Sciencemadness Discussion Board

H2SO4

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dazvo - 12-3-2003 at 08:43

FeS + HCl = H2S + Cl
H2S + H2O = H2SO4
??????????/
this is rait?????????/

I am a fish - 12-3-2003 at 10:16

Adding hydrogen sulphide to water will merely give you hydrogen sulphide solution (which is weakly acidic).


The equations you give don't even make sense. The two reactions written correctly are:

FeS (s) + 2HCl (aq) --> H2S (g) + FeCl2 (aq)

H2S (g) --> H2S (aq)


Have you any idea how dangerous hydrogen sulphide is? I strongly suggest that you learn some chemistry before attempting any experimentation. If you try to handle hydrogen sulphide with your current level of knowledge you will probably kill or seriously injure yourself.

Chris

Rhadon - 12-3-2003 at 10:35

dazvo, I don't know where you come from, but you might try a translation program like Babylon Translator :).

PHILOU Zrealone - 13-3-2003 at 03:29

To get sulfuric acid or sulfate, you need to oxydise the sulfur in the molecule to a higher degree of oxydation!
H2S --> H2SO3 --> H2SO4
FeS --> FeSO4
Thus you need an oxydiser!
HNO3, NH4NO3, KNO3, O2 depending on the case!

Why search complicated when you have it handy?
H2SO4 is in car batteries (30 to 50% H2SO4)!

Flying Dutchman - 13-3-2003 at 11:46

And offcourse if you need a higher concentration of H<sub>2</sub>SO<sub>4</sub> you can allways just boil it. Boil till white fumes are given off. I know, this is basic information, but if you spell "right" like rait, and giving equations that do not make any sence. Then I doubt that you knew this.

Cappy - 30-3-2003 at 22:42

How concentrated can you get sulfuric acid by boiling it? What about nitric and other acids?

Wouldn't heating decrease the solubility of the gasses?

PHILOU Zrealone - 30-3-2003 at 23:11

HNO3 will not boil well but you will reach an azeotrope mix of 68-69% HNO3 with water!
So strating from dilluted HNO3 you will boil first concentrated HNO3(68%) and then water!

H2SO4 will boil water and H2SO4 with increasing % H2SO4 upon time; thus here the conc H2SO4 goes out at the end or remain in the flask!
Beware of hot gaseous H2SO4/H2O fumes!

:cool:

Darkfire - 31-3-2003 at 16:21

Its likely to see the hno3 decompose before any real percentage is reached. Around mid high 90's can be reached with h2so4.

CTR

PHILOU Zrealone - 1-4-2003 at 16:46

I have never had any HNO3 decomposition while distillating at ambiant pressure in an oil bath!
I have distillated HNO3 conc from HNO3 69% /H2SO4 96% witout troubles and HNO3 conc from NaNO3/HNO3/H2SO4 without troubles eather!
Ok faint yellow NOx on top of the fluid but nothing dramatic!

I have used a glass rod distillator!

:cool:

PHILOU Zrealone - 1-4-2003 at 16:50

Of course the resulting conc HNO3 is white when cold and very pale yellow when hot and fumes a lot in the air.


:cool::cool:

hmmm...

Beanspike - 15-4-2003 at 21:57

Would you be able to boil drain cleaner (the hefty kind with the bag around it covered with warnings) and increase the concentration? or would this be pointless?

madscientist - 15-4-2003 at 22:24

Yes, that will increase the concentration. Typical H<sub>2</sub>SO<sub>4</sub>-based drain opener is about 94% H<sub>2</sub>SO<sub>4</sub>; boiling until thick white fumes appear (which are a mix of H<sub>2</sub>O and SO<sub>3</sub>;) yields 98% H<sub>2</sub>SO<sub>4</sub>.

Organikum - 16-4-2003 at 18:30

Boiling down battery acid (38% H2SO4) works perfect if a Liebig is attached to the top of the flask (no cooling water required) and the outlet is run in a bucket with water. No fumes at all escape.

Only the conc. H2SO4 got this way looks quite dirty, with particles floating around. Anybody knows a easy way to get ridof these impurities? If filtering what kind of filter is advised if you don´t have those nice Whatmans glassfiberfilters by hand?

Problem solved:
Filtered through some pressed glasswool worked ok. No problems.

[Edited on 18-4-2003 by Organikum]

Cappy - 20-4-2003 at 19:11

Could battery acid be boiled in a teflon-coated frying pan? Let me know what you think about using the pan for preparing food afterwards. :P

Also, when boiling H2SO4 and HNO3 and other acids/bases, will water always boil off first before the azeotrope is reached? Obviously a small amount of acid vapors would come off too, but I was wondering if distillation was required, or if simple boiling would work.



[Edited on 4/21/2003 by Cappy]

Ramiel - 21-4-2003 at 02:09

I may be wrong, but battery acid has a lot of impurity in it (mostly Lead). Hence boiling it in a frying pan might get you a fun case of lead poisoning.

Thinking of purifying sulphuric acid…
Could one boil a ‘sacrificial’ batch of acid until it gives off H<sub>2</sub>O and SO<sub>3</sub>
Then pass the fumes through or over either MgSO<sub>4</sub> or CuSO<sub>4</sub> such that you get mostly SO<sub>3</sub> fumes, and then pass these through sulphuric acid to get Oleum.

This just occurred to me, I think I’ll try it tommorow.

Cappy - 21-4-2003 at 18:31

Lol, yeah that would suck. Fortunately, my battery acid is store bought rather than canibalized from a battery.

:cool:

vulture - 21-4-2003 at 21:23

Also, when boiling H2SO4 and HNO3 and other acids/bases, will water always boil off first before the azeotrope is reached? Obviously a small amount of acid vapors would come off too, but I was wondering if distillation was required, or if simple boiling would work.

This depends on which side of the azeotrope you are....

For example, boiling 90% HNO<sub>3</sub> will cause mostly HNO<sub>3</sub> to vaporize till the concentration has reached ~68%.
If you boil 40% HNO<sub>3</sub>, mostly water will vaporize until ~68% is reached.

Once you have reached the azeotrope, boiling won't change anything, because the components will vaporize in the same quantity.

Ofcourse, if you heat it above 70C you'll be left with NO<sub>2</sub>, water and O<sub>2</sub>.

[Edited on 22-4-2003 by vulture]

[Edited on 22-4-2003 by vulture]

Blind Angel - 21-4-2003 at 21:41

Just to know, would it be possible to get anhydrous Sulfuric Acid from common source (like Car Batteries)?

Organikum - 22-4-2003 at 00:42

Cappy, you can boil the H2SO4 also in your open hand! For a very short time. :P

The described setup was for preventing the unhealthy fumes to escape which evolve when the highest concentration is reached. White fumes of SO2, SO3 and other shit. You can do it outside of course if you live in the outback. Poor kangaroos so.

The acid used by me was from the car-supply store and contained nevertheless lots of dirt as showed up by concentrating the acid. The acid from old batteries is stored by me as it is R1ngm45t3r´s favorite drink when he comes over for devastating my ambiente a little bit.

Cappy - 22-4-2003 at 06:39

The more I look into amateur chemistry, the more I'm convinced that a dedicated lab is needed. I guess a stove top "fume hood" could be damaged by the fumes, and probably wouldn't ventilate well enough even with the kitchen sliding glass door open. I guess I could work outside, but around here it's always either humid or windy. :mad:

trinitrotoluene - 23-4-2003 at 23:54

Coulden't you also distill your H2SO4?Of will it decompose?
If possable distilled H2SO4 will be high purity without those contamination. But on the downside distilling H2SO4 is extreamly energy intensive. The boiling point of H2SO4 is pretty close to that of lead.So it will take a while to distill.

HDPE

a123x - 24-4-2003 at 07:42

Does anyone happen to know how well HDPE would stand up to boiling H2SO4? I can't work outside so I need some way to overcome the acid fumes and sulfur oxides that are prduced while concentrating H2SO4. My thought is that I could attach an HDPE tube to the top of my flask and then have the tube a foot or two long and at the end of it have it covered with a piece of fiberglass cloth which holds some moist base(most likely NaHCO3) to neutralize the acid fumes as they pass through. I'm not sure how well HDPE coud stand up to the hot acid fumes and even if it could I'm not sure my set up would even work anyway. If you think this won't work and have a better idea please tell me.

Cappy - 24-4-2003 at 11:44

I'm sure HDPE is good for unconcentrated H2SO4, but I'm not sure about pure, hot fumes. Teflon is safe for fuming H2SO4 up until 200 degrees Farenheit according to the NIBCO Chemical Resistance Guide for Valves and Fittings. Unfortunately they don't list HDPE, but most plastics aren't any good for very hot, concentrated H2SO4.

[Edited on 4/24/2003 by Cappy]

trinitrotoluene - 24-4-2003 at 12:30

Those bottles sulfuric acid of drain cleaner you buy they are made out of HDPE.Yes HDPE should resist concentrated H2SO4 at room temperatute. But when I did try to put some hot H2SO4 at 80*C into a HDPE container it got really weak. I beleave if you increase the heating it would fail.

a123x - 24-4-2003 at 15:10

Thanks. I guess I'll just have to wait until the weather gets warm enough so that I can concentrate the acid outside.

PHILOU Zrealone - 2-6-2003 at 03:14

HDPE starts to become soft arround 80°C, the more you go up with the heat the more it soften until it becomes liquid.
HDPE could only be used for distillation under vaccuum where the heat is not excessive.

Another problem with HDPE is that being aplastic its thermical isolation effect is high and thus a cooler made with it won't be effective.

alchemie - 8-6-2003 at 08:26

You can easily get rid of the fumes by piping them outside.
Cover a one holed stopper(cork or rubber) with teflon tape, then insert a glass tube through it(can be a small one) and attach a hose(I used the transparent one from hardware store, PVC I think).
Insert the stopper in the GLASS flask with the battery acid and, as someone already said, boil until white fumes appear and you´ve got concentrated H2SO4.

I dont know how concentrated but, in my case, enough to make HgSO4 out of liquid Hg.

[Edited on 8-6-2003 by alchemie]

outside and outside

Organikum - 8-6-2003 at 23:13

Ehem, before venting the fumes "outsides" one should have a look where "outsides" these condense....
....or troubles ahead.

Not outside venting but in a bucket with water gives no fumes and no ruined fassade or worse. Whats the problem? Works fine costs nothing is safe as handling and concentrating H2SO4 can be.

Distilling CONCENTRATED H2SO4 is a adventure not to undertake without urgent need. And there is no plastic known to me going to stand the conditions. (KAPTON may for a short time, but I won´t bet on it). Ceramics might be the way for the amateur, siliziumoxide, titaniumoxide and silicates to hold it together. Thats a guess now.

suizide time again?

Organikum - 9-6-2003 at 11:13

yes whom the inner clock calls....

greetings to Ringmeister - you´ll see him soon I guess.....

inkognito - 20-10-2003 at 08:47

i didn't want to make a new topic just for one question so here is it : whats the highest conc. of h2so4 that can be reached by boiling car battery acid ??? i was by a battery recharger and he gave me 0.5 liter of sulfuric acid from some big contanier ( 50 liters , maybe more ) . well i don't know what that concentration is ??? please help . im very confused

ps. im not a kewl , i just don't have much knowledge in chemistry , and im not from USA or UK , but i think you can understand what i said

rikkitikkitavi - 20-10-2003 at 09:10

the battery acid is probably around 37 weight %.

The highest concentration achievable is 98 weight %, but before this there will be lots of sulfuric acid smoke=> high losses. Minimum 20 % of the acid will be lost during this process.

a more reasonable concentration is 95 % , good enough for making high conc HNO3.

/rickard

[Edited on 20-10-2003 by rikkitikkitavi]

inkognito - 20-10-2003 at 09:52

i have one liter of this battery acid , i can get how much i wan't so a 20% loss isn't that bad . can you tell me how much 90>% h2so4 can i make from 100 ml of this battery acid ??? what is the boiling point of h2so4 ? can you give me some direct information about this procedure , how much should i boil off ,and that stuff??? i will do some calculation by myself , but it would help if i know what you think . thanx

cmon guys , don't be laisy !

[Edited on 21-10-2003 by inkognito]

inkognito - 22-10-2003 at 10:42

i read on rougesci that the density of h2so4 is 1.84 , but what concentration ? i boiled my h2so4 from 100 to 60 ml , next day im going to measure the density . what concentration of h2so4 do they mean with 1.84 density . please don't be angry if i sound stupid , and that stuff . im new to this .

vulture - 22-10-2003 at 10:56

SEARCH!

And use the edit button! :mad:

Calling us lazy is so @#$%! hypocrite! Get off your ass and do some searching. This information can be found within less than 5 minutes.

You are really pissing me off mister...:mad:

And please make your posts readable!
[Edited on 22-10-2003 by vulture]

[Edited on 22-10-2003 by vulture]

madscientist - 22-10-2003 at 11:04

Quote:
cmon guys , don't be laisy !


I usually have to visit weirdpier to find statements as pathetic as that.

inkognito - 22-10-2003 at 11:10

you guys are realy no better than xinventions or totse . you can understand my posts , so than there is no problem . im sorry , that i called you laisy , but it isn't that hard to answer one question as easy as this one . don't be mad . ill try to find my answer on some other place . thanks for your "HELP" :mad:

[edit by madscientist: This is NOT a "we'll answer your inane demanding questions like slaves" forum. We are not your calculators. So forget it. We're here to discuss, not slave for you.]

[Edited on 22-10-2003 by madscientist]

I know the answer to your question...

DarkVigilante - 22-10-2003 at 17:25

However, I am too "laisy" to tell you.

DarkVigilante - 22-10-2003 at 17:30

Interestingly, this Inkognito character is the member of the day with 4 posts... I think I will have to post a few more times just to reclaim this record for those with meaningful posts.

Mumbles - 22-10-2003 at 19:04

At x-inventions you asked nothing. Well, assuming you still used the Inkognito moniker. The only thing I found is you complaining about not being able to get KNO<sub>3</sub> at a reasonable price, and thats why you make HE's. Theres also some stuff about party poppers.

You asked no questions there, so why attack? If theres something I've over looked, I'm sorry. Or were you just saying that it is inferior to this board? I couldn't tell from your post.

inkognito - 22-10-2003 at 21:03

no , guys . im not mad at you. i just don't like the administrators over here very much , that's all. and i was just kidding when i said lazy , so you don't have to mad . on xinventions i just searched for information , but as you see posted for some other stuff. on totse , i have a other user name .

vulture - 23-10-2003 at 05:55

Let's get this thread back on topic shall we?

I think inkognito has learned his lesson.

The purpose of an administrator is not being liked, but keeping the place clean and tidy. I couldn't care less about popularity.

Making H2SO4 with epsom salts...

DarkVigilante - 23-10-2003 at 20:29

Epson salts or MgSO4 can be electrolyzied and with the right cathodes and anodes the remaining products can be treated in such ways as to immediately make H2SO4 or make SO2 that becomes SO3 in the air. SO3 can be passed through water to make H2SO4. Concentrate and your there. There are lots of ways to do this, but I will leave other people to come up with their own cool ideas since thats half the fun.

rikkitikkitavi - 24-10-2003 at 09:54

intersting Cyclo. that you have had success with using only a foil used as a lid
(working as condensing surface for less concentrated acid) , I had troubles with acid losses (far more than 20 % ) in open pans. theroretically , around 20 % losses is the best you can get.

But with a pyrex bowl with a removable lid (with a small hole on top) losses where much reduced. Unfortunately the bowl cracked (quite sensitive @ 300 + C) but it was an easy matter aquiring new ones.

Instead of Fe2(SO4)3 you could try to heat a pyrosulfate , it decomposes at lower temperatures. But still , working with SO3 is a bitch.

And yes, it is possible to "distill" H2SO4 in a way, when concentrating it over a column , f e x in a Pauling concentator. By feeding diluted acid into the column, acid flows downwards and is contacted with hot vapours from below, coming from the bottom contains hot concentrated sulfuric and over the top leaves water with a little sulfuric acid.

/rickard

[Edited on 24-10-2003 by rikkitikkitavi]

blip - 24-10-2003 at 13:01

I'm quite sure O<sub>3</sub> would be able to oxidize SO<sub>2</sub> into SO<sub>3</sub>, although getting/making O<sub>3</sub> is another matter entirely. I always found the idea of using SO<sub>3</sub> to "recharge" H<sub>2</sub>SO<sub>4</sub> solutions interesting. I've read that one must boil H<sub>2</sub>SO<sub>4</sub> for ~20 minutes <i>after</i> the white fumes appear to really have it be concentrated.

chemoleo - 24-10-2003 at 13:23

well, a long time ago I produced SO3 by melting Na2S2O8 (sodium peroxodisulphate). Heaps of white fumes are produced, but they would not noticably dissolve in water (very much unlike when Cl2 is bubbled into NaOH) - and as far as I know, you will only get SO3 to dissolve in concentrated sulphuric acid to form H2S2O7 (oleum), which, upon dilution with H2O, produces H2SO4 (but obviously more than you started off with) once again.

rikkitikkitavi - 25-10-2003 at 08:30

ok, now I am with you Cyclo...

No it is very difficult to do it at home , but I have a prospect from QVF (www.qvf.com) for a sulfuric acid concentrator plant.

It is working under vacuum (to reduce boiling point , for technical reasons) and attached distillation column. Everything is made out of glass but the electrical heaters (tantal) but doing this at home is virtually impossible. It is run batchwise.

However, using vacuum to concentrate the acid might be an better idea since the
temperature will be reduced to around 200 C for the azeotrpic acid.

/rickard

Mendeleev - 25-12-2003 at 15:16

Sulfuric acid is the most widely manufactured chemical in the United States. How people have trouble getting it is beyond me. Lowes sells Roebic brand "drain flow inhibited sulfuric acid" drain opener, which you can see at this link: http://www.lowes.com/lkn?action=productList&catalogId=C0... (its the bottom of the three, notice its item number: 66830) and the MSDS for it is at http://www.roebic.com/pdf/DrainFlowMSDS.pdf which says that it is 90%. Although it contains buffers to prevent heat generation in the pipes, these wont affect nitric acid distillation for example because they don't distill at the temperature that nitric acid does. If you live in the USA then you probably have a Lowes within reasonable distance. If their website advertises it that means that they sell it and if its not in stock, just ask them to order it. NAPA auto parts also sells car battery acid refills at ~ 35% concentration, about $15 for five gallons.

[Edited on 25-12-2003 by Mendeleev]

Tacho - 26-12-2003 at 07:57

If you start with 200ml battery acid, d=1,25g/ml you have:

H2SO4 H2O conc. dens.
60 ml 140 ml 44,1% 1,252

H2SO4 is non-volatile, so, as you boil away the water you get:

60 ml 120 ml 47,9 % d=1,280
60 ml 100 ml 52,5 % d=1,315
60 ml 80 ml 58,0 % d=1,360
60 ml 60 ml 64,8 % d=1,420
60 ml 40 ml 73,4 % d=1,504

I always stop here, since I´m quite happy with 75%, but, in theory:

60 ml 20 ml 84,7 % d=1,630
60 ml 10 ml 91,7 % d=1,720

I attached an excel spreadsheet I made about H2SO4 concentrations

Attachment: dens_conc.xls (14kB)
This file has been downloaded 959 times

Mendeleev - 26-12-2003 at 08:43

Sulfuric Acid Concentratin vs Density Table

%--- density (g/mL)
0.5--- 1.0016
1--- 1.0049
2--- 1.0116
3--- 1.0183
4--- 1.0250
5--- 1.0318
6--- 1.0385
7--- 1.0453
8--- 1.0522
9--- 1.0591
10--- 1.0661
12--- 1.0802
14--- 1.0947
16--- 1.1094
18--- 1.1245
20--- 1.1398
22--- 1.1554
24--- 1.1714
26--- 1.1872
28--- 1.2031
30--- 1.2191
32--- 1.2353
34--- 1.2518
36--- 1.2685
38--- 1.2855
40--- 1.3028
42--- 1.3205
44--- 1.3386
46--- 1.357
48--- 1.3759
50--- 1.3952
52--- 1.4149
54--- 1.4351
56--- 1.4558
58--- 1.477
60--- 1.4987
70--- 1.6105
80--- 1.7272
90--- 1.8144
92--- 1.824
94--- 1.8312
96--- 1.8355
98--- 1.8361
100--- 1.8305

[Edited on 26-12-2003 by Mendeleev]

thunderfvck - 10-2-2004 at 19:16

Sorry to resurrect a dead thread but my thread had been closed earlier by the fearful vulture, so here I am, posting exactly what I had before. Perhaps some of you can help me out.
I did an experiement today to determine the percentage of H2SO4 in a drain cleaner product. It turned out to be 98% roughly, very exciting. The drain cleaner I had used had a red color to it, some kind of impurity. Anyway, when I diluted the acid in water (TAP water) a gas was formed. It was wispy white as I recall. What gas could this have been?

When I neutralized the acid with NaHCO3, the SAME stuff that had been diluted with the water that caused a gas to evolve, and the acid was fully neutralized, the color of the solution went from somewhat clear to red. I wasn't aware that my solution of drain cleaner with water was an indicator. What's going on?

H2SO4 + 2NaHCO3 ---> Na2SO4 + 2CO2 + 2H2O

So CO2 is released. While doing the experiment the gas released did not smell like CO2. THe gas smelled like burning death. I tried my best to refrain from the noxious vapours. What could have caused this?


Thanks.

Quince - 19-8-2005 at 23:53

Has anyone here actually tried distillation of H2SO4 from drain cleaner? Would that remove the buffers? Would regular glassware suffice?

Duster - 20-8-2005 at 02:08

From what I have read, many have tried, and while its possible to get some of the color or impurities out, most people still have the same color they did before.

Some succeed somewhat... I belive it was somewhere here last night I read about someone distilling sulfuric acid drain cleaner, and while their product was indeed clear, they lost a lot of it in some reaction that accidently took place...

Regardless, I have never heard of the color affecting any reaction that uses the acid. Sure it may look odd and may scare you, but I have never heard of anything go wrong because of it... But then again who knows...

As for normal glassware to handle it, you'll be fine. No matter the concentration, H2SO4 simply can not eat away at glass... flourine on the other hand....

BromicAcid - 20-8-2005 at 07:11

It was the battery acid thread of all places that I posted on my distillation of drain cleaner. I used regular glassware but I did the distillation under reduced pressure. I got very clean sulfuric acid from the process.

Of note is that I didn't use magnetic stirring and used boiling stones which is a no-no in a reduced pressure distillation as a result I would get occasional flash boiling. Also when initially distilling water would condense in the still head and drip back into the very hot sulfuric acid and would cause a poping in the flask shooting vapors and acid upwards, ruining my first attempt although I was more careful with my second attempt. If you did this with an apparatus under atmospheric pressure it may have come off better though I would have had to have used a better heat source.

Maybe wrap the still head in Ni-Chrome to keep it over 100C so water would not condense. Also note that at such high temperatures I probably shouldn't have used ice water in my condenser and I am somewhat lucky it didn't break, maybe use air instead.

h2so4smoke.jpg - 48kB

Quince - 20-8-2005 at 21:08

Well, I could do reduced pressure, but the issue is how long it takes to reach temperature.

I don't have a problem with the color of the drain cleaner, it's very slightly yellowish. I have a problem with the bits of cloudiness in it, which is either particulate matter (but probably easier to distill than find appropriate filter), or the buffers.

I assume with proper insulation around the still head, with the source flask in a heating mantle, it shouldn't be too bad. I'll probably give it a try next weekend, and I'll post the results.

Any use to add a vigreux column, to help with the water issue?

[Edited on 21-8-2005 by Quince]

Duster - 20-8-2005 at 21:30

From what I can recall, drain cleaner is about as close to pure H2SO4 as your likely to get, that is, the water has already formed its azeotrope with water... In which case you wouldnt be seperating any water from the acid. All your doing here is just seperating your acid/water from impurities.

What a long way to say a fractional distillation wouldnt make any diffrence.

However, if it would be battery acid, or anything under 98% (I belive) then it may be *somewhat* benifical... Then again water boils sooner than the acid anyway so...

Make of it what you will, but if your just going to get impurities out, then a quick and simple distillation should get the job done.

Quince - 20-8-2005 at 21:32

Will mineral wool (the kind used to insulate the walls of houses) be OK as a filter? I'm thinking filtration is much easier than distillation at 320*C.

neutrino - 20-8-2005 at 21:39

I don’t see how it would help. The acid has to be the same temperature to make it to the condenser regardless of what columns it has to pass through.

edit: Two responses while I was typing, that’s unusual.

The wool should do, just make sure there is no plastic in it.

[Edited on 21-8-2005 by neutrino]

Rooto

MadHatter - 21-8-2005 at 20:49

I've never encountered problems using the Rooto sulphuric acid despite its yellow tint.
The stuff is great for producing nitric acid.

wow...hot stuff!

((Blasta)) - 1-9-2005 at 09:28

I just found a place that sells Pro-Drain Opener. Its amazingly energetic stuff... it is thick and slightly amber colored and it fumes slightly. The pro's say it is 93.5% H2So4... it does Nitration REALLY well. So no sense on trying to concentrate it. I just made some triNitromethane... using the odd ball patent using Nitric Acid on Isopropyl Alcohol. Wow, can I say wow.
I post pics soon,

[Edited on 2-9-2005 by ((Blasta))]

woelen - 1-9-2005 at 10:37

Nitromethane from isopropyl alcohol? That sounds interesting. Can you explain this? What is the mechanism behind this?

Tacho - 1-9-2005 at 10:41

Really interesting. Patent number is?

((Blasta)) - 1-9-2005 at 23:08

United States Patent: 4,122,124

read up and try it* :) with rising fuel costs this might just be a money maker. ....being sarcastic
--------------------------
Instead of using liquid Nitric Acid...I used the chemical reaction between Sulfuric Acid and Potassium Nitrate inside a glass flask. Then I pumped the vapour into another flask containing warmed Isopropyl Alcohol. The product that condensed was yellowish and sweet smelling... yep, its pure Nitroform or tri-Nitromethane. I estimate 60% yield... which isn't bad since it was my first attempt.


[Edited on 2-9-2005 by ((Blasta))]

[Edited on 2-9-2005 by ((Blasta))]

The_Davster - 1-9-2005 at 23:16

Thats TRInitromethane, not just regular nitromethane which contains only one nitro group. Please note while messing with trinitromethane that it is quite carcinogenic.

((Blasta)) - 1-9-2005 at 23:22

oh, really? Yikes. I bet triNitroMethane could be useful in making PLX or a variation of it, right?

Quince - 1-9-2005 at 23:23

What the hell? This patent is for making trinitromethane, not nitromethane. Can't you tell the difference between CH(NO2)3 and CHNO2? Rising fuel costs? Talk about false advertising! Sheesh, just when I thought we had something interesting here.

Heh, I'm glad it's carcinogenic, maybe the fool will get cancer and stop spreading misinformation on this forum.

[Edited on 2-9-2005 by Quince]

((Blasta)) - 1-9-2005 at 23:29

I thought I had something interesting as well... well then again maybe I don't.
What use is triNitromethane then? I thought it could be used as a fuel of sorts with other chemicals? hummm... sorry guys
oh yea, in my origional post I did specifically state that this synthasis did create pure Nitroform/ tri-Nitromethane. Anyway what do I do with 120 mL of triNitromethane...
??

[Edited on 2-9-2005 by ((Blasta))]

[Edited on 2-9-2005 by ((Blasta))]

Quince - 2-9-2005 at 00:45

Further nitration to tetranitromethane for use in binary exlosives (but that's even more toxic, lethal in air is about 0.1 ppm). Check out roguesci.

[Edited on 2-9-2005 by Quince]

woelen - 2-9-2005 at 01:18

That's a pity... I was really hoping to get some (mono)nitromethane in pure form :(. The trinitro stuff is not interesting to me. Up to now I only succeeded in finding mixes with methanol or petroleum for model cars and karts, but I need the pure stuff. The mixes I found only contain up to 10% or something like that :(.

Quince - 2-9-2005 at 01:22

Yeah, but it would have more wear on the engine. Most aren't made for more than 10%, and a lot of plane glow engines are intended for 5% NM. Not to mention that the 2-cycle glow engine sprays non-fully burned fuel all over the place, as I found out the hard way...

catfish - 3-9-2005 at 04:35

Thunder-
you prolly smelled SO2 or SO3, and possibly saw water vapor leaving the solution.

Quince - 3-9-2005 at 05:14

SO2 does not smell like "burning death", it smells like burned strike-anywhere matches or firework smoke or a package of dried fruit that was just unsealed. The "burning death" description sounds more like the H2S, which as a far nastier stench than SO2, though I don't see how that could have come from the reaction. Now SO3, I don't know what that smells like, how it compares to SO2, so those that are in the know please describe it to us. Or maybe there was sulfur pollution in his water, as occasionally happens with tap water that's sourced from wells, and that also has H2S smell.

[Edited on 3-9-2005 by Quince]

neutrino - 3-9-2005 at 06:03

I'm guessing that the smell was an H<sub>2</sub>SO<sub>4</sub> mist.

12AX7 - 3-9-2005 at 08:03

SO3 is rather hygroscopic, so it forms H2SO4 (of some percentage H2O, because it is also hygroscopic!) which just burns when inhaled. I haven't noticed any smell from it where hot pyrolysis isn't involved (e.g. burning refractory sulfates like CaSO4 makes a lot of SO2).

Tim

Fleaker - 3-9-2005 at 08:10

Would it be possible to use a centrifuge to separate the dye from the acid? (referring the cheap black drain cleaner)

IPN - 3-9-2005 at 09:00

If the dye is only as a very fine suspension then yes. Remember to use strong tubes, preferably made from thick PP. No glass.

catfish - 3-9-2005 at 09:57

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.
Now how's about some SO3...?

[Edited on 3-9-2005 by catfish]

12AX7 - 3-9-2005 at 12:45

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

chloric1 - 3-9-2005 at 16:32

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.

The_Davster - 3-9-2005 at 16:49

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)) - 3-9-2005 at 22:43

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.

chloric1 - 4-9-2005 at 09:42

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!

12AX7 - 4-9-2005 at 09:53

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

((Blasta)) - 4-9-2005 at 09:56

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))]

Fleaker - 4-9-2005 at 12:53

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)) - 5-9-2005 at 00:26

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))]

12AX7 - 5-9-2005 at 08:19

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

Tim

((Blasta)) - 5-9-2005 at 13:46

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.

Fleaker - 5-9-2005 at 18:48

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 - 5-9-2005 at 21:35

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]

((Blasta)) - 6-9-2005 at 08:53

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. :)

Chris The Great - 6-9-2005 at 14:41

Tetranitromethane and RDX maybe? :o

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 - 10-7-2006 at 21:49

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.

Rooto

MadHatter - 11-7-2006 at 21:11

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.

tumadre - 19-7-2006 at 00:04

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.

Concentrate H2SO4!?

SAM4CH - 10-4-2007 at 12:54

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!!!!!!

not_important - 10-4-2007 at 14:44

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 - 10-4-2007 at 20:03

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?

not_important - 11-4-2007 at 03:59

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 - 11-4-2007 at 11:16

Can I use silicon iron alloy which used in electrical transformer as electromagnetic plates around the copper coils???!!

12AX7 - 11-4-2007 at 14:34

If you can melt and cast, or forge weld, it into a sealed pot...sure...

Tim
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