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Author: Subject: cleaning sulfuric acid
jimmyboy
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[*] posted on 5-4-2005 at 14:02
cleaning sulfuric acid


is there an easy way to remove the carbon sludge from the acid besides distilling or centrifuge? any ideas?

thanks
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runlabrun
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[*] posted on 5-4-2005 at 16:27


what conc is the acid?
Carbon sludge? where did you get it from a car battery?
Hmmm if its a car battery i would have thought the crap was lead sulphate....

-rlr
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HNO3
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[*] posted on 5-4-2005 at 18:03


I need to do more experiments, but in my production of Na2SO4 I noticed that when the acid was dilute, the colorant precipitated. Not very energy efficient, but you could try boiling, diluting, decanting, and then concentrating again.
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cyclonite4
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[*] posted on 5-4-2005 at 18:31


I agree with rlr. I haven't actually opened a car battery, but I assume it would be PbO, PbO2, or PbSO4.

It can't be filtered out can it?




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Blackout
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[*] posted on 5-4-2005 at 19:02


cyclonite4, you can't filter out something from a conc. acid with regular filter paper, you need glass fiber ones.

[Edited on 6-4-2005 by Blackout]
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sparkgap
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[*] posted on 5-4-2005 at 21:57


Glass fiber, or if you don't mind long-term safety (like here, for instance) asbestos sheets.

Maybe he can decant if there's a substantial amount of the sludge.

sparky (^_^)




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cyclonite4
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[*] posted on 5-4-2005 at 22:56


Quote:
Originally posted by Blackout
cyclonite4, you can't filter out something from a conc. acid with regular filter paper, you need glass fiber ones.

[Edited on 6-4-2005 by Blackout]


Maybe you should filter it out BEFORE you concentrate it?
And did I ever say use filter paper? No. I just said filter it.




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runlabrun
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[*] posted on 6-4-2005 at 00:57


car battery acid in itself is still to conc to use on filter papers, you could probably dilute it enough to do it tho.
I would think that the best way would be to decant the acid from the sediment sludge... does it form a sediment?

-rlr
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[*] posted on 6-4-2005 at 01:18


CAn anybody tell me what might be put in
Hardware store Sulfuric acid to act as a corrosion inhibitor?
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12AX7
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[*] posted on 6-4-2005 at 04:38


no personal derision.

[Edited on 17-4-2005 by Ramiel]
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12AX7
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[*] posted on 6-4-2005 at 09:32


once more, no derisionary comments.

[Edited on 17-4-2005 by Ramiel]
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jimmyboy
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[*] posted on 6-4-2005 at 12:07


lead sulfate is white - not black - i am guessing the black is from organics that were left in the acid
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[*] posted on 6-4-2005 at 12:41


The black stuff is lead (IV) oxide, also known as lead dioxide. This is no guess :P No really, that black powder was my raw material to start preparing some PbO2 for a potassium perchlorate electrolytic cell, until a really short time afterwards I learnt that it can can be produced by rxn between lead (II) and a hypochlorite. And well yes, some lead (II) sulfate is also present, since it is insoluble (especially in the presence of xs sulfate) but it's colour is white, as already stated.



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[*] posted on 6-4-2005 at 16:39


okay, I've boiled known battery acid and have never noticed much of any black lead compounds present...I think what some of us (or at least myself) are talking about is that nasty black concentrated sulfuric acid drain cleaner you get at the hardware store...does any body know how to seperate the black stuff out efficiently and easily? Using it is much cheaper than draining car batteries, at least for me...I couldnt imagine that it would be lead (IV) oxide...
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runlabrun
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[*] posted on 6-4-2005 at 17:21


Easiest way to get rid of the black crap?
find a different source....
There are many apart from the drain cleaner shit that is just watered down H2SO4... boil it down to get the goods... no problems.

-rlr
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[*] posted on 6-4-2005 at 18:24


Quote:
Originally posted by 12AX7
Quote:
Originally posted by cyclonite4
arrogant?


Hmm, the English language doesn't have a synonym (homonym whatever) strong enough to describe it...

Tim


I'm aware of what you mean by arrogant. I was asking if you were calling me arrogant.


runlabrun is right. Batteries are a crap source. I can't find drain cleaner, but what I found was 'low fume' pool acid. It was a 34% w/v H2SO4 solution. Just boil it down, no filtering. :)
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[*] posted on 6-4-2005 at 18:26


Add some high strength H2O2 to your sulfuric and heat to 150C or so, should oxidize the carbon to CO2 and any dyes too. At least speculating from my arm chair it would seem so.



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[*] posted on 6-4-2005 at 18:33


High strength H2O2?
Thats a waste!

Just find a better source of acid. ;)




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[*] posted on 6-4-2005 at 23:36


Hey guys, cool it. This ain't the place to be slinging at each other. :cool:

I must now ask: wouldn't adding concentrated peroxide cause some of Caro's acid to form? I shudder to even think about boiling it if so...

Why don't we have a "horrified" emoticon?

sparky (>_<;)




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[*] posted on 16-4-2005 at 12:35


Quote:
Add some high strength H2O2 to your sulfuric and heat to 150C or so, should oxidize the carbon to CO2 and any dyes too. At least speculating from my arm chair it would seem so.
Added 50 ml black drain cleaner to 15 ml 12% H2O2, the solution lightened slightly and vigourous fizzing ensued. Little droplets of hot H2O2 released hurt. The solution heated of its own accord and it was placed on a hot plate and put on a low heating setting with magnetic stirring. The mixture turned slighlyt yellow and was fairly clear, I took a picture with a beaker held next to it containing some acid before treatment. Being that the acid was clear and bubbles were still coming up like mad I added some more acid, it cleared up in a few minutes so I added some more, overall 15 ml 12% H2O2 treated a little over 125 ml concentrated acid. After a while the fizzing stopped and heating was discontinued. A fairly clean and simple procedure.

decolorized.jpg - 49kB




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[*] posted on 16-4-2005 at 20:36
Man thats GREAT!


Bromic acid, Let em be the first to congratulate you on a novel yet simple discovery.

It is uncanny how our thoughts cross paths so often at relatively the same time. I went to the Patent Office website earlier this week looking for information on inhibitors for drain cleaning acid. I dug up the following patent that presents evidence to support your claim and expereimental results.US 5,429,764


The patent suggest a fairly wide variety of cationinc and nonionic surfactants. Some fluorinated. Would boiling until white fumes ensue further purify the acid? well, that certainly seems plausable if not quite correct. I was alreay going to get this stuff to dry chlorine gas but now I guess it can prove further useful. Many stores here don't carry it so I found a couple that do and well I was relieved. I am sure the trend is going to eliminate this product soon enough.:(

I hope this patent helps shed light on the mysterious nature of the balck acid dilema.




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[*] posted on 14-6-2005 at 16:15


I tryed the same thing this afternoon. I started with a test tube of 10mL of acid. I then proceded to add 2mL of 25% H2O2. White bubbles and foam formed and then I stirred a bit. Finally I got a super clear product. I then tryed to heat the test tube. It boiled a small amount but I didn't want it to boil over so I stopped.

I noticed after a bit of heating however it started to turn back to a slight brown color.
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[*] posted on 14-6-2005 at 17:03


Quote:
Originally posted by ADP
I noticed after a bit of heating however it started to turn back to a slight brown color.


Could be ferric iron. Iron, common as it is, wouldn't be too suprising.

Tim




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[*] posted on 14-6-2005 at 18:40


An additional note on decolorizing H<sub>2</sub>SO<sub>4</sub>, I have found so far that nearly any strong oxidizing agent works in my case. When I use my black drain cleaner acid in my apparatus to produce chlorine gas by dripping it from a separatory funnel onto Ca(OCl)<sub>2</sub> the chlorine inevitably bubbles up through the acid when the stopcock is opened and as a result the acid becomes discolored ending up as off yellow from a starting color of dark brown/black. Also it should be noted that the acid I have contains any of a number of buffers and corrosion inhibitors, in all concentrations even after treatment with by boiling with H<sub>2</sub>O<sub>2</sub> the acid refuses to attack steel wool appreciably even after 24 hours in it, this is at dilute concentrations or moderate concentrations so it is some messed up acid, I really need to distill it.

Which brings me to greenyppol’s thread that was closed earlier, as I stated in another thread I have distilled drain cleaner and I plan to do so again. However it is imperative to have good stirring and above most else there must be some heating element on the top of the boiling flask/still head to prevent water from condensing and falling back into the drain cleaner during the early stages, otherwise each drop hits and causes a violent reaction bouncing the flask and shooting liquid up and sometimes into the condenser. This is similar to the setup for the decomposition of ammonium nitrate to yield N<sub>2</sub>O, the upper part of the flask is heated to prevent water from dripping back into the reaction flask which gives higher concentrations of side products. Anyway, just some notes.

Also, ADP, I didn’t get any additional discoloration on heating which was what I did to ensure the decomposition of the H<sub>2</sub>O<sub>2</sub> and to drive off some of the water, however as 12AX7 said Iron could be a possibility or maybe some organic matter from one source or another started to oxidize, something in the system unaffected by the H<sub>2</sub>O<sub>2</sub> at the lower temperatures maybe. One other thing ADP, how much did your reagents heat on mixing?




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[*] posted on 14-6-2005 at 18:59


Is the clearing of the acid a direct result of the H<sub>2</sub>O<sub>2</sub> or from the formation of a 'pirana solution'? I forgot almost all the information about it and where I heard it. A search of the forums yielded nothing. Can somone elaborate on this?
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