Progress with the Zinc Acetate Process

Progress with the Zinc Acetate Process

12.2.09… Placed 200g granulated zinc in 1 litre of 25% glacial acetic acid to dissolve over for over a month. 320g of Zinc Acetate crystals were produced which I ground easily to powder.

25.3.09... 50g Zinc Acetate set up in a 2 litre break-apart retort with distillation train and condenser, and gradually heat raised until acetone fog came over retort mouth. Continued for about 2 hours until acetate was exhausted. About 5-8ml of pale yellow distillate collected and a fair quantity of creamy white salt (Zn oxide flowers) was sublimated around the still head.





27.3.09... An extra 40ml. of distillate (mesityl oxide/ isophorone mix) from the Acetone/NaOH process was added to the 5-8ml and used to wash out the retort and condenser of zinc oxide sublimate, and all returned over the zinc ashes caput mortem. The retort head was removed and flask sealed, and mix allowed to digest at 40-50°c. for 5 days.

30.3.09... 50ml. of 25% acetic acid containing dissolved zinc was also added to the digesting mix.



1.4.09... The digest now appears 80% as a dark brown gummy solid with 20% creamy white coralline salt around the edge. I added another 40ml. of 25% acetic acid to the mix after breaking up the brown waxy crust. Then placed onto digestion again for another 4 days.



4 days later more ‘coral’ growths appear.

5.4.09... Now added a new 100g of dry Zn acetate to the mix, fitted the retort head and set up a second distillation, gradually raising the heat over a 9 hour distillation.



This is the appearance at the retort head late in the distillation after 90% of the liquids had distilled over.... swirling ‘fog’ depositing sublimated white to orange Zn salt (oxide?).



Approx. 150ml. of mixed liquid distillate collected, comprising of water, acetic acid, acetone, aldols and zinc salts of unknown proportions. The deep orange oil just below the surface may be the first sign of the oil we are looking for, but I will reimbibe it back over the ash residue this time.



6.4.09... This is the sublimed salt of zinc from the retort head. The remaining metallic zinc ashes (caput mortem) in the flask were finely ground with a mortar and pestle and placed back in the retort flask with the sublimed salt. The 150ml. mixed distillate was poured back over it, plus another 20ml. of distillate (mesityl oxide/ isophorone mix) from an earlier Acetone/NaOH process, and another 50ml. of Zinc-saturated 25% acetic acid. The flask was then sealed and the mix digested at 40-50°c for 2 weeks.

8.4.09... The digesting mix now has swollen x3 times, again looking like a coral reef, all liquids having been absorbed. Another 50ml. of 25% acetic acid was added and digestion continued.

13.4.09... The digestion was set up for for the third distillation and took 10 hours to complete. This time more zinc salt and orange-colored oil was sublimated in the retort head than previously, and 250ml. of distillate was collected, or which about 40ml. was an orange-red oil.





15.4.09... The orange sublimate was collected and added to the distillate, immediately dissolved, and was digested at 40°c for 4 days.



19.4.09... The red oil was separated from the whole distillate in a separatory funnel and then gently distilled in a 500ml. retort to remove acetone phlegm. About 8ml. of clear phlegm distilled off below 80°c, leaving nearly 20ml. of relatively pure and concentrated deep red oil of zinc, our Philosophical Mercury. This oil likely contains dissolved sublimate of zinc oxide, but this may be the key to the action of the PM.



20.4.09... 0.1g. of 24K gold leaf was placed in this red PM oil and macerated at 40°c.

21.4.09... No obvious dissolution of the gold leaf has occurred after 24 hours.

So Nick, why is this oil of zinc is not effective?
Can you suggest why I’m not getting the expected result?

This zinc acetate process was significantly edited/ updated by me, today.

Luce 7
Where did you get that retort. That's amazing!!


MO-1

magnum.opus1 wrote:

Luce 7
Where did you get that retort. That's amazing!!

MO-1

Hi Mag O,
Yes, break-apart retorts are very useful in alchemy, but you likely would have great difficulty finding one off-the-shelf. You need to have a friendly glassblower who does custom work and doesn't charge an arm and a leg. I'm lucky cause I know one who's into alchemy and likes making retorts. The piece in the photo I have had for over 20 years, and made by my glassblower who is still making me stuff. He is Swiss and 76 years old and we talk about alchemy while I watch him working on his glass lathe. Beautiful to watch but unfortunately scientific glassblowers are a vanishing species like too many other species. You may get lucky and find one in Dallas.

Good luck..... Don

Luce this work is wonderful.

You've clearly taken some steps that were suggested in the small excerpt at the bottom of Nick's zinc acetate page. I must commend you on the work, you've certainly done a lot and the photos are great. It's this kind of sharing that makes this forum a great place to be.
It's interesting that you haven't been able to dissolve the gold with this material though, my first guess is that it's too saturated with the zinc oxide to be able to dissolve the gold. Second guess is that it still needs more work (but I'm not sure of this), perhaps the chilling of the receiving flask or top of the retort with ice might help produce more material (not that that is easy to do, I've used a condensation tube for this with ice water and it works somewhat well).
Anyway I was going to suggest that you try to distill this concentrated red liquid off of the zinc oxide (so distill at a temp below where the zinc oxide would sublime) and use what distills over.
If this is the stuff it might be capable of reducing the zinc to something that is changed form the normal oxide but still sublimes when heated strongly, so perhaps it will be left behind as a gum much as gold and antimony would be left behind as a gum after the mercury is distilled off of them.
Once it's separated perhaps the distilled material would do better at dissolving the gold.

So far all I've been able to do in the process is produce a tiny amount of orange liquid and a good deal of the clear liquid you show, this is because I didn't use enough zinc acetate and my flask broke accidentally when I was putting it away one day so I've put it on hold. I've also gotten those growths, oddly they happened on some zinc acetate I left exposed to air (I hadn't distilled it yet though it was just sitting around), they look like little trees :-). I'm going to work more on it shortly and perhaps I can be of more assistance. Even this clear liquid did something to silver (turned it black) after I left it in there for about a month, it was interesting, but of course it's not what we're looking for.

Thank you for sharing the photos, I look forward to posting some of my own when I have some more success with the process. Best of luck with it, I'm sure you're close to getting a working material since it is much like what is described in the literature.

Blessings,

Bill

Blessings to you too, bonifaesh (boniface?)

It’s great to get some feedback from someone who is familiar with the process, and with whom I can have some discussion. Your first and second guesses re why I haven’t dissolved the gold (yet) are the same as mine. It would indeed help to conceptualize alchemically exactly what is happening here, in terms of the roles of sulphur, salt and mercury in the process. I distilled the separated red oil (sulphur of zinc?) below 80°c and about 10ml. of acetone-like “spirit” further separated. Was this “phlegm” or was it the “mercury of zinc” that I maybe should not have separated from the oil?

But like you, my first guess was that it was the zinc oxide, saturating the oil, that I should have removed. I left it in because it was carrying the sulphur (oil) during the sublimation, and I thought it might still be essential to keep this volatile salt of sulphur with the oil in order to dissolve the gold. But it may well be what is preventing the dissolution. So I will use a small retort (250ml.) and, like you suggest, gently try to distill off the oil before the salt sublimes again.

As to the second guess, I well may need more material and to do more redistillations over the zinc caput mortem, with extra feedstock of Zn acetate and acetic acid, which I have, because I will be running low on our red oil, particularly after I separate salt from it.

I haven’t been using extra cooling of the condenser simply because with the big 2 litre open-throat break-apart retort, condensation of all distillates seems to occur very easily and I have had a quite cold ambient temperature in the lab. I remember being encouraged into spending big bucks years ago on an over-the-top dry ice cooling system to get spirit of lead out of lead acetate, but then when I got the stuff, we didn’t know what to do with it. I still have about a litre of spirit of lead on the back of a shelf covered in dust.
Anyhow, it’s great to be working with acetates again and I look forward to some interesting results. I hope others can get hold of some retorts. Any competent glassblower can make a break-apart retort and it shouldn’t cost more than a couple hundred bucks, and will last a long time if carefully handled.

Thanks again Bill for your encouragement.

LVX... Don

Great job on doing the zinc acetate work. I'm stumped as to why your red oil won't dissolve the gold, and the only thing I can think of is this:


Did you use natural vinegar or did you use acetic acid from a chemical supply company? You wrote that you used "glacial acetic acid", which sounds to me like store bought acid, not natural vinegar. It's extremely important you use natural vinegar. Apparently this is not just a simple chemical reaction. But you still got the red oil, so now we know that the red chemical isn't what dissolves the gold like I had suspected.

But if the red chemical has no purpose, then why is it so mysterious and nobody can tell us what it is? When you get the oil assayed, they can't explain the red color. They do offer an explanation of what chemical it is, but there explanation doesn't match the written literature about the chemical properties; ie. the chemical they tell you is red actually can't be red.

Hi Nick,

Thanks for your comments. Yes, I did use 25% chemical supply glacial acetic acid to make my Zn acetate. Looks like I will have to start over with distilled wine vinegar.

In the meantime, I figured I would distill the red oil to separate the salt from it, so I put the 20ml. red oil (minus the gold) in a 250ml. retort and gradually raised the temperature. About 5ml. of clear liquid came over below 100°c. and then pale yellow oil (another 5ml.), and finally deep golden oil passed over up to about 200°c for a total of 15ml. distillate, when distillation was stopped. This left about 5ml. of almost black, tarry residue which immediately solidified on cooling. No sublimation of salt occurred and so it seems that the salt now is found in the deep red-black tar. I thought to myself, is this where the alkahest is to be found now?



*Distilling the red oil to a red tar*

I then thought that if I re-dissolve the dark red tar in some of the earlier volatile spirit (from the whole distillate) and re-distill several times, I could volatilize the tar with spirit. This would constitute the cohobation of Sulphur, Salt & Mercury, I believe, to form the Stone of Zinc.

So that’s what I’m in the process of doing at the moment.

But like you suggest, it may be all in vain, since hey, the red oil may not have the goods, not being made from natural vinegar. But it’s a really cool learning exercise.

luce7,

its a pity to see that all this work didn't result to a philosophical mercury but be sure that this path can lead to one. There are many credible sources mentioning that. Your attempt to "play" more with the distillate and salts is absolutely correct.

Quote :

About 5ml. of clear liquid came over below 100°c.

I believe that this is the ph. mercury you are looking after. Take a look at the "Way of the Crucible" at p. 177.
Speaking about the "menstruum foetens" (the bulk liquid you got):

Quote :

This liquid has the power to dissolve many of the metals, even gold if it is prepared in a finely divided state. By a very gentle distillation, the white wine spirit or aqua ardens will separate and come over at about 56 deg C. [...] This liquid represents the Philosophical Mercury of the metal.

If you still have those 5ml put them on some Sol leaf

I trust Robert Bartlett to the last "t", lol !

Wow, Foolish One,

That new alchemy book by Robert Bartlett is hot!
Thanks for putting me onto it. I didn’t know he had published a new, more advanced volume. Lots of enlightening practical hints and more.
The section on the Acetate Path of course is particularly relevant.

I notice that on p.152 we find.....”saith Ripley, I will teach you a general Rule: If you would make the white Elixir, you must of necessity divide your Tincture (the Blood of the Green Lyon) into two parts, whereof one must be kept for the red Work, but the other distill’d with a gentle Fire; and you will obtain a white Water, which is our white Tincture, our Eagle, our Mercury and Virgins Milk....”
This extract throws more light for me on the rectification.

Then on p.177, as you quoted, Bartlett expands and is more specific.
Great information for me.

And it just so happens that I had also taken that clear 5ml aqua ardens together with the pale yellow oil that distilled over immediately after it..... and added another 0.05g. of gold leaf to it to digest at 40°c, 5 days ago.

The gold doesn’t appear to have dissolved, BUT the menstruum has gone from yellow to deep red in 5 days. This sure indicates to me that in fact I am extracting sulphur from the gold and am getting a weak dissolution.

I will try concentrating the aqua ardens further to get a stronger dissolution. This has been a very valuable learning exercise and I now know several ways I could improve my results for starting over with a new process. Thanks again for “The Way of The Crucible”. Everyone should get a copy.

Quote :

The gold doesn’t appear to have dissolved, BUT the menstruum has gone from yellow to deep red in 5 days. This sure indicates to me that in fact I am extracting sulphur from the gold and am getting a weak dissolution.

I guess so, you extract Sulfur. It is a strongly positive observation.
I suggest also to try circulate/cohobate the aqua ardens on your leaf. Attempting to recover it by distillation for further use would be a nice idea in order to avoid making it again from the begining.

theFool wrote:

I guess so, you extract Sulfur. It is a strongly positive observation.
I suggest also to try circulate/cohobate the aqua ardens on your leaf.

Currently this is exactly what I am doing, using a long neck above the flask at 50°c. However, last night the glass stopper blew off the top of the tube and I would have lost subtle spirit. I thought I had secured it well, but no. C'est la vie. But most of the volume is still there. I will persist.

Thank you for your interest.

i have recently found myself blessed enough to have come into everything necessary to begin this process, so that i have.

over the course of a day, i collected 200 pennies all newer than 1982. i set out a bowl of some soapy water and washed every penny by hand, and then rinsed them all several times to make sure they were as clean as possible. please bear in mind i do not have any sort of laboratory equipment available or a real space to call my own. i found some vinegar bottles in a local co-op that are identical to beakers, so i bought them for the bottles. the vinegar inside had a preservative, potasium something-or-other, so I emptied the bottles and cleaned and dried them well. i bought a bottle of Heinz distilled white vinegar to use in the process. Nick said to score the sides of the pennies, so, figuring that i only need to expose as much surface area of the zinc as possible to the vinegar, i used 2 pairs of pliers to basically twist up, scratch up, and cut up every individual penny so that they looked as much zinc as copper. i put 100 pennies in each of 2 bottles i purchased, poured the vinegar in, and sealed the bottles air-tight using a layer of plastic wrap over the glass top with the plastic lid screwed on over it. i wasn't sure whether or not it would be faster to shake the pennies around on every once in a while or leave the bottle sit, so there one bottle i've been shaking periodically, while the other i have let set. it's been digesting for about 24 hours now, still dissolving, and i will have pictures on as soon as a camera becomes available. i intend to crystalize the zinc acetate into a different jar, clean these 2 out, and make them into a distilling system. i will drill a hole maybe 1/8" into the cap and put a rubber seal around it, and then i'm still waiting for a glass blower to make me a glass tube to attach to the bottles to make a distilling kit. he has things to do for a week, and then he'll make whatever i need. god has truly blessed me, i am eternally grateful.

Quote :

And it just so happens that I had also taken that clear 5ml aqua ardens together with the pale yellow oil that distilled over immediately after it..... and added another 0.05g. of gold leaf to it to digest at 40°c, 5 days ago.

Try separating the clear ardens from the pale yellow oil by quickly changing the receiver flask when you are distilling the liquid, and I bet the clear liquid will dissolve gold leaf, or at least extract a deep ruby red fire from the gold, which you can use to make the stone.

If you are able to again distill the clear solvent from the red gold oil, then you can digest the oil alone and it should change through the colors. But some say you should leave the solvent in with the gold oil and it will finish the stone much faster, and with multiplications the same applies. Doing the multiplications by just digesting in the water bath to make the stone an oil, then back in the sand bath to harden is a much slower way, and if you simply digest the red oil with the mercury solvent, you will complete it much faster.

NDC wrote:

Try separating the clear ardens from the pale yellow oil by quickly changing the receiver flask when you are distilling the liquid, and I bet the clear liquid will dissolve gold leaf, or at least extract a deep ruby red fire from the gold, which you can use to make the stone.

If you are able to again distill the clear solvent from the red gold oil, then you can digest the oil alone and it should change through the colors. But some say you should leave the solvent in with the gold oil and it will finish the stone much faster, and with multiplications the same applies. Doing the multiplications by just digesting in the water bath to make the stone an oil, then back in the sand bath to harden is a much slower way, and if you simply digest the red oil with the mercury solvent, you will complete it much faster.

Thanks for the tip Nick....

I am following your suggestions via 2 experiments :
Firstly the current digestion which has been going for 2 weeks (clear 5ml aqua ardens together with the pale yellow oil that distilled over immediately after it plus 0.05g. of gold leaf, digesting at 50°c.) .... this has now become a beautiful deep red and is clearly extracting sulphur.

Secondly I have distilled (sweated) at 30-40°c. more clear ardens from the original whole distillate and have placed another 0.05g. of gold leaf in this alone to digest and see if this also will dissolve or extract red fire.

Cheers.... Don

In the first case, following Nick’s suggestion, what I call the true ‘ardens’ (ie. the pale yellow oil/spirit which which was distilled from the 20ml. of red oil) which has been extracting sulphur from the gold leaf, was further gently distilled to separate the most volatile and clear fraction to test if this ‘clear ardens’ alone would extract sulphur from gold leaf, and the answer is YES... this has become obviously deep yellow after 3 days.

In the second case, this so-called ‘ardens’ has had no effect on gold leaf... no color at all after 4 days.

Now what I want to do with this ‘sulphur of gold’ is make a potable gold to imbibe.

I figure that since I only have about 5ml. or less of this probably weak, although deep red and almost solid sulphur (after the clear ardens has been distilled off), then I should make it potable, rather than trying to make a stone.

So my question for Nick is..... Should I add the ardens back to the thick sulphur and do repeated volatilizations until the sulphur/gold comes over with the ardens to volatilize the gold?
I guess this is the way to go.....

Then in your old Alchemy Illuminated website, you state..... “Step 4. Now distill out the Philosophical Mercury solvent using very gentle heat of only 120F, and then gold will remain behind as a gum. Take this resinous gum and put it in a fresh clean distillation system, and heat it until it vaporizes and sublimes in the neck of the apparatus. All that sublimes is ready, and all that remains behind must be treated further with the Philosophical Mercury.”

It will be a waste to ingest the gold oil as is. You need to combine it again with the alkahest you made, and digest it for 40 days in the water bath, and once it goes through the color changes and ends as red, then you will have the elixir of 1st order which is far more powerful than the dissolved gold is.

True potabile gold is the elixir of the 1st order. Gold that is just dissolved by an Alkahest is nearly useless, as Armand Barbult proved to us. He failed to bring his dissolved gold through the transformation process to make it into a proper elixir, so it was never opened, and therefor never made truly available for the physical and astral bodies to utilize when you ingest it.

If Armand had just digested his dissolved gold in his dew alkahest for 40 days, he would have an elixir that could have rejuvenated him to a great extent, and he would have live much longer.

Okay, Nick, thanks for the ongoing advice.

So, I have added all the true aqua ardens back over the thick gold sulphur, distilled it off again, added it back while still warm and then placed it all in a 50ml. flask with tall condensing tube attached and into the water bath at 50°c. for 40 days as suggested.

Assuming this putrefies to black > colors > back to red in 40 days, I guess then I will need to volatilize the gold oil, reduce it to a gum, and finally sublime it to get the final 1st order elixir?

Hi Luce,

I have read all your progress. You often use the alchemical word " VOLATILIZE ". Please, what does it mean and how you do that ?

Thanks.

Hi chercheur,

A volatile liquid (oil, solvent or menstruum) is one which has a very low boiling point or will evaporate (vaporize) very easily.

So to volatilize means to make volatile.

So you can add a volatile menstruum or solvent to a less volatile oil and by repeated distillation of the menstruum, the oil will become more volatile also, and will begin passing over with the menstruum. This is volatilization of the oil.

So thanks for asking and for your interest....... Don

Thanks for your clear explanation,

You shouldn't be using a condenser on the flask. You should have the flask exactly half full, with no condenser.

After the oil is made, then you distill out the solvent, and close the flask with the gold oil in it, and heat it in the sand bath until it becomes a hardened stone. It won't be a gum -- it will be a solid stone, a little grainy at first because it's not multiplied yet.

Nick,

Your helpful comments are noted and are being acted upon.
The saga rolls on!

LVX... Don

Hello brothers, I have been diligently trying to get this oil to dissolve gold, I notice some gold foil did infact break up in this oil I got, but I have never been able to get as much oil as luce7 did.

luce7 how did you do it? wonderful job!!
where did you find the convenient lab stand there for your hotplate? and what kind of flasks are those (in your second pic)?

I would love to come visit you and watch you work, in the meantime I look for alchemists in my own area to help me make this oil



I have recently purchased 50 liters good food-grade red wine vinegar at 10% acidity and am going to put it in the freezer to condense it to higher concentrations... as in http://pwp.netcabo.pt/r.petrinus/vinegar-e.htm

I got 5 lbs of Zinc Oxide to continue to try this path..

Can anyone contact me on Skype? My name is Delphinny
I would love to chat! Anyone? =)

Adam

NDC wrote:

You shouldn't be using a condenser on the flask. You should have the flask exactly half full, with no condenser.
After the oil is made, then you distill out the solvent, and close the flask with the gold oil in it, and heat it in the sand bath until it becomes a hardened stone. It won't be a gum -- it will be a solid stone, a little grainy at first because it's not multiplied yet.

I did follow this procedure and ended with a solid, dried-out red oil with which I made a strong alcoholic tincture (potable gold) and took up to 10 drops daily for over a week. However, I have noted no effects on my body or mind at this stage. I think my 'gold' was far too weak, but I have learned a great amount thru this process and plan a new strategy for my next acetate outing with my new knowledge. Ora et Labore.