Newbie to Extraction

[CelestialDragon]

Hi I'm new to extracting and I have run into an issue. I don't know all the "tech" talk but I ran an Acetic Acid and NaOH extraction with 50g MHRB. I could have trimmed down the aqueous to have a higher concentration of salts in my solution but grand scheme I was able to pull into naphtha. The problem I ran into was once my extract was in the naph. I tried freezing on my freezers lowest setting but I didn't have crystal formation. This could have been because I was checking on it too often I checked on it and moved and opened the container about 10 hours after it was in the freezer. I ended up loosing that extraction to condensation freezing on my glassware and water eventually getting into the naph. The next thing I tried was evaporating and freezing then repeating. This gave decent results. I would blow on the naph and a white precipitate would form and not dissolve back into the naph or melt. I lost this one to condensation freezing on my glass and water getting into the naph again. I did a 3rd pull on my aqueous and am just evaporating it. I don't expect much of anything from it im just trying to get anything to work. So far there are very small slightly brown "oily" spots that have formed. I plan on doing another extraction soon with 100g MHRB. If anyone has advice on how to get the extract out please do help. I live in a place with high humidity so if that's of any consideration

 

[blig-blug]

As you say, it seems like the main issue is humidity. I'm not too sure how to deal better with it because I don't live somewhere with very high humidity. What I do want to say is, if you get water into you naphtha, it's not lost! Don't throw it away. You can wash the naphtha and then pull again from the DMT containing water.
In general, an extraction is not lost until you throw something away, so it's better to keep everything around until the end.

 

[TransistorBass]

And remember even a bit of condensation will dry off when it comes out of the freezer given time and maybe a fan.

 

[CelestialDragon]

And remember even a bit of condensation will dry off when it comes out of the freezer given time and maybe a fan.

When I put the naph in the freezer the freebase didn't crash out in a way that I could harvest it. I did get a film at the bottom that looked like frosted glass and there were some filaments floating in the naph that were extremely delicate making pouring off the naph difficult. I'm thinking I got the results I did with freezing cause the concentration of freebase in the naph was low, however I also didn't get anything to crash out into a harvestable crystal when evaporating about 1/2 the naph then freezing after combining the naph with a second pull cause I did re-use as much of that first pull as possible (I lost some here and there to small experiments). This is where I found that if I take the naph out of the freezer then blow on it a white cloud would for and later coalesce into a small white granule. I got the most discernable results with freezing then evaporating but I don't want to rely on that strategy because of the humidity so I'm wondering if there is any temperature my freezer should be at or if I should consider looking into a different tech.

 

[CelestialDragon]

As you say, it seems like the main issue is humidity. I'm not too sure how to deal better with it because I don't live somewhere with very high humidity. What I do want to say is, if you get water into you naphtha, it's not lost! Don't throw it away. You can wash the naphtha and then pull again from the DMT containing water.
In general, an extraction is not lost until you throw something away, so it's better to keep everything around until the end.

yeah sadly I did loose this whole extraction trying to save what I could.

 

[BraveLilToaster]

Condensation isn’t a big deal at all. If you take it out of the freezer, let it warm to room temp before opening it to avoid more condensation. You can then pipette off the naphtha in to a clean dish/jar. If your naphtha isn’t saturated enough, evaporate some more. Then seal it really well. Some people use foil or plastic wrap before clamping the lid on to ensure an airtight seal. I personally like to use quarter pint wide mouth canning jars. I have thin ptfe squares I cut and place the ptfe on first, then the canning lid top with the gasket then the threaded ring really tight so the crinkled edges of the ptfe won’t let air in. Then I place the whole jar in a ziplock back that I suck all the air out of before closing. Then I throw that in the back of the freezer next to where the cold air enters the freezer.
When I decide it’s cold enough ~-20C with my infrared thermometer, I quickly take it out open it up and if there aren’t any floating crystals I just decant my solvent quickly and immediately close the jar again with the ptfe covering the lid and put it back in the freezer upside down. Wait 15 to 20 minutes for the rest of the solvent to drip off the crystals in to the lid. Remove from the freezer and keep it upside down so the solvent is on the lid instead of on the spice. let it reach room temp before opening it(the point of this is to avoid condensation forming inside the container) and finally I place it upside down on a grate that my air purifier fan blows upwards to make the crystals as dry as possible and solvent-less. Basically minimize the amount of time your container is open whenever the contents is colder than your environment because that’s what causes condensation formation, assuming your container is air tight and sealed properly, of course.
Depending on how old your solvent is and how long it has been left open in its life, it may have absorbed quite a bit of water from the air. You can try drying your solvent with anhydrous magnesium sulfate(baked Epsom salt). I usually throw a good amount in the bottom of my naphtha jug the first time I open it so I won’t have to worry about it in the future.

 

[Transform]

Yes, using a precipitation container with a lid is essential in general, as much to avoid naphtha fumes getting into your freezer as keeping out the moisture.

Working in front of a dehumidifier - especially if the output air stream can be confined to your work area - might also be helpful.

 

[blig-blug]

Working in front of a dehumidifier

Is there any risk of solvent fumes condensing inside the dehumidifier?

 

[Transform]

Is there any risk of solvent fumes condensing inside the dehumidifier?

How long are you planning to stand in front of the humidifier? There shouldn't be all that much vapour coming off freezing cold naphtha in the time it takes to pour it off the crystals. But, yes - make sure you move the naphtha away from the any electrical apparatus ASAP, and keep it in a tightly sealed container. The risk of electrostatic discharges should be fairly minimal if it's humid enough to necessitate the use of a dehumidifier. And do ensure that the fumes blown away by the dehumidifier aren't allowed to accumulate in an enclosed space since you'd be kind of doing things the opposite way around compared to a fume hood.

In fact, if you don't understand the safety implications of this don't work with a flammable solvent in the proximity of electrical apparatus at all.

 

[blig-blug]

How long are you planning to stand in front of the humidifier?

It was just hypothetical, I don't plan on doing it but I wanted to know in case some day I need it. Thank you for the safety pointers.

In fact, if you don't understand the safety implications of this don't work with a flammable solvent in the proximity of electrical apparatus at all.

Yes, that's what I have been doing so far.

 

[Transform]

It was just hypothetical, I don't plan on doing it but I wanted to know in case some day I need it. Thank you for the safety pointers.


Yes, that's what I have been doing so far.

Ah, therein lie the flaws of the English language having done away with certain aspects of grammar, and the commonplace use of "you" where in fact "one" would make for a clearer meaning. My initial question was at least partly rhetorical, and further parts of my reply were directed towards a more general audience. But yeah, still a very valid and thoughtful question that you made.