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Trouble with freeze precip

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macguyver

Rising Star
SWIM's having problems with freeze precip...

They followed Nomans tek (600ml water, 100g lye, 100g MHRB, 150ml naptha(Bartoline White Spirit from B&Q - in UK), 24 hrs with intermittent rolling of jar, 24 hrs freezer)...

SWIM has now tried 3 times to extract the crystals from the naptha:

1) Crystals were ALL floating in the naptha - NONE had stuck to the glass in the jar. SWIM attempted to pour through a coffee filter to collect & dry. When they poured the floaty filled naptha through a filter, a big lump of white DMT collected which SWIM then aimed a fan at to dry. They then watched in utter dismay as the lump dissolved to nothing - just left a tiny residue on the coffee paper, but no crystals. Fail!

2) Crystals all floating again, except this time there is some evidence of something sticking to the jar - possibly some oily residue... this time, having failed with the coffee filter SWIM poured the naptha back into the main jar (with lye & MHRB) leaving what looked like a lot of crystals stuck to the jar.. Success! Or so he thought - been drying under a fan for a few hours, and when SWIM went to collect they found all the crystals were stuck to the glass - an invisble sticky residue had been left which all crystals were stuck too. If it makes any difference, all crystals were small and uniform in size, none

3) Same as 2


So.. how can SWIM get the crystals off the residue, and where is the residue coming from / how can SWIM stop it?
 
residue is possibly some remains of the solvent that gets trapped and refuses to evaporate, or some plant oils and so on, or dmt n-oxide on your evaporation attempt.. or a mix of this all.

it has happened to SWIM before a couple of times, and sometimes making the exact same thing with exact same products and it works..

What SWIM would do, is first of all work in a way that nothing gets lost (if dmt melts into coffee filter, put it in warm naphtha to pick up the dmt again, for example).

Sometimes if the crystals dont stick its because the naphtha is not saturated enough (pre-evap some more), or the freezer is not too cold, or it wasnt in the freezer for long enough, or the container is not so good. SWIM uses simple flat glasses.

So SWIM would redissolve it all in small amount of warm naphtha, let evap slowly with a cloth cover until very small amount (not just till its cloudy), and then in the cold freezer for 24 hours at least.. Most should be stuck to the sides. Then either SWIM would have constructed an easy and very effective improvised vacuum filter, and take the stuff out of the freezer and quickly scrape the sides with the naphtha still inside. Then SWIM would pour it through the vacuum filter, and scraping whatever is left in the container and rubbing against the coffee filter in the vacuum setup. The crystals should dry quick enough to not melt into the filter.

Or SWIM would just pour off quickly the naphtha (passing through a filter just to catch anything that was not stuck)... Then with the crystals still stuck to the container, put it upside down, but using some support so it stays at an angle, so that any remaining naphtha can drop off, instead of warm up and stay inside. Also put a fan turned towards the container so that it can help drying up quickly.
 
Bartoline isn't really the best for freeze precip due to it having a mix of longer chain hydrocarbons(than normal naptha). Plus I can't remember if it contains aromatics which do not allow for freeze precip.
 
Can someone else confirm if Bartonline is no good for freeze precipitation? SWIMs checked the bottle and it says 'premium low odour' which he assume means it's non-aromatic? What is better in the UK, that can be bought in larger volumes than Swan lighter fluid? Is there anything?

How would SWIM contruct 'an easy and very effective improvised vacuum filter'? (EDIT: SWIM has found some threads on how to do this now)

Just to clarify what you're saying regarding the jars that have crystals stuck in residue - should SWIM add warm naptha to dissolve all back into the solution, then freeze again & then either use vacuum filter OR pour through coffee filter & leave jar at angle that drains as much naptha as possible?
 
A SWIM I know says that coleman fuel is very good in the UK and can be bought at a well known camp-store. Some people in the states say their coleman fuel contained a blue dye, but in the UK this isn't a problem.

500ml for about £5.
 
macguyver said:
Can someone else confirm if Bartonline is no good for freeze precipitation? SWIMs checked the bottle and it says 'premium low odour' which he assume means it's non-aromatic? What is better in the UK, that can be bought in larger volumes than Swan lighter fluid? Is there anything?

How would SWIM contruct 'an easy and very effective improvised vacuum filter'? (EDIT: SWIM has found some threads on how to do this now)

Just to clarify what you're saying regarding the jars that have crystals stuck in residue - should SWIM add warm naptha to dissolve all back into the solution, then freeze again & then either use vacuum filter OR pour through coffee filter & leave jar at angle that drains as much naptha as possible?
Click to expand...


yes exactly redissolve in warm naphtha, evaporate until its only small amount, then freeze again and proceed with one of the two options

good luck
 
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