How effective is backsalting per pull of water? (xylene)

[fathomlessness]

I want to start trying back salting my DMT after xylene pulls.

Just curious to know how much acidified water (vinegar) to use with xylene? Will less than 50:50 ratio water to xylene pull ALL the alkaloids from the xylene in one mix? Or like standard extractions are multiple pulls needed? I just thought that DMT may migrate to a polar solution much easier than it would to a non polar solution (especially if that polar solution is just plain clean acidic water).

 

[pete666]

I am doing back salting with HCl. Only little water is necessary. I use ratio about 1:5 (water:np)
Only one pull is necessary. I just add water to np and then 3,7% HCl in steps until pH 5.5
I then continue with basification and extraction by heptane, so I don't mind excessive acid. HCl could be evaporated from the result though, don't know whether acetic acid too. If not and I wanted to use the product at this stage, I would target pH 7, so there wouldn't be any acid left. But some alkaloids would stay in the np then.

Btw why do you want to uset acetic acid? Do you want dmt acetate or is it just middle step of more complex proceure?

 

[Northerner]

I use plain household vinegar (5%) as is at a 2:1 ratio acid:solvent. Remove the acid from underneath, base it and then pull once with the same amount of clean solvent.

I dunno if this is "right", but it works.

 

[fathomlessness]

I am doing back salting with HCl. Only little water is necessary. I use ratio about 1:5 (water:np)
Only one pull is necessary. I just add water to np and then 3,7% HCl in steps until pH 5.5
I then continue with basification and extraction by heptane, so I don't mind excessive acid. HCl could be evaporated from the result though, don't know whether acetic acid too. If not and I wanted to use the product at this stage, I would target pH 7, so there wouldn't be any acid left. But some alkaloids would stay in the np then.

Btw why do you want to uset acetic acid? Do you want dmt acetate or is it just middle step of more complex proceure?

I see, do you know that only one pull is necessary because you tested it before by doing a seperate second pull and basifying that?

I would of thought a ph of 3-4 is more preferable. I also read recently that the moles of acetic acid or hydroclooric acid have to be proportional to the amount of dmt otherwise the dmt wont react with the acids and transform. Whether or not only a little acid is required to convert A LOT of dmt is something i would want someone with more chemistry knowledge to chime in on.

I am using acetic acid because I have it and it's cheap and not as corrosive as hcl and the PH is really "set" at around 3-4 and doesn't fluctuate as hard as hcl. I have had a hard time before with hcl by accidentaly adding too much, so its just easier to use white vinegar. Why do you ask? Any benefits to hcl over actetic acid?

I was FASAing the dmt out of the xylene with acetone but it got expensive with all the acetone because i would have to evaporate that off the xylene and re-use the xylene. So now i am backsalting -> reducing -> cooling -> basifying -> drying -> acetone -> FASA -> DMT-fumarate.

 

[fathomlessness]

I use plain household vinegar (5%) as is at a 2:1 ratio acid:solvent. Remove the acid from underneath, base it and then pull once with the same amount of clean solvent.

I dunno if this is "right", but it works.

Yeah that is the same as I am doing, im just trying to get someone with technical knowledge of the limits of what i can scale down the solvent/water ratio to and whether or not repeated pulls are necessary on polar backwashes.

 

[Northerner]

I've tested it and found 0 alkaloids on the second +/-100ml pull on 200ml acid. 1.5g yield.

I've often wondered about the solubility of DMT in solvents and acids though, where the saturation points are.

 

[pete666]

I see, do you know that only one pull is necessary because you tested it before by doing a seperate second pull and basifying that?

No, it is well known so I follow this. I am getting total gain up to 3% (with this salting method), so I doubt anything is lost in the process

I would of thought a ph of 3-4 is more preferable. I also read recently that the moles of acetic acid or hydroclooric acid have to be proportional to the amount of dmt otherwise the dmt wont react with the acids and transform. Whether or not only a little acid is required to convert A LOT of dmt is something i would want someone with more chemistry knowledge to chime in on.

I am using acetic acid because I have it and it's cheap and not as corrosive as hcl and the PH is really "set" at around 3-4 and doesn't fluctuate as hard as hcl. I have had a hard time before with hcl by accidentaly adding too much, so its just easier to use white vinegar. Why do you ask? Any benefits to hcl over actetic acid?

With HCl you need exactly calculated amount of HCl, not more. You can calculate how much acid you need and it works perfectly, by added acid you can say how much alkaloids is in the solution (+=5%)
I would say with acetic acid it might be the same.
I might do the calculation fo you.
I've tried salting with FASW, but HCl seems to be better. You can check here

I was FASAing the dmt out of the xylene with acetone but it got expensive with all the acetone because i would have to evaporate that off the xylene and re-use the xylene. So now i am backsalting -> reducing -> cooling -> basifying -> drying -> acetone -> FASA -> DMT-fumarate.

Your procedure is similar to my procedure

 

[fathomlessness]

I see, do you know that only one pull is necessary because you tested it before by doing a seperate second pull and basifying that?

No, it is well known so I follow this. I am getting total gain up to 3% (with this salting method), so I doubt anything is lost in the process

I would of thought a ph of 3-4 is more preferable. I also read recently that the moles of acetic acid or hydroclooric acid have to be proportional to the amount of dmt otherwise the dmt wont react with the acids and transform. Whether or not only a little acid is required to convert A LOT of dmt is something i would want someone with more chemistry knowledge to chime in on.

I am using acetic acid because I have it and it's cheap and not as corrosive as hcl and the PH is really "set" at around 3-4 and doesn't fluctuate as hard as hcl. I have had a hard time before with hcl by accidentaly adding too much, so its just easier to use white vinegar. Why do you ask? Any benefits to hcl over actetic acid?

With HCl you need exactly calculated amount of HCl, not more. You can calculate how much acid you need and it works perfectly, by added acid you can say how much alkaloids is in the solution (+=5%)
I would say with acetic acid it might be the same.
I might do the calculation fo you.
I've tried salting with FASW, but HCl seems to be better. You can check here

I was FASAing the dmt out of the xylene with acetone but it got expensive with all the acetone because i would have to evaporate that off the xylene and re-use the xylene. So now i am backsalting -> reducing -> cooling -> basifying -> drying -> acetone -> FASA -> DMT-fumarate.

Your procedure is similar to my procedure

Fascinating, do you think the FASW method would work with xylene instead of tolune? I don't see why not hey?

I never even considered this as I thought fumaric acid wasn't that solubule in straight water.

If I had say a fair amount of DMT dissolved in the xylene and didn't know what quantities. Then could I add fumaric acid in to the xylene/water soup IN EXCESS and let it sink to the bottom before mixing it so that I make sure I react all of it? Or will it do the same thing as it does where you put FASA in xylene and the acetone combines with the xylene and doesn't dissolve anymore unreacted fumaric acid that may be lurking in the bottom so you just have to keep adding more FASA to precipitate the DMT in the xylene.

 

[pete666]

Fascinating, do you think the FASW method would work with xylene instead of tolune? I don't see why not hey?

I never even considered this as I thought fumaric acid wasn't that solubule in straight water.

If I had say a fair amount of DMT dissolved in the xylene and didn't know what quantities. Then could I add fumaric acid in to the xylene/water soup IN EXCESS and let it sink to the bottom before mixing it so that I make sure I react all of it? Or will it do the same thing as it does where you put FASA in xylene and the acetone combines with the xylene and doesn't dissolve anymore unreacted fumaric acid that may be lurking in the bottom so you just have to keep adding more FASA to precipitate the DMT in the xylene.

I think it would work. Excessive fumaric acid has to be removed from the evaporated result though.
But I would't use this route. As you can read there were some problems with FASW and toluene. Generally it worked, but it was not as good as salting with HCl. I just gave it only one try though, I might have done some mistake so it is still open. The main reason for not continuing with this approach is the fact that result has to be evaporated and even with precise titration (so there is not excessive fumaric acid in the result), it is very difficult to work with the result. Crystallization from water is giving much worse result than precipitation when doing FASA on freebase. Scraping evaporated fumarates is a nightmare for me.
Another reason is the purity of the result. It is very difficult to purify fumarate. So this is why I salt with HCl and basify for pulling/re-x by heptane and then doing FASA with freebase