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monomind
#161 Posted : 5/23/2021 9:26:00 AM

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Thanks benzyme.
I have another question if i may...
Does saline ( 0.9% saline solution ) have the same solvent properties as water ?
Meaning if a substance is water soluble ... can I assume it is also saline soluble ?

Cheers
 

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Sidisheikh.mehriz
#162 Posted : 5/23/2021 1:30:00 PM

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monomind wrote:
Thanks benzyme.
I have another question if i may...
Does saline ( 0.9% saline solution ) have the same solvent properties as water ?
Meaning if a substance is water soluble ... can I assume it is also saline soluble ?

Cheers


The 0.9% salt in that solution wont change much about the solvent properties of the water in the acidic phase of the extraction. I'm sure you can use 0.9% saline solution for extracting instead of just plain water. It's a good source of pure water if you have enough laying around and dont want to buy distilled water.
After that being said i use tap water with no issues i just boil it first to drive out the chlorine from. It. I just add slightly more citric acid than necessary to neutralise the calcium carbonate innthe water (hard water).
 
Sidisheikh.mehriz
#163 Posted : 5/23/2021 5:35:44 PM

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For so long I've wanted to ask these questions here at the chemistry section regarding making a reasonably pure hommade zinc powder for n-oxide reduction. Living in a third world country it's a challenge to procure chemical reagents and i have to improvise most of thet time.

Simply grinding zinc metal from a zinc anode or any peice of equipment that is made of zinc casting is just not going to cut it. It will almost surely contain toxic ammounts of heavy metals like cadmium. Recently though i found that medical grade zinc oxide is sold for cosmetics and for dentist purposes at a moderate price.

My first thought was to reduce this zinc oxide with active carbon in a heating vessel. I have tried this type of reduction on copper oxide and it worked quiet well due to carbon being much more active then copper this reaction was possible with a temperature that is lower than the melting point of elemental copper. I did a reduction on hommade iron oxalate successfully also yielding magnetic iron oxide (makes for a powerful thermite) and pyrophoric nano iron powder (spontaneously burn on contact with air).

Zinc reduction with carbon though is a different story since zinc is more active as an element than copper and closer to carbon. This reaction will require more heat that can easily melt the resulting zinc powder and one will have to grind the zinc afterwards.

So i searched around a bit more for an alternative reduction method and found that zinc oxide can be reacted with an aqueous solution of sodium hydroxide to yield sodium zincate Na2.Zn(OH)⁴ this sodium zincate can be reduced through electrolysis at the cathode end to elemental zinc sponge which can be later washed with distilled water and used as is for our n-oxide reduction purpose.

Some voltage and current experimentation and adjustment has to be made to ensure zinc is being reduced at the cathode instead of just hydrogen. lowering the voltage will minimize this. As for current one can control it through adjusting the distance between the Electrodes and also through controling the surface area of the electrodes (dip them deeper or shallower in the electrolyte solution. The less current the longer the reduction will take to finish. The basic nature of the electrolyte will allow for using less inert cathode. The anode though will be subjugated to a moderate degree of oxidation and must be moderately inert like nickel for exemple. Nickel is sold by electroplating kit suppliers fairly pure and i shall be trying it soon

The cathode is more forgiving as it's protected by the reducing power of the electric current as long a as the electric circuit is closed.

I got this idea from nurdrage's channel on youtube:
https://youtu.be/3X9c6epL7HQ

What the chemistry experts here think about this process?

Second question is regarding the prospect of using formic or oxalic acid for salting purposes.

As i mentioned above it's difficult to obtain reagents where i'm from but i found that oxalic acid dihydrate and 85% formic acid are both available as an organic varroa mite treatment in beekeeping and is globally sold for this purpose and i got my hands on both cheaply from a beekeeping hardware store.

I was more thrilled when i read that 5-meo-dmt and DMT research chemicals are sold in oxalate form and the scientific literature says that oxalate is there amongst the crystalline a and stable salts for dmt and 5-meo-dmt like fumarate and succinate (i cant find any of those and ordering them from abroad is not a choice for me)
Now i've seen in the phalaris analysis thread how phalaris can contain almost half its DMT and 5-meo-dmt in n-oxide form so my question is:
can i use zinc powder from the electrolysis of sodium zincate to reduce an extract from a positively tested good yielding phalaris brachystachys then base this reduced extract and salt it with oxalic or formic acid? Has anyone used these acids in an extraction before?

This paper here confirms the oral safety of calcium oxalate after consecutive use at doses much higher than for our purposes :

https://dmd.aspetjournals.org/content/33/2/282

One advantage of formic acid is it's high volatility even at room temperature. An advantage of oxalic acid is it's ability to be recrystalized through sublimation. Just simply place it inside a vessel with a cover. Heat the vessel on a very low heat setting. First water vapor will be released as the dihydrate crystals are being converted to anhydrous then the oxalic acid itself will sublime and recrystalize pure on the inside walls and cover's ceiling of the vessel (very pure stuff) while impurities will remain at the bottom of the vessel as a black brown sticky oily residue. Just don't breath near the heating vessel (micro oxalic acid crystals in the air and gaseous formic acid asa a thermal decomposition byproduct. I attached a picture of some pure oxalic acid crystals obtained by sublimation. (Feels good to know am ingesting a pure stuff). Even if the yield is low through sublimation i will take that because technical grade oxalic dihydrate is dirt cheap. It's sold as wood bleach too by the way but buying it from a beekeeper store it's more pure.

Formic acid is around 10 times the strength of acetic acid. It's the only carboxylic acid that has the reducing property an aldehyde has. I wonder if this property can be harnessed for our reduction purposes or if it's a destructive kind of reduction that will destroy my extract. Diluting the formic acid is probably good enough to avoid such an event? It cant be that reducing since some large molecules such as antibiotics are produced on large scale in formate salt form. When concentrated formic acid can readily form esters with alcohols according to Wikipedia. Maybe these esters itself could contribute as a solvent in an extraction same manner as ethanol and acetic acid when cooking a botanical can form ethyl acetate which is a good solvent)

This post is getting too long and i'm starting to blabber Very happy
Sidisheikh.mehriz attached the following image(s):
IMG20210512184947.jpg (3,220kb) downloaded 102 time(s).
 
downwardsfromzero
#164 Posted : 5/23/2021 9:41:09 PM

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Sidisheikh.mehriz wrote:
[...]
Your zinc electrolysis experiment sounds like a great idea! Clearly, food grade sodium hydroxide should be used for producing the sodium zincate if at all possible. I don't know how easy grinding up a piece of zinc sponge would be; a ball mill would make your life easier here but would present some hazards. You may be aware that, during the smelting of zinc, given zinc's relatively low boiling point (990°C) a good proportion of it distills out of the zinc smelter and is captured as zinc dust. This doesn't seem like it would be so easy to reproduce in the home laboratory but then again, nor does it seem unfeasible for a determined practical experimenter. Perhaps something with a plasma electrode and an inert atmosphere would be sufficiently compact. Obligatory disclaimer: Both of these preceding suggestions are fairly dangerous and you would need to know what you're doing!

Regarding choice of anode material, with a basic environment there's a small advantage in that nickel oxidation products will be practically insoluble, forming a layer of NiOOH if nickel-based rechargeable batteries are anything to go by. This will minimise the likelihood of nickel contamination in your zinc. Another thing worth considering is that some silver jewelry is rhodium-plated and thus may be another viable choice of anode material (if you happen to have a piece lying around): rhodium has excellent chemical resistance -
https://redox.me/product...trode-model-6-metal-mesh

Unfortunately, thermal decomposition of zinc formate appears to produce zinc oxide:
https://doi.org/10.1016/0022-1902(67)80317-8

Outside of a Leuckart reaction, formic acid would best be used with a catalyst such as palladium for reduction/hydrogenation. Some of the more competent practical chemists might be able to comment further on this.

Nice woolly oxalic crystals you've made there! You mentioned the low toxicity of calcium oxalate crystals but I would like to mention that I personally know someone whose health has been ruined by their long-term use of oxalic acid as a wood bleach. Oxalic acid and its soluble salts are a different matter from (than) practically insoluble calcium oxalate. Safety precautions apply.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Sidisheikh.mehriz
#165 Posted : 5/24/2021 11:41:11 PM

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Of course food grade lye or for soap making (not the drain cleaner grade) is required for this purpose. You don't have to grind the resulting zinc sponge it's just a mass of loosely connected tiny elemental zinc crystals that will collapse to powder when you try to scratch it off the cathode. I had that happen when reducing copper through electrolysis. The mesh size for the powder wouldn't be very fine though. I don't think this will matter much especially when using HCl for our n-oxide reduction purpose. I heard about the ball mill process in my early chemistry days doing pyrotechnics. The idea of steel balls colliding with each other and the inside walls of the mill very likely releasing some steel contamination (unless it's stainless steel balls) raises some concerns for me. Maybe i'm just being over careful here I don't know. I can be lazy sometimes and setting up a ball mill on top of an electrolysis set up seems already too much for just zinc powder for me.

You know that boiling off gaseous zinc to obtain nano zinc dust will require a nitrogen cooled chamber right? That's definitely not the kind of set up for an amateur home chemist whose only goal is an n-oxide reduction Very happy

Speaking of rohdium and electrolysis in general, i've spent quiet some time and practice in the past few years on a chlorate cell to oxidize Nacl to sodium chlorate NaClO3 for pyrotechnics purposes and i've experimented with rohdium plated anodes. Let me tell you the electroplated layer of rohdium on silver, or white gold is a very very thin layer that is not meant to last (on purpose) or else how a jeweler is going to profit from his gold plating kit if you never come back for replating. You might reach to some sort of deal with the jeweler for a thicker plated anode for an Extra price. That could work. But then again if you are going that far you might as well spend that money more economically on a platinum clad neobium anode sold for jewelry electroplating. It will be a very versatile item in your home lab for a wide spectrum of electrolysis at both acidic and alkaline mediums. If it's a genuine product it will last you for many years. A cheaper (around 50 bucks) but less versatile option is MMO (mixed metal oxide) titanium coated anodes these are widely used for commercial purposes like hypochlorite and chlorate cells, waste water treatment and swimming pool chlorine generators. Due to the high demand on these types of anodes by amateur chemists there are a lot of frauded ones so pick carefully.

Nickel should work fine and can be bought pure from electroplating kit suppliers. I just hope no nickel oxidizes into fine particles and incorporates into the reduced zinc sponge. Nickel is way more toxic than just zinc. A tiny bit of zinc can be even a good thing actually. Just like some chromium leeching out from stainless steel cookware is a good dietry source of chromium.
Leuckart reaction was an interesting entertaining read for me yesterday thank you for bringing that up. It's a shame though that it's an amination type of reduction and not just plain simple reduction. As for Formic acid reduction catalyzed by palladium on carbon i read that ammonium formate is more efficient than Formic acid and produce higher yields also hydrogen gas has to be fed to the reduction vessel in absence of oxygen for this to work. Why does all the cool stuff has to be so expensive like this Crying or very sad
At least and thankfully there are youtuber enthusiasts who has done these experiments for us to watch and live with them like hydrogenating olive oil into a margarine like saturated fat with carbon on palladium and hydrogen gas..or chalcone reduction into it's alcohols

Absolutely oxalic acid is no joke! Some ppl be like oxalic acid is in most vegetables we eat like it's benign.. well yeah you're not toutching vegetables bare handed everyday.. just take good look at the hands of any farmer who works with vegetables bare handed and see the awful cracks and blisters on their hands.. it's way worse than construction hands that's all the oxalic acid's work! It's deceivingly safe when handling it because you can't feel an instant burn on skin contact but since you cant feel it you might forget about it till after few hours you feel some burn and you notice you have blisters. You may forget washing your hands and then scrub your eyes!
Beekeepers vaporise oxalic acid inside the hive to kill varroa mite, i've used this treatment and wind blown those fumes back my way once and i breathed some of the oxalic vapor... Felt like sulfiric acid fumes in my lungs! Instant hard coughs! So yeah i totally understand your friend's misfortune.
 
downwardsfromzero
#166 Posted : 5/25/2021 12:59:51 PM

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Last visit: 16-Mar-2024
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Sidisheikh.mehriz wrote:
[...]
Sounds like you're on track with that and have thought it through quite thoroughly.Thumbs up

Now I'm eagerly awaiting your results!

Post a new thread in the Advanced Chemistry section and you'll be doing a great deed for the cause of entheogenic autonomy. I'll look into obtaining my own cosmetic grade zinc oxide with a view to replication of your method.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Sidisheikh.mehriz
#167 Posted : 5/27/2021 6:53:48 PM

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Consider it doneWink
 
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