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Quiz for the chemists! Options
 
Th Entity
#21 Posted : 2/7/2019 3:55:43 AM

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Yeaah, exactly right? Overkill
I feel like most of the cells (if not all) would be lysed during belnder and freeze/thaws.
Thanks!
 

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Th Entity
#22 Posted : 2/9/2019 1:25:13 PM

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Hey benz, during acidification and basification most people use heat? why?

(Most/if not all) cells would be broken down by the time one acidify (if he use powdered MHRB and freeze/thaw) and then one would either acidify/basify or would simply basify in which cells have no chance of surviving unlysed, i think (by the low/high pH alone, and during that, most would boil or heat the mix) why?

(And if one was to use heat during acidification for example, what would be the best temperature to do so and why?)
 
benzyme
#23 Posted : 2/9/2019 10:31:48 PM

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heat catalyzes the hydrolysis of cell membranes.
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Th Entity
#24 Posted : 2/10/2019 4:46:57 AM

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And what would be the best temperature to apply and for how much time (after acidifying)? Big grin Laughing
 
endlessness
#25 Posted : 2/10/2019 12:01:59 PM

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Not benz but... AFAIK I don't think this data is available, I don't think people did side-by-side with several different temperatures and timing to see exactly how much it affects it.

That being said, I think you are over-complicating things. People do a variety of different extractions here, some with heat, some without, some with one solvent, some with other, some with powdered bark, some with shredded bark, etc .. And in the end, the results are pretty much equivalent, people are getting around 1-2% DMT from MHRB.

Just don't throw anything away until you finish the extraction. That way if you don't get a good yield in your first try, you can always go back to an earlier step and try to do more pulls, or try to boil your bark again and extract from this last boil, or whatever.
 
tatt
#26 Posted : 2/10/2019 2:32:06 PM

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endlessness wrote:

That being said, I think you are over-complicating things. People do a variety of different extractions here, some with heat, some without, some with one solvent, some with other, some with powdered bark, some with shredded bark, etc .. And in the end, the results are pretty much equivalent.

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Th Entity
#27 Posted : 2/10/2019 4:15:41 PM

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Quote:
That being said, I think you are over-complicating things.
- thats me, exactly! Endlessness you nailed it.

Some questions might be strange but im just curious. Since we are here share your results about what temperature you apply during acidification and why? (what temp would promote cell lysis/hydrolysis of cell membranes?)

Edit: I read somewhere that short time with higher temp 80+ C is best in a biology lab.
 
endlessness
#28 Posted : 2/10/2019 4:30:06 PM

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It is totally fine and understandable to ask questions if you are curious about theoretical aspects. I certainly am a lover of theoretical questions myself Smile

When talking about extractions though, the practical aspect of it reigns supreme. For example, say the difference between 50 degrees celcius or 80 degrees celcius is a difference between 1.2g or 1.2001g ... If that was the case, then sure we can say that in theory more heat will help, but in practice it would make no difference and people shouldnt really spent their resources on this increased temperature.

Another thing is, regarding temperature I suppose you are talking about an STB, right? Because with an A/B people will generally boil their plant material so it will always be 100 degrees celcius (for that case you could question the effect of the time variable though). In the case of STB, if you use lye, it anyways by itself will already raise the temperature of the solution quite a lot, plus the lye itself will help breaking down cells. Are you thinking of adding extra heat to the whole thing?

Lastly, here's a proposal for you... You are not talking about lysing grapefruit cells, you are talking about DMT-containing plants, right? So this means you are interested in extractions of these substances.... So why not answer your own questions at least partly, through experiment, and letting us know the result so we all collectively grow our knowledge? This is as easy as doing a side-by-side extraction changing the temperature variable (or whatever other variable you are specially interested in) between the two groups.. I for one would love to read your results Pleased
 
Th Entity
#29 Posted : 2/11/2019 6:12:10 AM

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Ok


P.S. - Sorry if i annoyed you guys with these questions (on most of them i had opinion but i wanted 2nd one) big thanks to benz
 
Th Entity
#30 Posted : 3/5/2019 6:24:52 PM

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Hey Nexians!

Which solvent would be the best substitute for naphtha (for the pulls/extraction)? Maybe something not as selective as Heptane or?

Same question applies to the re-x part, which would be the BEST solvent for re-x of good product?
Same question applies to the defat part, which would be the BEST solvent for defat

- I pretty much have acess to all common laboratory solvents, so availability is no problem.

P.S. - I cant find a reasonably good naptha to use in extractions.

Edit: I just realised that probably if i'm going to defat i would have to use the same solvent like the one for pulls/extraction so keep that in mind. Wink Embarrased


 
downwardsfromzero
#31 Posted : 3/5/2019 7:15:04 PM

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Different solvents have their different relative advantages and disadvantages, so asking what the 'best' substitute for naphtha might be is useless without defining some further parameters. Also, I find it baffling that you claim to "pretty much" have access to "all common laboratory solvents" yet then state that you can't find a reasonably good naphtha. I thought petroleum ether was a common laboratory solvent and it's practically the same as naphtha.

[Does "pretty much" having access mean you walk past the open window of a laboratory from time to time? Big grin ]

As far as recrystallisation [of DMT] goes, heptane has a number of advantages - selectivity, low toxicity, favourable temperature/solubility curve, convenient boiling point, to name several.


Anyway, cyclohexane. Just use cyclohexane.
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Th Entity
#32 Posted : 3/5/2019 7:59:57 PM

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Quote:
best substitute for naphtha (for the pulls/extraction)? Maybe something not as selective as Heptane
something that has the "pulling" ability of naptha or better that can take all the non polars within the mixture, that can later be purified.

Yes i might use heptane for re-x thats my current choice, any other suggestions?

I can use cyclohexane too, do you have experience with it what are your results and opinions?

I can buy this: Cyclohexane for liquid chromatography, HPLC
Essential substance 99.5%
Water 0,01%
Acidity (μEq / g) 0.0005
Residue after evaporation 0.0005%
UV absorption:
210 nm max. 0.40
220 nm max. 0.10
230 nm max. 0.05
240 nm max. 0.01
350 nm max. 0.004

Quote:
[Does "pretty much" having access mean you walk past the open window of a laboratory from time to time? Big grin ]
it's just available to me and i can afford it so why not use the best for each situation. Laughing

I can buy petroleum ether too, its available. I thought about it, here where i live for some reason naptha is being sold as different things from store to store (different mixtures that sometimes drastically differ, i have no clue why). From 4 different brands only 1 evap clear but i dont think its actual naptha, more like some naptha distillate/derivative labeled as naptha (cant find msds and label is not very informative so i rather be on the safe side).

However heres the petroleum ether i can get:
Petroleum ether 40-60C, pure for analysis
Water max 0,1%
Aromatic hydrocarbons max 0,01%
Residue after evaporation max 0,01%
Sulfur pass test
Benzene 0,001%

Rolling eyes

 
downwardsfromzero
#33 Posted : 3/5/2019 9:59:32 PM

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Cyclohexane is great for degreasing. I've used it for fats analysis in waste stream samples. It's probably useless for freeze precipitation on account of its high melting point. Still good for a pull, backsalt/mini A/B with heptane.

Your petroleum ether appears to be largely pentane which would have the annoying habit of evaporating when warm enough to extract anything effectively, so now I understand your relative naphtha predicament.

All told, you just need to choose something and go with that. And I'd be particularly interested in what results you'd get with cyclohexane.

Quote:
4 different brands only 1 evap clear but i dont think its actual naptha, more like some naptha distillate/derivative labeled as naptha

Naphtha, in the most general sense, is just a petroleum distillate derivative (i.e. by hydrotreating to ensure stability) labelled as naphtha. It can be called by various names - petroleum ether, benzine (with an 'i' - careful there!), liquid hydrocarbons, paraffin, mixed alkanes, etc. When looking at proprietary products, I'd look for "Naphtha, hydrotreated, light" on the label, if that's any help to you.

In the past, I've had great results with medium naphtha - sold as a BBQ lighting fluid - followed by re-x with a clean-evaporating solvent. An octane/decane fraction seems to do a really nice job of pulling and has a great temp/solubility curve.

If you're really concerned about purity of OTC hydrocarbon solvents you could simply ("simply") fractionally distil them.
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benzyme
#34 Posted : 3/6/2019 3:37:22 AM

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cyclohexane is excellent for pulling and doing RT evap, or rotavap’ing.
Pet Ether is essentially VM&P, short-chain aliphatic hydrocarbons, C5-C9.
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Th Entity
#35 Posted : 3/6/2019 7:26:13 AM

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For solvent for Re-x the battle was between heptane and hexane, both of them i can get in those "forms" - pure for analysis, for liquid chromatography, for spectroscopy. Im leaning towards heptane tho, what do you guys think?

Heptane - pure for analysis
Essential substance min 99%
Water max 0,01%
Boiling point 98C
Evaporation residue max 0,001%
Free acids max 0,002%
Iron max 0,00001%
Lead max 0,00001%

Hexane - pure for analysis
Essential substance min 99%
Water max 0,01%
Boiling point 68C
Evaporation residue max 0,001%
Free acids max 0,002%
Iron max 0,00001%
Lead max 0,00001%

The other "forms" are purer and more expensive.

For pulls and defat i would like to use the same solvent, i thought about using heptane for the pulls/extracting and the defat, but from my little knowledge heptane is not the best choice for defat. Im not sure about cyclohexane maybe i could give it a try if i dont find any solution to this "problem". Any other ideas? DCM, THF, Toluene, Xylene? Maybe i can even try to find some of the not so common solvents if you suggest one that will work great. (I would also like it to be good for freeze percip, i dont have the knowledge nor the expertise to choose one, so i would greatly appreciate if anyone can suggest something that will work good.

Maybe if someone give "recipe" i could try to "cook" my own naptha. Laughing (mixing different solvents)

Here is another petroleum ether i found

Petroleum ether - pure for analysis
Contains 2% n-hexane
Boiling range (90 %) 40 - 60C
Density (20C) 0,64 - 0,66 g/cm3
Water (Karl-Fisher) < 0,03 %
Acidity / alkalinity < 0,0005 meq/g
Color < 10 APHA
Residue after evaporation < 20 ppm
Calcium (Ca) < 5 ppm
Copper (Cu) < 5 ppm
Iron (Fe) < 5 ppm
Lead (Pb) < 2 ppm
Magnesium (Mg) < 2 ppm
Potassium (K) < 2 ppm
Sodium (Na) < 5 ppm
Zinc (Zn) < 2 ppm
Total phosphorus (P) < 1 ppm
Total silicon (Si) < 1 ppm
Total sulfur (S) < 50 ppm
Bromine number < 5



 
Th Entity
#36 Posted : 3/7/2019 4:43:39 AM

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Maybe i could use heptane for pulls/extracting and re-x and use cyclohexane or other solvent for the defat, which solvent to use for defat?
 
benzyme
#37 Posted : 3/7/2019 5:08:47 AM

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you could use either, to similar effect. both are nonpolar. you could even use cyclohexane as a recrystallization solvent.
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Th Entity
#38 Posted : 3/7/2019 5:51:38 PM

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Benz is this comment on post #35?
Quote:
you could use either, to similar effect. both are nonpolar. you could even use cyclohexane as a recrystallization solvent.


I decided im going to use Heptane for pulls/extraction and the re-x.
Now im wondering what solvent to use for the defat (i will defat) maybe cyclohexane since @downwardsfromzero said he used it for degreasing and it works well, maybe something else you could suggest that will suck all the plant oils/fats effectively?

What about chloroform for defat?
 
Th Entity
#39 Posted : 3/10/2019 4:49:29 PM

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Im sorry for asking these questions!

I know you (longer members of the dmt-nexus) have answered these types of questions literally hundreds of times, i give you all my love and total respect to you and i really appreciate you!

Lastly, i want to ask this: would it be effective to use heptane for defat? Is it going to work properly?

P.S. - Im going to use heptane for pulls/re-x and i want to know if heptane is effective for defat?
Likes dissolve likes, i know but is it effective?

 
Mindlusion
#40 Posted : 3/10/2019 5:06:58 PM

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recrystallization solvents are typically poor extraction solvents.

Because recrystallization solvents you typically want one that the compound of interest has poor solubility in at room temperature, but OK solubility at high temperature.

With an extraction solvent, you want something that has good solubility at all temperatures.

The only benefit of using a poor solvent like heptane for extraction, is that it also has a poor affinity to impurities, or NMT in the case of acacia bark. So initially you get an extract that is more pure. But, doing that is a bit redundant because the whole point of the recrystallization solvent is to recrystallize the crude. And, its wasteful since you would have to do >5x pulls to efficiently extract the alkaloids, and use a lot more solvent. Cyclohexane is the least polar, and would be especially wasteful.

If you use something like chloroform, toluene, methylene chloride or ethyl acetate as your extraction solvent, you can extract virtually all the alkaloids with just 2-3x 50mL pulls.

The same principle applies to defat as well.
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