Can xylene pulls can be backsalted?

[Kalitechnik]

Hey folks please help me on this one as i am wondering, can my xylene pulls be backsalted?
Do i understand correctly that i can use water with citric acid to backsalt my xylene, and later add the base solution and do the pet ether pulls to freeze precip my xtals?

And how to do it corectly? If i will have around 350 ml of xylene, how much acidic water i should use, and how many times i should do it?

 

[acacian]

Yeah they can.. solution with a ph 4 is ideal but keep in mind contact with the freebase will raise ph. I don’t measure acidity when backsalting as I’m converting it to freebase very quickly - meaning if your solution is a little too acidic it’s not a big deal as it’s being converted straight away. Prolonged exposure would be another story. Good practice to keep around 4

 

[Kalitechnik]

Yeah they can.. solution with a ph 4 ideal but keep in mind contact with the freebase will raise ph. I don’t measure acidity when backsalting as I’m converting it to freebase very quickly - meaning if your solution is a little too acidic it’s not a big deal as it’s being converted straight away. Prolonged exposure would be another story. Good practice to keep around 4

can you please explain on the prolonged thing? is keeping our freebase changes into salt in acidic enviroment to long wrong? and whats with the PH?

i usually go quite low with the PH for the acidic phases? Is this wrong? and why if it is? i would apreciate explanation on this issue. thanx.

 

[Transform]

If your acidic phase ends up up going too low on the pH after the backsalting has been completed, it means at the very least that you have wasted acid and will subsequently also waste base when converting back to freebase (assuming you're not using a volatile acid and evaporating it down completely before adding base). As for the prolonged contact with acid, this is not so much of an issue for MHRB but the story for some other plants may be different - such as in the case of making full-spectrum acacia extracts.

 

[Kalitechnik]

If your acidic phase ends up up going too low on the pH after the backsalting has been completed, it means at the very least that you have wasted acid and will subsequently also waste base when converting back to freebase (assuming you're not using a volatile acid and evaporating it down completely before adding base). As for the prolonged contact with acid, this is not so much of an issue for MHRB but the story for some other plants may be different - such as in the case of making full-spectrum acacia extracts.

Ok, so saving acid and base is one thing, and also as i was reading @Loveall aproach he was saying some procedure of how to make backsalting in a way that we can change polymerized goey deems into white crystals. That would be mine aim to while working with the xylene pulls.

Backwash details that could minimize DMT polymerization:

- Stir in dilute acid overnight. With time, the most stubborn DMT polymers seem to be broken up. Like Jess said, don't use a lot of acid to minimize ionic strength in the next step.
- Add Naphtha before basing
- Add base slowly while shaking with Naphtha and sample the water pH. Target a pH of 10.7, to finish up (water will also stop clouding as base is added). I think we want to avoid cloudy water sitting around to minimize DMT polymer.

Not sure which of these matter more, but combined they turn yellow goo to white xtals.

So just to be sure i would like to ask you guys for the procedure of correct backsalting. If i got it right.
Lets say i will be working with 300-400ml of xylene.

How much of the acidic water for the backsalting i should be using? 100ml?
And should i do it once (as many places says) or 2-3 times similar to NPS pulls (i read in one place that someone adviced to do it 3 times, and combine the acidic water.

 

[doubledog]

Yes, it can be done. Use 50-100ml of water, and use a titration to not overacidify it. One backsalting cycle is enough, main focus should be on mixing of the layers.
You can also get freebase by adding some base to your backsalting water. Reducing of the water to half could help here. Dmt separates from the alkaline water in form of white precipitate/crystals and can be filtered out. After washing and drying, it produces slightly brown, waxy, sometimes oily material.

 

[Transform]

some procedure of how to make backsalting in a way that we can change polymerized goey deems into white crystals

I suspect that freeze precipitation from naphtha or heptane will producer whiter crystals than evaporating xylene would.

Is there a reason why you're persisting with the use of xylene?

 

[Kalitechnik]

I suspect that freeze precipitation from naphtha or heptane will producer whiter crystals than evaporating xylene would.

surely it will. and even whiter if averything is made in room temp (as my early experience shows). Previously what i was doing was following dptek (the tek developed at Mintys discord server).
1. Room temp 24h acid soak
2. Adding previously prepared salt and lye solution
3. Adding quickly icy water to keep the temp of the pull at 21-22C
4. Pulls with pet ether

that usually produced me with nice white crystals.

Is there a reason why you're persisting with the use of xylene?

The xylene came to my world after researching the fullspectrum spice. As people claimed it has different qualities (which i will not focus on that now).
So first i did some xylene pulls with spent bark (mamma mia, what i lost with so much thrown spent bark before ). And i discovered i can have some more stuff. After reading more i realized that mostly what is pulled is dmt anyway with few traces of additional stuff. So in general i realized that xylene pulls much more dmt.

And that is my main reason now. Yields.
Before with the above mentioned cold pulls procedures i was getting 0,7 - 1,2% yield with 1,5% once as a maximum.
With crude xylene pulls i started to get 1,8 - 2,2% yield from the same bark, which after first mini A/B`s was 1.6-2%.

So that is my main reason. And since "jungle", goey, waxy spice seems to be dmt in different forms (as some call it polymers) my idea is to pull as much as possible with hot xylene pulls, instead of evaping as before backsalt it, and later give it some treatment to make it as white-pure-crystaline as possible.

And some of @Loveall work and threads on this subject is my inspiration, as he was showing that he could change some quite goey yeloow stuff into whitey xtals. BTW is he somewhere around as it would be nice to hear from him about how it was developing.

I am attaching my last xylene goey pulls, which was mini A/B`d.

 

[Kalitechnik]

Yes, it can be done. Use 50-100ml of water, and use a titration to not overacidify it.

I checked what a titration is and kind of understood it. But i am wondeing how can i measure what is the actual PH of a water solution under the xylene? I dont have pro lab meters.

One backsalting cycle is enough, main focus should be on mixing of the layers.

So i should focus on mixing, shaking very well, few times to be sure that all will be trnasfered from xylene to the acidic water?

You can also get freebase by adding some base to your backsalting water. Reducing of the water to half could help here. Dmt separates from the alkaline water in form of white precipitate/crystals and can be filtered out. After washing and drying, it produces slightly brown, waxy, sometimes oily material.

Hmm. That is super interesting. So in general i could skip the pulling with naptha, and just filter it in a buchner? And by washing you mean pouring more clean water on the filter to rinse it out from the lye remnants?

 

[Transform]

I checked what a titration is and kind of understood it. But i am wondeing how can i measure what is the actual PH of a water solution under the xylene? I dont have pro lab meters.

What you do is take a known amount of the xylene solution and backsalt it into a known excess amount of acid of known concentration. Then you titrate the amount of acid remaining using a standard solution of base. From that figure you can work out how much acid is required to neutralise the rest of the DMT in the xylene.

 

[doubledog]

Liquid pH indicator (I use red cabbage as a source) is very convenient tool for titration, its colour shows you pH without need to disturb xylene layer.

Yes, washing is exactly that - as you filter out fb, it stays wet with alkaline water on the filter, so you have to wash it with plain water. It is also quite possible that you can have issues with back extracting into naphtha - polymorphic dmt is not very soluble in it.

 

[Transform]

Liquid pH indicator (I use red cabbage as a source) is very convenient tool for titration, its colour shows you pH without need to disturb xylene layer.

Yes, washing is exactly that - as you filter out fb, it stays wet with alkaline water on the filter, so you have to wash it with plain water. It is also quite possible that you can have issues with back extracting into naphtha - polymorphic dmt is not very soluble in it.

Thanks, I forgot to mention including an indicator in the titration method, but then again, the fundamentals of titration will be explained elsewhere on the internet already.

Miareczkowanie – Wikipedia, wolna encyklopedia

pl.wikipedia.org

 

[Kalitechnik]

Liquid pH indicator (I use red cabbage as a source) is very convenient tool for titration, its colour shows you pH without need to disturb xylene layer.

Oh thats interesting. I watched some YT videos on red cabbage juice used in ph indication. Very handy. Just one thought. Will this give some reddish colour to the freebase

Yes, washing is exactly that - as you filter out fb, it stays wet with alkaline water on the filter, so you have to wash it with plain water.

Let me repeat that again so i can understand it correctly. After backsalting and getting rid of xylene, i can base my solution and simply filter it to get the freebase? That sound very interesting. And now when i think about it, it reminds me the harmala extraction, where harmalas freebase are crashing out in the basic solution. Is this the same principle?

It is also quite possible that you can have issues with back extracting into naphtha - polymorphic dmt is not very soluble in it.

As i was reading some of @Loveall post, we should be able to change the polymorphic goey dmt into xtals, by some procedures. Looks like some long acid treatment is one of those steps....

Backwash details that could minimize DMT polymerization:

- Stir in dilute acid overnight. With time, the most stubborn DMT polymers seem to be broken up. Like Jess said, don't use a lot of acid to minimize ionic strength in the next step.

 

[Kalitechnik]

So thats how my first backsalting went.

After mixing few times acidic water with xylene to be sure all was transfered, and after removing as much xylene as possible with pipette (i guess i will need a proper separatory funnel for that in a future) this is what i got. I have seen how white cloudy preciptates occurs in the water it was quite stunning. And some layer of xylene is visible, which i needed to evaporate before adding lye.

After adding lye soluting and pet ether and shaking i got quite nasty layer of emulsion. Is there any way of minimizing it?

Pulling with pet-ether and fully evaping it left me 2% waxy yellow nice smelling deems. (Started with 45g of bark.)

I also wanted to se what abou the nasty emulsion thing, and i pulled it on some surface. After drying it gave me some 170mg, of dmt smelling substance, i guess thats dmt also right?

I should add also that this time i used used xylene for extraction, and also used pet-ether, and i left it for full evap, and i guess thats the main resson for getting waxy goey product.

 

[doubledog]

Oh thats interesting. I watched some YT videos on red cabbage juice used in ph indication. Very handy. Just one thought. Will this give some reddish colour to the freebase

Colour from indicator is washed away, And if any remains, it's still just cabbage

Let me repeat that again so i can understand it correctly. After backsalting and getting rid of xylene, i can base my solution and simply filter it to get the freebase? That sound very interesting. And now when i think about it, it reminds me the harmala extraction, where harmalas freebase are crashing out in the basic solution. Is this the same principle?

Yes, it's same principle, alkaloid in freebase form becomes insoluble in water, when base is added. It differs in properties, harmaloids are more dense, and settle down, dmt is more fluffy and floats in water.

Emulsion is probably a mix of dmt and some impurities from the water.

 

[Kalitechnik]

Emulsion is probably a mix of dmt and some impurities from the water.

ah. thats why distilled water is adviced for this process?

 

[doubledog]

Yes, that's probably the main reason for that.

 

[1Starway7]

Warning about ...xylene... It can be smelled atleast 30 or 40 feet away...unless covered air tight...It will stink up your freezer...

Hope your doing your extraction in total privacy! ..... you dont need unwanted atention

I would never use that stuff unless i was out in the country far from a nosey neighbor.... just venting exylene fumes out an open window doesnt guarentee your saftey and privacy.. ... if you live in an apartment building...!

Oders from ..Napatha... are far easier to control than exylene! GOOD LUCK!

 

[bodymechanics]

Excellent work Kalichnik!
I’m about to try this very same procedure on 200g bark.

 

[bodymechanics]

Warning about ...xylene... It can be smelled atleast 30 or 40 feet away...unless covered air tight...It will stink up your freezer...

Hope your doing your extraction in total privacy! ..... you dont need unwanted atention

I would never use that stuff unless i was out in the country far from a nosey neighbor.... just venting exylene fumes out an open window doesnt guarentee your saftey and privacy.. ... if you live in an apartment building...!

Oders from ..Napatha... are far easier to control than exylene! GOOD LUCK!

I put my xylene pulls out side on the balcony. It’s definitely got odor, but I doubt the neighbors smell it. It doesn’t smell any worse than minor painting