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Reverend Necroticus Rex
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Registered: 15-6-2004
Location: Right behind you.......
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I don't think you need to add SO3+H2O2 to make caro's acid, i was trying to dissove some lead just today, it didn't do shit in conc.
H2SO4, even with the oxides and whatnot scrubbed off, swapping the H2SO4 for equal parts of acid and peroxide make quite a difference, as my ruined
shirt and burned thumb can attest to.
I shudder to even THINK what SO3 and conc. H2O2 would be liked mixed together,
Nothing I will be going anywhere near anyway.
[Edited on 23-6-2004 by Reverend Necroticus Rex]
The sun is shining on a brand new day
Blackened corpses burn where they were slain
Self-flagellation prompts him to confess, Bless me father, for I made this mess.
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newby
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Caro's acid H2S05, is used in the gold mining industry to remove cyanides, it is very unstable and decomposes quickly with the loss of oxygen,
reverting back to H2S04. For this reason it is made on site. I am submitting a theoretical(because I ha'vnt tried it) process for the cleaning
of discoloured concentrated H2S04 by the dropwise addition of a 50% solution of H202 with stirring to a solution of discoloured concentrated H2S04
from battery acid. The literature states a temperature of 80c, never having tried the process I am unaware if there would be a rise in temperature by
the addition of dropwise amounts of H202, if not, some heating may be required. Theoretically, your discoloured concentrated battery acid, should
turn clear and upon standing any H2S05 in solution, should very quickly revert back to H2S04, obviously you would have lowered the concentration of
your battery acid by H20 and would need to re concentrate. I think you should take a few more precautions when working with corrosive substances,
goggles with side shielding, full face shield, surgical gloves
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Mendeleev
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My acid also turns yellowish, but it is only a slight tinge and it goes away once it cools down, it is only present at 200 C +. Now if you could get
a way to clean drain cleaner that would be something. I believe activated carbon was mentioned as a possibility.
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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Zac
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Registered: 28-6-2004
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Drain Cleaner
Hi, I bought some of this drain cleaner (the black stuff) Tried everything but distilling to get the black stuff out, freezing, filtering, charcoal,
nothing worked, did notice after I heated some and let it cool and poured the contents out that this black stuff had stuck to the bottom of my
flask seems to be some type of charcoal mixed in with it. Kinda thinking about
distilling it at high temp to see what comes over, bottle says it's 96% conc H2S04 inhibited, carbon would be a good choice to screw up the use
of this stuff for anything else
Weighed down By Gravity and lack of freedom, Float and be free.
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BromicAcid
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When I made hydrobromic acid reacently I used 'black' drain cleaner. The solution turned yellow after a bit of heating and a layer of red
floated to the top, seperating from the rest, I should try this with no additives and see if it would work for purification.
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tom haggen
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Hello all,
I have begun a project that involves concentrating my sulphuric acid and storing it. Well a few particles of fuzz managed to get into my H2SO4 and
went unnoticed for a few weeks. However, after a few weeks my acid really started getting a darker yellow. I'm just wondering if this will make
it so I will get poor yields if I try to use this acid in any syntheses later on down the road.
N/A
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tom haggen
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Anyone?
N/A
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The_Davster
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I don't think it will cause you to get poor yields. I am assuming your intended use is nitrations, right? Lots of people use draincleaner for
their sulfuric acid and their yields are still decent, and draincleaner acid is pretty impure. I don't think that a few tiny bits of fuzz
discoloring your acid will suddenly make your acid useless.
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tom haggen
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Ya I guess i'm just over cautious.
N/A
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BromicAcid
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Back when I boiled down my sulfuric acid from battery acid till it 'fumed' I let it sit for quite a bit. From say October till April, when
I came back to it in april a off-yellow precipitate of sulfur was apparent at the bottom. Never figured out exactly why, the acid was clear still and
had substantial dehydrating abilities still.
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The_Davster
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Thats strange Bromic, just today I was looking through some old cleaning supplies at home and I came across some sort of polish(cannot remember what
for) that said it contained sulfuric acid. At the bottom of the bottle there was a crystalline precipitate that was sulfur yellow. BromicAcid, was
your precipitate actually sulfur or just sulfur colored?
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BromicAcid
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I filted off my precipitate and heated it, that was the only test I did, it melted and formed a thick similar to sulfur at a high temperature
(pre-thermometer days). Therefor I assumed it was sulfur, but I could have been wrong.
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MadHatter
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Registered: 9-7-2004
Location: Maine
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Rooto
Polverone, I strongly agree with you on this one. I paid $14 for 1/2 gallon
of the Rooto at my local Ace Hardware. It's the best OTC H2SO4 I've
ever used ! Before I found that I was using the Roebic Drain Flow
that I purchased at Lowes. Despite the carbon coloring it did a good
job. As for concentrating the acid, an Erlenmeyer flask on a hot plate
with a hydroaspirator does a great job. It carries the noxious SO3 fumes
down the drain as well as lowering the boiling point of everything
involved leading to less decomposition of the acid.
The reference to Red Devil Lye as a source of NaOH hit the nail on the
head. I bought 18 LBS when the local Mars Supermarket had it
on sale. I use it for chemistry of course, but in a 5% solution it's also
one of the best degreasing solutions I've used in pressure washing.
Magpie, I get the impression that you're an older researcher such as
myself. Out of curiosity, what is your age ? I just recently celebrated
my 46th birthday. Ah, to the good ole days ! 20 years ago I could buy
red phosphorus with no questions asked. Now I couldn't find the
shit to save my ass !
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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HankeyPoo
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Someone I know, used to work in a automobile repair shop. Just a couple of days after he started working there, someone ordered him to get some water,
during a repair.
He was quite new there, so he found a outlet, and filled a bucket. He brought it back, and the mechanic told him that it was battery acid.
Can you imagine that? H2SO4 from a wall outlet 
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BromicAcid
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I guess this is the best thread on sulfuric acid to put this in, guess what I did today...
I distilled drain cleaner!
Yes, I heated it to boiling, watched the scary wispy white fumes travel though my system and condense, dripping drop by drop into my receiving flask.
It went from almost black to nearly clear, but it scared the hell out of me.
So I guess distillation is another viable method for H2SO4 purification, bring on the black drain cleaner! 
[Edited on 8/9/2004 by BromicAcid]
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FrankRizzo
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Bromic,
Are you sure that it was sulfuric acid that you were distilling over? IIRC, 98% sulfuric acid boils at over 300C.
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BromicAcid
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I had it distilling under vacuum, it was coming over at 238C. It carbonized sugar readily and otherwise appears quite potent. I took some pictures
of the crazy fumes and other strangeness that took place during the distillation, I will post them some day.
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Quantum
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Interesting thead
Believe it or not I still don't have good H2SO4! I am considering boiling it down on the hotplate but I only have a rubber stopper with a hole in
it to make the fumes go away so I think it might melt.
This rooto stuff sounds good. So far I have tried robeic but its dark color prevented me from seeing anything and it got all over filter paper.
What if, what is isn\'t true?
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mick
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battery acid
This is probably well out of date but anyway-
I was reading the bit about mercury from the thermometer.
I have been using these cooking temp probes, some now have a turkey sized ss probe attached to wire so you can keep the box of tricks well away from
what you are doing. The ss seems pretty good for general work but to do corrosive stuff it would not be hard to put the probe in a bit of glass
tubing, sealed with a torch at one end and a bit of PTFE tape at the other. The bit I like is that the ones I use have a max and min recall temp, so
you can tell if there was an exo or endo reaction while you were not looking.
Mick
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FrankRizzo
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What sort of container have you guys been using to concentrate battery-grade sulfuric acid? I would imagine that heating a Pyrex pot to ~300C would
probably destroy it.
Or, has anyone found a decent online source of ACS grade acid? The alchymist and few other places sell 1L of 95-97% for $30 + shipping.
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rift valley
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I've used my 1000 ml heavy duty pyrex beaker, but in a fit of stupidity I cracked it when I removed it from the heat and placed it on the wet
ground. From what I could tell the beaker was not damaged by the acid
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thunderfvck
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I use a 1000 ml pyrex measuring cup (made of glass). This works quite well even though it directly states that the glassware shouldn't be used
for lab purposes. The acid doesn't destroy it. The only way you could really wreck it is by shocking the glass, so it's best to let it sit
on the hot plate and cool down to ambient temperature before removing it. If you're concerned with the strong acid sucking up moisture in the air
(98% H2SO4 is after all can be used in dessicators) you can put a book or plastic whatever over the top. It will cool down more slowly though by doing
this...
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MadHatter
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Glass
I've never had a heating problem with any borosilicate glass. As stated
previously - just let it cool down slowly. If you don't have access to labglass
then pyrex baking dish will work only you may have a harder time getting
rid of the fumes.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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acx01b
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i had a flask a with little crackures, but was far to be borken just looking it you could think was broken but was not, i did many reflux in it never
had problems
but one day i tried to conc. 30 H2SO4 (distillation) : it worked i got the dirty black oil, then i tried to make ptsa refluxing conc H2SO4 with
toluene: worked too, i thought cool i made ptsa..
i used half of my ptsa, and i have let the H2SO4 layer stand in the flask about 1 week... 1 week later the H2SO4 had passed throw the crackure and
the flask was not a flask anymore, the crackure became an escape for liquids, the pyrex and the H2So4 reacted together, maybe the ptsa catalysed the
reaction...
just be carefull with non perfect flask and acids.
finally i founded some 80% H2SO4 -> higher purity than the black oil i got by concentrating the 30%: it is quite brown, but clear... (less than
0.5% impurities)
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chloric1
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| Quote: | Originally posted by thunderfvck
Well I want to Auto Parts Pincourt, my local auto parts supplier, and YES!!
I got 20 L of 35% H2SO4 for $20!
Amazing deal. AMAZING. Thanks Tom, for pushing me to get off my ass. I am now ecstatic. TWENTY LITERS! I'll be able to make like 6 L of high
purity H2SO4, enough for ages. Excellent. |
Oh Dammit! I paid $9 for only 5.77 Liters on Friday! I guess I will shop around more too!
Fellow molecular manipulator
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