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AJKOER
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For those having trouble either freezing the SO2 or forcing it into a solution of H2O2 to create H2SO4, I would suggest a closed system approach
involving the convenient generation of H2S from Sulfur and Aluminum scraps.
Caution: Perform outdoors given the broad range toxicity (including skin absorption) of H2S (similar to HCN) that might occur in the event of a leak
and the smell of H2S is usually unappreciated by yours neighbors. Note, H2S gives an initially powerful odor followed by a deadening of ones sense of
smell increasing its ability to induce a fatal dose with a characteristic delayed fatality effect. Have Bleach (NaClO) on hand to neutralize the
reaction if the need arises.
Step1. Heat powdered Al and S to form Al2S3. Avoid exposing the Aluminum sulfide to moisture.
2 Al + 3 S --> Al2S3
Step 2. When ready add water and heat to generate a flow of H2S:
Al2S3 + 6 H2O --> 2 Al(OH)3 + 3 H2S
Step 3. Capture the H2S in H2O2:
H2S + 4 H2O2 --> H2SO4 + 4 H2O
Note, one may find adding an air pump to the H2O2 solution may help in oxidizing the H2S although aeration by itself is known to be effective in only
low H2S concentrations.
Note, insufficient H2O2 yields Sulfur as does treating H2S with NaClO:
H2S + H2O2 --> S + 2 H2O
H2S + NaClO --> S + H2O + NaCl
Step 4. Depending on the hardware design, one could burn any excess unabsorbed H2S in air or direct into a Bleach (NaClO) solution. One could also
collect the SO2 from the H2S combustion for adding to the product of Step 3.
2 H2S + 3 O2 --> 2 SO2 + 2 H2O
Obvious problem with this method (other than dealing with the smell) is the generally dilute H2SO4 formed.
For those lacking a source of Al, heat a mixture of sulfur and paraffin wax to form H2S.
[Edited on 8-9-2011 by AJKOER]
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Gui316
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I've tried to oxidize sulfur in a vaccum flask with potassium nitrate, but it did not worked. Then I tried to oxidize it with calcium hypochlorite. It
worked! I lead it to hydrogen peroxide and it turned yellow...Why? Also, I've split some molten sulfur on my microwave. It have solidified and I don't
know how to clean that mess...Ideas?
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watson.fawkes
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Quote: Originally posted by Gui316  | | Also, I've split some molten sulfur on my microwave. It have solidified and I don't know how to clean that mess...Ideas? |
Toluene. You may have some trouble keeping the toluene in contact long enough to dissolve the sulfur. Be creative. A cloth and
wick-into-reservoir system might work.
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AJKOER
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Mixing Sulfur and Ca(OCl)2 is really only fun to watch and too dangerous to perform oneself. On YouTube:
http://www.youtube.com/watch?v=52wqqz0YKO8
Super heating the Sulfur in the rapid exothermic reaction with Ca(OCl)2 most likely generates Sulfur vapor, some SO2 and perhaps some Cl2 and sulfuryl
chloride, SO2Cl2.
A better and safer idea, make HClO by mixing an aqueous weak acid (capable of forming a soluble calcium salt) with the Ca(OCl)2 Bleaching Powder.
Distill to obtain pure HClO. Add Sulfur to form HCl and H2SO4 per the reaction scheme I previously noted.
Note, Carbonic acid, H2CO3, forms an insoluble CaCO3, so avoid. It is noted that the reaction with Ca(OCl)2.CaCl2 (Bleaching Powder) and CO2 liberates
Chlorine (reference Wikipedia as one source), while Cl2 is not created with the reaction of NaClO and H2CO3, just HClO. My attempt at the reaction
sequence:
H2CO3 + Ca(OCl)2 --> CaCO3 (s) + 2 HClO
Sufficient dilute HCl could also be created from:
H2CO3 + CaCl2 <---> CaCO3 (s) + 2 HCl
So as to produce Chlorine from:
HCl + HClO <---> Cl2 + H2O
[Edited on 16-9-2011 by AJKOER]
[Edited on 16-9-2011 by AJKOER]
[Edited on 16-9-2011 by AJKOER]
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Gui316
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I don't think that HOCL can be distilled. It would decompose. Maybe using a vaccum distillation....But I don't think so. But I'll give it a try. What
acid you think that I should use?
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Gui316
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Just more one thing. You said that burning sulfur in presence of calcium hypochlorite yield sulfur vapors, sulfur dioxide and some sulfur-chlorine
compounds. I've tried to make an solution of calcium hypochlorite and then I add sulfur to it. The reaction takes a while to get going, but once it
does, it is a quite interesting reaction. I think that once the reaction takes place into water, it will not get very hot. Max 100 degrees. That would
avoid formation of sulfur vapors and the formation of sulfuryl chloride, am I right? And...What does sulfur dioxide smells like? I tried to burn it,
and it release a puggent smelling gas...Makes you feel pain in your noise and it actually reassemble the smell of chlorine...or maybe the smell of
nitrogen dioxide...is it correct?
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White Yeti
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| Quote: Originally posted by Gui316 | | And...What does sulfur dioxide smells like? I tried to burn it, and it release a puggent smelling gas...Makes you feel pain in your noise and it
actually reassemble the smell of chlorine...or maybe the smell of nitrogen dioxide...is it correct? |
Did it also sting your eyes? I accidentally got a whiff of that stuff, it burns your nose, it burns your eyes and it will close up your bronchi if you
inhale too much of it. Oh, and it also kills your nerve cells in your nose that allow you to smell, so don't try to inhale it on purpose. It's nasty
stuff, watch out.
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Endimion17
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If you want to know the smell of sulfur dioxide (and you simply must, those are the basics), take a pinch of sulfur and set it on fire for a few
seconds, then extinguish it and disperse the smoke with your hand. You'll notice a "smell of burning sulfur". There's no other better description. It
doesn't smell anything like the halogens or nitrogen dioxide.
You can dissolve some potassium metabisulfite in few mL of water and take a whiff or two. It hydrolizes and produces the dioxide gas.
Given the amounts produced, there's no danger of injuring or killing yourself. At higher concentrations and prolonged exposure (it's easy to
overexpose yourself and get symptoms later), it causes a great deal of pain upon lung dilatation during breathing and induces a shitload of coughing.
Painful coughing. Worse than chlorine. This one just makes you cough and cough, and your bronchi try to close.
Eye stinging comes at even greater exposures, or if a streak of smoke touches your eyes.
It's not very toxic per se, but it is very, very irritating for the mucous tissues, and has somewhat delayed effects.
I was exposed to it for the first time when I was in junior elementary school. My grandpa used it in his vineyard and I remember stricking a match
and, while it was just starting to burn, sticking it into a small pile of sulfur. And then I inhaled. After my bronchi dilated back  , I though to myself: "This is a hell lot of fun!"
Here's a nice set of photos by famous photographer Grunewald at Ijen in Indonesia. I can imagine how their lungs look like. Their teeth corrode, too,
because they use a wet cloth in their mouth to breathe through. Poor people.
[Edited on 17-9-2011 by Endimion17]
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White Yeti
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Those pictures are breathtaking!!
Thanks for sharing.
I warned Gul316, not because sulphur dioxide is excessively dangerous, but because some people are more sensitive to it than others. I'll get a little
personal, but I burned less than a gram of sulphur just to know what SO2 smelled like (and to see a nice blue flame), and a streak of smoke touched
both my eyes and nose. Just that little bit of gas was enough to close up my lungs for several minutes and induce wheezing for several hours
afterward. I have some symptoms of asthma but I never though sulphur dioxide would affect my lungs that much. I was more careful with sulphur ever
since 
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Gui316
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Cannot be worse than chlorine. Chlorine fills your lung with fluid and cut your lung's capacity by maybe 70%. You try to cough, but you can't because
there isn't enough air to cough. Ah well...That is weird, because I've burned sulfur here, and it smell like chlorine or nitrogen dioxide...Something
between both. I'll try to do it with the metabisulfite, if I can get my hands on it. Just more one thing. Burning sulfur in presence of platinum would
yield sulfur trioxide?
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Endimion17
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Oh well, chlorine allows you to crawl on the floor and try to calm down by recovering yourself with small breaths at the time. Sulfur dioxide will
painfully choke you to death and won't let you calm down because you won't be able to stop coughing, and inhaling will be very painful. There's no
accounting for taste.
Either your olfactory system is damaged, or it wasn't just sulfur. The smell of SO<sub>2</sub> does not relate to halogens, which relate
to nitrogen dioxide nd ozone. Those are two distinctive groups. Oxidizers and a reducer. Halogens smell like cleanliness, hospitals and analogue 35mm
film canisters, and sulfur dioxide smells like volcanoes, strucked pieces of pyrite and medieval image of hell.
White Yeti, people with pulmonary issues tend to react more dramatically, that's true.
Yes, photos are amazing. Makes me want to take a small boat and go around the 0.5 pH acidic lake, like this man did.
Metabisulfite is extremelly common where I live. It's usually in regular stores, next to gelatin, vanilla, baking soda, etc. People put it in homemade
jams and grape must. It's a cheap and
great antioxidant.
How would you burn sulfur in presence of platinum? That's not so easy to achieve. Just putting a piece of Pt in a jar with burning sulfur won't help.
[Edited on 17-9-2011 by Endimion17]
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Gui316
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(un)Fortunately we don't have volcanos here in Brazil...I guess that this country is one of the worst countries for those who are in love with
chemistry...Well...Is there any test for sulfur purity? My olfactory system seems to be fine...Well, since my problem with chlorine, i think that I'm
more sensitive to it, but i don't think that it would make me identify chlorine smell from...sulfur. Well, burning that yellow powder really produces
a white smoke that smells like nitrogen dioxide. I'm very disapointed to know that my sulfur is not as pure as I thought that it was...
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