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Cleaning before or after freezing? Options
 
dakkapel
#1 Posted : 3/13/2013 9:54:06 PM

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This weekend swim did his first extraction! Tonight his crystals are drying Smile
But swim is not sure if he did the cleaning on the right moment. Most of the tek's are talking about cleaning with soda after drying? Does anyone know what's the difference in effect?

Swim is thankful in advance!

So these were globally swim's steps of extraction:
1. mhbr powder mix with naoh then wait
2. add nafta then wait
3. pull and add nafta. this step 5 times.
4. add (1/4 of total amount of ml) sodawater shake and pull sodawater
5. add sodawater shake and pull again
6. add water shake and pull
7. add MgSo4 shake and separate
8. put in freezer
9. pour off nafta
10. let it dry


"All is knowing."
 

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ymer
#2 Posted : 3/13/2013 10:23:48 PM

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With sodawater you mean water with sodium carbonate dissolved in it? if you do then yea the process is fine, a bit overkill on the washing part but looks good to me Thumbs up
 
dakkapel
#3 Posted : 3/14/2013 7:54:22 AM

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Yes that is right. Swim dissolved baking soda in warm water till it was saturated.
Why you think it is an overkill on the washing part?

Btw swim just weighed the amount and has 2,5g out of 330g. So it that is a 0,75% extraction. The crystals are little and hard. The color is quite yellow.

Swim is doubting if he should clean it once more with baking soda and do a re-crsytalisation. But maybe it is unnecessary. Swim knows there are a lot of different opinions about this, but still would like to know what other members think. Is the washing before freezing enough? Cause the yellow color is an indication that it is not pure yet...
"All is knowing."
 
ymer
#4 Posted : 3/14/2013 3:03:00 PM

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I just said a bit overkill because you did 3 washes, not that it's a problem but maybe you lost some DMT oxide in there which is the one that makes your spice yellow (In my opinion I prefer yellow spice)

If you want to get rid of the DMT-Oxide you will have to Re-X with warm hexane/heptane or naphtha but the former are preferred, when you do it discard the yellow sludge at the bottom (I wouldn't do it myself but if you want white spice discard it)

After that you will have mostly DMT, you can Re-X all you want until you get your desired result.
 
d*l*b
#5 Posted : 3/14/2013 3:28:29 PM

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I don't think you need the MgSO4 wash. The sodium carbonate wash is a good idea though, it will remove any NaOH/MHRB solution that may have got caught in suspension. One wash will probably do the job in most cases but if you are really worried two won't hurt.
D × V × F > R
 
dakkapel
#6 Posted : 3/15/2013 4:09:09 PM

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ymer wrote:
I just said a bit overkill because you did 3 washes, not that it's a problem but maybe you lost some DMT oxide in there which is the one that makes your spice yellow (In my opinion I prefer yellow spice)

If you want to get rid of the DMT-Oxide you will have to Re-X with warm hexane/heptane or naphtha but the former are preferred, when you do it discard the yellow sludge at the bottom (I wouldn't do it myself but if you want white spice discard it)

After that you will have mostly DMT, you can Re-X all you want until you get your desired result.


So you say the yellow color is the result of DMT-oxide in the spice?
And if swim is recristalizing the spice the DMT-oxide will be left in the nafta? Or will it be changed to normal DMT?

Secondly you say you prefer dmt-oxide in your spice. Why do you prefer that in a comparison with white spice?
"All is knowing."
 
dakkapel
#7 Posted : 3/15/2013 4:23:42 PM

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d*l*b wrote:
I don't think you need the MgSO4 wash. The sodium carbonate wash is a good idea though, it will remove any NaOH/MHRB solution that may have got caught in suspension. One wash will probably do the job in most cases but if you are really worried two won't hurt.


So far I know the MgSO4 is to attract the H2O in the nafta. Which should make it easier to separate the H2O from the nafta. So I have two questions.

First of all I actually don't know (for sure) why it is problematic if there is some H2O in the mix.

Secondly is there a downside on a wash with MgSO4?

Thirdly if the downside is loss of yield. Is there some estimation on how much yield you loose?


"All is knowing."
 
 
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