How did you go about recrysallizing ?

I'm glad it works for you and you yielded a gram of spice but I don't get this at all.

I'm curious, why did you "cook" the bark without acid and then freeze thaw it? Why the strange amounts like 100.7 g ietc, and strange numbers like that? Where did you come up with these volumes?

Anyway, yeah right on you got some spice out of it.

Curious, I re-x'd because some droplets of basic soup fell on the pulled naphtha

null, in the tek, the first step is the freeze/thaw, and then comes the acid cook. A bit after having done this, I read around here that is better to do the acid cook first, isn't it?
The strange amounts are there because I wote exactly what I used, for example I had to use 100g of MHRB but when I weighted it there were 100.7g, so I wrote it down in my extraction notes, so if there was any rpoblem related to the ammounts I could exactly know what was going on. The volume of water was bigger because I did not know that all the bark gets on the soup in the end, and when I was about to cook it i poured a bit of water in order to make the tiny amounts of it in the walls of the vessel to go down, so I ended with more water than necessary. Thats why also I used more acid, because I thought that as I had more water than I should, to lower the pH I would have to use more acid. I put first 60mL, then 20, and then 20 more, and I stopped when it was at pH 4.

Thank you both for replying

Yeah you got some spice anyway which is the main point. I was just wondering how you re-x'd it, since you lost so much product ?

Sorry, I didn't understand what you meant. I weighted the product, put it in a clean glass, and poured 40mL of naphtha at 55ºC. Stirred, waited until a layer formed above the naphtha, and decanted the naphtha in a clean dish, in torder to freeze precipitate it. Then, i washed with 15 mL naphtha at 55ºC the remaining layer in the glass, did the same procedure, and then repeated once more, these two last washes were put in a same dish. Freeze precipitated everything, collected crystals, and evaped remaining naphtha, which gave the golden wax.

Like null pointed out, I wouldn't recommend cooking the bark before the freeze thaw. Just freeze thaw as the first step.

When you do the freeze thaw cycles, your bark does not need to be submerged in water to burst cell walls. Just wet enough it clumps up & is thouroughly & evenly moist.

What I do is stick it in a plastic water bottle dry & then add distilled water a few ML at a time from a syringe, shaking thouroughly between adding water.

This way you do not end up with an excess of water before you start extraction.
Acid cooks, as mentioned, are best done after the freeze thaws. If you freeze with vinegar in the bark the water will freeze & most of the acetic acid will stay liquid or get semi-frozen like slurpee & just pool in one spot in the bottle.

I'm planning a side-by-side comparison with some of these variables in a coming extraction and will post my results.

I first plan to do hundred grams with the freeze thaw and then to one without and do everything else the same, and compare yields.

TY concombres , I usually do add a dash of vinegar in the water that I freeze with. I didn't know that it didn't freeze as well.

It may not matter much, but I am not sure. With mhrb, i did a side by side with cybs tek a while back & freeze thaw didn't produce a noticeable increase in yeild. Acacia seems to like holding onto the goodies a bit more though so it may be beneficial.
I also do my acid soaks in a constant heat bath at 150F for 8 hrs so that may have something to do with yeilds being high with no freeze thaws.

Also, the vinegar thing may be false, i have not tried using it with freeze thaws, but I do recall reading that freezing vinegar will essentially separate most of the acetic acid from the water, i believe it may have mentioned it forms an azeotrope at a certain percentage ala ethanol so it will never get 100% pure that way, but it is worth freezing some vinegar to see how it behaves.

Please do post your results when you do a side by side, i`m interested in seeing how each variable effects extraction but unable to extract at the moment.

I started today an extraction with a little acid soak done before the freeze thaw, as some members told me that they did it. Didn't read until now that it is unnecesary, but I expect it is not detrimental...

The rest of the procedure will be the same as before, except for the salt ammount, which I think should be a bit bigger in order to fit the total ammount of water (if i remmember well, cyb wrote that it is recommended to add 80g of salt for every litre of water).

Also, will try to improve the pulling technique... I'm thinking about dividing the total ammount of basic soup in two flasks, in order to ease the procedure (my extraction vessel is 12.5 cm wide and the naphtha layer is like 0.5 cm aprox, which makes way more difficult doing clean pulls).

I'm writing down everything involving the procedure and will post results. Thank you all for your advice!

I am waiting for another vessel to come in order to be able to do side-by-side extractions, which will be very helpful in determining which variables are better to change and which ones not, for the moment, everything I can do is to write down the procedure...

What type of vessel did you get? IMO the best option seems to be a 1L erlenmeyer flask with a ground glass joint & a ground glass stopper to fit the neck.
This way the stopper & flask are totally inert & you can carefully shake/roll rather than stir. The pyramid/cone shape of erlenmeyer makes pipetting much easier than with jars or round bottom flasks.

It is a 2L schott duran glass jar, the one in the pic has 1L capacity, but the design is exactly the same... But much more wide.

Nice

I was looking into some reagent bottles similar to that recently to store acentone after drying with MgSo4 & keep it moisture free.
When kept in a jar acetone fumes melt the rubber rings. Deffinitely do not want rubber & plasticizers in my spice

It can be a bit hard finding apprppriate vessels with glass lids/stoppers & i do not trust plastics with solvents. Compatible plastics are one thing, but caps for bottles made with obscure types of plastic are just as hard to find as glass stoppers.

It is really useful for every step on the procedure... But when it comes to pull, it is a complete nightmare. That's why I was thinking about getting some flasks to pour the soup into before pulling.

^ I went through the same problem using a boiling flask with a long neck, jars, etc.

Looking online they are a bit hard to find. There is maybe one or two I saw when I looked & one looked to be cheap Chinese glass, but like I mentioned above, an erlenmeyer with a 24/40 ground glass joint for the neck & a 24/40 ground glass stopper seems like it would be nearly the perfect extraction vessel.

I have been on the hunt for something perfectly shaped that would allow for a deep solvent layer even when using a small ammount of solvent & a tapered neck like an erlenmeyer with a smooth transition vs. Liquor bottle style neck. Erlenmeyer is the closest I can find without having one custom made & working out the dimensions length wise, angle for the taper, height, etc. While still remaining at 1L capacity, not being too tall, & incoporating a ground glass neck & stopper so shaking/rolling can be done without having to worry about a plastic lid leaching unwanted phthalates into the solvent.

Something like this? They work great, and neck holds about 80ml for easy pulling.

I have looked into those before but I see two problems with them.
When you shake/roll, since the bottle has shoulders like a liquor bottle does, it creates a bubble that has a tendency to float up & cause mild emulsions & generally makes it hard to shake/roll gently. This is one of the things i did not like about the boiling flasks with a long neck.

Also, the caps. I would rather not use cork or a plastic/metal lined with plastic cap. They drive me nuts. Not only do they leak, they potentially leach phthalates into your solvent & contaminate your product.

The first thing I mentioned is not so much a big deal, but number two really gets me.
I have a tendency to go a bit overboard regarding purity of acids & reagents used & also to ensure any tools I use are 100% inert.

Ideally my thoughts were something very close to an erlenmeyer flask, only taller & skinnier so the solvent layer is deep & easy to draw off down to a few ML without sucking up any basic soup.

I agree fully with your reservations, and so remove the plastic liner from the cap before use.

It doesn't leak, if screwed on tight, while I roll it around in my lap.