Thinking about purchasing a funnel separator.

Would this be a good choice for alkaloid extraction?



SEPARATORY FUNNEL GLOBE SHAPED, BOROS. GLASS,WITH DETACHABLE PFTE STOPCOCK AND ST-PE_STOPPER, 500 ML, ST 29/32 BORE OF PLUG 2,5 MM PACK. = 2 PCS.

And what other (basic) lab materials and house hold appliances can make life easy?
also considering filters, simple scale, funnel, jar, evaporation plate, glass cilinder.

Any tried and true tips welcome really...

That would be useful for small-scale stb, and seperation of NAOH and Naptha .

do you say this by experience ?

I cant see how a separatory funnel would work for an STB using lighter-than-water solvents like naphtha.. Did you ever notice how the black basified liquid sticks to the walls of containers? So lets say you make a pull with naphtha... then what? Then you have to drain all the bottom layer, which is this sticky stuff.. maybe pieces of jurema blocks your funnel.. but even if not, then still, as you drain it, the major liquid would come down but a little would be all over the walls and parts of your funnel.. and then you would drain the naphtha finally, but it will def come with little bits of the basic liquid that is still slowly dripping from the sides of the separatory funnel. The only chance would be an A/B, but even so the liquid still tends to stick everywhere..

unless someone has experienced otherwise and can prove me wrong...

Because otherwise, this would be more useful for heavier-than-water solvents like DCM (but then again, DCM seems quite toxic and it would also pull loads of gunk together appart from dmt, so I wouldnt use it)


Useful things to have? A vacuum filter set up (bucher, vacuum pump, good filters, etc).. a food dehydrator.. A good blender.. But one of the things that seems the most useful, pro, automatic, effective, is a soxhlet.. Wish this would be possible, but too expensive and no space for it

For soxhlet, dont you think it would effect the yield if you are unable to basify the bark. you certainly couldnt add a basified solution to the powdered bark while its in the thimble or it would end up going through the siphon into the solvent/concentration chamber. With the bark powdered the hot solvent would probably pick up little bits of spice and over a long time of running it would be fairly concentrated but dont you think the base is nesescary to drive the extraction to completion based on le chateurs principle? Just not sure how it would work

But as for the sep funnel, my friend uses a liter sep funnel for his small scale extractions and he says its fine and dandy. Yes some sticky basified solution will stick to the walls a bit, and yes if you do not have some practiced decanting skills you will most likely clog your stop cock with powdered jurema, which is a massive pain to try and unclog while not making a huge mess and not loosing any solution, but it is doable. My friend also said he did not notice any problem with bringing left over base with the solvent into the freeze precip jar but even so if your recrystalizing it shouldnt matter much either way. There are defintely other ways to go about it and pipetting off solvent layer is pretty easy as well, but my friend thinks its just easy with sep funnel and somewhat time saving as well, thats just his opinion though.

some macac used to use 250mL funnels
'twas tedious, but they worked

a hotplate-stirrer is always a good thing to have. the stirrer can save SWIY emulsion headaches
if SWIY gets a collection of lab glass going, a mantle is also a good addition for re-distilling solvents.

as was mentioned, a vac and buchner funnel are also essential for filtering biomass from the aqueous phase.

the macac uses all the above, though he needs larger sep funnels (he broke his 250s and is stuck with a 125)

tip: if an item of glassware gets stained or coated, try washing it with hot dilute sodium hypochlorite solution (bleach), or carefully rinse it with sulfuric and hydrogen peroxide.

Disregard soxhelt comment, friend did not understand the concept

A sep funnel is just about the best thing you can own. When that sticky red goop sticks to the walls dont panic, remove aqueous out the bottom, np out the top with spice and then WASH THE FUCKING THING (all it takes is 4 seconds of hot water, rinses right out) then do a sodium carbonate wash in sparkling glassware. Thats how you get things nice and white.

Thx dude
Was hoping for this kind of reply. Was planning on doing it the way you describe.
But was worried though about how to clean it... but you also answered that one : )

Guess the basified water with plantmaterial should be filtered before putting it into the funnel. Any suggestions on the filter to be used? Coffee filter? Or should it be finer? (to prevent powder material from entering the stop).

I got 3 different sizes of seperatory funnels.
VERY useful.
Couln't imagine doing an extraction without!

I use a plastic bottle with that sucking thing on it, as a seperatory funnel. However hard to open when its full and upside down. And its not very usefull actually, used it once for SC wash and splashed everything on my face eheheh

Using narrow and long jars that exactly fits when all the mixture is added, is better because taking pulls are easier. You should find the most suitable jar for yourself i use one that exactly fits 50gr, and another one fits 100gr extractions. Also have a big one i never used.

For pulls i found that a syringe with no needle is good. Have a 3ml plastic pipette and a big turkey baster, but syringe works far better for me unless im extracting a huge amount.

heres a short lis of things i mostly use and their purposes ;
+A little deep, square and wide plate for evap,
+A wine/champagne glass for recrystalization,
+A small freeze precipt jar with no curves (straight glass is always easier for scratching all the yield) and wide mouth so its better to scratch it
+A bigger and very wide jar for freeze precipt (this one is really nice for drying after freeze precipt)
+3 little plates for drying the yield on it (one for the crystals, other for clean white stuff, and the last one for yellow-orange stuff to be purified)
+2 scales, one is 0.001-20 for dosing and stuff, other is 0.01-100 for weighing Naoh and mhrb
+A pH meter, (this is good for experimenting but not necessary if you have your ratios for the TEK and its working good). Also a thermometer is good while experimenting with recystalization but not vital for extraction.
+A pyrex with ml measure on it i use for mostly mixing naoh+water
+A plastic ml measuring cup mostly used for naphta
+A spoon, A knife, A scalpel, N95 dust mask, plastic goggles, latex(vinyl whatever) and dishwashing gloves (i find it easier to work with powder free latex gloves, but dishwashing gloves are good for washing the dishes )
+I always keep few extra jars and a glass for naphta heating, naphta transfer and so on...
+Few glass vials for storing the yields. (I keep white stuff and yellow-orange stuff seperate)

if i remember more i will write later but its all i can remember now

all glass pipette! I can't even imagine how easy pulling solvents would be with one...

Pipettes, HDPE bottles, Small beaker, evap dish.

Add to that limitless improvisation on whatever's lying around

I would like a distilation setup though.

A litlle pricier and really not wildly nesescary but super fun to play with and defintiely facilitates some good yields is a Magnetic Hot plate stirrer.

Reaaal expensive retail but my friend got his on ebay for 56 bucks.
Awesome for heating NP solvent
Heating mixture of solutions
Also by leaving the stir bar in the extraction vessel on real low and turning the heat up just weencey bit you can leave it like that forever and the NP/Basified Bark solution will be constantly heated(allowing Non polar to effectively mix in with basified water) as well as constantly slowly stirred to get a large amount of contact between your NP and the other basified solution(more solution to pull alkaloid from), and since its a nice slow stir you never get an emulsion.

And if you do any at home chem experiments just to dick around like my friend does it makes damn near anything waaaay easier

Yes some1 else also talked about this.
I can see how it would help very much indeed (motion, temperature), to bring alkaloids over to the NP, and also to avoid/break emulsions.

So far the monkey is set on buying two 500ml funnel separators. Though he would really like a plate stirrer. At the moment the monkey is checking out E-bay and sites like that. Maybe hes lucky...

Any1 filtering before mixing solvents? can imagine it to be important to get solid particles out, so to prevent clogging of the stop...
Any1?

ahaaa : )
but filtering using a vacuum will require even more of the expensive equipment.
Who is using filtering techniques without use of vacuum?
Any monkeys using coffee filters?

you can improvise your own vacuum filtering using vacuum cleaner, funnel, coffee filters, hdpe jug, some strong tape and a couple of tubes that fit the end of the funnel

like this, except its much better to use hard hdpe container than PET plastic bottle because first of all depending on what chemical you use it can dissolve PET plastic, and also with the vacuum the plastic bottle crumples up while the HDPE stays normal...

The trick is to approach the vacuum to the tube slowly, because the vacuum cleaner is too strong and might rip the filter

good idea!

but if using coffee filters then maybe the vacuum is not needed?
just rinse the filter and filterresidue with basified water so all alkaloids are washed out?
can imagine vacuum is needed for very fine filters only...

Still wondering if a coffeefilter will be fine enough
will fine particles clog the funnelseparator?

well the vacuum makes everything a billion times faster, thats all, but gravity by itself would work..

If for example one pours some naphtha with dmt crystals through the filter, instead of waiting minutes/hours for it to completely dry, in a few seconds the vacuum pulls all the liquid down and dries it...

as for 'fine particles and clogging'... dmt will stay on top of coffee filter, it wont pass through.. Harmalas also, but hamalas are quite fine so some gets 'lost' inside the filter (just dip the filter in acidified water to retrieve alkaloids).. Harmalas filtering can be a pain though, specially the first steps because the oils from syrian rue tend to block coffee filters very very fast.. Gotta filter while its in acidic solution with the dissolved alks using a cotton plug in the funnel, repeating a few times to get rid of unnecessary filter-clogging particles around, so when you do have to filter properly to get the alks, these dirty oily particles are out

i've gotten to be quite the virtuoso with a pyrex turkey baster at this point....it's actually something that warms the very cockles of my O.C.D. heart.... i LOVE syphoning off saturated spice!!

1600mL pyrex mason jars, 5L hinge and seal top WIDE-MOUTH glass jars (i got big hands....), a beautiufl glass funnel (not sep or buchner....just a good solid glass funnel... these are my tools o' the trade..

oh- also, if you can get a large pyrex baking dish or large storage bowl WITH AIR-TIGHT LID, your freeze precip will thank you for it.

LOVE AND GRATITUDE!!