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Is not putting cling wrap over my freeze precip causing problems with melting crystals? Options
 
Jaurk
#1 Posted : 6/18/2016 8:18:38 AM

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What is the point of the cling wrap?
I'm okay with my naptha evaporating in the freezer,
I have an empty freezer (no food) & a lot of naptha.

I'm just trying to figure out why my yields are nothing at all.
My crystals keep melting.





1. 100g ACRB placed in 500mL water.
2. Freeze/Thaw x2
3. Vinegar was added to pH 5. HCL ~2mL added to reach pH 2-3.
4. Overnight acid bath at 50C.
5. 80g NaCl (Salt) added
6. 55g NaOH (Lye) added, turned black. pH = ~12-13.
7. Warm naptha pulls after soup cooled down.
8. Placed into glass precipitation dish, put into freezer.
9. NO CLING WRAP PLACED ON DISH
10. 8 hour freeze showed some crystals on the bottom.
11. Poured naptha off into 2nd precip dish to air evap.
12. CRYSTALS MELT WHERE THE HELL AND WHY IS THERE SO LITTLE!!

I soaked what I could in cannabis, i don't know if it's ice water but it's partially active.
 

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Chan
#2 Posted : 6/18/2016 9:58:58 AM

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As a general rule, don't deviate from teks until you fully understand what you are doing. We're not trying to get rich on cling wrap stocks Wink

You're not going to evap significant quantities of naptha at freezer temps. It's the drop in temp which makes the spice less soluble in it, causing it to "crash out" as crystals.

You DO want to evap as much naptha as possible BEFORE putting it in the freezer so you have a nice saturated solution ready to drop lots of material once it freezes down. Evap (using a fan) until you start to see specks appearing, or it turns milky.

Sounds like you're getting some condensed water vapour in there too, without the cling wrap, and that's coming out as wet crystals, possibly with much of your potential yield left behind in the unsaturated solution... You can still put it under a fan and try again, but any water will be hard to displace now.

And cannabis and spice don't usually enjoy one another's company...



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sbc1
#3 Posted : 6/18/2016 11:06:56 AM
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Always cover your dish, your going to get condensation, ice into your dish which will melt your dmt plus water and naphtha don't mix so you'll have 2 layers, water layer will freeze the naphtha won't so always cover your dish
 
Jaurk
#4 Posted : 6/18/2016 11:08:05 AM

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Chan wrote:

Sounds like you're getting some condensed water vapour in there too, without the cling wrap, and that's coming out as wet crystals, possibly with much of your potential yield left behind in the unsaturated solution... You can still put it under a fan and try again, but any water will be hard to displace now.


I think that's the case, really.
I see the crystals when it's frozen, but after I pour the naptha off they just melt.
That's what I soak the cannabis in (partially active).

Well, I have another one in an acid bath at the moment.
If anyone else has had this problem, I will put cling wrap on this one.
I will also evap naptha off to make the freeze precip more condensed.

Be back tomorrow.
Open to any more replies Smile
 
Jaurk
#5 Posted : 6/19/2016 10:31:15 PM

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Well unfortunately I only had abilities to evap precip.
Resulted in goey blobs.
I am thinking this is due to no defat step with ACRB.
I have one more trial I could do, in time.


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I like to try things my own way first and I guess I learnt Razz
 
Rick Sanchez
#6 Posted : 6/19/2016 10:52:35 PM

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Some samples of acacia bark contain higher levels of the beta-carboline NMT than others. This means that while some samples with lower NMT content will yield perfectly clean spice without any additional cleanup steps, others will require more work if a greater purity is desired. Smoalking the goo itself will produce a more than satisfactory experience for most people. Freezer precipitation is a great way to yield clean spice in that the crystals form in the precip. vessel while a few impurities may remain dissolved in the solvent. If you are trying to crystallize solely by evaporationg, the solvent has to be very clean. As long as you perform the mini a/b that EW describes in his tek or a method similar to this toremove the fats/ yellow coloring from the solvent you should be ok. Another easy alternative to crystallization is redissolving the goo and making changa! good luck
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Running Bear
#7 Posted : 6/19/2016 11:02:10 PM

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I think its ice that's melting not crystals. I also believe that you're either using bad naptha or that you have weak ACRB. Stop evaporating your naptha before you put it in the freezer and make sure you cover it. The same thing happened to me when I started so buy some better bark and if that doesn't work buy some new naptha.



one more thing,
nice picture lol...
 
arcologist
#8 Posted : 6/20/2016 4:21:28 AM

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Goo with ACRB usually means a significant portion of NMT is present in the extract. You can turn goo (dissolved in NPS) into crystals using dry ice to remove the NMT.

When freeze precipitating it can also be good to cover the dish (use something not plastic) to reduce the formation of condensation/ice on the glass. This can also be avoided by placing the dish in the refrigerator beforehand to cool down the glass before putting in the freezer.
 
endlessness
#9 Posted : 6/20/2016 9:38:30 AM

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Apart from what arcologist said, check the FAQ for melting crystals problem.
 
 
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