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MY soxhlet Tek techinical but very efficient from what i understand Options
 
chemisch
#1 Posted : 1/15/2012 9:37:01 PM

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1) Acetic Acid Aqs is poured a round bottom flask the ph of the acetic acid must be 2-4(muriatic acid for cheap so i personaly will use this instead to avoid the fumes of hot acetic acid not tastey.)

2) the soxhlet thimble is cottoned off and filled with plant matter

3) Set-up the soxhlet apparatus as standard begin to run water and bring the Acetic acid solution to a rapid boil

4) 3-8 hours later depending on the rate of siphoning stop the boiling and allow to cool This solution should be Dmt in salt form

5) pour the dmt acetic acid aqs solution into a seperatory funnel and add naptha not sure of emulsion so dont mix to vigorously separate the vinegar/water/dmt salt from the naptha keep the water may want to add more naptha and try and redissolve more crap but most likely unnecessary

6) now we need to basify to 12-13ph NaOH(lye) will be added slowly so we dont go over to avoid having to add water to the solution to bring it back to were we need it because it is very easy to highly basify the solution and have to add tons of water like gallons

7) now add dcm or naptha to this basic solution in the sepatory funnel mix but not to vigorously and let it separate and siphon repeat this step with the basified water and pool the naptha/dcm at this point there is dmt which can be freeze precipitated or evaporated

Cool taking about 50 ml of Distilled water and placing it into a flask and adding sodium carbonate to it. Just add a pinch to the water. It doesn't take much. You will only be using this mixture for the first wash. Do not use it for the second and third washes. A little dab will do yah here, add only a small amount of the water/sodium carbonate solution to your naphtha. If you have 300 ml of naphtha then you want to put around 25 ml of the sodium carbonated water. Mix the 2 together and then place them in a seperatory funnel. Shake the hell out of it this is the only mixing step where the liquids separate almost immediately so no worries about too much agitation. Separate the water from the naphtha and discard the water.
For the second and third washes you want to use only distilled water nothing should be added. 25 ml per wash is sufficient. Perform the same procedure as above. You should not leave the water in the naphtha for too long. This means no sitting for hours letting it 'soak' you need to get it in and out. (stole some of the wording here from "vovin's tek" )

9) should allow to evaporate or reduce and freeze evaperate after you have yielded crystals you can redisolve in a super saturated solution of dcm/naptha and re crystalize for even purer pure even tho it should be quite pure

i have not yet used this procedure but i will soon and i will update when i do my yeilds preciously from 500grams of mhrb(thats what i am ordering soon)
if you can bassify in ammononia and extract with dcm why not smoke it?
 

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benzyme
#2 Posted : 1/15/2012 10:22:55 PM

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20 mins ultrasound-assisted extraction > 7 hrs soxhlet cycling
"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
 
tripkabouter
#3 Posted : 1/15/2012 10:29:32 PM
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I am very interested in this, as I will be ordering my own soxhlet apparatus soon. Hope it works!
 
chemisch
#4 Posted : 1/16/2012 1:28:02 AM

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benzyme wrote:
20 mins ultrasound-assisted extraction > 7 hrs soxhlet cycling


i'm not gonna debate which is better in my opinion soxhlet works better yet takes more time i would rather spend 7 hours cylcing than have to pull from an straight to base tek 5-6 times and have to evap like 5 galloons of naptha now dcm wouldnt take that long but who wants to evap that much dcm
if you can bassify in ammononia and extract with dcm why not smoke it?
 
benzyme
#5 Posted : 1/16/2012 1:52:28 AM

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I wouldn't mind, since it has a higher vapor pressure, and only requires one pull. I only use dcm, and the apparatus in my avatar.

soxhlet is fine for salvia extracts and extractions of polar molecules, but for alk extractions, it's actually not very efficient. a pressure cooker, vinegar, NaOH, dcm, and heptane is all one would need to do a complete extraction in four to five hours (from raw material to final product). an ultrasonic cell disrupter drops that time to one to two.
"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
 
tripkabouter
#6 Posted : 1/16/2012 8:51:16 AM
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Chemisch, you may have already read this https://www.dmt-nexus.me...mp;m=198336#post198336. I think the soxhlet is fine for alkaloid extraction when you use it in a initial extraction, from where you perform A/B. This does have the advantage of using minimal amounts of solvents, that can be reused after the extraction. The pressure cooker idea sounds fine too, but, dunno, it just isn't the same as using clean glass.

Bit off topic but benzyme, I thought salvia extraction was better when performed with ice-cold acetone, so you don't pull all the other crap?
 
Shaolin
#7 Posted : 1/16/2012 9:05:30 AM

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chemisch wrote:
benzyme wrote:
20 mins ultrasound-assisted extraction > 7 hrs soxhlet cycling


i'm not gonna debate which is better in my opinion soxhlet works better yet takes more time i would rather spend 7 hours cylcing than have to pull from an straight to base tek 5-6 times and have to evap like 5 galloons of naptha now dcm wouldnt take that long but who wants to evap that much dcm


What was your experience with sonication ? With 5 gallons you can extract 18,9 kg (1g/1ml ala NoManSTB)of MHRB. Hefty Pleased
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benzyme
#8 Posted : 1/16/2012 8:58:23 PM

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flushing with hot solvent won't do you much good if those cells aren't lysed. I've already posted a ref with data showing
the yield advantage sonication has over soxhlet...won't even get into how much more efficient it is.
Gotta do it in batches or use a flow cell reactor
"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
 
chemisch
#9 Posted : 1/17/2012 6:14:27 AM

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i had not heard of using sonication for extraction and pressure cooker idea sounds intriguing can you link me to a tek so i can wrap my head around it? the main reason i wanted to use a soxhlet is becuase i wanted to make sure i am getting all the alk's from the MHRB where i didnt feel just placing it in jars and letting it soak would yeild as much.
if you can bassify in ammononia and extract with dcm why not smoke it?
 
chemisch
#10 Posted : 1/17/2012 6:32:01 AM

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why...... does a sonicator have to be 3 grand? that makes me sad Sad

at that point droping 3grand into extractions of mhrb i would personaly would rather synth dmt
if you can bassify in ammononia and extract with dcm why not smoke it?
 
Shaolin
#11 Posted : 1/17/2012 1:47:38 PM

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chemisch wrote:
pressure cooker idea sounds intriguing can you link me to a tek so i can wrap my head around it


From what I remember BenzPCTEK(TM) would go something like this.
____________________________
All regular pressure cooker regulations (look at your instructions manual) still apply.

3 runs @ 120C @ 15 psi @ 40min*

- fill the stainless steel pressure cooker 1/3 with water.
- load up your glass jar(s) with 1:1 (volume/volume) mimosa and vinegar mixture.
- keep the jar(s) less than half full.
- lid(s) of the jar(s) should be loose** but tightly wrapped with foil.

Filter/decant. Basify. Extract. Etc.

*of boiling so 40 minutes without counting the initial PC warmup to the desired pressure
**closed lids might implode
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benzyme
#12 Posted : 1/17/2012 3:05:15 PM

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that's it.

the PC should be stainless steel, of course. Presto, etc.
sonicators are not cheap, but they don't have to cost three grand either.
I got an analog one (200 W) for $199. A gregar extractor is more expensive.

I posted a similar idea about soxhlet three years ago;
after some tinkering and thinking, I figured a regular simmering A/B, or better, pressure cooking, would be more effective, timewise and yieldwise. It would be awesome if dcm or chloroform could be implemented in the soxhlet extraction, but its vapor-pressure is too high, and a water-cooled condenser isn't enough to condense it. you'd need acetone/dry-ice in a Dewar condenser.
"Nothing is true, everything is permitted." ~ hassan i sabbah
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The Traveler
#13 Posted : 1/17/2012 3:49:24 PM

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Shaolin wrote:
chemisch wrote:
pressure cooker idea sounds intriguing can you link me to a tek so i can wrap my head around it


From what I remember BenzPCTEK(TM) would go something like this.
____________________________
All regular pressure cooker regulations (look at your instructions manual) still apply.

3 runs @ 120C @ 15 psi @ 40min*

- fill the stainless steel pressure cooker 1/3 with water.
- load up your glass jar(s) with 1:1 (volume/volume) mimosa and vinegar mixture.
- keep the jar(s) less than half full.
- lid(s) of the jar(s) should be loose** but tightly wrapped with foil.

Filter/decant. Basify. Extract. Etc.

*of boiling so 40 minutes without counting the initial PC warmup to the desired pressure
**closed lids might implode
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chemisch
#14 Posted : 1/18/2012 3:46:17 AM

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alright sweet, i'm thinking about maybe making a tutorial on shulgins synth of mescaline is that something you'd like me to post or is that way to sketch i'm so excited
if you can bassify in ammononia and extract with dcm why not smoke it?
 
benzyme
#15 Posted : 1/18/2012 4:11:04 AM

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synthesis posts are against forum rules, thus prohibited.
extraction is a different story, since most of the chemicals involved aren't particularly controlled.

but yeah...shulgin's book reads like a betty crocker cookbook; except LAH isn't quite as innocuous as baking powder.
"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
 
chemisch
#16 Posted : 1/18/2012 4:32:50 AM

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alright good to know, and it kinda does hahaha and LAH is very noms what you talking about???
if you can bassify in ammononia and extract with dcm why not smoke it?
 
chemisch
#17 Posted : 1/18/2012 4:34:28 AM

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benzyme do you have an occupation in some chemical feild you seem pretty smart
if you can bassify in ammononia and extract with dcm why not smoke it?
 
benzyme
#18 Posted : 1/18/2012 4:36:28 AM

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I'm a biochemist in the biotech industry.. with 15 years of chemistry experience.

and thanks; I've forgotten a lot of the theory (i.e. name reactions), but still know application and understand reaction mechanisms. I especially know the tools of the trade with respect to sample prep and purification, and how to analyze samples with GC-MS, CE-MS, LC-MS, and HPLC-UV.
"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
 
chemisch
#19 Posted : 1/18/2012 5:08:05 AM

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ah, i just love chemistry i'm gonna try and get into phoenix's chem program just want to understand synthesis completely make new drugs(: like sasha
if you can bassify in ammononia and extract with dcm why not smoke it?
 
benzyme
#20 Posted : 1/18/2012 5:11:02 AM

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hehe, I was like that too.
then I fell in love with analytical chemistry. gotta learn some of it, or you'll be flying
blind while making things.
"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
 
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