWIM uses a flat bottom boiling flask and a very accurate digital hotplate. SWIM doesn't like using round bottom flasks. The only time they are needed is when doing things in a vacuum. Unless you plan to do plant extractions in a vacuum, don’t bother with the awkward heating mantle and dangerous round bottom flask. Get an accurate digital hotplate and a safer flask that can stand up on its own. I’ve never liked round bottom flasks because they can’t stand up on their own. I avoid them like the plague! They are accidents waiting to happen!

As for the Soxhlet, SWIM uses a 1000 ml one and doesn’t use a thimble. The thimble is NOT NEEDED. SWIM used to use it long ago before he knew better. All you need is a few cotton balls at the bottom of the Soxhlet to prevent anything from falling out into the boiling flask below it.

Take a look at this setup. No thimble is used. You can fit more herb in that way:

257px-Soxhlet_Extractor.jpg


Here’s the Soxhlet swim uses:

48577f3e15a60_10550b.jpg


It’s available here:


Another tip, if you powder your herb and mix it with a little diatomaceous earth (about 4:1 of herb to DE) for improved drainage, you can fit far more herb into the Soxhlet and extracting time is improved.

You’ll always need to put something to keep the glass connecting joints from sticking together. SWIM recommends using PTFE joint sleeves instead of joint grease (stopcock grease). PTFE joint sleeves are pricey but they last forever and aren’t messy. SWIM also uses PTFE tape sometimes (the kind used for plumbing). It’s cheap and not messy. Some people frown on that practice, but SWIM has used PTFE tape many times without any problems. He hates joint grease!

Yeah, I know, SWIM is a little opinionated sometimes. Sorry about that. SWIM is just not the "follow the crowd" kind of guy.
 
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