Jan e Kharabat
Established member
I thought about writing a separate post since benzoic acid has not received much attention so far. The greatest benefit of benzoic acid is that it can be used to detect the presence of even very minute amounts of DMT in the NPS. It also allows one to complete the extraction in a single day by salting out each pull consecutively. This also reduces the amount of NPS one has to use since you no longer need to freeze precipitate every pull separately. You can also perform an entire extraction in one sitting.
I'll write my preferred method but you can change a few things if you like, such as skipping the freeze/thaw step or going straight to base. Also, I don't think I write in a very organized manner, so please feel free to rewrite this and tidy it up if you can. So here's the Tek:
1- powder your bark as fine as possible, pass it through a sieve and do multiple runs if you have to.
2- add the bark powder in a sufficiently large borosilicate glass bottle, add enough water to cover the powder, add some citric or acetic acid, or HCl if you like, check with a pH strip If the pH is below 3.
3- leave the bottle in the freezer overnight. Take it out and leave it to thaw in the morning. Repeat this process at least 3-4 times.
4- now add in NaOH, I usually just eyeball it so... Can't tell the exact amount. But I try to use as little as possible. One method I found useful was to add until the pH reaches 14, then add naphtha and shake. If it doesn't separate well, add some more and shake again. The right amount of NaOH is that which let's the layers separate somewhat neatly within 15 minutes.
5- if you haven't added naphtha to the bark soup already, add it and then shake, let the layers separate, shake again, repeat a couple of times.
6- prepare a saturated solution of benzoic acid (henceforth BA) in 100-200ml naphtha in a separate bottle. I use a small 250ml borosilicate bottle. You can also warm the bottle to allow more of BA to dissolve.
7- pull the naphtha out of the bark soup bottle and into a 400-500ml beaker or any large enough glass container.
8- add the BA solution and stir. White clouds of DMT benzoate will appear and upon stirring, DMT benzoate will quickly crash out and settle at the bottom. You can do it over a magnetic stirrer if you have one, or just stir manually and keep adding the BA solution to see if more clouding appears. Add smaller amounts by the end when the clouds become fainter so that you don't have too much excess BA in the naphtha by the end. Stop when no more clouding occurs upon adding BA solution
9- let the solution sit for a while, 15-30 minutes ought to be enough.
10- put some of the naphtha from the beaker back into the bark soup bottle and some into the BA solution bottle (just to keep the equilibrium), use filter papers as the DMT benzoate is very fine. The naphtha poured back in the bark soup bottle will likely turn milky, but that is just excess benzoic acid reacting with NaOH. Just shake a couple of times and it will clear up.
11- make the next pull the same way, add BA solution to your pull to crash out the DMT benzoate, then pour the exhausted naphtha back into bark soup bottle through a filter paper.
12- you can separately weigh the DMT benzoate from each pull, or you weigh it together after 6-7 pulls. After that, clean up the beaker, dissolve all the DMT benzoate stuck to the walls of the beaker in hot water, it will take a while. Pour that water into another container and keep it aside.
13- pull again and see how much DMT benzoate crashes out, if the amount is too little, you can either stop extracting or pour the naphtha back into the bottle and leave it for a week or so. After a week, you can pull again and see if enough DMT benzoate crashes out. If it does, leave for another week and repeat.
14- collect all the DMT benzoate, dissolve it in hot water, add it to the container you set aside after cleaning the beaker. You should have all your DMT benzoate in a single aqueous solution in one container, let's call it the mini A/B container
15- add sufficient amount of NaOH to the DMT benzoate solution and pull with small amounts of naphtha until the solution is clear and the DMT swimming on top of the aqueous layer is gone. Collect all the pulls and freeze precipitate.
16- you can check if there's still any DMT left in the mini A/B container by making another pull, and adding a few drops of BA solution. If there's even a few milligrams in there, the solution will turn cloudy. If sufficient amount of DMT benzoate crashes out, dissolve it in water, add it back to the mini A/B container and pull again.
17- Alternatively, you can also perform a dry conversion tek, mix your DMT benzoate with sufficient amount of sodium carbonate, moisten the mixture, let it dry, then pull with small amounts of dry acetone and evap the acetone. The extract obtained in the end can easily be redissolved in hot naphtha and recrystalized, that way you can avoid the mini A/B.
This way, you can control and measure multiple things, the amount per pull, difference between warm and room temp pulls, difference between clean and reused naphtha, number of pulls and amount of NPS needed for the mini A/B step etc. And that too, without having to wait for freeze precipitation of several individual pulls. You can simply collect all the benzoate, weigh it and calculate the amount of freebase.
Benzoic acid can be easily made from sodium benzoate. Simply dissolve sodium benzoate in hot water and add HCl and benzoic acid will crash out immediately. You can calculate the amount of HCl needed for this reaction, but I'm too lazy to do that, so I just eyeball it, then filter out the left over water, add some more HCl to it and see if anything crashes out. The benzoic acid can further be purified by recrystallization from boiling water. Simply dissolve it in boiling water, let it rest and cool down over night, pour out the water, collect and wash the BA crystals with small amounts of cold water and dry them.
I'll write my preferred method but you can change a few things if you like, such as skipping the freeze/thaw step or going straight to base. Also, I don't think I write in a very organized manner, so please feel free to rewrite this and tidy it up if you can. So here's the Tek:
1- powder your bark as fine as possible, pass it through a sieve and do multiple runs if you have to.
2- add the bark powder in a sufficiently large borosilicate glass bottle, add enough water to cover the powder, add some citric or acetic acid, or HCl if you like, check with a pH strip If the pH is below 3.
3- leave the bottle in the freezer overnight. Take it out and leave it to thaw in the morning. Repeat this process at least 3-4 times.
4- now add in NaOH, I usually just eyeball it so... Can't tell the exact amount. But I try to use as little as possible. One method I found useful was to add until the pH reaches 14, then add naphtha and shake. If it doesn't separate well, add some more and shake again. The right amount of NaOH is that which let's the layers separate somewhat neatly within 15 minutes.
5- if you haven't added naphtha to the bark soup already, add it and then shake, let the layers separate, shake again, repeat a couple of times.
6- prepare a saturated solution of benzoic acid (henceforth BA) in 100-200ml naphtha in a separate bottle. I use a small 250ml borosilicate bottle. You can also warm the bottle to allow more of BA to dissolve.
7- pull the naphtha out of the bark soup bottle and into a 400-500ml beaker or any large enough glass container.
8- add the BA solution and stir. White clouds of DMT benzoate will appear and upon stirring, DMT benzoate will quickly crash out and settle at the bottom. You can do it over a magnetic stirrer if you have one, or just stir manually and keep adding the BA solution to see if more clouding appears. Add smaller amounts by the end when the clouds become fainter so that you don't have too much excess BA in the naphtha by the end. Stop when no more clouding occurs upon adding BA solution
9- let the solution sit for a while, 15-30 minutes ought to be enough.
10- put some of the naphtha from the beaker back into the bark soup bottle and some into the BA solution bottle (just to keep the equilibrium), use filter papers as the DMT benzoate is very fine. The naphtha poured back in the bark soup bottle will likely turn milky, but that is just excess benzoic acid reacting with NaOH. Just shake a couple of times and it will clear up.
11- make the next pull the same way, add BA solution to your pull to crash out the DMT benzoate, then pour the exhausted naphtha back into bark soup bottle through a filter paper.
12- you can separately weigh the DMT benzoate from each pull, or you weigh it together after 6-7 pulls. After that, clean up the beaker, dissolve all the DMT benzoate stuck to the walls of the beaker in hot water, it will take a while. Pour that water into another container and keep it aside.
13- pull again and see how much DMT benzoate crashes out, if the amount is too little, you can either stop extracting or pour the naphtha back into the bottle and leave it for a week or so. After a week, you can pull again and see if enough DMT benzoate crashes out. If it does, leave for another week and repeat.
14- collect all the DMT benzoate, dissolve it in hot water, add it to the container you set aside after cleaning the beaker. You should have all your DMT benzoate in a single aqueous solution in one container, let's call it the mini A/B container
15- add sufficient amount of NaOH to the DMT benzoate solution and pull with small amounts of naphtha until the solution is clear and the DMT swimming on top of the aqueous layer is gone. Collect all the pulls and freeze precipitate.
16- you can check if there's still any DMT left in the mini A/B container by making another pull, and adding a few drops of BA solution. If there's even a few milligrams in there, the solution will turn cloudy. If sufficient amount of DMT benzoate crashes out, dissolve it in water, add it back to the mini A/B container and pull again.
17- Alternatively, you can also perform a dry conversion tek, mix your DMT benzoate with sufficient amount of sodium carbonate, moisten the mixture, let it dry, then pull with small amounts of dry acetone and evap the acetone. The extract obtained in the end can easily be redissolved in hot naphtha and recrystalized, that way you can avoid the mini A/B.
This way, you can control and measure multiple things, the amount per pull, difference between warm and room temp pulls, difference between clean and reused naphtha, number of pulls and amount of NPS needed for the mini A/B step etc. And that too, without having to wait for freeze precipitation of several individual pulls. You can simply collect all the benzoate, weigh it and calculate the amount of freebase.
Benzoic acid can be easily made from sodium benzoate. Simply dissolve sodium benzoate in hot water and add HCl and benzoic acid will crash out immediately. You can calculate the amount of HCl needed for this reaction, but I'm too lazy to do that, so I just eyeball it, then filter out the left over water, add some more HCl to it and see if anything crashes out. The benzoic acid can further be purified by recrystallization from boiling water. Simply dissolve it in boiling water, let it rest and cool down over night, pour out the water, collect and wash the BA crystals with small amounts of cold water and dry them.
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