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Author: Subject: H2SO4 by the Lead Chamber Process - success
Aqua_Fortis_100%
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shocked.gif posted on 13-11-2007 at 05:44


Some months ago I was just experimentating with this interesting subject.. The first experiment I did was the described in a link posted above ('pop bottle process') . I've used a PETE 2.5 L pop bottle , some sublimed sulfur , KNO3 , 10mL or so of water, and a encurved teaspoon adapted to the lide of the pop bottle.

This is a extremely mess process, because you often became exposed to nauseous SO2. I simply have putted the KNO3 in the encurved spoon and heated with until melted,and the adding the S8 (I've found that is much better doing this than heating both simultaneously,because less sulfur is just burned in open air and hence less is wasted(since when mixed the sulfur ignites pretty fast)) which in turns gave a red-brown melt and ignited instantaneously (but smoothly ;) ) and quickly puting this in the pop bottle.. I did this 10 times(waiting ~30 mins between each burn,and letting some O2 come into the bottle), but sometimes the sulfur-KNO3 melt have fallen in the solution and causing more mess..:mad::mad:

after this , I've filtrated the suspension of sulfur in the acid misture .. then I used the procedure described in a link posted by tupency h. wherein a cooled (-10*C) solution of H2SO3 + O2 can yield H2SO4.. So I've put the filtrate in a container and this in a salt-ice bath for 20mins.. when I back to the place where the solution were standing, I've noted a white precipitate (KNO3 from the mess or any salt formed in situ like KHSO4, KHSO3, etc ¿¿¿)..

This gave me a great grief and foul thinkings :mad::mad:

so I dumped the contents on the cement floor , in backyard..and the stuff made some bubbles and the caracteristic 'whoooosh' from acids on the things.. So , at least this gave me some happy thinkings..:D (however this can also probebly by due by the H2SO3)...:(




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[*] posted on 13-11-2007 at 13:25


Quote:
Originally posted by Aqua_Fortis_100%
Some months ago I was just experimentating with this interesting subject.. The first experiment I did was the described in a link posted above ('pop bottle process') . I've used a PETE 2.5 L pop bottle , some sublimed sulfur , KNO3 , 10mL or so of water, and a encurved teaspoon adapted to the lide of the pop bottle. ...:(


I suggest using a copper endcap instead of a spoon. Less chance of producing a mess of KNO3 in the resulting acid. See http://cavemanchemistry.com/cavebook/chsaltpeter3.html
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[*] posted on 13-11-2007 at 15:49


One last idea i omitted in my prior post. Would using N2O work as well?

Chemkid




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[*] posted on 13-11-2007 at 16:25


Quote:
Originally posted by chemkid
One last idea i omitted in my prior post. Would using N2O work as well?

Chemkid


N2O would definitely not work. The nitrates produce NO2, not N2O.
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[*] posted on 13-11-2007 at 21:45


sorry i've been away so long...

@The_Davster, the water won't flow back into the sulfur burner because its under pressure from the pump. the wick is a good idea, i have yet to attempt to build the burner. i've lit a pile of it outside and it burned quite nicely just in a puddle.

@bilcksneatff, the metabisulfite is a good idea, especially if the sulfur burner turns out to not work... but i don't think i can easily get ahold of any, im not exactly in wine country. and i would guess that its quite a bit more expensive that plain old sulfur. worth a try anyway.

thanks for the input. i'm sure theres plenty more to improve on the overall design. unfortunately it might be a while until i have to time to build one... but i will.

[Edited on 13-11-2007 by 497]
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[*] posted on 13-11-2007 at 21:51


Open the burner to add more sulfur? Power failure? A couple more feet of pipe could prevent a nasty/annoying accident.

I once cast some sulfur around a thick cloth wick for a sufur candle. Whether or not you would like to use cloth is up to you, but a tight coil of some metal mesh would have the same effect without the potential contamination of the produced acid.




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[*] posted on 13-11-2007 at 21:58


you are right, having it run back in would be a pain in the ass. as soon as i have a chance i will test some different designs for sulfur burners.
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[*] posted on 14-11-2007 at 03:14


Quote:
Originally posted by bilcksneatff :
I suggest using a copper endcap instead of a spoon. Less chance of producing a mess of KNO3 in the resulting acid. See http://cavemanchemistry.com/cavebook/chsaltpeter3.html


Yes that's the link I'm refering in the post. I've used the spoon solely because in the time I did the procedure I didn't have ANY copper/iron wire or endcap laying around, and lazy to go to the local (6 km far from my house :mad: ) hardware store... So I've did the necessary improvises..

[Edited on 14-11-2007 by Aqua_Fortis_100%]




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[*] posted on 14-11-2007 at 04:05


Quote:
Originally posted by Aqua_Fortis_100%

Yes that's the link I'm refering in the post. I've used the spoon solely because in the time I did the procedure I didn't have ANY copper/iron wire or endcap laying around, and lazy to go to the local (6 km far from my house :mad: ) hardware store... So I've did the necessary improvises..

[Edited on 14-11-2007 by Aqua_Fortis_100%]


I understand, I was just thinking a copper endcap would be less likely to spill KNO3 or sulfur into your acid.

Quote:
Originally posted by 497

@bilcksneatff, the metabisulfite is a good idea, especially if the sulfur burner turns out to not work... but i don't think i can easily get ahold of any, im not exactly in wine country. and i would guess that its quite a bit more expensive that plain old sulfur. worth a try anyway.

[Edited on 13-11-2007 by 497]


I would check www.midwestsupplies.com/Products/ProdByID.aspx?ProdID=4938

They have a one pound bag of potassium metabisulfite for U.S. $14.50.

[Edited on 14-11-2007 by bilcksneatff]

[Edited on 14-11-2007 by bilcksneatff]
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[*] posted on 14-11-2007 at 04:34


Note that in N America sulfur should cost $1 to $1.50 per pound for garden grade, which should be washed with water to remove (organic) wetting agents before use.

Burning a pound of sulfur will give you about 2 pounds of SO2, while adding acid to a pound of bisulfite will give you less than a pound of SO2.

The trick is in getting a small size sulfur burner to work well.
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[*] posted on 14-11-2007 at 06:12


Quote:
Originally posted by not_important
Note that in N America sulfur should cost $1 to $1.50 per pound for garden grade, which should be washed with water to remove (organic) wetting agents before use.

Burning a pound of sulfur will give you about 2 pounds of SO2, while adding acid to a pound of bisulfite will give you less than a pound of SO2.

The trick is in getting a small size sulfur burner to work well.


One pound S --> ~1.5 pounds SO2
One pound K2S2O5 --> ~1 pound SO2

Didn't really think about it that way!

Quote:
Originally posted by 497
so i decided a batch process would be much more effective. coments?


I thought of another idea. Would 10-15% H2O2 be cheaper for you than HNO3? You can simply bubble SO2 through 10-15% H2O2 to get H2SO4. The only problem I see is the fact that the HNO3 will be regenerated, whereas the H2O2 will not.

[Edited on 14-11-2007 by bilcksneatff]
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shocked.gif posted on 14-11-2007 at 17:51
Upscaling...


This Drawing is my new backyard chamber..(I dont have a cam at the momment, So I did a fast drawing)..This was did quite a some days, and didn't post before together with the earlier posts because of the hurry I'm in..

I've did some simple calculation on gases before the pratice and will present below. Please, if anyone find in my calculations some weird or wrong thing, feel free to tell and correct me..

(I)

Descripition:

PETE bottle is a fairly resistant material against many diluted and weak acids, I often store filtrated battery acid in it without any problem, and also is a fairly inexpensive material to get(usually free if you like drink or 'hunting' in the weird and funny neighbourhood trash).. That's the reason I've did chosen and used this material in my experiments.

My chamber consists of a (more or less irregular :D ) serie of pop-bottles straight on the floor (the generator are also in the same position..My drawing mess up in this also ; be aware to not think the pop-bottles are upside-down in a weird position )and with some wet cloth on it ,( to help cooling the inlet gases). Each of them being connected to the other by means of 8 cm piece of common aquarium tubing and with the help of hotmelt glue.

At one extreme of the chamber, the aquarium tube is connected in a side of a empty kerosene metal can(with some PTFE, to give good seal), which in turns holds a pierced cork stopper with generous amounts of PTFE around it ( to both protect the cork stopper and to improve seal) with an radio antenna Al tubing which is jointed together with a old refrigerator copper tubing (PTFE is used also here, since the temperature, IMO, isn't that great at the point). The copper tubing is connected in the Rojek lid of my 'reaction vessel' ( a tomato 'tin' can ) and some plaster of paris (I just used this because is the most common and the only that I know somewhat..I've great problems with sealing and soldering tubes to vessels (speciallity the first),because the hardware store here recently don't appear to be an friendly place to visit..high prices and very few interesting things). The edges of the tin can were wrapped with some Al foil, to help keep the lid in the correct place(the rojek lid seem to have tiny amounts of a plastic material in it..bad news) and the lid pressured in the place... The holder of the reaction vessel in the drawing is a iron type paraphernalia, but in my experiment was simply 2 common bricks and the alcohol burner under the tin can...

The reactants were impure (CaCO3 - gardening) sulfur ,tap water (10mL in each pop-bottle) and double saltpeter (NaNO3/KNO3,1:1 - without wax additives, which were removed-, which I just considered as KNO3 to dont increase the trouble..)
..

(II)

Consulting Axehandle rxns an overall one can be made, based on the natural sulfur allotrope...

S8 + 16/3 KNO3 --------> 8/3 K2S + 16/3 SO2 + 16/3 NO


S8 => 32.1*8 = 256,8g
16/3 KNO3 => (16/3)*101.1 = 539.2g
------------------------------------------
8/3 K2S => (8/3)*110.3 = 294.1g
16/3 SO2 => (16/3)*64.1 = 341.9g
16/3 NO => (16/3)*30 = 160g

========================

(III)

So, the sum of gaseous products is NO + SO2 , what means 16/3 + 16/3 mols => 32/3 mols of gas

arbitrarily (because neither of my thermometers are reliable to measure) considering the final temp (after passing the last pop-bottle and venting to outdoor) as 30°C, PV=nRT can be used to determine the final volume of all gases in the system:

1*V = (32/3)*0.082*303
V= ~265.02 L

======================

(IV)

Next step is calculating the total volume of all pop-bottles connected to each other...(desprezing minor volumes like the tubing and can volumes,water, etc)..

pop-bottle type: PB Amount: Volume(L):

1.5 L........................3.....................4.5

2.0 L........................23...................46

2.5 L........................1.....................2.5
Total PB: 27 Total Vol: 53

So, by dividing the total vol of the chamber by the arbitrary value found at (IV) we will find the theoretical necessary amount of reactants needed to fill all the chamber:

53L/265.02L = ~ 0.2

so,

16/3 SO2 * 0.2 = ~ 1.067 SO2
16.3 NO * 0.2 = ~ 1.067 NO

Now looking also (II):

If to produce 16/3 moles of SO2 we need 256.8g of S8, what is the amount of S8 needed, if we need only 1.067 mols of SO2 ? AFAIK: x = ~51.4g S8

Doing a similar calculation with the KNO3 we will find: ~ 107.87g KNO3..

So again arbitrarily, I've just cutted the amounts aproximately by half: 25g S8 and 55g KNO3 by shoot...

the results of my experiments I will post tomorrow, because its getting late here.. (the results were very weird at principle..but just funny) :D

[Edited on 14-11-2007 by Aqua_Fortis_100%]

h2so4[1].bmp - 1.8MB




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[*] posted on 15-11-2007 at 12:02


why not do the same thing but in water, like my design? it seems much simpler and easier, not to mention more compact. and if using HNO3 you don't need to screw around with KNO3. and if you do decide to do a gas phase reaction, there are much more effective containers (5 gallon HDPE buckets.) it will be a nightmare getting all those tubing connection to seal, belive me i've been doing alot of that for another project.

H2O2 might should work, but i like the HNO3 better because its not consumed.

on another note, i've had some more success producing HNO3. more details in the thread in technochemistry.

[Edited on 15-11-2007 by 497]
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[*] posted on 15-11-2007 at 17:57


@497, yes your method seems to have much less labour than my one..but you are using HNO3 and this isn't very much OTC in most countries, because of its very interesting and 'popular' properties/uses..;) .. Additionally most people here and in other places wants H2SO4 actually to make HNO3 , not the opposite(well..the lead chamber process can be used just for fun, like my project, or then for real production of H2SO4, which is very hard to worth, because which sulfuric is still a widely avaliable chemical, even if will not be OTC in concentrated form..also is difficult to have near 100% no losses in HNO3 and hence , at a given time you will need to replace some, more on that latter).

Ironically, the initial results of my 'lead chamber' were... NITRIC ACID ! While I've just carefully watching the heating of the rxn vessel, large brown/red clouds evolved during the start and filled the kerosene can , the first and 2nd pop-bottles..I´m very sure that this stuff is NOx, not only by their colour but because also of it foul and toxic smell.. after, when the rxn vessel started to evolve white fumes of SO2, the improvised sealing on the rxn can failed and started to leak out..what forced me to remove the can immediatelly from the heat source and allowing to cool down..inside the can a black boiling mass..

This is weird for me, because the sulfur tends to react in open air with KNO3 in a manner completelly diferent: burning imediatelly and evolving SO2, and I did tried this many times.. but I just thinked before that the KNO3 itself are able to give some oxygen to S8 and start a oxidant/combustible type reaction and burning without O2..,But inside the can the only thing happened was the boiling of the mass (without fire..even when the lid was removed).. So my next try would be adaptating a hose from the aquarium pump to the reaction vessel and allowing lo force some air along it..this will prevent this mess to happen , fire the mix , reduce the nitrate consumption and also give a more homogeneous distribution of the gasses along the bottles..But also maybe requires more volume to work properly, without leaking out too much gasses before they react (which means more bottles attached) or lower amounts of reactants per shoot..


Quote:
and if you do decide to do a gas phase reaction, there are much more effective containers (5 gallon HDPE buckets.) it will be a nightmare getting all those tubing connection to seal, belive me i've been doing alot of that for another project.


497, I didn't found make these plastic connection as mess to do(was even fun!), although the sealing between the metalic, heat exposed parts was a bitc* ..If anyone can advise me about how to give good seal these parts I will appreciate a lot..

And about the HDPE containers, I know most people here like of it, but I insist in several PETE connected together, because ,chiefly , a much more effective reaction area is obtained, whereas using a HDPE container you will have only a tiny area of the liquid at the bottom. And I found experimentally, also by accident, that the surface area of the water is even MUCH more increased when the bottle chamber is exposed to the sun : the water evaporated condenses on whole wall of the PETE containers , creating many tiny drops and huge surface area to reactions take place..



ah... For some reason I'm just happy somewhat with my very diluted < 1-2%(?) nitric acid..maybe because was created too weirdly..




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[*] posted on 16-11-2007 at 18:11


well why don't you just use that nitric you got in my process??? :P but really you have a point, nitric isn't the most OTC.... one reason i'm working on a nitric acid producing apparatus, see: https://sciencemadness.org/talk/viewthread.php?tid=1518&page...

and as for the surface area issue, i agree the PETE bottles will have more. but i think that could be solved by agitating the water in an HDPE bucket. either way you're having fun, and thats what really matters. :D

another thing, i don't think you really need to heat the reaction KNO3/S8 reaction. from what i've read earlier in the thread all you need to do is light the mixture with a lighter and it burns just fine after that. 3S + 2KNO3 --> K2S + SO2 +2NO, etc.

anyone know a good way to measure the concentration of nitric acid? i have a pH/conductivity meter, but i don't trust it's accuracy above very dilute acid.
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[*] posted on 16-11-2007 at 18:24


Quote:
Originally posted by 497


anyone know a good way to measure the concentration of nitric acid? i have a pH/conductivity meter, but i don't trust it's accuracy above very dilute acid.


Titration with NaOH solution(standardize against an acid of known concentration first) using the pH meter as an endpoint indicator.

How accurate is your scale? Density is convenient to measure the concentration of acid. http://www.efma.org/publications/NitricAcid/Section15.asp




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[*] posted on 16-11-2007 at 18:51


Ah, make your own! My large balance is accurate to at least 0.5g, at weights up to 10 kg! A small scale one can be readily made with little more than coathangers. Your accuracy is only limited by measurements on the beam, friction and your test weights.

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497
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[*] posted on 16-11-2007 at 18:58


heh, you just read my mind, i was just thinking about what materials i could find to make something like you describe.

also i just found online some sodium metabisulfite for $2 a pound plus shipping when you buy 23 pounds. thats pretty good, it seems a bit easier than burning sulfur.

23 pounds = 55 mols Na2S205 = 3.5kg SO2 = 5.4 kg H2SO4

pretty good for 50 bucks

and also the resulting Na2SO3 can be made to produce another mol of SO2 by Na2SO3 + 2HCl ---> 2NaCl + H20 + SO2. if you can HCl thats cheap enough.

[Edited on 16-11-2007 by 497]

[Edited on 16-11-2007 by 497]
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[*] posted on 19-11-2007 at 08:53


497, where did you find that Na2S2O5?

This is a random question, but if you burned KNO3 or NaNO3 with charcoal, would you get K2CO3, CO2, and NO?

2KNO3 + 2C --> K2CO3 + CO2 + NO



[Edited on 19-11-2007 by bilcksneatff]
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[*] posted on 19-11-2007 at 12:02


http://www.chemistrystore.com/sodium_metabisulfite.htm

i've never heard of that reaction, i dont know...
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[*] posted on 24-11-2007 at 10:52


Here's something very interesting from http://www.ucc.ie/academic/chem/dolchem/html/comp/h2so3.html...

"Reactions of Sulphurous acid
The solution when heated in a sealed tube at 150 deg.C. deposits sulphur.



3H2SO3 ===> 2H2SO4 + H2O + S


Sulphurous acid can be oxidised by the use of strong oxidising agents.

Oxidising of Sulphurous acid by Oxygen



2H2SO3 + O2 + 4H2O ===> 4H30(ion) + 2SO4(ion)


Sulphurous acid solution is slowly oxidised by atmospheric oxygen to sulphuric acid.


Oxidising of Sulphurous acid by Permanganate ions

When Sulphurous acid is added to permanganate ion which is coloured purple, SO2 will decolourise the MnO4(ion) when it is reduced to the colourless Mn(ion).


2MnO4(ion) + 5H2SO3 + 4H2O ===> 2Mn(ion) + 4H3O(ion) + 5SO4(ion) + 3H2O"
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[*] posted on 25-11-2007 at 10:39


Here is another sulfuric acid making idea that is somewhat close to this thread. I am not sure if this works but here it is....

Na2SO4 + 2CH3COOH --> 2CH3COONa + H2SO4

Would this work?

Chemkid

[Edited on 25-11-2007 by chemkid]




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[*] posted on 25-11-2007 at 10:53


Compare the Ka (acid strength) values for acetic, H2DO4, and HSO4(-). Also think as to which has the lower boiling point and so could be distilled away from a reaction mix.
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[*] posted on 25-11-2007 at 11:14


Quote:
Originally posted by chemkid
Here is another sulfuric acid making idea that is somewhat close to this thread. I am not sure if this works but here it is....

Na2SO4 + 2CH3COOH --> 2CH3COONa + H2SO4

Would this work?

Chemkid

[Edited on 25-11-2007 by chemkid]


I know that it works in the opposite direction.

H2SO4 + 2CH3COONa --> 2CH3COOH + Na2SO4

If it even works at all, it would probably require a lot of energy.
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[*] posted on 16-2-2008 at 13:05


Why wouldn't this work?

SO2 + H2O ==> H2SO3
3H2SO3 ==> 2H2SO4 + H2O + S

Sulphur is burnt in a small container with a little air coming in from the sides, then sealed up when smoke starts coming out and the flame allowed to die..

SO2 is produced and water is at the bottom of the container. SO2 is soliable in water. (See first equation) - or does this need a special temperature. (somewhere between 0-100C?)

There we have H2SO3, this is then placed inside a sealed tube and heated to 150C.

We have a diluted H2SO4 with a little sulphur. Is sulphur solible in Sulphuric acid? If not could it be seperated?

Btw I'm new here but I've been reading through your site with some interest.

I guess what I am asking is.. How is sulphur dioxide disolved in water?


[Edited on 16-2-2008 by Pixicious]
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