• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

freeze percip question...bottom layer has turned to ICE!

Migrated topic.
B

Bananaman

Rising Star
SWIM has set the pulled naphta aside in a container and put it in the freezer...swim has decided to check on it tonight before pulling it out tomorrow...the only thing is, a good portion is now ICE!


what does SWIM do next? SWIM has never heard of it freezing in all the freeze percipitation teks he's seen. :?:
 
Sort by date Sort by votes
a friend usually stirs it all up right before dumping it through the coffee filter. remember that this all has to happen very fast in order to still have freezing cold naphtha. the naphtha must be VERY cold for filtration of the crystals. otherwise they will redissolve in the solvent and pass through the filter. a friend also tends to stick his collection jars back in the freezer for another 2 nights or so in case some more decides to fall out of it.
 
Upvote 0 Downvote
sounds like you had some water?? you would have noticed it when you put it in...it would have made a separate layer in the naphtha...not sure whats going on there
 
Upvote 0 Downvote
Definitely sounds like there's some water impurity in the naphtha. Certain brands of naphtha as well as some solvents (e.g. xylene, toluene and isobutanol in my experience) take some time to separate properly from water.

Initially, separation can be a bit more hazy; Even though an interphase between the two phases may be apparent, particles of water can still be present in the NP layer and particles of the NP solvent may still be present in the aqueous phase.

Just wait more for the layers to separate, in the end one's NP layer should be clear, not too cloudy. Patience is a virtue.
 
Upvote 0 Downvote
also it could be water vapor from the freezergetting into the naptha and colleecting at the bottom and freezing into crystals,1 or 2 drops is ok as it acts as seeds crystals,but too much water in there could be a bad thing,i always had some water vapor get in my naptha but not enough to worry about,as soon as all the naptha has evaporated i take it out and put a slow fan on the baking dish to evap the water droplets.(this is if you are using a baking dish to evap the naptha in)swim has steered away from putting naptha in jars and freezing the jars because dmt crystals have a tendancy to collect on the side of the jar and are a pain to get off.swim likes baking dishes for the freeze precip part.
 
Upvote 0 Downvote
Infundibulum said:
1shot2 said:
1 or 2 drops is ok as it acts as seeds crystals
Click to expand...
Water crystals do not act as seeders for spice crystals, spice crystals on the other hand can act as seeders for spice:wink:
Click to expand...

well excuse my ignorance but, can´t anything with irregular surface be a seeder for spice crystal^? I cant see why a tiny speck of ice wouldnt work as such

not that one should make it on purpouse, of course, because the water in the end will be a pain, but just theoretically...
 
Upvote 0 Downvote
I always use a mason jar with a screw on lid to prevent any moisture build up (and spills) from happening. Never had any ice form in my naphtha.

Let thaw, seperate water from naphtha and stick back in the freezer in a jar with a lid.
 
Upvote 0 Downvote
and when you go to pour the naphtha off..do it very quickly..and then close the jar again to make sure very little water will condense on the inside of the glass...and then let it sit upside down...on the lid so any other bit of naphtha or water wont be reabsorbing your spice as it warms up...then once water stops forming on the outside of the glass open it up and dump out the naphtha that collected on the lid...and then sit the jar upside down on a piece of paper towel to dry some more...and then let it sit right side up until it dries completely(dont want crystals falling off when they start to dry upside down)

then scrape and voila!

what you can do next helps with dosing...once you have all your spice..pile it up on a very flat piece of glass...and then drip heptane or naphtha whatever...onto the spice until it becomes slightly pasty...what this will do is condense your spice...so spread a layer of this paste across the glass...make it nice a uniform...and then let the naphtha/heptane..whatever..evaporate...

what you get is this hard puddle of spice..get a razor blade and scrape up the spice...you will notice that it is very powdery now and less crystally...break up all the little chunks that didnt powder up..and now you have a pile of whitish spice...its much more dense this way...and you can put way more of it in your smoking device because its now more potent by volume...mess around with the dosage...but SWIM has found it easier to manage this way..and it also reduces the amount of air/oxygen that can sit in the spice
 
Upvote 0 Downvote
I always use a mason jar with a screw on lid to prevent any moisture build up (and spills) from happening. Never had any ice form in my naphtha.

Let thaw, separate water from naphtha and stick back in the freezer in a jar with a lid.
Click to expand...

Yup, You need to get an air tight seal!!

If the freeze precip jar (or whatever) is not sealed, the oxygen in the jar, and in the freezer, will condense inside your precip jar. Which ends up creating ice in your precipitation. This makes filtering the crystals out of the Naptha difficult because the ice sits on top of the filter with your crystals & melts causing the DMT around it to not only stay damp longer but it also dissolves some DMT crystals and allows them to pass through the filter. Basically ice in the Naptha makes getting the DMT out of there, a giant pain in the ass and you end up with a smaller yield from that first freeze precip. You'll have to re-freeze the Naptha again to try to get the rest of the crystals back out etc... Still, Some of the DMT will remain stuck in the filter, so you will lose some almost every time if you get ice in your freeze precipitation container.

Although to tell you the truth, it sounds like you have a whole lot of ice in there, so I would guess that you didn't get all of the water out of the Naptha in the first place.
So make sure you get any water out of the Naptha, before putting it in the freezer. Then make sure you have an airtight seal on the precipitation jar!!

Before putting my precipitation jars in the freezer, I will set them out, on the counter top for a while, with something sitting under the jar, lifting up one side of it, so it sits at an angle.
Any water thats still in the Naptha should fall to the bottom of the jar, as little clear balls.
With the jar sitting at an angle, they will then "roll" to the lower side of the jar and coagulate together, forming bigger "balls" of water.
Swirling the jar around, gently, will help to get the little balls of water to coagulate if they don't do it by themselves.
I then use an eyedropper to decant the water off the bottom of the jar.
A baster is usually much too big to pull out only the hopefully small amount of water, leftover in the Naptha.

I'd go with what acolon_5 recommended above, to get the water out of your Naptha & refreeze it.
It should be fine if the only problem is just ice in the Naptha.
Make sure to get a good seal on the precipitation container for sure, to help avoid this in the future!!

WS
 
Upvote 0 Downvote
Back
Top Bottom