Re-X Help

[NikkiPotnick1981]

Hello all. I need some guidance on a my Re-x technique

I have done this before with success, but it was some time ago and I kinda forget. Also, apologies, Im having a hard time navigating the search function on the site.

Process:

- I give a heat bath to 50ml of naphtha in a small beaker

- I then dump 1/2 gram of dmt into the warm naphtha

- I swirl the dissolved dmt/naphtha around for 30 seconds, thus separating the impurities

- once the impurities settle into the bottom of the beaker, I stick in the freezer for 45 mins

- due to the short freeze the impurities should stick to the bottom of the beaker

- after the 45 mins I remove beaker from freezer and then dump the dmt/naphtha into my pyrex dish

- I wrapped the pyrex and stick in the freezer for 18 hours

- next day remove pyrex, scrape and weigh


Any issues with this technique?

Thanks all

 

[AcaciaConfusedYah]

Hey NikkiPotnick1981,

That could be ok - though maybe a few minor adjustments.

Heat as much naphtha (safely, and not anywhere near an open flame) as you want - but, You may not need all of it.

I'd only add as much heated naphtha as it takes to dissolve the DMT. A more saturated solution will likely be easier to retrieve the most goods via the precipitation.

So, instead of dumping the DMT into the beaker; place the DMT in a separate beaker and slowly add the solvent, while stirring, until dissolved. A little extra won't hurt, but may not be needed. (I'd try to use as little as possible.)

If there are solids that are remaining after the DMT has fully dissolved, and they appear to be impurities, then I would suggest vacuum filtration to remove the solids. If you don't have the setup - then yeah, allow it to settle and then decant the solution from the solids and then freeze precipitate.

Take Care,
ACY

 

[NikkiPotnick1981]

Thanks so much. Made me feel better!

I love that I can use as much naphtha as needed to dissolve the DMT. I have been wasting a lot. I have a lot of yellow naphtha now stored away. Perhaps you know how to clean this? I heard we can decant it to bring it back to clean.

Im not sure if its necessary to clean the naphtha. But I notice when I reuse the yellow naphtha it doesn't separate as easily and makes it much harder to pull without getting impurities.

Thanks friend!

 

[AcaciaConfusedYah]

Thanks so much. Made me feel better!

I love that I can use as much naphtha as needed to dissolve the DMT. I have been wasting a lot. I have a lot of yellow naphtha now stored away. Perhaps you know how to clean this? I heard we can decant it to bring it back to clean.

Im not sure if its necessary to clean the naphtha. But I notice when I reuse the yellow naphtha it doesn't separate as easily and makes it much harder to pull without getting impurities.

Thanks friend!

Oh shoot! Thanks for reminding me! I've been meaning to post a pictorial guide that shows my method of reclaiming solvent without the equipment that would be used in a lab setting. Someone else asked about this same thing earlier this week; and I said I'd put together an easy guide.

We're in the process of clearing our home and packing for a relocation - so things have been busy. I have old solvent that needs to be cleaned and returned to its original container so that it can be transported or disposed.

I'll see if I can swing it, tonight, and maybe get the guide posted. I'll post the link to the thread once it has been created.

Take Care!
ACY

 

[AcaciaConfusedYah]

Procedure for Reclaiming Used Non-Polar Organic Solvents

This procedure is very simple. In fact, writing it out likely complicates it more than anything. The quantity of materials will be arbitrary and can be adjusted to suit your needs - scale as needed.


Materials:
Used non-polar solvent
Old pickle jar with HDPE film underneath the lid (make sure the lid will seal completely)
Deionized or distilled water
Sodium carbonate
Seachem Matrix Carbon
Glass Pipette or Glass Syringe
Old solvent container (Storage of the freshly cleaned solvent)

Safety:
Goggles
Gloves
Long pants
Closed toed shoes



Method:

1. First, decide how much solvent needs to be cleaned. A large volume can be cleaned in smaller batches or in a larger single batch. The primary confliction of a larger scale will be finding the appropriate size jar. If the total volume of the jar is 1000 mL, then that is fine. If it is 500 mL, that is fine. Pick a jar that is appropriate for your volume. For the sake of this experiment, the volume will be 1000 mL.
2. Saturate some of the deionized/distilled water with sodium carbonate. If the water is not saturated, that is ok.
3. The Seachem Matrix Carbon is a spherical activated carbon product sold for aquariums. The spherical shape of the carbon increases surface area. High amounts of surface area means that you can effectively remove the discoloration and fats, while using less of the activated carbon.
a. Depending on the amount of solvent that needs to be cleaned, choose a quantity of Seachem Matrix Carbon and rinse it with tap water. Rinsing the carbon removed the carbon dust that results from the spheres grinding against each other during shipping.
b. I usually use between 1/8th to 1/4th cup of Seachem Matrix Carbon for a 1000 mL jar.
4. After thorough rinsing, place the carbon in the jar.
5. Using the sodium carbonate solution, fill the jar until roughly 1/3 to 1/2 full. (including the carbon). **If the water begins to turn black, then the carbon was not rinsed well enough**
a. You can fill it with more or less water – as mentioned in the beginning, many quantities are arbitrary.
6. Once the sodium carbonate solution and carbon are added to the jar, some of the carbon might float – that’s ok. Some will sink - that’s ok, too. Add the non-polar solvent.
7. Shake vigorously, as long as needed, until the non-polar solvent is colorless.
a. Allow some time for the layers to separate and verify that the solvent is the desired color.
8. After separation has finished, decant the non-polar solvent and store it in the original container.



Essentially, that’s it. You can take it further if you’d like. Some folks may want to use a drying agent, such as anhydrous magnesium sulfate or anhydrous sodium sulfate, to dry the solvent before returning it to the storage container.

 

[NikkiPotnick1981]

Wow acacia! great write up thank a lot. Looks like I'll have to find some of these materials.

Hey a bit of a snafu with my rex. I re-x'd 500mg as a tester and lost half of it. Its crazy to think that I lost half of the weight.

So I then re-x'd 1.5g all at once and I froze it over night... however There is minimal crystal. Looks like I lost 90% of my dmt.

What could've went wrong?

I placed the pyrex in the freezer about 8pm 2 nights ago. I did face a power outage at 1:30am until around 3pm the next day. I didnt open my freezer once so I didnt think it would be a huge deal. I removed last night to check, and minimal crystal. So I left it to freeze one more night. Pulled it out today and till hardly any crystal?

What might I be doing wrong???

I feel like I lost all my previous extracted dmt. Bummer

Maybe I'll leave outside to evaporate. If that doesn't work I guess I never had much dmt to begin with. Which is strange bcause I have the same bark and materials that I've always used with great success. And the dmt I was purifying looked overall really nice. Just some spots of base material I wanted to clean.

 

[AcaciaConfusedYah]

Hmmm. That is really odd. Precipitation should be dependent on solubility, which is dependent on temperature.

Can you identify how you are getting base soup in the precipitation dish? Sometimes, I'll collect a pull and then transfer it to a beaker, or jar; allowing any water to settle on the bottom. Due to water having an affinity to the glass, the solvent can usually be decanted with little (usually none that is visually noticeable) base-soup making it into the precipitation tray.

I'm not sure why you're having such loss. I generally avoid the evaporation method, but others seem to find it useful. Unfortunately, the solvents that I prefer are no longer offered at the large box-stores. So, I'm limited to online ordering (nah, too sketchy for me) or hoping that the smaller hardware stores still stock the desired solvent. OR I have to reclaim the solvent.


Hopefully you'll get it figured out!

Take care,
ACY

 

[NikkiPotnick1981]

my pulling technique has become pretty good. So im not pulling much base material globs. But its almost as if the base material is bleeding into the naphtha/dmt during separation process.

Im not getting as good as a clear crisp separation as I once did. So my pulls are picking up bleeding base material whereas before I'd get strictly naphtha with suspended dmt.

Im not sure why the reaction is not as black and white as before. Im using the same materials as I always did. Only I havent extracted In 6 months. Can age of materials really affect the seperation so much.

Maybe my rolling technique has been lacking and im getting issues there?

Anyhow, im drying this now and I see clearly there is DMT but its so fine! Ive always had moderately larger crystals before. This looks like a fog all over the bottom of my pyrex. Fingers crossed I didnt lose too much. I'lll let you know the weight difference from before and after

 

[AcaciaConfusedYah]

You used all the same materials? Same solvent as well? I ask because I am wondering if the solvent companies have begun to add something that would cause this effect.

I haven't purchased naphtha in a while, so I'm not sure if they've changed the blend.

Have you done an evap test on the solvent to see if there is any residue?


Take Care,
ACY

 

[NikkiPotnick1981]

I only ever had 1 gallon of naphtha. Still using it.

I tried the evap test on my cook top. It leaves minimal evidence however Im not sure if that is residue or just a clean spot on a cook top lol. I believe there is a tiny amount of residue since I cleaned it before I tested.

Its V.M.P Naphtha
Reducer #3

Whatever that is.

 

[AcaciaConfusedYah]

Ah, gotchya. I don't know how "Reducer #3" plays a role. In chemistry, a reducer would imply that there is something added that would become oxidized. Unfortunately, I could not find any information regarding "Reducer #3" in relation to naphtha. It could mean a variety of things, pending on the context. Maybe it implies that the naphtha "reduces" (the "thickness" of) paint. (It is often sold for painting applications.)

I found the SDS of a few different brands of V.M. & P Naphtha. They imply that the contents are between 95-100% "light" naphtha.

Well. Hopefully it'll all come together.

Take care!
ACY