??

what, like these?

the first one is a std. size for semi-macro/macroscale, about 19" tall. the last one is about 3 feet tall...pretty big.

sep funnels get expensive, especially >500mL. a 500mL is a good size, 1L even better, but a 2L is thug.
swim would definitely get a 2L is he had some extra $$
(swim is messing around with a 250mL with a broken spout and a 125mL...very tedious to work with)

What size Soxhlet Extractor and boiling flask is SWIY using, 500ml? Is it really worth it to spring for the 2L Separatory funnel?

How much easier will it be for SWIM using a 500ml Sox and 1000ml LLE with a 2L Separatory Funnel?

well, ...easy. a 2L sep funnel is obviously advantageous to work with larger volumes. one could easily extract from 250g root bark with 3 (instead of 12 with, say, a 500ml funnel) solvent extractions.

it's just a bit on the pricey side, but convenient.

A 1000 ml Soxhlet is best for 100-300 grams of herb, depending on the herb used. 1000 ml is the liquid capacity of the Soxhlet. But once it’s filled with herbs, you’ll end up using only about 600 ml of liquid, with 200-600 ml being in the boiling flask below. If you shut off the heat right before the Soxhlet siphons, the flask below will only have about 200 ml of liquid in it. That’s the best time to get your liquid. So although you’ll need a 1000 ml boiling flask, at the end you’ll only be getting out about 200 ml of solvent if you collect your solvent from the flask while the Soxhlet is nearly full of solvent.

A 1000 ml CLLE, the heavier than water kind, is meant to be filled 4/5 with water and 1/5 with DCM or chloroform. So keep that in mind. If you have a CLLE with a shutoff valve on the return arm, you don’t need a separatory funnel for it because the CLLE itself works as one (a little awkward though).

SWIM uses a 1000 ml Soxhlet, a 1000 ml CLLE (because that’s pretty much the only size you can find) and a 500 ml separatory funnel. He rare ever needs a larger separatory funnel, but when he does, a 1000 ml one is good enough for him.

Great advice, 69ron. About how much ~P. Viridis foliage will fit in a 500ml 55/50 24/40 Sox?

Nearly everything recommended or needed is in place now.Besides 2 final things 2 teflon joint sleeves, they come in packs of 3 and right now there are 2 joints unprotected. A 45/50 on top of the CLLE, and a 55/50 on the bottom the Allihn condenser, should they just be wrapped in plumbers thin PTFE tape from the hardware store instead to protect them? Will that hold up to the heat?

Also, what to use to hold up the CLLE as it would be sitting higher up off the lab table surface than both the hotplate + the 500ml FBF, does the CLLE get too hot to prop up with flammable supports?

The 2L Seperatory Funnel is is a sweet piece of kit. However the stopper is polyurethane plastic, should my sugar glider buy a glass stopper in the correct male joint size?

Notes: (Thermolyne HP1915-B 750W [755w AC draw])
33g of Whole Hawaiian Chacruna as experimental run
T = 00:00 --
300ml methanol/ethanol solution first siphon
100ml " " " " halfway to second soxhlet siphon


---

550 watt = fifteen minutes to first siphon (3 times)
475 watt = 30 minutes to fourth siphon (2 times)
350 watt = 45 minutes to sixth siphon (until end T = 04:00)

---

Alkaloids are crashing out in my sugar glider's freezer right now, using naptha for the final nonpolar extraction.

very nice


yeah, get a pennyhead TS stopper; that looks like a size 22(mm)

Thanks, benzyme I think it's called 29/32 according to the top of the stopper.

Slight anomaly with my sugar glider's extraction process, using 88 grams of finely chopped foliage in the 500ml soxhlet body. The plant fats and bits are collecting inside of the bottom the siphon arm. Both the condenser and soxhlet siphon tube are condensing and dripping steadily. It has siphoned twice so far...

My sugar glider assumes since he was aggressive with the packing pressure from the top, using 1 cotton ball on the bottom, and 4 on top for a total of 5, seven seems a better number to use [3 on the bottom].

edit:

at some point the sugar glider may want to look into a pressure-equalizing dropping funnel, to attach to the soxhlet, so he can reduce the volume in the RBF, and recover his clean solvent

the general setup looks like this

*edit* gee whiz ..
look at the brief ultrasound-assisted extraction tech at the bottom

ULTRASOUND-ASSISTED EXTRACTION



A dynamic ultrasound-assisted extraction method prior to the gravimetric determination of total fat content in bakery products was proposed (Ruiz-Jimenez J et al., Anal Chim Acta 2004, 502, 75).
Samples were inserted in a stainless steel extraction chamber drained by the extraction fluid (hexane). The tube was immersed in a water bath in which an ultrasonic probe (Branson 450 sonifier) was immersed.
After testing several parameters, the most efficient approaches was an open system where fresh extractant was pumped in forward-and-back steps. Two grams of sample were optimally extracted with 25 ml of hexane for a time much shorter than conventional Soxhlet extraction. Comparisons with the Folch reference method have shown no significant differences when food samples were extracted (Ruiz-Jimenez J et al., Anal Chim Acta 2004, 525, 159).

Sweet deal!

Does that mean you can skip the Soxhlet altogether in favor of a metal tube in a resonating aqueous bath?

that's what it sounds like.

*chin-stroking* this warrants further investigation

Benzyme, what is a good local source for pure methylene chloride, diethyl ether seems to be regulated as a drug precursor?

OR

Should my sugar glider simply produce another solvent by reacting sodium hypochlorite (Clorox) with 95% ethanol alcohol to simply make CHCl3?

haha, that's an old school tech

would work, but would also liberate lots of chlorine gas.. very dangerous if done outside a fume hood. also the product may contain carbon tetrachloride, a rather nasty solvent.

check local small chem supply shops for methylene chloride, it's not very suspect. still used as a plastics solvent, i.e. pvc work

After doing a Noman's STB on the first 23g test extraction and freeze precipitated absolutely nothing in the freezer jars. So my sugar glider decided to do an 88g Soxhlet run and still STB'd it to get next to nothing just a thin film of crystals on the coffee filter. .4ml/per g of foliage of heated (~110F) Naphta was used in 3 pulls. 3 Seperate jars all yielded virtually no spice from that 80g, what gives?

Should my sugar glider switch from Klean Strip Denatured Alcohol [45-50% ethanol + 45-50% ethanol + 1-4% MIK], to 90% IPA?

Also, to what level is the CLLE intended to be filled to. I know the 200ml of diethyl ether or DCM will be just at the bottom, so the red line should be 1000ml of liquid. In a diagram found on google it makes it look like the entire FBF and the tube at the green line and the CLLE should be entirely filled with water/solvent/organic material. How much liquid should reach to what line in the CLLE body?

SWIM has had many batches of mimosa that yielded next to nothing using techs that yielded about 2% with other batches of bark. My guess is that some of the mimosa out there is now fake. Its getting more and more popular, so I think some people are selling mimosa look alikes to make a quick buck. This has been happening with Hawaiian Baby Woodrose for ages and seems to now be happening with mimosa.

SWIM has never had chacruna that was fake or very low yielding. He calculated how much money he has lost from fake or low yielding mimosa and determined that even though chacruna contains less DMT, the money saved from being burned by fake mimosa was worth the change to chacruna.

Now SWIM almost never uses mimosa.


A 1000 ml CLLE should be filled with about 1000 ml of solvent. The extracting solvent should be about 1/5 of the total liquid in the main solvent area of the CLLE.

If using water and DCM to defat it, you'd need a heavier than water CLLE, the kind in your photo. They are designed to hold 200 ml of DCM and 800 ml of water. But because these handmade CLLEs are not that accurate, the actual amount they hold varies a little. Before running it, make sure you have about 100 ml of DCM in the flask below it and make sure the CLLE is filled 1/5 with DCM and is right about to drain into the flask below. If you add as little as 1 ml of water, a few drops of DCM should drain out. If not, it doesn’t contain enough water so add a few ml more water until a few drops of DCM drain out of it into the flask.

The water should not be less than 4/5 of the liquid capacity of the CLLE. The less water you have, the longer it takes to defat or extract.


For a lab stand, I recommend this one below. It’s cheap, very well made, and large. At just $12.50 it has a 2-hole 7x11.75" base and a 1/2x35" rod. It’s one of the best you can get. I don’t like the tripod kind at all.



http://www.cynmar.com/it...l.aspx?ItemCode=12030382

Yeah, I've been thinking the same thing for a while now.

Most reactions progress much, much speedier when under the influence of ultrasound. For instance: in his lab, SWIM must reduce the MnO2 sediment of a Hg-determination with hydroxyl-ammoniumchloride. Because the manganese dioxide sticks to the bottom of the beaker like a sonofabitch, this can take half an hour, with glass-rod scratching. Dipping the bottom of the beaker in a running Ultrasonic bath however, accomplishes this in about 5 seconds. One can see the particles shake free of the beakers' bottom, literally exploding in the solution, and reacting a split-second later to dissolve into nothing. Getting a reagent with low solubility to dissolve goes the same. Hell, perhaps even FASA can turn in to FASSA (fumaric acid super-saturated acetone), as if that would accomplish anything.
Unfortunately, a lab-grade Sonic-bath like this is prohibitively expensive. Swim's been dreaming up a big pile of money, to purchase one of these babies and reducing his extraction times to 10% of what they used to be.
Whenever he can find the time and the balls, he'll do a quick comparison using borrowed time.

yeah, lab-grade sonic baths (Crest, Branson, etc.) regularly go for $250-300 on ebay.
they have stronger transducers than consumer-grade ones used to clean jewelry.

DCM is not very environmentally friendly (CFC), and potentially carcinogenic/toxic according to the back of the bottle -- or possibly a mutagen. Would diethyl ether work better/evaporate from the CLLE body, 1/5 diethyl ether-ethyl oxide to 4/5 of water until the water siphons a bit.

http://www.coleparmer.co...uct_view.asp?sku=8800924
http://www.coleparmer.co...uct_view.asp?sku=8807325

Also, apparently this dichloromethane is mixed in solution with ethanol, and ethylene glycol, and when added to water a wax-like white cloudy substance forms on the bottom of the container. Is this ethylene glycol or is the giant white glob at the bottom the DCM???

$250 - 300 is still cheaper than a complete soxhlet setup.
From the little information out there on the net it seems to me that ultrasonic extraction (maceration?) betters soxhlet for reducing time and the ammount of solvent used in alkaloid extraction. There's mentions that ultrasound might destroy alkaloids if not the right frequency and time used, but they use probes that are a lot more powerful than these cleaning baths.

I started to put together a soxhlet but seeing how much money I had to spend to complete it I would go for a sonic bath instead. My main reason for buying a soxhlet is to reduce the ammount of solvent I need and work without fumes as I live in a houseshare. If I understand correctly I could achieve this using a sonic bath + I could use it as a liquid-liquid extractor too.

I'm tempted to give it a go and find out if it's usefull or not. I've found this Crest for a price that I can always sell it for if it goes pear shaped. Do you think it might work?

yes.

Crest ultrasonic cleaners are industrial-strength, it's a very good brand. specs on that one says avg 90 watts, peak 270. to give you an idea how strong this is, some of the more powerful commercial ones for cleaning jewelry average 45 or 50 watts, and usually go for around 150, $160.