Q21Q21 Recovery Help (Calcium Chloride :( )

[relent]

Hey all,

Following Q21's tek for the first time, I soaked 100g of MHRB in distilled vinegar overnight, added it to a 5qt pot with 100ml of distilled water and reduced it to a thick, soupy consistency. I then proceeded to add the "pickling lime" I had picked up, roughly 80g thereof, immediately noticing the very small fine print which stated:
"CONTAINS: Calcium Chloride"

Expletives were sounded, and now I'm here, wondering if this batch is at all recoverable. Will the Calcium Chloride interfere with basification or the end product if I can find calcium hydroxide on short notice? Or should I throw the whole batch out and start over?

If any of our resident chemists could offer their opinion, I'd appreciate it. It's my understanding that Calcium Chloride does NOT raise pH.

Moral of the story: Read labels thoroughly, take nothing for granted.

R

 

[Vodsel]

To help our real resident chemists show up and whack my ass, I will offer my amateur chemist two cents as a bump.

Calcium Chloride is a salt, so as you say it shouldn't alter the pH of your mix. However, in aqueous solution it appears to be slightly basic (don't ask me why, in my chemical fact sheet it appears with an acidity of 8-9 in solution). It is also quite more soluble in water than Calcium Hydroxide.

Now - speculations ahead: I'd say the acetates in your mix are perfectly fine, and that you just slightly increased the pH of the mix. Also, solvents in your mix are pretty more saturated (CaCl2 is very soluble in both water and acetic acid). I'd say you still can add Ca(OH)2 to basify, but probably you need to compensate for the salt added with more water/vinegar before basifying properly.

Someone correct me, please.

 

[Electric Kool-Aid]

I am interested in this too!
because someone said adding salt to the mix will bring the spice out.
so maybe this will be the best of both worlds! just add sodium carbonate and boost up the ph.
please dont quote me on that! chems isnt my thang.

 

[relent]

To help our real resident chemists show up and whack my ass, I will offer my amateur chemist two cents as a bump.

Calcium Chloride is a salt, so as you say it shouldn't alter the pH of your mix. However, in aqueous solution it appears to be slightly basic (don't ask me why, in my chemical fact sheet it appears with an acidity of 8-9 in solution). It is also quite more soluble in water than Calcium Hydroxide.

Now - speculations ahead: I'd say the acetates in your mix are perfectly fine, and that you just slightly increased the pH of the mix. Also, solvents in your mix are pretty more saturated (CaCl2 is very soluble in both water and acetic acid). I'd say you still can add Ca(OH)2 to basify, but probably you need to compensate for the salt added with more water/vinegar before basifying properly.

Someone correct me, please.

Vodsel.
I am with you for the most part. CaCl2 is a salt, pH wasn't the worry so much as screwing up the acetates or unsavory reactions down the line (be it with Ca(OH)2 or naphtha).

Adding more vinegar and reducing a second time is fine, assuming that's the next logical step. Though my understanding is that CaCl2 would be soaking up the excess water/vinegar(?), so adding more may not even be necessary except as a precaution?

Either way. Right now I have the slurry in a sealed jar in the back of the fridge until I can pick up some Ca(OH)2 tomorrow, assuming I can find it. All we have nearby are hardware stores and Indian groceries. We shall see! It may be interesting to complete the extraction just to see what happens.

 

[relent]

Update. After adding roughly 100g of Ca(OH)2 (verified), my crumbly mixture became the cosnistency it was supposed to, but was black/ashy and very smelly. Did my first pull, we'll see how it goes.

 

[Vodsel]

The usual rootbark-vinegar-Ca(OH)2 mix has a slightly reddish-grey color at first, and once stirred and exposed to air acquires an ashy-grey color in the surface. The darker color is probably because of the chloride (I'm guessing since it's the only difference in your extraction). Also, there is a characteristic smell after adding in the lime.

I assume you pulled solvent and are attempting now FP. Let us know how it goes when you wake up.

 

[relent]

Morning report.

First pull is still in the freezer, a very clouded solution with what doesn't appear to be much crystals at all on the bottom. While there's disappointment with yield, at least it wasn't a complete loss!
Used a heated naphtha soak for approximately 30 minutes, followed by another hour heating the naphtha for evaporation (which did not occur...).
If the solution is still a very dense cloudy white, is there still compounds precipitating out? A probable complicating issue is that this is 200ml of naphtha in a quart Ball mason jar. If this evening there has been no increased yield and the naphtha is still cloudy, may need to figure out a way to evaporate the solvent and try again.

Second pull will need to use significantly less solvent, and that may help matters. Something broad and flat like a glass baking dish is available, but there is no way to cover it except saran wrap, which with using Naphtha seems less than ideal. May need to find a better solution than a glass jar.

Updates tonight. Suggestions welcome.

R

 

[Vodsel]

Cloudy is good. I've seen solvent getting cloudy within twenty minutes of being placed in the freezer... if it takes much longer than that, it's because it's less saturated. Either that, or your freezer is not too cold. Just leave it there for at least six hours and check again, if all is well the cloudiness should slowly disappear leaving precipitate in the bottom and/or floating crystals in the top layer.

200ml sounds like a lot of solvent for just one pull, but wait and see how it goes. However, the only weak spot of this tek IMO is that it might not be particularly solvent efficient. And in your case, I don't know if the presence of calcium chloride in the mix will increase the solvent absorption. Are those 200ml the same amount you added to the mix, or have you noticed solvent loss after pulling?

If it does not precipitate properly, evaporating is as simple as leaving the jar open for a while, with a little air flow on top if you want to speed it up. Flame-free heat will also make it go faster but it's not needed.

And mason jars (I like particularly the ones with a rubber ring below the lid) work fine, as long as the inside is smooth enough to scrape the obtained crystals. I did not scrape, though... I used a little paint brush to scoop everything, and then wash the insides of the jar with a little solvent, to recover the stuck traces of crystals, then use that solvent in the next pulls. Whatever container you use, glass or pyrex are best IMO, make sure it closes tight.

 

[relent]

Next update.

Last evening was punctuated by a still extremely cloudy/milky solution with minimal crystals having actually formed, as though the rest had failed to entirely fall out of solution.

1. Warmed up the first pull, proceeded to evaporate from 200ml to 100ml soln.
2. During this time did another pull with significantly less solvent (50ml).
3. Noticing a definite "wetness"/clumpiness (not a crumbliness) to the root bark, the mixture and 100ml of distilled water were added to a pan and cooked down again to a crier consistency, though not bone dry, for a future third pull if these two go well.

As of this AM T-8hrs of freezing for both pulls, the larger first pull has an almost salt-like cloud in solution though little has actually dropped out or adhered anywhere inside the jar. The second pull is much less opaque but still looks promising. Further evaporation of the first pull may be necessary.

PROBLEM: A very small amount of water had settled into and frozen in the bottom of the first pull, along with a negligible amount of dust from the evaporation process (no decent cover ). A problem?

 

[Vodsel]

PROBLEM: A very small amount of water had settled into and frozen in the bottom of the first pull, along with a negligible amount of dust from the evaporation process (no decent cover ). A problem?

I have no experience in dealing with water/ice drops inside of the solvent, but this thread might help.

And as long as it's cloudy, goodies are there. If there's no precipitation after 6-8 hours, just evaporate more. 200 ml was indeed a lot, I just re-checked and saw you used 100g of root bark. That amount suggests around 50 ml solvent per pull. Otherwise you will need to evap a lot and waste too much solvent.

 

[relent]

Cliffnotes:

First and second pulls had small crystal formations, so despite a very low yield, it seems to have been successful. I decanted the naphtha for further evaporation and more freezing. What I could scrape out of the first-pull jar was placed in a vial, and then a few ml of heated naphtha was added to it, swished around until the stuck waxy crystals were dissolved, and poured into the vial immediately resulting in a very dense/cloudy solution. This was put in the freezer.
The second pull jar is still drying to see if the waxiness was an issue of lack of evaporation.

Meanwhile a small square of paper towel pulled apart into a single thin layer was used as a filter during decanting. This was dried and scraped into a shotglass, with a total crystalline yield approaching that of each jar. A small bit of the decanted naphtha was warmed, added, mixed, and set to freeze along with the vial.

The decanted naphtha seems to still contain a good deal of goodies, being somewhere around 150ml (only able to evap the 200ml first pull to 100ml after hours and a hot bath. This has largely complicated the whole process. Second pull was around 50ml). This will be reduced as much as possible and allowed to freeze.

Meanwhile another 100g batch is sitting in 100ml 3%vinegar and 75ml of dh2o in an HDPE2 jug; originally I was only working with mason jars and stainless steel pots, which made pouring (solvent or otherwise) extremely messy and unreliable. I'll be posting in the proper section soon regarding sources of glassware/lab equipment, since I would like to be more analytical in future extractions instead of MacGyvering everything.

I'll conduct a more normal Q21 tek with this next batch and compare results. A third batch will be done utilizing the recent salting method (properly), but perhaps a smaller amount of mhrb.

Things I've learned so far:
**Quart Mason jars are excellent containers for mixing the slurry of vinegar/lime/mhrb, but terrible for reducing the mix if needed (water bath), drytek sticks, and pouring off solvent runs down the side resulting in a significant loss. The lids contain BPA and can't be used with solvent.
They're also atrocious for freeze precip/evaporation due to again an inability to poor off the solvent through a filter accurately, and scraping up the remnants proved more difficult than anticipated. Might get more shotglasses or a more proper recrystallization dish. Glass baking dishes are fine but I have no lids.

**Something to measure out solvents is a must. Even pouring from the can is messy, so a glass syringe/baster is a must.

**Fan evap seemed must more efficient than a heated bath, but caused some dust debris in the final product. Considering I have some left over, calcium chloride acts as a dessicant. Perhaps a glass container (or large lidded pot) would be good to place the precip container in, with CaCl2 to draw out mousture. Solvent may not be drawn but should still evaporate readily.