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:
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 :
Calcium formate is a water-soluble salt of an essential mineral nutrient with potential for use as a dietary calcium supplement. Formate ion is a product of endogenous and xenobiotic metabolism, but sustained high plasma formate concentrations (such as occur in cases of methanol poisoning) are...
dmd.aspetjournals.org
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 :d
