Author Topic: purifying tech. grade H2SO4  (Read 204 times)

poisoninthestain

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purifying tech. grade H2SO4
« on: April 10, 2009, 08:41:21 PM »
Most technical grade H2SO4 solutions are contaminated with additional dyes and metal ions, either from the industrial synthesis process or by the chemical addition by the companies(such as dyes).

All grades can be purified by adding a small amount of H2O2(preferably 30-35%) to oxidize the ions in the solution reducing the pigment color. H2SO4 in a pure state is an almost water-clear color. H2O2 does this beautifully with the addition of heat to provide some activation energy to get the rxn going.

Prepare your H2SO4 solution. I used the glass apparatus below. It's a 500ml FB attached to a stoppered 105 vac. adapter with heavy walled tubing attached at the nipple leading outdoors.

Pour your H2SO4 into the flask and add the H2O2. The molar ratio of H2SO4:H2O2 should be 1:1/50. This can be scaled up or down relatively easily. Pretty much a capful of 35% H2O2 will clear up most of the color of 1000ml con. H2SO4. Feel free to experiment with ratios as they aren't really important. I have tested this and excess is much better than too little, the only thing is the more H2O2 you add the more you'll have to boil off.

Anyways, heat this up. BEWARE as the H2SO4 will release colorless choking odors so make sure you're doing this outside or venting outside(I did all this in my lab  :P).

This is where paths diverge. Some brands are very dark. Some are less so. Mine was a light yellow-orange as seen in the pic below. Typically the darker your H2SO4 is the more the impurities will foam up. Mine hardly foamed as you can see in the pics below...and when it did it was white, innocent looking bubbles.

You'll know the rxn is complete when as your adding heat the bubbles start to form(effervesce), and then more, and MORE, and then finally the foam comes roaring to the top, and then it settles down(all while the heat is still going), and finally dies...lastly, let the whole flask cool down and you're done.

Your purified H2SO4 should be relatively free of color. Mine was a nearly 100% crystal clear. Many thanks to Sedit for the original idea that inspired this writeup.

-PStain.

« Last Edit: April 10, 2009, 08:50:49 PM by poisoninthestain »

Sedit

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Re: purifying tech. grade H2SO4
« Reply #1 on: April 11, 2009, 04:01:27 AM »
Many thanks to Sedit for the original idea that inspired this writeup.
-PStain.

Your mighty welcome Poison.
You like that pretty H2SO4 dont ya? Do drink it now thinking its H2O ;D .

OK, any oxidizing agent will work here to break down the gunk. Theres not much of it but it looks like shit and is annoying.
Some people use Nitric acid to perform the same effect but I always keep some H2O2 on hand so no need to waste my hard to earn HNO3. I also have some improvements I was just thinking of today. I dont know how to test there effectiveness but it seems like a good plan.

When boiling your clear H2SO4 down till white fumes come off(This denotes 98% and up) it would probly be a good idea to throw in some activated charcoal. This will suck up any remnants(~sp?) of organics and probably some of any metals floating around.

How concentrated was your H2O2 poison? Im hoping to get away will good ol 3% as to not waste any (even if it is a cap or two) of my peroxide on this if not needed. Iv always done it with 35% and my H2SO4 looks way shittier then yours before hand but the end result appears the same. I get ALOT more foam then what appears in your picture.

LMAO Honestly tell me,  from now on, what the first thing your gonna do when you get a new bottle of sulfuric 8)....

Enjoy yall.

~Sedit
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You pissed off the wasp now enough is enough!!!

poisoninthestain

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Re: purifying tech. grade H2SO4
« Reply #2 on: April 11, 2009, 05:08:19 AM »
I used 35% H2O2 in the run below.

I tried about 5ml of it on 100ml and it was still tinted so I added another 10 or so and it cleared right up.

I still have to purify the rest of my bottle...so that's what I'm doing tomorrow among other things.  8)

I'm guessing my H2SO4 is ~95% straight from the bottle. I never did bother getting up to fuming. I'll give it a try!

I'm sure this will work for taking out dyes on most other things too. Well, hopefully.


Sedit

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Re: purifying tech. grade H2SO4
« Reply #3 on: April 11, 2009, 07:10:53 AM »
I think next time Im going to do some test tube drop by drop to see how little i can get away with. It takes a moment before it clears up so hopefully Ill be able to add the heat and very little H2O2.

BTW how big/thick/color was the head of your foam? Mine looks like shaving cream sort of. ... but  my liquid lightning is a helll of alot darker then yours. Save that source cause I may been needing it soon.  ;)
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poisoninthestain

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Re: purifying tech. grade H2SO4
« Reply #4 on: April 11, 2009, 02:23:17 PM »
My foam wasn't big at all, maybe a 1/4' high and white like shaving cream mixed with H2O2 bubbles.

Vesp

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Re: purifying tech. grade H2SO4
« Reply #5 on: April 11, 2009, 06:07:29 PM »
You might be able to concentrate H2O2 by freezing out the water, not to sure though if it is very effective. I know it can turn 3% H2O2 into "turn your skin white" H2O2.

Liquid lighting.. Oh I can totally relate to the gunk you are talking about sedit. That was the first drain cleaner I bought, and it was horrible. I decided to just buy a gallon of 93% H2SO4 from a chem supplier instead. It works for most of my needs. I'll have to work on making my liquid lighting better thought. I have a bit of nitric acid I could mix and reflux with it I guess. the nitric acid isn't enough for anything other then dissolve a a bit of metal or making a small amount of NC so its not of much use.
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Sedit

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Re: purifying tech. grade H2SO4
« Reply #6 on: April 11, 2009, 07:10:01 PM »
This is Liquid Lightning vesp...

You know how shitty this stuff normaly looks and its always 93% from the bottle. Now its greater then 98% and looks like this.
The H2O2 cleansing clearly has its place in everyones tool box.


EDIT:

On review I found the product I started with is 43% H2SO4.... But damn look how purdy it is now at 98%
« Last Edit: September 17, 2009, 08:27:24 PM by Sedit »
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Vesp

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Re: purifying tech. grade H2SO4
« Reply #7 on: April 11, 2009, 07:19:06 PM »
Holy sedit! That almost looks cleaner then the stuff I bought from a chem supply! amazing, but does it actually get rid of the impurities, or does it just make the sulfuric acid clear?
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Sedit

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Re: purifying tech. grade H2SO4
« Reply #8 on: April 11, 2009, 07:28:53 PM »
Dunno thats something me and poison where talking about. I would think that if someone skimmed off the foam then it would be like when h2o2 is put on a cut and all the stuff its oxidizing is drawn to the surface as a foam.(The oxygen bubbles are attached to the junk bringing it up).

This would suggest that a skim of the thick shaving like foam and all the bad shit goes away. This would possibly include metals contaminants that are in it.

PS:Keep in mind Vesp that pic does no justice. It even looks a little tinted in that picture... its not.
There once were some bees and you took all there stuff!
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poisoninthestain

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Re: purifying tech. grade H2SO4
« Reply #9 on: April 11, 2009, 07:57:49 PM »
I believe if it foams a lot then a skim could be in order. I think once all the dyes and ionic crap are oxidized you shouldn't have to worry even if they are still present in the H2SO4 solution. Just in case, you can always bring the BP up til fuming 98% which should boil away a fair bit of the remnants.


Vesp

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Re: purifying tech. grade H2SO4
« Reply #10 on: April 11, 2009, 08:06:19 PM »
I don't know if the foam would take out the contaminants, is that a method for purifying things?
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timecube

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Re: purifying tech. grade H2SO4
« Reply #11 on: April 12, 2009, 06:04:51 AM »
I think a lot of the contaminants should be gone, as any hydrocarbons should have been oxidized to CO2 and H20.

It seems like basic distillation should clean it up equally well, but if course it will depend on how hard your crud is to separate from your acid and this way is probably a bit quicker.

Sedit

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Re: purifying tech. grade H2SO4
« Reply #12 on: April 14, 2009, 04:05:22 AM »
I don't know if the foam would take out the contaminants, is that a method for purifying things?

Well when you think about it the foam is formed when the contamination is oxidized so it would be simular to when you pour peroxide on a cut and the foam draws the dirt out. I just did this with a bottle of the worst sulfuric I ever had just for the hell of it. The sulfuric was "virgin" with 12 buffers<-IE JUNK....  It was dark black nasty junk that was over 15 years old. After adding the h2o2 it almost compleatly cleared up with a hint of yellow to it. I wish I took pictures because I was amazed it was able to handle this junk.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

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Re: purifying tech. grade H2SO4
« Reply #13 on: April 14, 2009, 04:11:12 AM »
I guess it would work based on density, or something like that, I just don't see why it would be selective for organic molecules vs sulfuric acid, but I get what you mean with the H2O2/blood thing. This reminds me of the flotation mining or whatever else they do with it to separate stuff.
http://en.wikipedia.org/wiki/Froth_flotation
That has to do with hydrophobic or hydrophilic properties though.
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Sedit

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Re: purifying tech. grade H2SO4
« Reply #14 on: April 22, 2009, 03:33:49 AM »
SOoooo..... What exactly is that thick cloud that comes off of concentrated H2SO4 when its heated to long? Anyone know?SO4
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Vesp

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Re: purifying tech. grade H2SO4
« Reply #15 on: April 22, 2009, 04:56:32 AM »
If I get what you are asking, it is just SO3, and H2O, which obviously recombine forming tiny droplets of H2SO4 in the air.

Ammonium bisulfate something very similiar decomposing into NH3, H2O, and SO3.
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Sedit

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Re: purifying tech. grade H2SO4
« Reply #16 on: April 22, 2009, 05:35:55 AM »
Possibly but it didnt have any sort of irritating oder like I expected. I kept a rag over my face while hurrying to shut every thing off and there was a thick cloud I was in but no burning of the eyes nose or mouth at all like I would expect from vaporizd H2SO4.

Side note: When More H2O2 was driped in it produced huge amounts of Ozone.
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Vesp

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Re: purifying tech. grade H2SO4
« Reply #17 on: April 24, 2009, 10:36:02 PM »
Interesting information about the ozone, are you sure it was O3?

I don't know what it could be then, perhaps some sort of oils they mix with the sulfuric acid?

Another side note: I know electrolysis of some concentration of sulfuric acid can produce decent amounts of ozone.
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Sedit

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Re: purifying tech. grade H2SO4
« Reply #18 on: April 24, 2009, 11:32:26 PM »
Na they explained it to me over at SM.
H2SO5 in concentrated Sulfuric decomposes to O3 in the presents of H2O2 releasing alot of ozone. I was really caught off gard because Iv used so much high voltage that Im very use to the smell of ozone and this was stronger then anything my tesla coil ever put out and thats saying alot.
There once were some bees and you took all there stuff!
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Vesp

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Re: purifying tech. grade H2SO4
« Reply #19 on: April 26, 2009, 08:29:59 PM »
Hmm that could be useful. Good to know Ozone is produced that way. Probably isn't the best way to make O3 though.
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