Non-Chemical 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

 

[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.

 

[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.

 

[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.

 

[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.

 

[qst42know]

Where is that located?

 

[qst42know]

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

 

[Noxx]

I never tried but I will soon.

 

[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

 

[Noxx]

Lol !

 

[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.

 

[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.

 

[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.

 

[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

 

[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.

 

[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.

 

[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:

 

[viacin]

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

 

[viacin]

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

 

[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.