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Author: Subject: H2SO4
catfish
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Tim-
thx for the tip on CaSO4>SO2! What temperasture does the salt decompose...wait never maind I got it, wtf? Over 1193'C? That's not real practical.

[Edited on 3-9-2005 by catfish]
12AX7
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Heh yeah, all the alkaline earths have high decomp temps. Mg is around 2000°F = 1100C, Ca seems to start around there and slowly complete up to absurd temperatures (1400C?). The lowest temperatures appear to be the transition elements from Fe (or so) to Zn.

Hmm Mn can hold a lot of sulfate ions, no? That might be a better SO3 holding device

Tim

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chloric1
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I have an ebook I loaded from this forum that states antimony sulfate decomposes to sulfur trioxide at a fairly low temperature. The Handbook gives a straightforward preparation of antimony sulfate. I believe it is an anhydrous salt as well making the SO3 isolation less tedious.

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The_Davster
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Which handbook is this? I have some antimony powder so I could potentialy give this a try, but antimony is rather difficult to dissolve.

EDIT: All Sb dissolves in is aqua regia and HNO3/tartaric acid mix(I wonder the mechanism for that disolution...)

[Edited on 4-9-2005 by rogue chemist]

((Blasta))
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 Quote: Originally posted by Fleaker Would it be possible to use a centrifuge to separate the dye from the acid? (referring the cheap black drain cleaner)
Have you not tryed to buy the professional drain cleaner at Janitorial Supply places? Man, its pretty much an over the counter thing without any kind of paper work. The acid is 93% usually, with several varieties of Rooto and Drain Clean-O at 96.5%-98% H2SO4!! The black stuff is heavily dyed and doesn't usually seperate out and I think the percentage of acid is only 60% If I remember clearly.

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chloric1
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The cheap black stuff I bought is 90%. If diluted with water the black separates. It is charcoal. I get crystal clear dilute acid but why trouble with the boiling scenario. Would like to try rooto or that stuff labeled "liquid fire". Any case any of these would be satisfactory for drying chlorine or other gasses that don't dissolve/react,dissolving ammonium chloride to make anhydrous hydrochloric acid,catalyst in ester or ether prep etc. If you decide to concentrate the dilute acid by heat make sure it boils at 338 degrees C!

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12AX7
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I once made a 50% solution of acid (to have offhand) and it was a little yellowish. I anodized a piece of lead in it and it became colorless. Just thought I'd mention

Tim

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((Blasta))
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Carbon.... humm, thats intersting that it would be in the acidic solution. Wouldn't Carbon be used as a catalyist during the reaction with water? Yeah, I just found some "black" acid drain cleaner and it says in bold letters 90% strength and I guess I was thinking of the "red" commercial drain opener which is only 58.5% H2S04...which can be had at some of the lumber house supply places, like Home Hardware and Home Depot...which is aweful shit and 1.5X the price of the Janitorial Drain Opener.

1L of Home Hardware Drain Opener (58.5%): $12 1L of Janitor's Grade Drain Opener (93.5%):$7.20

------
The Sulfuric Acid that I have is amber in color. I don't know if it is a dye or if it is excess S03 in the acid? When I heat the acid to 130C the color begins to fade rather rapidly and the water by this point dissapears and I lose 5.5% of volume. These are all very good signs...I think.

[Edited on 4-9-2005 by ((Blasta))]

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Fleaker
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Well if it's just carbon then it shouldn't interfere in too many reactions. I was buying the amber colored liquid fire version. I didn't think to check a janitorial supply house for bulk purchase. No reason to buy that now.

Why?

Well I found a source for 18M, reagent grade sulfuric and it's extremely cheap (less than a dollar per liter). Unfortunately, it's only in bulk (as in 15 gallons of it bulk). Group buy I'm thinking? There is a deposit you have to put down to buy the 'keg' (basically a stainless drum with a teflon spout) Now to hope that they'll sell to me.

[Edited on 4-9-2005 by Fleaker]
((Blasta))
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Wow! Cheap...bet your going to need a licence for that.
18M in a drum sized container is really cool, but I hate to see a 15 gallon spill of 98% H2SO4! Talk about a bad day...

[Edited on 5-9-2005 by ((Blasta))]

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12AX7
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You think that's bad? He keeps taunting me about a similarly sized keg of nitric acid!!

Tim

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((Blasta))
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Quote:
Originally posted by ((Blasta))
 Quote: Originally posted by 12AX7 You think that's bad? He keeps taunting me about a similarly sized keg of nitric acid!! Tim

oh great stuff! While I speak I'm making Nitric Acid from my drain opener with Ammonium Nitrate. Damn, its the white fuming kind.... Seems to be going well so far.....no leaks! It is condensing in a pyrex flask so it does have some contamination from the by-products of the reaction. The acid is slightly yellowish and thick like light mineral oil. Very energetic stuff and fumes violently.

use caution---explosives in transport
Fleaker
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Yep and just make sure not to leave it out in the open lest you want all of your nice metal equipment (computers etc) ruined. It's quite as bad as HCl when it comes to rusting things. If I need concentrated nitric of the thick and oily variety, a vacuum distillation @ 10C of NaNO3 and H2SO4 does the trick.

On a side note, I find that heating it to distill over the nitric acid can lead to unwanted nitrogen oxides. I once left the distillation and came back to see a green distillate! Just remember to use an aspirator if you do vacuum distillation of corrosives or else your pump will go bye-bye (without a trap that is).
Quince
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Blasta, if you have a sealed fume hood, you should try to turn the trinitromethane in tetranitromethane. Then mix with stoichiometric amounts of toluene and enjoy.

[Edited on 6-9-2005 by Quince]

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((Blasta))
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I've been able to test my trinitromethane as an explosive. It is quite powerful when mixed with an amine...much more so than standard PLX. I've already added more nitrating solution to my trinitromethane...we will see if the very powerful tetranitromethane forms.

No, mixing toluene with tetranitromethane is quite a bad idea from what I've been told. It kinda like playin' with a liquid which has the same stability as peroxyacetone but has nearly 2X the power as TNT. So, no.... I'm not really wanting to die right now. Besides I have 100 grams of RDX ready to be shaped.

use caution---explosives in transport
Chris The Great
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Tetranitromethane and RDX maybe?

I think that the toluene/TeNMe mixture is more stable than AP, but a little less than nitroglycerin. It has an insane VoD, but dinitrobenzene gives a higher lead block test, at a much lower VoD. TeNMe mixtures are weird, some have insane VoDs but lower power, while some with a 6.5km/s VoD (dinitrobenzene) manage 650 for a lead block test.

Anyway, back to the reguralirly scheduled topic.
Magpie
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I wanted to add my experience with concentrating H2SO4:

I set up for simple distillation at atmospheric pressure with about 75 mL of Rooto that I thought was about 86% based on a crude density meaurement. I placed this in a 250 mL RBF. I used no thermometer or keck clamps on the hot connections as I knew plastic/rubber would get trashed. I wired the condenser to the adapter per Roscoe's advice - this worked well. Per Organikum's advice I installed a trap followed by a water bubbler (submerged 1-2") using Tygon tubing off the vacuum adaptor vent.

Upon heating the straw colored Rooto the acid turned dark brown then light orange. Smoky vapors came off almost immediately upon reaching a boil. When the condensate drops fell back into the RBF mini explosions occured. These were unnerving at first as I thought one might blow out the unsecured glass stopper. I boiled this for about 1/2 hour and only got about 2 mL of condensate.

Since the going was so tough - and I saw the "white smoke" right off I thought I might have grossly underestimated the strength of the Rooto. I stopped and titrated the acid in the pot with standardized NaOH. Results were 35.7 N! So it seems like I had con. sulfuric acid all along and didn't know it.

The single most important condition for a successful synthesis is good mixing - Nicodem
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Rooto

Magpie, that Rooto is some great shit isn't it ? I've never had a problem with it. Even
Polverone recommended it. It sounds like your condensate was mostly water that fell back
into the flask. We all know, of course, what happens when water is poured into concentrated
H2SO4. Given that the acid in the flask was already hot - oh well, take it from there.

I had good luck even with the Roebic stuff despite its black colour. It's just annoying to
look at. I have over a gallon of the Rooto and I'll be using it until it's removed(GOD ! NO !)
from the shelves. I've been looking at the "Misty" brand lately. They claim 93%. It
might be a good idea to stock up on these wonderful sources before the wankercrats
outlaw it completely.

Power comes from the barrel of a gun !
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I also want to add my experience with battery acid

I had about 800 ml at 1.2 grams/ml in a quart jar
and as it boiled away it turned yellow like piss at about 400-300ml

and I accicently left it on the hot plate for 5 hours unattended
luckly the temperature stabilized below the boiling point and now I have about 200 ml of a black liquid with a white material on the inside of the glass

I had done exactly the same thing the day before, and the "white smoke" appeared at about 1/3 the initial volume.
so why there wasn't any "white smoke" at 1/4 the initial volume is a mystery to me. The shed was nevertheless filled with "white smoke" but the acid was obviously stable at that temp and volume.
same black color though.
SAM4CH
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Concentrate H2SO4!?

How can I concentrate 35%sulfuric acid to 90-96% using cast iron "I have an experiment using cast iron cookware but my pan had high corresive points in few hours" and I do not like to use pyrex or other glassware!!!!!!

Sam
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 Quote: Originally posted by SAM4CH How can I concentrate 35%sulfuric acid to 90-96% using cast iron "I have an experiment using cast iron cookware but my pan had high corresive points in few hours" and I do not like to use pyrex or other glassware!!!!!!

You can't. You need silicon-iron alloys, or other acid resistant materials. On top of that heating sulfuric acid in that concentration range tends to generate acid mists that are difficult to absorb and which will trash whatever is nearby.
SAM4CH
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I have read an article which talk about using cast iron "Pauling boiler and process for the concentration of sulphuric acid" patent No. 4857281, please advise!
and what about specification of silicon-iron alloy used for concentrate H2SO4?

Sam
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Seeing as you are reading patents, see US4032622 - 1977-06-28 "method of concentrating sulfuric acid using a boiler of improved cast iron"

Patents often omit much information "know to practitioners of the art". However both of these patents do mention "acid of greater than 70%" as the starting point, suggesting that perhaps cast iron does not do well with more dilute acid. Another bit of information is that lead resists sulfuric acid up to strengths of around 80%. Put those together, see why maybe cast iron cookware does not do well with 30% acid.

On the small scale glass and ceramics are your friend, except around acid fluoride. It is possible you might be able to use non-stick cookware, provided the coating is intact - ie new.

When boiling sulfuric acid open containers are not your friend. Picture tiny droplets of sulfuric acid drifting about. Imagine what they can do to your stove top, your clothes, your skin, your lungs. Now go back and look at what a "Pauling boiler" looks like, then search for images of "flask".
SAM4CH
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Can I use silicon iron alloy which used in electrical transformer as electromagnetic plates around the copper coils???!!
12AX7
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If you can melt and cast, or forge weld, it into a sealed pot...sure...

Tim

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Electronic Design, from Concept to Layout.
Need engineering assistance? Drop me a message!
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 Sciencemadness Discussion Board » Fundamentals » Reagents and Apparatus Acquisition » H2SO4 Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues   » Detritus   » Test Forum