Non-Chemical kill two birds one rock, making HNO3, CuSO4, Gold from pins

[butcher]

you pretty much have the picture,
what you are calling a scrubber, is not really a scrubber,
but a collection bottle (to collect and condense the gas (cool back to liquid) gas bubbling these gases in water(H2O2 can help to NO2 gas in solution, and assist to make a nitric acid) this reciever collection bottle is sitting in Ice water bucket, to keep it cold so gas change's to liquid,
after the acid is made in this reciever bottle, the acid is moved to a storage bottle, or used as needed.

I can see where you see it as a scrubber, as a reciver bottle can be used to scrub or destroy the acidic gasses ( called scrubbing the gas), but the chemistry is different in that use of the collector bottle.

a lab beaker, boiling flask, erlenmeyer flask, or a chemistry distilling lab glass rig ( best), can be used instead of old pickle jar, the sand bath is to protect the glass from heat and sudden chenges in temperature, (glass does not like that), I just like the wide mouth of the jar.

the good fitting teflon lid is important if making nitric acid, as nitric will eat rubber and can react with some materials. and hose type is also important, a lab distilling unit would be the best it's joints are ground glass tight fitting,

read it good before trying it and ask questions if you are not sure about something, it is really simple just hard to explain.

 

[golddie]

Hi Richard
Thanks for your help.
I have been reading reading this thread carefully and I find it very helpful
Here are some questions and observations

1)
2NO2(g)
what does the g stand for

2)
you didnt use hcl to drive off the nitric

3)
how much is the amount of water you add to dilute the syrup.

4)

nitric bottle with proper lid put of light in safe place for later use in recovery or refining

what do you mean by put of light

Thanks again

 

[Barren Realms 007]

4)

nitric bottle with proper lid put of light in safe place for later use in recovery or refining

what do you mean by put of light

Thanks again

I think he ment to say out of the light

 

[butcher]

Yes keep your nitric acid from light, it breaks down in light, that is why they use amber bottles (brown bottles) to store it in. even then I keep it in a dark place. (I edited typo in original post thanks for catching that).

(g) in the formula stands for gas.
(aq) is a solution in water

In this we do not use HCl to drive off nitric, that is a different process.
Here we are driving the gas from nitric, with its boiling point, this NO2 and NOx gas is bubbled into the reciever with water forming nitric acid.

Sulfuric acid acts a a dehydrating agent, beside making nitric from fertilizer by giving the hydrogen to the nitrates, and giving the sulfate to the copper.

Copper can help to form the NO2 gas we are using to make nitric acid with, copper also heps to drive these gases out of the boiling flask.

We add just enough water to dissolve the copper sulfate salts when cool, so we can get the gold flake's seperated from the soluble salts of copper sulfate. If we did not have the gold in with the copper we would not need to dissolve them.

 

[golddie]

Here we are driving the gas from nitric, with its boiling point, this NO2 and NOx gas is bubbled into the reciever with water forming nitric acid.

Hi Richarcd
Are you driving the gas off with sulfiuric acid or jus water

 

[butcher]

Goldie, it is only heat that drive's off gas from our boiling solution.

In the boiling vessel we are making a poor mans nitric acid, using the nitrate fertilizer, for this we are adding a sulfuric acid (which will have some water in it), the more concentrated the sulfuric the more concentrated the nitric we will produce, the reason for not using pure sulfuric is we dont need too strong of nitric, about 68% or less.(this is about as strong as we could get it unless we done thing's differently like changing pressure), now this boiling vessel we are also dissolving copper (to get gold off of pins).

there is something call azeotrope and acids and water(concentration) in solutions have certain azeotrope's they will determine the boiling point of the NO2 gas in the solution, and the concentration of the solution will determine which will boil out of boiling flask as gases first,the acid cation, or water
nitric acid and water has an azeotrope of 68% this is why it is sold at that concentration. when boiling a solution with a lower than 68% concentration of nitric acid, mostly water comes out as vapor, and solution concentrates untill it gets to 68% concentration then the ntiric will boil off as NOx gas untill dry. or if we started with a very concentrated nitric say 98% and 2% water, and boiled this the water does not boil out first, if we boil, we boil off NO2 untill solution reaches azeotrope 68% and then if we further boil we still just boil off NO2 till dry. so you can see from this we can not concentrate it to a higher concentration by boiling,(we would need reduced pressure and minimum water in the mix).

Also different concentrations of acid (water) have different boiling points, when we work with these acids and heat, knowing this can help us to know what temperature we need to keep our NOx (cation) in solution or to boil it out of solution which ever we are trying to do.

Sulfuric acid acts as a dehydrator, this means it helps to absorb the water, here sulfuric in solution can help keep water in the boiling flask and our nitric we are making will be somewhat stronger.

To answer your question we are using neither sulfuric or water to drive the gas from solution.
We are using heat, and the boiling point to drive these vapors out of the boiling vessel, (now copper in this solution helps this also, as copper dissolves it releases the NO2 gas from the nitric).
what boils out depends on concentration, temperature, pressure, and the acids azeotrope.

 

[golddie]

Hi Richard
Thanks for taking the time to explain

 

[maynman1751]

One more question Richard. How much H2O, H2O2 do you put in the receiving vessel? What's enough but not too much that it would require less evaporating(not boiling ) to concentrate the resulting Nitric? Would a longer, thinner column of water (vessel) have a tendency to collect more from the bubbling gases? Thanks as always.

 

[publius]

Here is a labware type.

I really find this picture somewhat disturbing. I recall s a story of an assayer who kept the out put end if his mercury retort, under water to collect any Hg vapors that might not have been condensed within the water jacket. One day the gas when out. The retort began to cool and sucked water into the hot end of the retort. Long story-short: BOOM! :shock:

No one hurt. But there could have been.

As long as there is some kind of vacuum breaker on your system there should not be a problem.

Now someone asked about the long(er) column being more efficient. The answer is yes and no. The colder the liquid is the more efficiently it will absorb a gas. The more pressure that liquid is under the more gas can be absorbed. so if you column is 1 meter tall the pressure is greater at 1 meter than it is at 500 cm. If the fluid is chilled to near freezing the greater the absorption is. If you reduce the size of the bubbles the faster they will diffuse into the fluid. Each of these factors has an optimum pressure/temperature/and diameter.

That being said, Because you are relying on pressure developed from a boiling a fluid and then cooling it to condense some component, you may not have enough pressure to push past the pressure developed by the column of fluid (H2O and H2O2 in this case) to even be able to develop a bubble.

Then re-read the first part of my post, for what I expect to happen is something goes awry with the system...

 

[Geo]

my redneck condenser.

 

[kuma]

Hello Butcher , how are tricks?
I hope your well chief!

this reciever collection bottle is sitting in Ice water bucket, to keep it cold so gas change's to liquid,

This is another case of it's so simple , it's genius!
I probably wouldn't have thought of that off of my own back , it's 'lil tid-bits like that that seem to make all the difference , especialy to noobs like myself , so once again thank you chief!
All the best for now , and kind regards ,
Chris :mrgreen:

 

[butcher]

Kuma, thanks I am doing good, we learn tricks from each other.

Geo, very nice condenser, and it is long enough to condense the fume to liquid.

maynman, I use the least water to start I can, as it will develop more liquid in the receiver as it distills.


publius,
yes you are correct distilling this hot liquid and bubbling it into a receiver is very dangerous if not done properly, the boiling flask if heat is removed becomes a vacuum source, and if it is cooled without removing the condenser tube to the cooler liquid this liquid will suck back and hit the hot glass full of boiling liquids and will break the glass.

I am glad you brought up the caution, as the details of the warnings and dangers involved should not be taken lightly, If a person wanted to distill and did not wish to bubble into a condenser, they could, as long as condenser was capable of cooling the gases to liquid, they can then leave the tube open to atmospheric air and drip condensed liquid into the receiver, there would be some gases that may escape, and some NOx gas loss, and it would be safer if you did not pay much attention to details of the process, there are several details of the process that can be dangerous if you do not pay attention to warnings, or how you perform the task, but if you do pay attention to details it can be done safely.

 

[maynman1751]

Geo, what did you use for the center tube on your condenser?

 

[maynman1751]

Butcher, instead of concentrating battery acid could you use 98% sulfuric? If so, how much to balance the recipe?

 

[Geo]

Geo, what did you use for the center tube on your condenser?

i bought some glass tubing from a local neon sign company.its pyrex and melts with a small propane or mapp gas torch. that particular piece is 3/8" and 4' without the bend. i buy it at $2.00 a stick. i got 5 each of 1/4",3/8" and 1/2".

 

[butcher]

I found that some water in the reaction worked better, so diluting the 98% sulfuric would work well.

Again, this is dangerous and requires attention to details:
Always dilute the acid by pouring it into water.

(Never pour water into concentrated sulfuric acid):!:

copper is major player in making nitric acid in this process helping to generate NOx gases, the nitrous oxides need oxygen to convert to nitrogen dioxide gas or the will just bypass the condense and escape the system, the nitrogen dioxide gases need water to convert to nitric acid.

You want to try and get about 60% to 70% nitric acid, other members are much better at the math

Here is how I look at it you will have 40% water in the 60% nitric acid,

0.40 X 6cups = 2.4 cups water

6cups total – 2.4 cups water = 3.6 cups of 98% sulfuric acid

2.4 cups water divided by 3.6 cups sulfuric 98% = 0.6 (60% acid and 40% water)

We could calculate by density and milliliters, but I would try this and see how it worked, my math skills need work, you can test the density of the nitric made to see if you need to adjust recipe.

 

[Topher_osAUrus]

Just had to bump this old thread.

Butcher, you are a brilliant man, and very detail oriented.

I used a combination of this and a couple other threads to set up a type of still/scrubber unit to recycle the HNO3 ive wasted on dissolving copper, but only doing it part way (impatience as a noobile, not letting the reaction finish before adding another bit of acid..

Only problem with this thread, is the title... You, good sir, are getting 3 birds with 1 stone... The nitric...the copper sulfate...and the gold. Three very beneficial things in one fell swoop..

Recycle, recycle, recycle.

 

[butcher]

If you wish to recycle as much nitric acid as possible, remember, the more NO2 gas that leaves the reaction the less nitric you will be able to recover from nitrates.
Diluting a reaction will help, also add a little H2O2 can help, this has been discussed many times on the forum.

I am glad you like recycling or making some of your own reagents.

I have made several post on that topic, many other forum members have very good topics on it.

 

[Topher_osAUrus]

If you wish to recycle as much nitric acid as possible, remember, the more NO2 gas that leaves the reaction the less nitric you will be able to recover from nitrates.
Diluting a reaction will help, also add a little H2O2 can help, his has been discussed many times on the forum.

I am glad you like recycling or making some of your own reagents.

I have made several post on that topic, many other forum members have very good topics on it.

(i couldnt choose color on my phone, but for some reason could make it ridiculously large)

I usually run my acid diluted to cut back on loss of NO2, but i havent tried h2o2 in mt AR or when I run silver in nitric. I believe i read(when i first started my scholastic journey a year ago) of someone adding h202 in the middle of their process (AR-unknown material[at least i dont remember it]) and it caused him some problems.

Was this because he used too much h202 and did not replenish the nitric?

I only use h2o2 to help capture and convert the NO2 gas to HNO3 when i have the still set up...

Although, admittedly, i bought 4 gallons when i was going to the schoom of youtube, thinking i would need it in my AP just as much as HCL....such a fool.. But, you dont know what you dont know until its right in front of you sometimes... If only i would have found this forum before those videos..

Thank you butcher, you are a brilliant man and an absolute blessing to this forum. Your contributions to my learning have no bounds.

 

[butcher]

The only thing that comes to mind is too strong of hydrogen peroxide with silver.

Strong H2O2 can reduce silver, we can use the H2O2 aspect when converting silver chloride using H2O2 and NaOH, to reduce silver chloride to powders of metal silver.

Also using too strong Hydrogen peroxide with silver can be dangerous in some instances, or under some conditions silver can act as a catalyst, giving a violent reaction, (makes me think of a think Jet engine in your beaker of acid.

What I was referring to was a little dilute hydrogen peroxide, 3% for example that is mostly water, and a solution dilute with water. We only need a little peroxide to provide some oxygen to convert the NO gas to NO2 gas, then the water converts the NO2 gas to HNO3.

This is a small example where I will study well before I try something I read, This is basically chemistry we are working with. Some things can get dangerous, if we do them wrong, or we do not know, or understand enough of what we are doing.

I want to be able to understand the reaction or what could happen, or how to use the information I read. Many times we may read a little about something, but do not get the whole picture, or understand all of the possible reactions. in our educated mind we may think we know enough (we read a few pages of info and watched several you tube videos, and we could try something. which may turn out to become a mess, or even worse a dangerous lab accident, a foam over if we are lucky, a possible explosion if we are not, being blinded, or worse, from the glass beaker we had in our hands.

Like reading HCl and nitric acid dissolves gold,We can do that sounds really easy, so we pour some HCl in a beaker, add a gold ring and dump in some nitric, well we could have many problems from here, some of our gold may dissolve as we cough and choke on the red clouds of deadly gas. then we may have other problems not getting much of it to dissolve, or trouble getting it back out of solution... All because we got in a hurry and did not research enough, thinking we done research...

Study everything, and study it more, and keep studying. You can never learn enough in this field of chemistry, and the other arts associated with precious metal recovery and refining.