Freebasing DPT HCl, plan and questions

[m3dt34ch]

I have just bought 0.5g DPT HCl, and have made a plan for freebasing it. Looking for feedback, should this go well?

Ingredients:

• 500mg DPT HCl~
• 94.4mg Na2CO3~
• 5-10ml Acetone
• trace DI water

Equipment:

• Shot glass
• Pipette
• Stirrer
• Microwave
• Funnel
• Small filter paper
• Storage vessel (10ml aluminium pot)
• Tray/Grate
• Boiling water
• Fan (optional)

Plan:

1. To a shotglass, add 94.4mg Na2CO3~
2. Add 0.89ml DI water for 1.0 M
   Mix/agitate
3. Add 500mg DPT HCl
   Mix/agitate // DPT 'oils out'
4. Emulsify into paste, leave to set and complete reaction
5. Return after an hour or so, then microwave shotglass as is until water completes evaporation
6. Add 5-10ml anhydrous acetone, stir until DPT oil is collected
   Impurities residual soda ash / formed NaCl are insoluble in acetone, leaving behind only table salt in ideal case
7. Pass through a 1" funnel / coffee filter, decanting off impurities where possible, into end storage vessel // 160mg~ nacl + excess soda ash will remain on the small filter
   // In my case, this is a short wide aluminium pot around 5-10ml
8. Fill a tray with boiling water, on a suitable support place the vessel
9. Allow to evaporate for an hour, aid with gentle airflow from fan

Ratios were worked out as described in reply, based on exactly 500mg source material i.e. 94.4mg~ Na2CO3 / 64.9mg~ HCl

Questions:
Is it crucial to aim for the weight of soda ash to be as accurate to the source material as possible? I do not want to have residual soda ash in the fully evaporated extract.
Understanding that both sodium carbonate and sodium chloride are insoluble in acetone. If the required DI water is enough, it could be pulled with that?

Also, acetone boils at 56c. Can I be assured my end product wont trap solvent? a heat bath like that should boil the shit out of acetone, right?


I think these questions are quite important, as it involves the satisfaction / effectiveness of using the result DPT oil with concentration pads of a vaporizer, I'd be worried that this method could leave any harsh caustic byproducts or acetone in the result that would fuck up a dry herb vape and your lungs.

 

[m3dt34ch]

Just adding the bits worked out for the weights/measurements, in-case that is critical or desired


The balanced chemical equation for the reaction between sodium carbonate and hydrochloric acid is: Na2CO3+2HCl→2NaCl+H2O+CO2
This makes the molar ratio requirement of base to acid 1:2
_____________________________________________________________________________________________________________________________

(A) Mass of HCl per source material * (E) Molar Mass Ratio = Mass of Na2CO3 required to basify
i.e.
A * E = Na2CO3 g
((x)g * 36.458/280.84) * 1.453590433E
^ Enter x as source weight of DPT HCl
_________________________________________________________
A = Mass of HCl per source material
A = Source Mass * (HCl Mol/g / Salt Mol/g)
A = (x)g * 36.458/280.84 = Mass of HCl per mass of DPT HCl
Change x based on recorded source material mass
_________________________________________________________
E = Mass conversion ratio given by the balanced chemical equation (1:2 1Na2CO3 2HCl)
Two moles of HCl = 72.916g/2mol
One mole of Na2CO3 = 105.99g/mol
E = 105.99 / 72.916 = 1.453590433

_____________________________________________________________________________________________________________________________

EG.
(0.5g * 36.458/280.84) * 1.453590433E = 0.09435087595g soda ash per 0.5g DPT HCl

This could then be added as a 1.0 M solution to the DPT HCl

1.0 M = mass of Na2CO3 / molar weight of Na2CO3
=
0.09435087595 / 105.99 = 0.000890186583L or 0.89ml DI water




On the concern that the amount of water used or created could carry any byproduct NaCl/unreacted soda ash to the final product,
taking 0.5g to be the exact weight of source material
64.9mg hcl + 94.4mg na2co3 = 159.3mg max possible contamination byproduct unreacted soda ash / table salt | na2co3 / nacl

Na2CO3 solubility in water 49.7g/L, NaCl solubility in water 35.9g/L
0.89ml * 0.359 = 319.51mg max solubility of NaCl in amount of DI required for 1.0 M solution
0.89ml * 0.497 = 442.33mg max solubility of Na2CO3 in amount of DI required for 1.0 M solution

QUESTION: Microwave off H2O before introducing acetone?

So if both possible byproducts are easily soluble in the amount of DI water required to make a 1.0 M base solution, my assumption this may help a proper freebase reaction.. is it possible to microwave the fully reacted mixture before extracting with acetone?

My thinking here is that this paste will still be saturated with twice the amount of water needed to dissolve all possible reaction byproducts it has just finished producing during agitation. If acetone was added now, that water would drag all the soda ash / nacl that remained still fully dissolved, straight into the solution.

The old microwave comes in here seeing as the DPT has a melting point around 175c, so all this water could be eliminated without risk of damaging the DPT freebase
Without any water to retain the suspension of NaCl / remaining soda ash, they both are insoluble in the acetone used to collect the DPT freebase.

99.8% non-anyhydrous acetone should have 20ul of water per 10ml, this could dissolve a maximum of 9.94mg soda ash, and 7.18mg nacl

Assuming soda ash weight is matched as accurately as possible to source material needs, having no excess of required would mean the only possible contamination is 7.18mg of nacl of the 160mg~ that will be made as guaranteed by the successful complete reaction. To eliminate this potential byproduct, making the acetone anhydrous by baking epsom salt- (magnesium sulphate heptahydrate)- anhydrous magnesium sulphate is acquired (250c for 2 hours). Practically, you would need 4-6g for enough surface area and efficiency to draw the water content out of 1l of 99.8% acetone, with water its major impurity. This should act as a desiccant and make it mostly anhydrous / approaching pure. From only 7.2mg of potential contamination to approaching zero. This seems like a good step to take for minimal cost, effort and risk it should be easy to add



At this point I would really love some feedback to verify this should work, or not and why. I'm so far confident this is relatively straight forward as far as chemistry goes, and by following these steps, there is no chance for impurities in an achieved final product.



Once I have gone ahead with this I'll update on results and experiences if any.

 

[Transform]

Pass through a 1" funnel / coffee filter,

You'll want a tiny filter for that small amount, or too much of it will just soak into the coffee filter. Get hold of some glass Pasteur peipettes if you haven't already, and stuff a very small wad of cotton wool down to the end of one. Then you can use that as a miniature filter for a few mL of acetone without losing so much. Residual DPT trapped in the cotton wool can be washed out with a little more acetone. Granted, a small filter disc can also be rinsed, especially if you're using suction.

If your acetone's a tad damp (it's quite hygroscopic), it may pull a little of the SC along with it, but you should be able to rinse this off with DI water once the acetone has evaporated away from the solute (hopefully mostly DPT).

Your scheme looks well enough thought out, although I've basically skim-read it and not checked the actual figures, since you appear to be well enough equipped with the faculties to do so yourself

 

[m3dt34ch]

You'll want a tiny filter for that small amount, or too much of it will just soak into the coffee filter. Get hold of some glass Pasteur peipettes if you haven't already, and stuff a very small wad of cotton wool down to the end of one. Then you can use that as a miniature filter for a few mL of acetone without losing so much. Residual DPT trapped in the cotton wool can be washed out with a little more acetone. Granted, a small filter disc can also be rinsed, especially if you're using suction.

If your acetone's a tad damp, it may pull a little of the SC along with it, but you should be able to rinse this off with DI water once the acetone has evaporated away from the solute (hopefully mostly DPT).

Your scheme looks well enough thought out, although I've basically skim-read it and not checked the actual figures, since you appear to be well enough equipped with the faculties to do so yourself

You mean I can fill one of these pipettes with the wool, then reabsorb the end acetone through that wool to wash off any salt that makes it through?

I have a 1" diameter funnel I planned on trimming a coffee filter to, barely a circle bigger than my thumb, then passing the collected acetone directly through that to the vessel, and passing a little more acetone to wash any oil through the filter

 

[Transform]

You mean I can fill one of these pipettes with the wool, then reabsorb the end acetone through that wool to wash off any salt that makes it through?

No, I mean you can stuff a tiny sub-pea-sized blob of cotton wool all the way down the pipette from the wide end, then pass the solution through that as a filter. Don't pack it too tight!

The idea is to minimise the amount of filter substrate which remnants of solution can clings onto.

Trimming coffee filter is a bit of a pain - it's best if you can cut really (impossibly) neat and accurate circles - and I find they normally tend to let fine particulates through unless you use an Aeropress filter, which is a far finer grade.

I mean, it will work the way you're planning to although you might end up with a tiny bit more SC particulates in the semi-crude isolate, along with possibly a bit more in the way of losses if you're restricted to gravity filtration.

 

[m3dt34ch]

No, I mean you can stuff a tiny sub-pea-sized blob of cotton wool all the way down the pipette from the wide end, then pass the solution through that as a filter. Don't pack it too tight!

The idea is to minimise the amount of filter substrate which remnants of solution can clings onto.

Trimming coffee filter is a bit of a pain - it's best if you can cut really (impossibly) neat and accurate circles - and I find they normally tend to let fine particulates through unless you use an Aeropress filter, which is a far finer grade.

I mean, it will work the way you're planning to although you might end up with a tiny bit more SC particulates in the semi-crude isolate, along with possibly a bit more in the way of losses if you're restricted to gravity filtration.

As in, an unplugged glass pasteur pipette, add a tiny amount of cotton wool to that

I have just ordered glass pipettes, if I stuffed whatever tiny pin of wool I can far down into one that would work more effectively at grabbing the salt? You mean blocking the path of the pipette, but not too tight, catching the first pass then rinsing off the wool is better than coffee filters ?