# Keeping the Genie in the bottle. (controling the BFRC)



## qst42know

To conserve acids and control the (as Steve had described it) the "Big F'in Red Cloud". I was trying to mimic the action of a lab glass condenser without the expense. The lid of the bottle was left on but slotted so no marble could plug it up if the poly net bag the marbles had come in had failed. The net bag has to be melted or knoted shut no staples to contaminate your solution. I kept the marbles wet with a spray bottle throughout an AR reaction. It worked great up to the peak of the reaction when I had to resort to adding a few ice cubes. The ice did dilute the reaction a bit but I consider the experiment a complete sucess. Almost No visable fumes were expelled, with the added benefit of keeping the acids in the reaction I was able to use half of the expected acid to complete the job. As a further improvement and to prevent dilution, I added one of those gel ice packs made for lunch boxes being careful to select one that is sealed not the type that has a vent cap, keep the ice pack upright when in use just in case the seal would fail. 
Keep in mind the fruit jar was a failure it will not take the heat and I almost had a major spill when the jar developed a crack. I now use a commercial coffee pot and a slightly larger top bottle.
This technique could be up sized to any operation to great advantage, cost savings on acids, reduced polution for open air reactions, or far less fumes up the flue.

As a safety note always wash the ice pack thoughly and keep it in a sealed container away from food when you go to refreeze it you don't want to poision anyone.

https://photos.buckeye-express.com/albums.cfm/4302


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## qst42know

Is anyone here using true lab glass condensers to return the nitric to the primary reaction? And is anyone using lab glass (or something else) to collect the nitric for reuse from the boil to a syrup second step? I have yet to come up with a dirt cheap second step condenser. The primary collector cost all of about $7 bucks, ice pack and marbles combined.


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## Noxx

Nah the brown fume you see is NO2, that's not nitric acid. 
If you bubble the fume through water, I'll will make weak nitric acid.


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## qst42know

That is why the marbles were misted with water at the start to collect the NO2. And return it to work on the metals. The ice pack kept the marbles cold, they stayed wet from the warm moist vapors and the acid kept on working. Watching it steadily drip back in was quite satisfying knowing I was getting the most of my acid dollar. Why let it just blow away when you can get more use of it.

It's also more efficent to catch it at the source than a flue based collector as some have contrived.


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## Noxx

Have you see the Hygdogen Peroxide patent ? It states that you can eliminate all NOx fumes. The fumes redisolves in the acid, thus making more nitric acid.


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## qst42know

Where is that located?


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## qst42know

I found the post. Has anyone here used the peroxide technique described? And how did it work.


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## Noxx

I never tried but I will soon.


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## viacin

I just spent big bucus for pyrex brand beakers cuz I was afraid other glasses wouldn't hold up to the heating and acids over time. I have TWO WHOLE CASES of 1000ml mason jars that my sister GAVE me! Too bad they wont work!! I'm glad you told me before I decided to try it. Gah..ooh well, ever since I was a kid I've wanted beakers anyway (Yes, I was one of those kids) 

Great pics btw, really illustrate the point. What size marbles are they? 1" ? and I suppose the colors they use will not come out and contaminate it? Is that a 2 liter soda bottle with the bottom cut off?


Ooh, and BFCR is in the dictonary now! "BFRC Big Freaking Red Cloud "

http://acronyms.thefreedictionary.com/BFRC


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## Noxx

Lol !


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## qst42know

The marbles are from the craft store and are 3/8". I looked for solid colors with no metallic coating. The original experiment was a water bottle on a pint jar. I now use a two liter bottle two ice packs and marbles inside on a commercial coffee pot. Add only part of the expected acid at first.

It helps to have an empty container to hold the top bottle upright when adding more acids or stirring.

Your vapors and foaming in an AR reaction will carry off values, by capturing them you will even recover more gold. The amount is small but so is the plating on some of the materials I collect from.

Save the canning jars for vacuum filtering.


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## butcher

dont see where wet marbles no matter how cool would do much of anything to convert NO2 to HNO3, bubbling NO2 into water will , industrially they use steam or water sprays,
wouldnt subject the chemical bags of cold packs to this the nitrates and plactic is bad enough but the chimical mix can be dangerous if developed leak ect, yes peroxide helps to keep nitrates oxidized in aqua regia at low heat to disolve with but has its limit it breaks down to water quickly with heat to form water vapor,
thin canning glass such as pickle jars can be used with sand baths and proper heating not thermally shocking glass, do not use rubber nitric disolves it, teflon works also the chemical resistant milky clear hard plastic hose(polyviny type? im not sure of ecact name of type I use)
I wouldnt worry about keeping the genie in the bottle, I would let her out and capture her in another bottle, bubbling her through water of coarse.


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## qst42know

Warm moist vapors collect on any cold surface. Doesn't your beer can sweat? A quantity of water is held between each marble where they contact each other. When enough has collected it drips. 

It is no different than bubbling it into a large quantity of water only the amount of water is tiny most of it comes from the reaction itself and the acid is not diluted any more than it already was. It drips right back in to keep working.

The ice packs I use are the hard polyethylene type, fairly inert. The active ingredient is ammonium chloride used for PGM collecting. I don't use ice pack bags.


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## viacin

if this keeps the fumes out of my neighbors yard, and the epa off me, then it's a great idea. The extra nitric acid is a plus


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## qst42know

I know it looks a bit silly, perhaps too silly for the old pros to chime in here.

But it works and works well. The science is there.

Its not a sealed system and there will be some fumes to protect yourself from but not enough to see. There will not be any BFRC to alarm the neighbors. Where privacy is a concern you won't find a more cost effective solution.

Its my understanding that 50% of your nitric acid is driven off as NO and NO2. Collecting it and getting the most from it makes good economic sense as well.


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## butcher

I kind of missundertood what you were trying to accomplish with this.
yes it looks like it would collect SOME of the fumes and convert them back to nitric acid.
I think I would get rid of the cemical cold pack, and why not use ice maybe some mixed with marbles.
My belief there would still be NOX gas from this maybe not seen but still dangerous.
The gas would probaby pass through not mixing with water and air long enough to convert all of it. 
How strong your nitric was in your jar and how fine the metals would determine how much gas evolved.
You still dont want to breath it, or work with it in an enclosed enviroment,or around your neighbors new car.


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## qst42know

Marbles only work until they have warmed. Ice is quickly over come by the heat of the reaction and dilutes your solution. The cold packs are necessary to outlast the reaction. I suppose they could be individually placed in a poly zip lock bag for added protection. 

If you still see the fumes you need a larger top vessel and more or smaller marbles. You want a long meandering path through them.

And you are correct it does not make this operation benign, but it is quite well controlled. 

There aren't any smoke signals to call the troops. :wink:


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## viacin

I will be giving it a try this weekend. I'll post my results.


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## viacin

btw qst, how many 3/8" marbles do you use? do you fill the 2-liter 3/4 full like the water bottle?


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## qst42know

Two of the small ice packs 8oz. by weight. Rough measurements 3x5x1 . squeeze them before you buy to see they are sealed. One brand I stayed away from because they use a vent cap rather than a seal. I weighed the marbles about 3 pounds. Cold marbles from the freezer would help. It works out to about 3/4 or a little better in the 2 liter bottle. A couple spritzes from a water bottle to get it started.

You said you had purchased beakers to work in, plug the pour spout with a cotton ball other wise all the fumes will take the path of least resistance.

After the reaction is finished rinse the marbles into your beaker.


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## butcher

guncotton?


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## viacin

aah yes, the spout. Good advice. Ty for the specs. I don't know how popular this technique is, but it sounds absoutly wonderful. Less BFRC, and more nitric. Which means less worries from the neighbours, and less time spent on production. That is two of my biggest brids solved with one stone. This should be in a book, really.

Frozen marbles above a exothermic solution? You have no problem with cracking or breakage?

but about the cotton.... 
"Nitrocellulose (also: cellulose nitrate, flash paper) is a highly flammable compound formed by nitrating cellulose through exposure to nitric acid or another powerful nitrating agent. When used as a propellant or low-order explosive, it is also known as guncotton. Henri Braconnot discovered in 1832 that nitric acid, when combined with starch or wood fibers [cotton], would produce a lightweight combustible explosive material"

From what I gather, it takes a good soak in nitric acid and sulfuric acid to make true guncotton. But I wouldn't toss the cotton near a flame after I'm done either.


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## qst42know

I have used cotton balls in my test tube trials. Keeps the bugs out and the vapors slight. I never considered they may have had pyrotechnic secondary uses. :wink: I'll have to give that a try. I think you are right about the sulfuric. Carbon, sulfur, and nitrate, would be gun powder after all.

"Frozen marbles above a exothermic solution? You have no problem with cracking or breakage?"

The marbles don't touch the solution just vapors. So I don't believe they will be under much thermal stress. Your reaction will foam up by itself as the heat builds. Don't overfill your beaker, start small till you get a better idea of what to expect. Surprises aren't welcome when dealing with acids.


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## butcher

Good got ya learnin and reading, the knowledge will be useful,in doing and not doin things.


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## viacin

qst42know said:


> Surprises aren't welcome when dealing with acids.



So true. I'm 99% ready, but the strainer I have procured to place my coffee filters in does not fit the container it's going in very well, it's oval and the container is round. Now I learned in kindergarten that this doesn't turn out well, and one wrong move could send a filter full of acid spilling everywhere. I really wanted to get this rolling today, but my time may be better spent shopping for a new strainer. Better Safe Than Sorry

I'm going to look at some other options, see if I can use my funnel. It doesn't fit the filters though, too small. Technical problems at the last minute, as always. :roll:


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## qst42know

As near as I can tell you will be the second person to use a marble condenser. 

If you want to see what you will be avoiding, carefully lift the condenser a bit when your reaction is working strong. The dense red fumes form immediately.

The use of Lab Glass condensers have been around for a very long time. The biggest drawbacks to using these I saw was all your materials must fit through the narrow neck joint of a boiling flask or you had to invest in an expensive wide mouth glass reactor. And they require a source of flowing chilled water.

Hopefully more will adopt the technique as it is a safer, cheaper, more responsible way to use nitric or AR.


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## Oz

When using coffee filters I have found that instead of using expensive buekner funnels that an old coffee pot basket is an inexpensive option. They set well on or into beakers depending on sizes used.


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## viacin

Oz said:


> When using coffee filters I have found that instead of using expensive buekner funnels that an old coffee pot basket is an inexpensive option. They set well on or into beakers depending on sizes used.



Great advice Oz, ty. I was aiming for a plastic seive like in lazersteves videos, but amazingly found my local stores severly lacking. I sent my wife on a shopping exedition and instructed her as to what I required. Unfortunantly either my instructions or her ears are not working. I have learned not to argue which.

The oval-shaped contraption she brought back just falls over when sat on the beakers. I COULD make it work, but the holes are layed out as such that just one wrong move could send acid dripping out. I have decided to wait untill a better container can be found. Your coffee pot basket is my first item of choice. I wish I had just knew about buchner funnels before I began buying everything. That's why I believe we need a good equiptment list.

Why we are on the subject, I found one I like. It has a nylon mesh screen. Is nylon and PP safe to use with nitric acid and, later on, AR?
http://cgi.ebay.com/ONE-1-NYLON-MESH-PERMANENT-BASKET-COFFEE-FILTER_W0QQitemZ360096857509QQihZ023QQcategoryZ20671QQssPageNameZWDVWQQrdZ1QQcmdZViewItem


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## Oz

I would stay away from nylon screen. What you are looking at is an insert to use instead of paper filters in a coffee maker. I was talking about the part of a coffee pot that you put your paper filters in. they usually have ridges to hold the filter out so the sides as well as the bottom can filter. You can find old coffee pot being thrown away at curbside or for a few dollars at a Goodwill Store.


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## viacin

aah, like the image below. That was what I first looked for, but became side tracked with glass funnels. Ty Oz, will try again.

[img:300:300]http://i2.ebayimg.com/04/i/001/12/9f/3f5d_1.JPG[/img]


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## qst42know

A new funnel from the auto parts store in polypropylene can serve pretty well. For about $1.50. Follow Hokes paper folding tips and adjusting to fit the angle of the funnel.


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## viacin

qst42know said:


> A new funnel from the auto parts store in polypropylene can serve pretty well. For about $1.50. Follow Hokes paper folding tips and adjusting to fit the angle of the funnel.




Been there, tried that, the funnel bottom hits the bottom of the beaker. I wanted something more "formal" anyway, but now I'm back down the same old road. I could just cut the funnel's tube off to get by.

It looks like I'm going to have to wait for marbles in the mail. I was forced to order them online. I really do not know what is wrong with the stores around here. Aparently they don't think restocking is good business practice. Come on, how can wal-mart be out of marbles! They obviously do not care for the homemade refining equiptment connaisseur. It really makes me mad when you go to town with a whole page of things to buy and only find three items.


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## Oz

That picture is exactly what I was talking about, you can see how it will rest on or in the mouth of a beaker depending on size. As to the funnels, I don’t care for them unless they are made for filtering with ridges on the sides as only the portion at the hole in the bottom can filter efficiently.


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## qst42know

:lol: Same thing here. I'd bet I had stoped at 7 different stores. I finally found marbles at a fabric/craft store.


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## Pawnbroker Bob

I use an absorption train to keep my gasses in check. It works really well. 

It consists of four equal sized ElM flasks. They are all stoppered with 2 hole stoppers. 3 stoppers have a short glass tube that goes no deeper than the neck of the flask and a long tube that goes to almost the bottom of the flask. The remaining stopper has a short tube and a thermometer or plug the thermometer hole if you don't need it. 

Flask 1 contains the AR and gold heated on a warmer. It also contains the stopper with the short tube and optional thermometer. 

Flask 2 i empty

Flask 3 and 4 contain distilled water and several ounces of sodium hydroxide. (lye)

You want to have no more fluid in 3 and 4 than you have of AR in flask #1. ie: Flasks 1 - 3 - 4 600ml each flask 2 is empty. 

THE IMPORTANT PART!!!! FOLLOW THIS CAREFULLY!!! The orientation and connetion of the tubes is critical!!!
You are dealing with a closed system... the idea is that the gasses given off by flask #1 flows into empty #2 Then bubbles into the lye soultions in 3 & 4 neutralizing the gases. As #1 flask cools a vacuum is created and will suck the solutions from 3 into 2 and 4 into 3. If the stoppers and tubing are not placed properly the solution will get sucked into flask #1 and ruin everything. and or shooting out of flask #4. My reference in numbering is working from left to right. 

OK connecting tubing to stoppers: From the SHORT glass tube from flask #1 connect with hose to the SHORT on flask #2. From LONG #2 to LONG #3, from SHORT #3 to LONG #4. SHORT on #4 ventd to air. To simplify... left to right... SHORT to SHORT, LONG to LONG, SHORT to LONG, SHORT vents to air. 

If you diagram this out you will get the idea. Gas flows left to right and upon cooling solutions flow right to left filling empty flask #2 and emptying #4. The short tube in # 2 keeps solution from flowing into #1 as #2 fills. 

After cooling swirl #2 flask to absorb the remaining gas into the lye solution. There will still be gas in flask #1. Remove the stopper and quickly replace with a sold one. If you have not completely boiled down your AR you can swirl #1 around and the gases will dissipate or remove to outside or a fume hood, remove the stopper and vent. You will find that you will have very little gas to deal with. 

Pawnbroker Bob


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## qst42know

Your system is environmentally responsible neutralizing the acidic fumes in lye. And I congratulate you for reducing the air pollution as a result of your refining.

An improvement to your process would be to add a condenser vertically above your #1 reaction vessel so that the condensate is returned to the reaction to continue working. Reducing the acid required and the volume of liquid wastes.

Your number 2 empty flask collects some condensation till it warms correct? This would have acidic values that could perform more work for you.

Whatever remaining fumes that pass through the condenser could then be bubbled through the lye solution. A system like this could be near 100% fume free.


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## Lou

'Atta boy Bob!!


I'm most impressed by the responsibility that some of us here on the board have. This is going above and beyond the call of duty for a small time operation. My commendations.


We need a hats off to you smiley icon.


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## Pawnbroker Bob

Thank you all for the kudos!  

I have thought about a condenser and it would save some nitric. And yes there is condensation in flask #2. Of course all this is neutralized as the lye solution flows in reverse. 

I should add another important note about the lye. When added to the water ithe soultion is going to heat up. Wait until the lye solutions cool down before putting in the stoppers or you may have fluids running all over the place.  

The system may sound complicated but it is actually very simple and easy once set up. You can use the lye solutions a few times before discarding. I rotate in a fresh flask of lye now and then at #4 moving the used #4 solution to #3. This way I get a litle more life out of them. 

I'm not much of an artist but perhaps I will sketch out what this is supposed to look like and post it. 

I'm sure something like this could be adapted to several 5 gal buckets. With no direct heat using a bucket, very little vacuum is created. Perhaps the AR bucket could vent bubble into 2 others holding lye soultions? Heck put a vent fan on the last lye bucket and a small hole in the AR lid. You could draw all the gases and air throug the solutions. 

PB
"Doing my best for the environment and everyones health!""


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## Anonymous

Having drawn out what you have described PB, you are correct in saying it sounds complicated but is really very simple.

My question here is, rather than discarding the lye solution containing the dissolved and neutralised Noxx fumes, would it be possible to dissolve the Noxx fumes in distilled water and then distill this solution to produce new Nitric acid?


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## Pawnbroker Bob

Hi Marty,

I am no chemist just have some experience. My goal with this set up is to create a high purity of gold and not kill myself, my animals or my neighbors. Reclaiming chems is of no use to me. That being said Noxx bubbled through water will create nitric acid as to purity and strength who knows. You also have chlorine gas being released which bubbled through water creates hydrochloric acid. With both of these compounds with air, heat, and other contams who knpws what kind of strange AR soup will be created in the water. I guess evaporating/distilling this down may produce some type of HCL and HNO3 mixture of unknown concentrations. 

For my purposes fresh AR chems are the only way to go. 

PB


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## viacin

marty said:


> would it be possible to dissolve the Noxx fumes in distilled water



What a awful thing to say. Why in the world would we want to dissolve noxx in distilled water? He's a pretty cool guy, what did he ever do to you.


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## Anonymous

I'll take that one on the chin Viacin :lol: 

PB, good point, I was forgeting about the other fumes involved in AR,
maybe it would be possible when dissolving base metals in Nitric.


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## viacin

lol marty, I couldn't resist. I was speaking of the humble creator of this forum, Noxx. http://goldrefiningforum.com/phpBB3/memberlist.php?mode=viewprofile&u=2

I just couldn't resist


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## Noxx

Ahhahh  Why would one wants to dissolve me ? :shock:


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## Noxx

marty said:


> PB, good point, I was forgeting about the other fumes involved in AR,
> maybe it would be possible when dissolving base metals in Nitric.



Getting back on topic,

If I remember correctly, Hydrogen and NO fumes are not soluble in water in a significant amount.


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## Anonymous

Noxx said:


> marty said:
> 
> 
> 
> PB, good point, I was forgeting about the other fumes involved in AR,
> maybe it would be possible when dissolving base metals in Nitric.
> 
> 
> 
> 
> Getting back on topic,
> 
> If I remember correctly, Hydrogen and NO fumes are not soluble in water in a significant amount.
Click to expand...


Thanks for your response Noxx, if what I proposed isn't possible then thats something I've learnt today. It was just a thought that maybe we could control the BFRG and reclaim and reuse some chemicals rather than dispose of them. At least by using lye the Noxx fumes are controlled and neutralized


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## Noxx

By the way, It is NOx fumes not Noxx...

The x represent a number. Like there are NO2 fumes and NO (nitrogen oxide) fumes.


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## Pawnbroker Bob

Sorry for the insult Noxx! Sometimes my fi9ngers just type random keys.  

PB


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## qst42know

Noxx said:


> If I remember correctly, Hydrogen and NO fumes are not soluble in water in a significant amount.



NO2 forms nitric acid when combined with water. NO is soluble in Nitric acid. Nitric acid is used in commercial scrubbers to collect NO. Nitric acid is also present in the marble collector.

http://mattson.creighton.edu/NOx/NOx_Info.html


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## viacin

I put qst's idea to the test today. I must say it worked wonderfully! My BFRC stoped immediately and the nitric began dripping back down in a matter of minutes. It is simple, easy to set up, and works great. I recommend it to anyone running nitric or AR. It also kept the neighbours from calling the EPA/911, so big A+'s there as well.

Be careful though, your gold can bubble up inside the bottle if you have a vigrous reaction. So don't forget to wash it out over your filter! Also, have another beaker or something handy to place it in while stirring or boiling your solution, as it will tip over.

I give it 5 stars out of 5 and plan to use it for a long time. Maybe once I get set up in a permanent shop I will get a bit more technical, but this is all one needs to control their BFRC effectivly.


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## Pawnbroker Bob

As requested here is a diagram and and instruction of the absorption train.

Enjoy!

PB


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## wop1969

qst42know, now that is what I like to see creative thinking 
That is so simple its better then great. add a fune hood to that and it dont seem like theirs much left to worry about.


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## rainmaker

What, if anything is in flask # 2?


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## qst42know

wop1969 said:


> qst42know, now that is what I like to see creative thinking
> That is so simple its better then great. add a fune hood to that and it dont seem like theirs much left to worry about.



Thanks. I hope to hear how it works for you. 

Though it appears to be a rediscovery of an old technique. After I began using this condenser I have seen one old lab glass cylinder full of marbles on eBay, and another 1 pound lot of tiny marbles from a well known lab supplies company. 

Anyhow it is within reach of anyone wishing to keep fumes under control. I no longer worry when my dogs need to come out where I'm working.


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## qst42know

rainmaker said:


> What, if anything is in flask # 2?



Pawnbroker Bob stated on page three of this thread #2 is empty.


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## wop1969

Pawnbroker Bob 
very clean, simple and effective.

I think I will try both, put a cylinder between flask 1 and 2 that is full of mables and you got the best of both techniqunes 
put flask 4 under a fume hood and life is good (if nothing goes wronge)


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## qst42know

If you are using HCL/CL any condenser will work to reduce fumes.

But if you are using AR approximately half of the nitric acid is driven off as gases. The effervescence (fizz) can carry away PM values. 

If you can keep the marbles above the vessel so that they drip back into your reaction you retain most of the nitric usually lost as a gas and return the PMs to your reaction vessel. 

Before I started using the marble condenser It was common for me to find purple speckles of colloidal gold on the outside of the pot, on the top of the hotplate, and on the work surface. Granted the amounts are small but can add up over time. If you have a filtered fume hood you can collect these values in the filter and process them periodically, but I feel it is more efficient to collect them at the source.


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## wop1969

qst42know said:


> If you are using HCL/CL any condenser will work to reduce fumes.
> 
> But if you are using AR approximately half of the nitric acid is driven off as as gases. The effervescence (fizz) can carry away PM values.
> 
> If you can keep the marbles above the vessel so that they drip back into your reaction you retain most of the nitric usually lost as a gas and return the PMs to your reaction vessel.
> 
> Before I started using the marble condenser It was common for me to find purple speckles of colloidal gold on the outside of the pot, on the top of the hotplate, and on the work surface. Granted the amounts are small but can add up over time. If you have a filtered fume hood you can collect these values in the filter and process them periodically, but I feel it is more efficient to collect them at the source.




Half the nitric, that is allot, no wonder the gas is so bad 
I aggre, collect at the source.
I will run the marble setup on mine at the least


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## hosef

Could you make a combination of the two where the marble scrubber could be combined with the four beakers lye/water solution to neutralize all of the NOx that escapes from the marble scrubber?


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## Noxx

Yes why not ?


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## hosef

Cool, that means that I could have zero fumes and collect back as much of the nitric as possible.


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## qst42know

hosef said:


> Could you make a combination of the two where the marble scrubber could be combined with the four beakers lye/water solution to neutralize all of the NOx that escapes from the marble scrubber?



That would be very similar to the #3 No Air Dilution scrubber GSP described in this post. Though it uses solid materials for neutralizing. 


http://goldrefiningforum.com/phpBB3/viewtopic.php?t=4284&start=0&postdays=0&postorder=asc&highlight=


In small scale I don't know how much pressure the vapors can produce to push through a fluid. Tightly sealed would be even more critical. And you may have to pull it through with some type of vacuum pump to keep it bubbling.


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## Anonymous

Once upon a time for lack of investment capital to purchase Pyrex glassware, I built a reflux condensation reaction system to process organic reactions... The apparatus can be adapted for aqua regia dissolution, then, modified for distillation and recovery of nitric acid with no toxic discharge into the atmosphere...

I originally planned to provide instructions only for the condenser... But my detail oriented system design mentality took over, causing me to put on my chemical engineer hat and delve into the reflux condensation reaction system, finally leading me to providing operating instructions with an emphasis on safety... I'm posting this to the discussion of condensation and evaporation as applied to the aqua regia process... 

In the spirit of Hoke, I hope my composition is understood by the non chemist... 

PARTS:
From Tri-Ess Science Supply in beautiful downtown Burbank... 
1- 20mm X 48" Pyrex tube ... $6.00 ... (will make two condensers and 60 degree distillation insert)
1 - 1 liter Kymax - Erlenmeyer flask $9.50
1- Rubber stopper - w/20mm hole ... $2.00

From Home Depot
10 ft - 10 mm inside diameter plastic tubing ...$4.00
2 - 8/10 mm Teflon wedge fittings ... $1.50 each
1 - Tube kitchen/bath silicon caulk ... $3.50
1 - Evaporative cooler pump ... $ 16.00 (optional)

From beverage supplier 
1 - 2 liter plastic Dr. Pepper bottle $1.00 plus CRV (California Redemption Value)

From Salvation Army store
1 - Used hotplate - $2.50

Assembly instructions...
-Drink Dr. Pepper and rinse bottle...

- Insert 20 mm Pyrex tube through rubber stopper so end is flush with the neck- bottom of Erlenmeyer flask when stopper is inserted... Approximately 1" below the stopper...

-Cut 20 mm hole in bottom of soda bottle, insert tubing in top of soda bottle through 20 mm hole... Bottle will be mounted up-side-down... Allow 4" - 6" between top of stopper and condenser bottle... Scratch Pyrex tube with glass cutter, 4" above inverted bottle... Remove tube from bottle... Support the tube horizontally on both sides of scratch...Tap the scratch from the bottom with metal end of glass cutter while turning the tube... As the tube is tapped, you will see a crack develop... Tap at the end of the crack and follow it around the tube until it snaps in two pieces... Or cut tube with tile saw...Fire polish with propane or Mapp gas… 

Cut holes for Teflon wedge connector in side of soda bottle 2" above the neck and 1 " below the (inverted) bottom… Insert wedge fittings and seal with silicon caulk
Insert Pyrex tube through bottle and seal with silicon caulk... Allow 24 hours for curing...

To supply water to the condenser, the 10 mm intake tube can be connected to a water faucet in a sink and discharged directly into the sink drain or attached to a garden hose and diverted to the tomato patch…

For a portable water supply, attach 10 mm plastic tube from lower wedge connection to a 600 cfm (cubic feet/minute) evaporative cooler pump secured in the upper part of a 5 gallon bucket ... Attach another 10 mm plastic tube from discharge wedge fitting into bottom of bucket to re-circulate the water... 

Water circulates from pump, securely submersed at top of 5 gallon bucket, to lower intake, fills the condenser and discharges at the top, passes through tubing to bottom of bucket... 

To mount the condenser independent of Erlenmeyer reaction flask I drilled a 20 mm hole through the ends of two - 2"X 2" X 24" - pieces of pine... Supports are mounted above and below the condenser, then clamped or bolted to a well anchored shelf unit or work table... 

I can't overstress the critical importance of pre-testing the condenser while it is mounted independent of the reaction vessel... Fill the 5-gallon bucket with cold water, activate the pump and watch for leaks... 
The condenser will supply adequate cooling for up to a twenty liter reaction vessel... In the portable system, the coolant water gradually heats up... The coolant can be changed periodically simply by moving the discharge tube into an empty bucket or diverted to the tomato patch while adding cold water from a garden hose... 

For reactions that use organic solvents, like alcohol or benzene, the Pyrex tube can remain open at the top without losing solvent by evaporation... For acidic solutions, I recommend capping the top of the condenser to avoid losing acid vapor... Or attaching a 20 mm plastic tube at the top and submersing the other end in a water collection vessel...

Nitrogen oxide, NO, is a corrosive gas compressed into a pressure vessel... Nitric acid, HNO3, is nitrogen oxide dissolved in hydrogen dioxide H20 (water)... The balanced chemical equation is NO + H2O = HNO3 ...

When a solution containing HNO3 is heated, the gas, NO is released by evaporation... The reflux condensation system enables one to boil the solution in the reaction vessel, the Erlenmeyer flask... The vapor rises in the condenser tube that protrudes through cold water that circulates through the 2 liter pop bottle condenser... The cold water on the outside of the Pyrex tube causes the acid vapor to condense and drip down to return into the reaction vessel... It’s like an artificial thunderstorm...

When the condenser test is complete, there are no leaks and the condenser, pump, intake and discharge tubes are securely mounted, I recommend testing the system with the reaction vessel filled with plain water... Boil the water by heating over the hot plate... Run the system and monitor the coolant water temperature to get an idea of how often the coolant water must be replaced... Smaller vessels at moderate temperatures (150* to 180 * F.) should run an hour before needing to be cooled ... If you have access to ice, you can cool the water quite rapidly... The reaction flask must be securely mounted independent of hot plate and independent of the condenser, so the hot plate can be removed, the flask disconnected and lowered away from the stopper which enables filling or removing the solution... 

If you haven't operated a reflux condensation reaction, you should run the system two or three times so you become familiar with the mechanics... For me, designing, building and operating chemical systems is just as exciting as completing a pure product... I've had my share of surprises, a tube separates causing coolant to spew on a hot plate, or a crucible of molten metal slips from the tongs causing me to jump and dance to avoid shoes full of molten metal and a 911 emergency… My tiny research lab is located in the garage… Beside the garage I have a 2.5 cubic foot natural gas pottery kiln – 2350* F. It sits beside a 3 crucible capacity smelting furnace built in December 2008 – tested to 2400* F. 

My home is located between two hospitals with 24 hour emergency service… 5/8ths mile each direction… Think about what you are doing before hand and set up the essential equipment so you can safely shut down a reaction... My first and only serious industrial accident occurred in the same garage while I attended high school in 1968… Summer field science/ chemistry, biology and geology… 

Fellow student develops cool contact bombs and graciously shares technology – .25 gram potassium permanganate / .25 g red phosphorous wrapped with a few BB sized granite pebbles in 2” X 2” aluminum foil, the size of a cherry bomb… Device explodes with nice flash-bang when hurled at the ground or a wall… 

Dr. Glazo decides to expand the experiment off campus… He correctly theorizes a bigger bang can be obtained by adding .25 g potassium chlorate… He mixes the first test bomb in garage (95* F)… Holding the piece of aluminum foil in one hand, he adds ingredients with metal spoon, only to discover the addition of potassium chlorate oxidizes at 85* F… Mixture detonates causing 2nd degree burns on both palms… Enough said… Impressive learning experience…

The condenser can be remounted to slope down for distillation... A 6" - 8" length of Pyrex is bent in the middle with Mapp gas torch to a 60 degree angle, annealed properly, then, inserted between the reaction vessel top and the end of the condenser tube... When the AR solution is boiled, the nitric acid condenses as it rolls down the slope through the condenser tube and collected in a suitable glass container... 

With care and caution, this simple apparatus should provide years of service for AR reactions and subsequent distillation...

I'm going to post before catching a few winks... I'll probably modify and update before posting in the equipment category... I look forward to comments, questions and hopefully constructive critique...

Dr. Glazo... 8) 8)


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## yvonbug

All the idea's and info in this one thread! You guys are all great. The reading of all this info is more fun than, uh, well, it's lots of fun! Anyways, I think I'll try the inverted soda bottle with the marbles. I don't really need too much as I'm out here in the sticks. And that seems to be easy and quick. I mainly just worry that my goat will get too much a wiff of the stuff. I can't stand it, why should he? Thanks again guys! You make it fun as well as safe for us backyard refiners! -Yvonne-


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