posted 05-09-99 03:30 PM         

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This is a modification that my chinchilla filled me in on the other day. He says you'll need: a 70-90mm buchner funnel with any thin filter, a STRONG suction devise (chinchilla used a recently ripped off refridg pump, although "mouth suction" will work somewhat to take out the yellow color but wont make the sass clear), a 250ml filter flask, tubing to fill on the sidearm, frozen sass in a 10 oz liquour bottle (with screwcap) or larger.

Turn your fridge and freezer up to the coldest level possible. It will take 2 or 3 days for it to get down to that max temp(amount of time depends on how much you have in your freezer, and the more you have in there, the more stable that temp becomes after it is reached, so have alot of frozen foods to act as an insulator). After 3 days the temp should be between -18c and -22c (most will go to -18c), warmer than -18c was not tested, so dont know if it will freeze if
-17c. DP Harma's freezing technique is excellent but seems a little meticulous, its actually much easier than he makes it to sound (so he needs more credit for that writing than he's been getting. Getting the stuff to freeze is the trick. Usually, if you place a bottle of sass in the freezer, it wont freeze without opening it after it reaches it max cold point. It usually requires you to get it down to -18c or colder and then open the bottle up to expose it to air. The more air/liquid surface area exposure, the better chance of freezing. So, dont use those little 1oz NOW brand bottles to freeze it in. Use a liquor bottle. Chinchilla used a 750ml malabu run bottle filled to the rim with oil with a screw top. Open the bottle and let it sit at room temp for 5 min, put it back in the freeze with the cap closed and let it sit for at least 30 minutes. If it doesnt freeze, dont worry, it will upon doing repetitions of this. If it does not freeze after 2 attempts of this and the temp is -18c or lower, then put it in the fridge section with the cap open and let it sit in the coldest part of the fridge, bottle open, for 10 or 15 minutes. Put it back in the freezer closed cap or open cap, probably doesnt matter. But close the cap after 15 minute of being in the fridge if not frozen by then. If you still have no luck then you need to switch to using a open glass container (flour jar, etc), that has some surface area to expose the liquid to air while its at its lowest temp. Take the large top off of this glass container and expose it in the freezer (in the coldest area) for 1 hour or more. When your oil is at its coldest, pour only a capful of oil or just enough to cover the surface of the container with a thin film of oil. It might start developing crystals immediately or may not. Either way, throw it back into the freezer with the cover/or not the cover, may not matter. Within a day at the most, it should crystalize. If not, then intermitently expose the open container to room temp for 3 minutes and place back in the freezer. crystals should come out in hours or even minutes. If not then You need to try a differnt oil. Something is wrong with that shit you got. Chinchilla has tried this with at least 5 different brands and only the NOW brand was the most difficult to freeze. The key to getting the cyrstallization to begin is to expose the ice cold oil to air (usually room temp is the only way it works), but dont let it stay out more than 5 minutes. Once you've gotten the capfull to freeze over, scrape that frozen sass into the ice cold mother load of sass you got. The shit should start instantly turning into slush from the neck of the bottle down to the bottom (temp must be max cold before you transfer). This whole 750 ml of oil turns to a milky slush in 10 minutes. Dont shake it within the first 30 seconds of it changing its state, or it will stop or reverse. By using good judgement, estimate when you can start shaking the mix so it DOES NOT change completly to hard ice where you cant get it out of the bottle. Shake it so the rate of freezing is at an equilibrium of the rate of reversing it back to a slush mixture. You can tell this by the sound of the shaking. Put it back in the freezer for 10 minutes with freezer blowing and let it get slightly colder. In the meantime, put your buchner funnel in the freezer for 5 or ten minutes to let it cool down. Then, place it over the top of the filter flask and get the vacuum source connected to the sidearm. Shake the large bottle of continuously freezing slush enough to loosen the ice up from blocking the bottle neck and to make it into a homologous slush mix. Pout the slush into to buchner and turn the vac source on, YOU WONT BELIEVE how yellow liquid get sucked into the flask and an snow-white ice stays in the funnel as a compacted frozen solid. You can keep doing this as long as you feel the ice is significant enough to freeze the remaining slush that you pour in. Its a hell of alot easier than im making this out to be, as I saw a chinchilla do this on 2 attempts, both successfull. You can even break up the frozen shit in the buchner and mix it into a slush again to filter out the remaining frozen yellow crap. By doing this over a 8-10 minute time, chinchilla obtained: an ugly yellow cloudy mix in the flask (a maximum of 50% the original liquid) and then an ice white stuff in the funnel that could fool anyone to be ground up ice to be topped with their favourite flavour. Once that was melted, the stuff came over in its melted form as a clear water. NO SHIT! If you only get it to be a cloudy white then you have good suction, but if you get it to come over clear when its melted at room temp, You got kick ass suction. If you got cloudy white, you can put that bottle under hot water for 3 minutes and it turns clear and then back to cloudy white when at room temp. Chinchilla's fridge pump broken in the second process of doing this and he used his mouth to suck the stuff from the filter flask instead. But instead, he changed the buchner funnel to a 250ml sep funnel and shook the stuff in that to make it slush and filter it out of the sep funnel into the flask. Worked enough to get it cloudy white with no yellow. The smell of the clear stuff is nothing like the smell of out of-the-bottle sass or the left over yellow shit. It much lighter in smell, not strong at all, has a degree of a differnt spicy bouquet. As this is the first time ever seeing this stuff, does it sound like it's goods? (DP Harma, thanks for Your inspiration on this experiment)

posted 10-25-1999 11:23 PM         

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Now any jackass can freeze sass. No more, it cant be done remarks, it can be done! We're all aware vacuums lower bp's. So, on the opposite end, most liquids, when put under pressure will have a different mp/freezing point. Higher pressures will raise freezing points. And thanks to Ketones KRV/SRV any jackass can freeze his favorite oil.

Prefreeze your oil as cold as possible.
Make a KRV/SRV with the standard tire valve but try to obtain a 3 liter bottle instead of a 2 liter bottle.
Put the bottle in the freezer for 1 hour.
Pour in your prechilled (~ -12c) oil in the KRV and pressurize to 50 PSI.
Put back into freezer and let the think do its own while you go masturbate.
After 1 hour the amount you pour in (~ 125 ml or so) will freeze.
Release the pressure, add the remaining oil to this frozen solid and voila!
The rest is history. It will freeze and stay frozen like this very easily from then on.

posted 10-26-1999 11:12 AM         

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I'm not sure, but I guess opening the bottle helps because dust or frozen humidity from the air could act as initiators to the crystallisation. If the oil is stubborn, try adding a boiling stone or scratch with a wire.
Does pressure really have an effect on freezing point? If at all I'd expect pressure to lower the freezing point instead of raising? Whatever works for you.

I always used the freezing of safrole to further purify my pre-honey. It works very well with distilled material. But you have to approach this a little differently:
1) Always let it crystallise very slowly. The slower the better.
2) It helps to have some seed crystals in the freezer, although this is not really necessary unless you are in a hurry.
3) When most of the safrole is frozen, carefully pour away the still liquid portion. Do not discard it, collect and recycle.
4) Repeat several times. Each time the purity of the safrole will be higher (proven by measuring crystallisation temperature).
5) Work up the decantations, by either collecting the same fractions or combining and refreezing them or redestilling them.
6) Result: great yields of (soon-to-be difficult to find) safrole, with almost textbook-perfect melting point.

posted 10-26-1999 12:01 PM         

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Thenk yew, thenk yew very much!
schwam you are too cool

dpHarma

posted 10-27-1999 06:02 PM         

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I had a hard time freezing the oil at first. I got radical on it by using a dry ice-acetone bath, and it worked. I kept the seed crystals.

So chill your raw oil to at least -15 C, dip a stirring rod into your vessel of seed crystals, and place stirring rod in chilled raw oil and - presto! Beautiful ice!

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