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Color of backwash, ok? Options
 
Jees
#1 Posted : 11/23/2015 11:40:22 AM

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Hello to all,

what do you think about the color of this backwash?
It's yellow - green - ish.
It's 150 ml of demineralized water + some glacial acetic acid, so pretty clear in its own nature.

Because it is a backwash I presume the yellow/green in no plant fats at all (those remaining in the pulls) right?

It came of 75 gr mimo that was first HCL'ed and then NaOH'ed, the mimo soup got pretty warm-to-hot when dumping in the NaOH.
Then pulled few times with a coincidental mix of 50% light naphta + 50% toluene.
The mimo soup pulls were done at aprox 40 - 50 deg C (100 to 125 deg F).
Then these pulls were washed with sod carb before being backwashed with the acetic A.

Experience tells: When basing this backwash + pulling with naphta (now the naphta will turn yellow and the BW will become clear) + freezing it's gonna be yellow fluffs for sure, and a tiny oily layer at the surface. Potency is no prob at all but it calls for Re-X few times to separate the wax from the whiter fest.

Questions:

- are your backwashes anything like this color?

- is the color an indicator of something that can or cannot be tweaked by changes in the protocol?

- can the green/yellow be simply oxidized deems? Motive for some zink dust reduction of the backwash?

- This color is strictly mimo source material dependent?

- wondering if the hot mimo soup is factor to the color by dumping the NaOH in all at once, in that stage the FB deems got warmer than the regular pull temp. Going gentler next time?

Any hints are welcome,
may the force be with you,
J.
Love
Jees attached the following image(s):
backw.jpg (80kb) downloaded 142 time(s).
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
pitubo
#2 Posted : 11/23/2015 3:21:34 PM

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Jees wrote:
I wonder if the hot mimo soup is factor to the color by dumping the NaOH in all at once, in that stage the FB deems got warmer than the regular pull temp. Going gentler next time?

Hi Jees,

I'm not sure about the other questions, but IMHO adding solid lye directly into the mimosa soup is inadvisable. The dissolution of NaOH is strongly exothermic, to the point of causing the surrounding liquid to boil. Near the dissolving lye, there will be a solution of hot and very concentrated lye soloution that is very corrosive and may cause all kinds of side reactions. The localized sudden heating may even cause cracking in glassware that has poor resistance to thermal shock.

For best results, dissolve the lye in a steel container and mix it into the mimosa soup after the lye has completely dissolved and the lye solution has cooled down sufficiently.

Also, if you want to use salt to increase the ionic strength of the mimosa soup, it is better to add and dissolve the salt before the lye. Lye will still dissolve in salt solutions, pushing any surplus of salt out of solution, but salt will hardly dissolve anymore in a strong lye solution.

Gloves, eye protection, yada yada.
 
Jees
#3 Posted : 11/23/2015 3:33:26 PM

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Thank you P
yes salt was used too (forgot to mention that) and pored in together with the hard lye.
The glass was a thick borosilicate flask giving confidence not to crack it.
 
Hiyo Quicksilver
#4 Posted : 11/23/2015 6:48:27 PM

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pitubo wrote:
Jees wrote:
I wonder if the hot mimo soup is factor to the color by dumping the NaOH in all at once, in that stage the FB deems got warmer than the regular pull temp. Going gentler next time?
For best results, dissolve the lye in a steel container and mix it into the mimosa soup after the lye has completely dissolved and the lye solution has cooled down sufficiently.
While steel or iron are very resistant to lye solution, care should be taken when selecting a metal vessel for handling them.
It should be noted that stainless steel is merely resistant to corrosion, as it does not form a protective black oxide layer. Strong lye solutions can cause corrosion stress fractures in thin stainless steel containers of most types under heat (such as that caused by adding lye to water). Stainless steel flasks and drinking containers should not be used for handling strong bases during reaction, as this can cause a sudden and rapid rupture in the metal, especially near seams or welds.

Galvanized steel is common for making buckets and tools, and contains zinc. The zinc will react with the lye and leave a bunch of Sodium Zincate in your solution.

Solder and other metals used in steel tools can be highly vulnerable to corrosion, however (this is why pure lye is not recommended for cleaning copper/tin plumbing). Aluminum, brass, bronze, tin, zinc and cadmium are commonly used in metal fittings, fasteners, welding materials and solders, and are all vulnerable to corrosion by lye.
These reactions produce chemical contaminants and gaseous by-products which can cause a potential fire hazard without ventilation, and can quickly turn a great extraction into a toxic mess (Take my word for it, I've been there before).

Aluminum containers should never be used to handle strong bases. It's just all bad; Trust me. Wink

Here is a MSDS for Sodium Hydroxide solution (link), and a reference for the chemical resistance of stainless steel, as well (link).

Furthermore, in the presence of heat and oxygen, alkali metals can cause a dark oxide layer to form on steel that can be very hard to remove (this is called bluing). While it's not likely to contaminate your end product, it's worthy of noting when selecting a container. There are commercially-available products to remedy this problem, which are most commonly available at firearms and gunsmithing stores.

....When in doubt, use pyrex. Big grin
 
Jees
#5 Posted : 11/23/2015 8:20:59 PM

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Thanks for the heads up Hiyo.

Meanwhile that backwash "urine" got based and pulled with light naphta, omg there's now enough beautiful golden wax to start a little wax museum Shocked

Joe Swimmer doesn't mind some wax but there are limits Big grin
He hopes to catch some xtals too.

 
Jees
#6 Posted : 11/27/2015 11:23:33 AM

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He got the loot in from 75 gr Mimo bark.

0.64 % white feast
1.12 % hardened brown chips

1.76 % total

When basing the "urine" immediately above/on top of the surface of the "milk" some heavy oil drifted by surprize. It got all pulled with light naphta. Funny thing: 3 layers in the sep-funnel
- the watery below, discarded.
- the naphta op top giving the white feast by freezing
- in between these layers a third distinct layer of liquid golden brown "oil?" giving the hard brown chips afterwards.

The sep funnel could easily separate the 3 and it looked as this was pulling and re-x all in one go. So there was no Re-x afterwards necessary. Perhaps this combo of initial [naphta + toulene] pulls on the bark (before the backwash) made this possible.

He tends to believe substantial nn was dragged into the brown layer, explaining the fairly low white feast yield (super dry, no oil), and the fact that the brown stuff became almost glass hard and remained not goo-ish. It was goo in first, but after a methanol add + thorough evap it became really non sticky hard.

Jees attached the following image(s):
result.jpg (204kb) downloaded 274 time(s).
WF2.jpg (244kb) downloaded 87 time(s).
 
Jees
#7 Posted : 1/9/2016 4:13:53 PM

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Jees wrote:
... Funny thing: 3 layers in the sep-funnel
- the watery below, discarded.
- the naphta op top giving the white feast by freezing
- in between these layers a third distinct layer of liquid golden brown "oil?" giving the hard brown chips afterwards.

The sep funnel could easily separate the 3 and it looked as this was pulling and re-x all in one go. So there was no Re-x afterwards necessary. Perhaps this combo of initial [naphta + toulene] pulls on the bark (before the backwash) made this possible.

I am now pretty confident the middle oil layer, pushed out of the base water, and not accepted by the naphta, yielding the brown stuff, is mainly dmt n-oxide.

The initial toluene pulls took it out of the bark (bark which supposedly was rich in dmt N-oxide to start with) and the naphta from the mini a/b could not dissolve it, hence 3 layers in the sep funnel. Twice this bark yielded little whites and a majority in the brown.

I consider it an advantage to make the first bark pulls with toluene because it CAN take the n-oxide out, something naphta simply can't. Later, during the mini a/b with naphta the n-oxide will present itself separately (layer) from the naphta containing the dmt.

The dmt n-oxide is active in oral, rectal and smoked. There is a shallow difference to notice though, maybe a notch less brutal.

In future, before basing the mini a/b, a zinc treatment will be done to confirm the ideas in the best case.

So the former idea:
Quote:
He tends to believe substantial nn was dragged into the brown layer, explaining the fairly low white feast yield
had to be corrected, the nn was not really dragged into the brown section, it was simply oxidised nn in the bark material. This made the backwash color (in acid state) much more yellow (urine like) than usual.

chances are: to be continued Wink

(Comments are very welcome.)
 
 
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