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How long is needed for freeze precipitate? Options
 
StrangeLoop
#1 Posted : 6/11/2010 1:55:43 AM

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I had a dream I did my first ever extraction and within ~2 hours I had a dish covered with crystals. I always hear 18 hours for freeze precip, so if this were ever to actually happen, should I just be patient and wait the full time? If I saw crystals that fast in real life I sure would be antsy to test them out Very happy
 

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wade
#2 Posted : 6/11/2010 1:58:52 AM

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the longer the precipitation, the harder and denser the crystals

sure, in two hours you will see precipitation, but if you wait twenty four it will precipitate completely

 
dg
#3 Posted : 6/11/2010 2:56:32 AM
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if you were in a big hurry, you could alternately,
pour off the remaining np, salvage crystals for vap
reduce np w/ fan or under heat (saftey firts yo!) and re-freeze
 
Sublime
#4 Posted : 6/11/2010 5:37:33 AM

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That is true. Thanks to some users input, it is a good idea to evaporate about 25-50% of your naptha to make it more potent, if you will. Also your freezer should be a certain temperature, because I have found mine is not cold enough, I sometimes leave my jars in there for a few days, and each day more and more crystals appear.
"That which I avoid I will become a slave to, that which I confront I will master."
 
dg
#5 Posted : 6/11/2010 6:59:32 AM
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evap increases concentration, and cold decreases soluabilty
warm or hot np holds a ton more than cold.
i first discovered that when recrystalizing a large amount, and having the np get cloudy as it dripped from the funnel into a mason jar. i thought, why not toss it in the freezer?!
 
Trickster
#6 Posted : 6/11/2010 11:48:21 AM

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dg wrote:
if you were in a big hurry, you could alternately,
pour off the remaining np, salvage crystals for vap
reduce np w/ fan or under heat (saftey firts yo!) and re-freeze


Being in a hurry swim once freeze-preciped supersaturated naphta for ~3 hours and got 99% of spice. There was no spice in the remaining naphta after evapping it completely. Yield was 1.34%.
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BGTM236
#7 Posted : 6/11/2010 12:22:16 PM
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Trickster wrote:
dg wrote:
if you were in a big hurry, you could alternately,
pour off the remaining np, salvage crystals for vap
reduce np w/ fan or under heat (saftey firts yo!) and re-freeze


Being in a hurry swim once freeze-preciped supersaturated naphta for ~3 hours and got 99% of spice. There was no spice in the remaining naphta after evapping it completely. Yield was 1.34%.



I have the same yield. I use Heptane for my pulls, I never Freeze for less than 4 hours, but if im ready, and have the time to pull again, I dont go longer. I evaped my pull after a 4 hour freeze, just to see how much i was leaving, there was virtually nothing left. Additionally, I reuse my solvent, so anything left behind has the potential to crash out in the next pull.
 
collision_course
#8 Posted : 6/12/2010 9:30:45 PM

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i think its mainly about temp, the colder it is the quicker the precipitation
Once I had, a little game
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you should try, this little game
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Forget the world, forget the people
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This little game, is fun to do
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Elliot
#9 Posted : 6/12/2010 10:16:23 PM

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Dry ice is THE way to go.
I get it for about 1.50 a pound in my area.

It works WONDERS.
All of my posts are fictional.
 
StrangeLoop
#10 Posted : 6/13/2010 6:01:51 PM

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I think it's the temperature of the freezer. It's so cold that stuff on the left side of the fridge will often freeze.

My problem now is how to best recover the spice from a quart mason jar? The only way I've been able to so far is to use a spatula to scrape it up and stir the crystals into the naphtha and pour through a coffee filter, although I'm sure this is leaving a fair amount in the solvent and there's definitely still some spice on the jar. Maybe a different container than a mason jar? I can't really fit my hand all the way in there.
 
hyperspacing
#11 Posted : 6/15/2010 5:27:14 PM

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ya you definitly don't want to freeze precip with a big jar. You need a 1/2 pint jar. I would either try and use a big knife or heat up some solvent, pour it in, melt your crystals, and refreeze in a smaller jar like a shot glass or 1/2 pint mason jar.
Also it might just be my freezer but my best crystals weren't fully formed until 48 hours. Ya I had some after 24 but 48 was much better.
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sleeper
#12 Posted : 6/17/2010 9:54:04 AM
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SWIM gets crystal clusters starting around 4 hours. He gets sizable results after ~12hr. He gets best results after ~24hr. With the 3rd, 4th, 5th, etc extractions (if still producing results), his crystals keep growing even after 48hr, and chooses to leave the final extraction sitting for 7 days and freezing for 72hr.

Happy dreams,
sleeper
 
 
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