The Dry Distillation of Copper Acetate & The Radical Vinegar
The ore was collected from a former copper mine in Sth. Australia. It consisted of a mixture of blue azurite copper and green malachite that are classed as carbonate hydroxides. Azurite Cu3(CO3)2(OH)2 slowly oxidises into malachite Cu2(CO3)2(OH)2 so early painters who used blue azurite for their sky ended up with it pseudomorphing into green.
After crushing the ore to a powder a 600ml cellulose paper thimble was filled and topped with a filter paper seal and glass beads on top to prevent splashing. The thimble was inserted into the soxhlet chamber.
The menstruum is one third rectified red wine vinegar and two thirds distilled water (called in the old system a 6N ratio).
900ml was placed in a 1 litre flask with the soxhlet attached and condensor on top.
Extraction was begun on a Friday with the heating mantle set to 7 during the day and evening for four weeks.
The vinegar was assumed to have been exhausted and upon dismantling there was no smell of vinegar in the upper chamber and only slightly from the flask. The flask had a tan coppery hard coating and the crystal mass was dark green. This was removed en masse and the remaining acetate with distilled water.
After this amount of time the ore in the thimble had decreased in volume by approximately half.
The saturated result was gently evaporated on the sandbath to dryness.
The dried crystals were placed in a 1 litre B34 flask and buried in a pot of sand.
The dry distillation train with its system of three receivers; one- ice cooled; two- the water trap; and three- charcoal filter were connected.
The dry distillation began 7:00 am Friday, just prior to the
9:00 – Bubbles via water trap
10:53- Droplets in the stillhead
11:20- Distillate steady
3:05pm – Heat has been raised incrementally to Hi
5:50 - Dragon body is coppery red, Greenish-white frosty sublimate in stillhead
9:30 – Earlier sublimate mainly disappeared but a reddish powdery sublimate remaining. Condensor quite dry; distillate tinged orangey yellow. Turning down heat.
10:00 – Heat decreased incrementally
12:10am Off. First receiver disconnected to prevent vacuum forming and sucking up water trap.
The dregs or red dragon
The distillate was redistilled becoming darker with heat and concentration. No acetone was detected.
While testing for acetone from the first few drops of distillate using an old silver plated spoon it did this within a short time. Probably reacting with the underlying copper.
The second distillate still had a orange/brown tint with a pH 1.5 and the oily remainder became deep brown.
The second distillate was distilled a third time; the first drops pH 1.5 and clear and the remainder being amber orange with a strong acetic smell.
Distillate of third rectification - Radical Vinegar pH2
The Radical Vinegar of copper can be used on other mineral or metal oxides, hydroxides and carbonates.