First extraction (A/B), need help!

[justine]

Hi!

I am about to make my first extraction and I plan on using an A/B method.

I have a pound of MHRB but I'm gonna extract only 100g for my first time and I have a few questions :
I bought all the material needed for Vovin's Tek. So I plan on using HCL/NaOH and Naphta.
1) I'm also thinking about washing with Sodium Carbonate, do you think it is a good idea ?
2) Do you know how much I should reduce my acid soup (I'm thinking about 300ML so it will fit in my separatory funnel) ?
3) And how low should my PH be when extracting MHRB (what about 3? I read it should be in the 2-4 range but I wonder what the optimum is) ?
5) Can I boil my MHRB when extracting and reducing (opinions seem to be contradictory here) ?
6) Should I do a defat of the acidic soup after decantation or is it somewhat useless with MHRB as I read here and there ?
7) Should I still add some NaOH when the solution turns black to reach a PH of 13-14 or is it useless ?
8 ) And more important, how much naphta should I use for my pulls (I'm thinking about 3x30ml) ?
9) And should I shake the separatory funnel or only turn it end over end as vovin advises ?
10) Also should the naphta be warmer than the basic solution or can I warm both in a heat bath before pulling ?

Thanks!

 

[endlessness]

ok as I posted in your other thread:

sodium carbonate wash is good specially if separation of solvent from mimosa wasnt perfect and you feel there might be traces of the basified liquid there

hmmm.. 300ml isnt much water.. At least one problem I can see is, if its so concentrated like this, any small spill will mean a lot of lost alkaloids....

Personally I would reduce to maybe 500ml, but then you would have the problem of having to do two rounds on the separatory funnel. I think either way its gonna work fine actually


As for the pH, truth is, you dont have to acidify much at all.. Even if it was, say, pH 6, it would already be enough.. Actually even if you didnt add any acid, the alkaloids should naturally be in a water soluble form so you dont have to worry about it. Just add a little bit of acid and thats enough. As a side question: why hcl? why not vinegar, if its food-safe and so easy to find and works just as well?

Yes you can boil MHRB on the acid step and when reducing.

Add NaOH till the solution turns black, and maybe a bit more.. Too much wont be a problem. If you have trouble with emulsions, just add plenty more NaOH or some pure salt, and this should get rid of the emulsions.

3x30ml seems very little naphtha.. Maybe better do, say, 6x30-50ml.. Freeze precipitation instead of evapping is recommended. Check this out for some tip on how to retrieve the crystals from freeze precipitation to avoid melting dmt problems. Dont throw your basified mimosa solution until you have yielded all your crystals, in case your yield is very small it might mean a lot of it is still in the mimosa solution

Shaking the separatory funnel might create some nasty emulsions.. you can add lye to break them but its definitely better to just avoid emulsions, and mix by stiring/turning over end.

You can both warm up just the naphtha or the whole thing, I dont know how much it matters, any of the ways will work fine... Just obviously take safety precautions like never heat a solvent with open fire, or dont heat anything in a closed container, etc.. Also be careful when working with lye, always used safety goggles and gloves.

good luck!

 

[justine]

Wow, thank you endlessness!

As a side question: why hcl? why not vinegar, if its food-safe and so easy to find and works just as well?

Well i've read somewhere on the forum that less dmt salts are formed with vinegar than Hcl, but if it works just as well I will definitely go for it! Do I have to use a special kind of vinegar ?

3x30ml seems very little naphtha.. Maybe better do, say, 6x30-50ml..

Do you mean 3x30-50ml for each round (considering I reduce to 500ml) ?
Let's say I go for 2x3x50ml, how much should I evap the 300ml of naphta before freeze precipitation and how much time would it take (I would like my dmt to be ready in 5 days) ?

Thanks!!

 

[endlessness]

yeah vinegar works just fine... people have 1-2% yields with vinegar, Ive never heard of significant increase in yield with HCl, but to be honest I neither have seen anybody do a side-by-side extraction to compare it exactly. I would say go ahead with vinegar, any pure white vinegar from the supermarket or natural food stores should be fine. Read the label and check if it doesnt have anything weird added to it.

I mean 6x50 ml naphtha total, counting all pulls.. So you add 50ml, mix, separate, put that in the freezer. You add another fresh 50ml, mix, separate, etc... do this 6x.. So that it is efficient, you could, say, make 3 pulls in one day, put the 3 pulls overnight in the freezer for maybe 12 hours, the next day you get your crystals and reuse the naphtha for making another 3 pulls. So it might take, a few hours for the acid boiling step, a couple more hours for the first three pulls, half a day for precipitation, another few hours for next pulls, another half day for final precipitation, and a couple more hours for air drying the crystals.. you could definitely do it in 5 days.

 

[justine]

yeah vinegar works just fine... people have 1-2% yields with vinegar, Ive never heard of significant increase in yield with HCl, but to be honest I neither have seen anybody do a side-by-side extraction to compare it exactly. I would say go ahead with vinegar, any pure white vinegar from the supermarket or natural food stores should be fine. Read the label and check if it doesnt have anything weird added to it.

I mean 6x50 ml naphtha total, counting all pulls.. So you add 50ml, mix, separate, put that in the freezer. You add another fresh 50ml, mix, separate, etc... do this 6x.. So that it is efficient, you could, say, make 3 pulls in one day, put the 3 pulls overnight in the freezer for maybe 12 hours, the next day you get your crystals and reuse the naphtha for making another 3 pulls. So it might take, a few hours for the acid boiling step, a couple more hours for the first three pulls, half a day for precipitation, another few hours for next pulls, another half day for final precipitation, and a couple more hours for air drying the crystals.. you could definitely do it in 5 days.

Thanks!
By the way should I add distilled water to the white vinegar ?
And would you say that cooking 3x1h (using an erlenmeyer flask in a frankly boiling heat bath) is enough to get all the alkaloids ?

 

[endlessness]

yeah 3x1 hour should be enough for most alks.. what I usually do actually is do first an overnight soak, filter this, and then do 3x1 boils, dont know if it makes a big difference but it certainly wont hurt

distilled water is not necessary, tap water will work fine to mix with the vinegar. Btw, as for the naphtha msds you posted in the other thread, the 'desaromatisé', it seems better.. It says 100% hydrotreated naphtha.. im not sure how hydrotreatment affects it, lets see if any of the chem experts here can answer, but I suspect it will work just fine.

In any case always do an evap test before using any solvent for the first time

 

[justine]

yeah 3x1 hour should be enough for most alks.. what I usually do actually is do first an overnight soak, filter this, and then do 3x1 boils, dont know if it makes a big difference but it certainly wont hurt

distilled water is not necessary, tap water will work fine to mix with the vinegar. Btw, as for the naphtha msds you posted in the other thread, the 'desaromatisé', it seems better.. It says 100% hydrotreated naphtha.. im not sure how hydrotreatment affects it, lets see if any of the chem experts here can answer, but I suspect it will work just fine.

In any case always do an evap test before using any solvent for the first time

I just saw it is heavy naphta, isn't it better to use light naphta ?

 

[justine]

I went to castorama after work, checked on solvents and found a bottle of 'essence F' (='gasoline f')
which is 100% hydrotreated light naphta (cas 64742-49-0), do you think I should use this rather than
heavy naphta ?

 

[endlessness]

I looked at the msds, I dont see anywhere saying its 100% naphtha (or anything else for that matter hehe), but maybe my french is just not good enough or I didnt look careful enough...

I found weird the name of the product has "5%" in it (ESSENCE F-5%)... is it anything to do with the content? But yeah if its 100% light naphtha as you said it should work perfectly. Do the evap test and if its clean, should be good

 

[justine]

I looked at the msds, I dont see anywhere saying its 100% naphtha (or anything else for that matter hehe), but maybe my french is just not good enough or I didnt look careful enough...

I found weird the name of the product has "5%" in it (ESSENCE F-5%)... is it anything to do with the content? But yeah if its 100% light naphtha as you said it should work perfectly. Do the evap test and if its clean, should be good

Well on page 2, under *3 you can read the "informations about the components" (informations sur les composants) if there was anything other than CAS 64742-49-0 it would be mentioned, wouldn't it ?

As for the 5%, it is probably related to european regulations but maybe I'm wrong...

By the way it is often used as a longer-lasting replacement for Zippo lighter fluid.

 

[rOm]

Castorama !! haha DIY power !

 

[justine]

By the way, last night I acidified 100g of MHRB (2h/1h/1h in a boiling heat bath) and vacuum filtered
the acid soup each time and discovered interesting phenomenons :
- My first batch was cooked with 200ml of 8% white vinegar and when I started pouring it in the büchner and
pumped... nothing happened, or rather should I say that only 1 drop fell every minute even at -700mmHG.
Then I poured it back in the erlenmeyer and added 100ml of water and it solved everything, once more the
resulting filtrate was surprisingly clear.
At first I though it was only due to the fact that my first batch was initially too thick so for the
second batch I used 300Ml of vinegar. However I wound up with the same issue I had with the first batch
and needed to add 100ml water to solve it. I was once again very surprised with the purity of the
resulting filtrate and the cleanliness of the filter. Later, as the batch I was pouring in the buchner 50ml
at a time was cooling I also realized that filtration was getting much faster.
In the end I didn't even need to decant.

So to sum up, it seems to me that :

- MHRB acidified with pure 8% white vinegar is nearly impossible to vacuum filter (at least with a hand pump) but
adding some water considerably speeds up filtration and the resulting filtrate is much purer than when using the HCL+water method (since decanting seems to be mandatory with vovin's tek).
(if I had to venture a theory as to why I would say that vinegar and water enhance the property of the filter but i don't know exactly how)
- When using white vinegar + water filtration speed is inversely proportional to the temperature of the acidified MHRB.

What do you think about it?

 

[rOm]

I have no clue. SWIM got clogged up filter many times but just filter out the NPS, so he is generous with adding NPS and get very good yields.

Maybe ask Vovin directly, I don't know how much free time he has, or if he answer PM but he will know the How's & Why of his tek ...

 

[corpus callosum]

Fantastic OP, Justine.

And much credit to Endlessness for answering your queries so beautifully.

I am a firm fan of le tek de Vovin because it yields a very pure product if one follows the tek closely without omitting any of the steps.For some reason, working through the tek in a leisurely fashion is most satisfying.

Ive tried a few variations just to see if it alters the outcome and I have found that boiling your acidified solution does lead to a lesser yield and the product tends to be tinged yellow-the reason for this is unclear to me.Ive also found that to cover 50g of MHRB with the HCL solution as the tek suggests it takes 100-150ml if using a 500ml conical flask.When done 3 times and after Buchner filtering and decanting I have had 300-450ml of deep red liquid which does away with the hassles of having to reduce the volume for the subsequent steps.Ive never had to reduce the volume at this stage so I cannot say if using more HCl solution and then reducing the volume would increase the yield.

Life becomes easier if you dont have to split your basified liquid and I always pull the freebase with naptha thats uncomfortably hot to a dipped-in finger with the basified liquid being at room temperature.Six pulls of 50mls naptha is my preferred method.Evaporating this gives a bigger yield but freeze-precipitation is not far behind.

Ive had yields of over 1% but quite as high as 2% but I guess the quality of the MHRB must play a part in this.

And I applaud Endlessness for the suggestion that you keep your basified liquid until after youve freeze-precipitated your naptha to yield the crystals just in case the yield is low so you can re-work the basified solution some more.Such a simple point but so valuable.Plus you can re-use your naptha following this to pull again if required.Lastly, this naptha can also be evaporated to yield a little more tackle right at the end.

I also really like the last solvent wash step in vovins tek-I prefer to freeze precipitate from this as the crystals come out alot whiter-provided of course you get all the gummy muck out.

 

[Explorateur]

Justine, I'd like to know if you manage to get good results with "Essence F" (cas 64742-49-0) as alternative to VM&P Naphtha ?

 

[Rivea]

By the way, last night I acidified 100g of MHRB (2h/1h/1h in a boiling heat bath) and vacuum filtered
the acid soup each time and discovered interesting phenomenons :
- My first batch was cooked with 200ml of 8% white vinegar and when I started pouring it in the büchner and
pumped... nothing happened, or rather should I say that only 1 drop fell every minute even at -700mmHG.
Then I poured it back in the erlenmeyer and added 100ml of water and it solved everything, once more the
resulting filtrate was surprisingly clear.
At first I though it was only due to the fact that my first batch was initially too thick so for the
second batch I used 300Ml of vinegar. However I wound up with the same issue I had with the first batch
and needed to add 100ml water to solve it. I was once again very surprised with the purity of the
resulting filtrate and the cleanliness of the filter. Later, as the batch I was pouring in the buchner 50ml
at a time was cooling I also realized that filtration was getting much faster.
In the end I didn't even need to decant.

So to sum up, it seems to me that :

- MHRB acidified with pure 8% white vinegar is nearly impossible to vacuum filter (at least with a hand pump) but
adding some water considerably speeds up filtration and the resulting filtrate is much purer than when using the HCL+water method (since decanting seems to be mandatory with vovin's tek).
(if I had to venture a theory as to why I would say that vinegar and water enhance the property of the filter but i don't know exactly how)
- When using white vinegar + water filtration speed is inversely proportional to the temperature of the acidified MHRB.

What do you think about it?

I have always been amazed as one reduces the water content how much solid material precipitates out of the acidified solution. I have had deep reddish purple solutions with not a sign of solids at room temperature. Cooled for an hour turns it cloudy and makes it very difficult to filter. I tend to filter, cool, and decant ending up with darker purple solution and no solid content. If I reduce this, as soon as it cools it clouds and becomes difficult to filter.

 

[Trickster]

I tend to filter, cool, and decant ending up with darker purple solution and no solid content. If I reduce this, as soon as it cools it clouds and becomes difficult to filter.

I used to do that but now I simply put the solution in a fridge for a day. All solids settle and after careful decanting there is no need to filter.

 

[Explorateur]

Justine, I'd like to know if you manage to get good results with "Essence F" (cas 64742-49-0) as alternative to VM&P Naphtha ?

Justine reply "yes" via PM...