Sciencemadness Discussion Board

Battery acid

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thunderfvck - 3-4-2004 at 02:22

I just got some car batteries from a friend of mine and I'm planning on concentrating the H2SO4 inside them. I am sick of my disgusting drain cleaner. It is disgraceful.

I am concerned about the lead/other impurities, however. When I drained the batteries (used batteries), you wouldn't believe the mess it was. BLACK as night, so much garbage is in there. However, I filtered a bit of it with some coffee filters and the resulting liquid was pretty clear looking. So I can get rid of the color, thank god (a problem I wasn't able to solve in the drain cleaner). So, what kind of impurities are we talking about here? Are these impurities extremely BAD, do I risk screwing up further experiments as a result?

I know I am probably better off buying the electrolyte directly from an auto parts dealer, however this is more exciting. Besides, I had gone to Canadian Tire and they just kind of scoffed at me. I haven't tried anywhere else but I'm sure I could find it. Anyways, I assume this electrolyte refill would be pure H2SO4, well dilute anyway?

After spending a good half hour trying to pry open three of the batteries I had gotten, I wonder, why do they sell refill if it's almost impossible to open the batteries? How are you supposed to get the electrolyte inside without tearing the lid off?

Thanks a bundle.

Esplosivo - 3-4-2004 at 02:31

Lead impurities are very few. We are talking about a very small quantity of lead sulphate in solution (lead sulphate is very very slightly soluble in water, and even less soluble in sulphuric acid) and some lead (IV) oxide (PbO2) which passed during filtration. The black solid you filtered off is mostly PbO2 - if you collect it and decide to use that for any experiment just wash it in water and filter a couple of times.

Some battries, like the ones I have at home, have screw openings at the top from where sulphuric acid may be added. In Malta I have seen only a few of these sealed battries, most of which are used for power supplies such as for USPs (old ones).

Out of point but lead (IV) oxide can be used to carry out many reactions, so don't throw it away. It can be heated to form PbO. PbSO4 can be made by passing SO2 gas through PbO2, and also by mixing PbO2 with sulphuric acid (-ie if next time you want sulphuric acid out of your battries, charge them first - this will give you a better 'yield' ). PbO2 can also be used to produce chlorine by reaction with HCl, together with other reactions.

[Edited on 3-4-2004 by Esplosivo]

Mumbles - 3-4-2004 at 13:19

Were the batteries recharged or just left uncharged?

If charged the impurities should be manageable. If uncharged the Acid would be pretty weak, and probably not worth concentrating. It addition to that it would be decently contaminated.

Quantum - 3-4-2004 at 16:06

How did the auto store owner scoff at you? I would try and look clean and neat and if that dosn't work then just yell at them that your going to a diffrent store that wants to *gasp* make money.

tom haggen - 3-4-2004 at 20:17

First of all when you go to an auto parts store you have to show a little intelligence. Going in there asking for electrolyte isn't going to get you anywhere. All that shit is, is water with some type of electrolyte in it (NaCl, KCl). You must ask for battery acid. If they flip you any shit just tell them that your going to be anodizing some aluminum. There are countless applications for using H2SO4 in the shop besides making explosives. I think your crazy for wasting all that time filtering acid out of a battery. You were better off recharging those batteries so you could have a 12v power source lying around.

[Edited on 4-4-2004 by tom haggen]

thunderfvck - 4-4-2004 at 00:15

I don't know whether or not they were charged. A friend of mine had them lying around his house so I assume they're uncharged.

The guy at Canadian Tire looked at me strangley and told me that if I needed to have my battery refilled I'd have to bring it in and they'd do it for five dollars. He told me they don't sell battery acid and in stating this he made it seem like it was ridiculous to ask about it. Like, who the hell sells battery acid? That's the impression I got from the guy. I guess I should do some more searching.

I should add that when I asked many of my friends about obtaining battery acid, they all had no idea about it, as though it isn't even for sale. And these people are car fanatics, you'd think they'd have seen this before. Could it be possible that it just isn't available here in Quebec?

Yes, so assuming these batteries are uncharged and I have mega impurities. I filter it using coffee filters until the solution is clear. How massively contaminated is this solution? Will it pose a threat to any future experiments? How might one go about purifying this, if it is at all possible?

Once I get my scale (I've been waiting about three weeks - those fuckers) I'll be able to tell all of you how concentrated this solution is.

Thanks.

[Edited on 4-4-2004 by thunderfvck]

unionised - 4-4-2004 at 05:15

There is a lot to be said for keeping chlorides out of lead acid batteries.

tom haggen - 4-4-2004 at 08:26

Thunder, I'm telling you, don't even tell them that your wanting to refill your battery. That is ridiculous and its a waste of time to do so. Thats probably why they were playing games. Find a new store and tell them that your going to be anodizing some aluminum. A lot of auto parts stores infact don't sell sulphuric acid. I've had good results with NAPA.

[Edited on 4-4-2004 by tom haggen]

thunderfvck - 5-4-2004 at 08:18

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.

thunderfvck - 5-4-2004 at 14:56

Now to purify it...

I've done my reading on the subject. Seems pretty straight forward, however I have a couple of questions..

So I boil the stuff. Alright, wait until I see the thick white fumes and then stop. Correct? Or do I let it fume out for awhile to ensure that it's 98%?

I am using a huge 6 liter flat bottomed flask to do the boiling. Is this bad? The flask is pyrex, blah, so I guess it can withstand the temperatures. However I read something about steam exploding? I don't know, this doesn't sound right. But the flask has a fairly narrow top so I can imagine the steam inside would get quite hot and concentrated. Anyway, is there any problem with using this? The flask is half full...

People have said that heating directly on the hot plate is bad. Well how bad is this? I have read that sand should be used or a high boiling oil. I do not have access to this at the moment, what kind of risks am I taking by just heating directly on the hot plate?

It is being stirred, BTW, no boiling stones though...I guess I should smash a mug or something...

Thanks guys.

tom haggen - 5-4-2004 at 15:18

You only have to worry about steam explosions if your distilling H2SO4. I think. but your just concentrating so you shouldn't have to worry.
Just check the weight of your acid against a density chart to determine concentration. You'll have to heat it well past the point that it starts fuming. It will put off massive amounts of acid vapors. It's a process that could potentially draw a lot of attention to your "lab" But if you don't have any illegal explosives lying around you shouldn't have much to worry about. I put my flask directly on a hot coil all the time, thats not to say that it is safe. But I stand back while the water boils out of my acid, and its out in the garage. So if the worst case scenerio were to happen (the flask cracking during concetration) I would be prepared. Just keep in mind that if you were to splash boiling hot H2SO4 on your skin it will burn through it immediately. By the way did they question you when you bought your acid this time?



[Edited on 5-4-2004 by tom haggen]

thunderfvck - 5-4-2004 at 16:02

Nope. No questions asked. Worked wonderfully. Last time I go to Canadian Tire.

It looks like this is going to take a long time...It's been going for four hours, it took two hours just to start boiling. Man.

It had the density written on the box. It coressponds to 35%. However I'm going to bring some to my drug dealer friend and use his scale to double check. Chemistry is fun.

Quantum - 5-4-2004 at 18:22

I got a cheap but good scale. It can hold 100g and is 0.1g accurate. Cost = 28$

This guy sells them cheap and he is funny:
http://www.oldwillknott.com/cgi-bin/htmlos.cgi/37104.2.4710613738612779157/triton_miniscale.html

tom haggen - 5-4-2004 at 20:12

I have a density chart for sulphuric acid if you want me to email you a copy.

thunderfvck - 5-4-2004 at 20:31

Nono. I ordered a scale. 0.01 g resolution for $50. I'm just waiting for it to come, it's been three goddamned weeks.

I don't need a sulphuric acid density chart, I've found one. But thanks for offering.

Okay, well I tried checking the mass percentage of H2SO4 in the sample, and I got 74%? Wrong. Definitely not right.

It took 7.5 g of NaHCO3 to neutralize 11.8 g of the acid. I added water halfway because the mixture was getting nicely gooped. Could this have caused something to go awrong?

Quantum - 5-4-2004 at 23:41

Wow! 0.01g you say? Please provide a link.

I really want to get some battery acid myself. After making 5 liters of sulfuric but finding out that the yeild couldn't be more than 10ml I got pissed as my mood shows. I will need to get a cheap hotplate from walmart as the only source of portable heat I have is a colman that burns costly fuel. Strong sulfuric is a staple to the home chemist. Making sulfates, making nitric, drying things out and a whole host of other uses abound! I will not pay 7$ for 1 piss poor liter of nasty ass black as night second hand etheopian rejected drain cleaner! 15$ for 20L resulting in 6liters of the good stuff(sounds a bit like drugs:o) sounds a lot better to my ears.

tom haggen - 6-4-2004 at 05:43

I used to have a scale that weighed down to .01 grams back in my younger stupid days. It was design for weighing gun powder. It dissappeared like all things not earned honestly.

[Edited on 6-4-2004 by tom haggen]

Mendeleev - 6-4-2004 at 08:06

I boiled down drain cleaner directly on a hot plate. It worked just fine for about 6 times or so, but then I noticed cracks in the beaker recently. They say you can put it directly onto a hot plate or burner, but apparently you can't. I will be writing those assholes, I want my fucking beaker replaced. I don't mind drain cleaner on occasion, it works just fine for distilling nitric, however I try to use the clear sufuric from NAPA unless I will be distilling something out of it. The advantage of drain cleaner is that you just pick it off the shelf in the hardware store. At NAPA, they remember your face after you ask for sulfuric refills several times(and you do have to ask for it, it's in the back). I hate fucking suspicious assholes. I had a guy at home depot ask me if I was building a bomb because I bought an oxygen tank. Stupid gestapo fuckface...

[Edited on 6-4-2004 by Mendeleev]

thunderfvck - 6-4-2004 at 08:33

http://scales.net/mn_prods/myriad_scale/myriad50_summ.php

It's only a little piece, one of those portable scales. However it's 0.01 g, and quite frankly I don't care how small it is. Most jeweller's scales for at least $100 on ebay, so this is a great deal.

Quantum, you should really get a hotplate via ebay. I'm telling you man, CHEAP. The one I have is a piece, the stirring mechanism doesn't work until the 4th setting (this can and must be repaired) hwever I only paid about $70 for it.

Mendeleev, what kind of beaker did you use? How serious are the cracks?

I'm getting pretty sick of using my 6 liter FB flask. It's taking the better half of the century to boil off all that water. It has been running since 4 pm yesterday, it is now 1230pm of the NEXT DAY and I've lost about a liter of water. It's because of the small opening I have on my flask, it doesn't allow much water to leave the flask. So I believe I will put it in nice glass pot when I get back from school, and boil the living hell out of it.

Saerynide - 7-4-2004 at 02:37

Quote:
Originally posted by thunderfvck
Mendeleev, what kind of beaker did you use? How serious are the cracks?


My pryrex beaker died on a gas stove. It was only on there for about 10 min too :o

thunderfvck - 7-4-2004 at 05:30

I went to the store yesterday in hope of finding some glassware I could use. I found pretty much nothing except a Pyrex measuring cup (1 L) that looked pretty decent. The glass was THICK. Anyways, so I bought it and brought it home, and the first thing I do is remove the Pryex sticker..."Not for lab or stovertop use" is written underneath it, well son of a bitch!

Saerynide - 7-4-2004 at 07:49

What kinda pyrex glass dies that easily?? :o

vulture - 7-4-2004 at 08:20

Strange. I only have borosilicate 3.3 glass, be it from Schott or Normag. This will stand up to pretty abusive spot heating on a ceramic hotplate/stirrer.

thunderfvck - 7-4-2004 at 09:01

Fuck me.

You know what just fucking happened? Oh am I fucking PISSED FUCKING OFF.

I wanted to check the temperature of the goddamned H2SO4, but the level of it was way low and I couldn't get the thermometer in there with the clamp I have. So I used my shirt to protect me from the heat while I lowered the thermometer. When I was raising it out of the fucking thing, the motherfucker slipped and hit the bottom of the glass. My heart stopped. NO. NO!! THen nothing, I was thinking, okay, I'm alright, thank god. Then I see mercury pouring its ugly head out of the fucker and all onto the bottom of the flask. I now have murcury in my concentrated hot sulphuric acid. So there's definitely going to be a reaction going on. So my once pure H2SO4 is now contaminated. And I can't stand for this. So I stopped the heat, removed the flask. DUmped the hot H2SO4 in a bucket and recovered the murcury. There was some yellow shit inside the flask and this only fed my fury. I first took my keys and threw them across the room, knocking some movies over the shelf. I broke part of my keychain. Then I took the thermometer and also threw that across the room to vanquish the evil forever. Now there's probably murcury lying in my basement in those damned little beads of death. Fuck. THe stupid things you do when angry...

And this is the SECOND thermometer I've broken. The first time was completely retarded as I shocked the glass in cold water, it cracked and I was miserable. Now I broke the SECOND fucking one, AND I fucked my H2SO4. I've been concentrating the H2SO4 for about two days now, it takes forever in that flask. I am so angry. Like seriously, I am really, very unhappy right now. Now I have to order yet a THIRD thermometer, AND start all over again with the H2SO4.

Or maybe not, what do you guys think? Should I ditch all the acid or what? How contaminated is it? It seems to have formed a yellow precipitate, so if I filter it, would I be okay?

I'm such a fucking stupid fucking retard.

BromicAcid - 7-4-2004 at 17:58

How concentrated was your acid at this point? Production of either the mercurous sulfate or the mercuric sulfate is temperature and acid strength dependent. If you managed to get the mercurous sulfate it is almost insoluble in cold concentrated sulfuric acid according to Hawley's Condensed Chemical Dictionary (Note, mercurous sulfate is listed as being white to yellow in color). However the mercuric sulfate is readily soluble supposedly. You could always do a quantitative test to determine the extent of mercury contamination.

The only one that I know of though is bubbling H2S through the mix, preferably in a small test tube. The sulfide would precipitate out hopefully.

I would be more concerned about the mercury spill. Not that I have some inherent fear of the stuff, but in that the EPA could very well designate your house a Superfund site, they have done it before over one thermometer. I believe it cost the owner of the house in upwards of $40,000 for clean up.

[Edited on 4/8/2004 by BromicAcid]

Quantum - 7-4-2004 at 21:55

I wouldn't use it; mecuric compounds give me the willies! I hope the EPA dosn't hear about the Hg spill:o its retarted to get so upset over less than a gram of the stuff.

I think if you use a wide mouthed glass next time it will go much faster. Possibly sucking the water vapor/SO<sub>2</sub> fumes off with a pump would keep them from slipping back into the acid.

We all have our stupid days:( I remember I destroyed a printer because I got mad at it. It was a lexmark; shitty printer dosn't like Linux.

tom haggen - 7-4-2004 at 22:52

Theres a small possiblity of refluxing with a narrow necked flask but I wouldnt worry about it. Thunder you got so much H2SO4 I would just pitch what you have already contaminated with mercury. I have recently lost a thermometer so I feel your pain. However, you need to calm down. Your going to waste a lot of supplies as a begginer, take it in stride.
Trust me I have wasted a lot of supplies. By the way, you really shouldn't have to monitor temperature when concetrating sulfuric acid.

[Edited on 8-4-2004 by tom haggen]

thunderfvck - 7-4-2004 at 23:18

I know I shouldn't have to montior temperature, but I was curious. I mean, I'm a beginner, and I have a thermometer, so what do you expect me to do. BTW, the temperature was 120. haaaaaa. My sulfuric acid is now kind of yellowish in color. I've read that mercurous sulfide precipitates out of the solution, so any that I may have would precipiate, no?

It's not the fact that it's contaminated, really. OI mean, that pisses me off enough as it is, it's just that I've spent a good three days concentrating this stuff and for what? A contaminated solution. You probably understand why I blew it.

I swept my basement floor and found no mercury balls. The last time this happened, I dropped a ball of the stuff and it splattered all over ym table. However, I was able to clean it up once I cleared my table off, I cleaned off many little metallic balls. I didn't find any this time, while I swept. But these things are SO small, so it's likely that I entirely missed them. How dangerous is this stuff? Assuming I have like mg quantities scattered on my floor.

The mercury didn't seem to react with the concentrated H2SO4. When the thing broke, it just spilled out and remained a tiny ball. It didn't bubble or anything. I've read that while preparing mercuous sulfate, you have to reflux it at HIGH temperatures (about the same I had going I suspect) for quite some time. I had it sitting in there for no more than 3 minutes. I don't know though. When I emptied the flask, there was some yellow/white crystallized sbtance on the walls of the flask. Things I didn't have thetre before so I accredit it to the mercuous sulfate. Should I REALLY just get rid of this? I've spent so much time boiling off the water, t'd be incredibly frustrating to just get rid of it all.

And BTW, how do you dispose of it? I know I'm supposed to neutralize it first, but I wasted like half of my sodium hydroxide trying to neutralize the used battery acid I had retrieved directly from the battery, and it stil wasn't neutralized. I ended up dumpoing it directly into the sewer. I know that this shouldn't be done, but reagents aren't cheap. That doesn't justify my dumping it however, but, what am I to do. I'm really not willing to uyse most of my NaOH to neutralize something I'll just end up throwing away. Oh, I'm so evil.

But when that thermometer dropped, I just lost it. There was a brief period where I thought I was okay, then I saw the mercury, and I flipped. Thermometers are so bloody senstive.

My approxiametly 1 L of H2SO4, from about 3L, gives off what looks like white fumes. However, I believe it is still water that is being driven off (STILL!). I blow on the vapour, and it turns whiter, presumably because I'm condensing it even more and it turns white because of it. But the fumes that it's been giving off are not WHITE white, you know? It's just like water vapour. It dissipates quite rapidly and isn't very irritable to the lungs.

Anyways, I've written quite enough. I'm mainly concerned with the yellow color, I've seen sulfuric acid (concentrating, fuming) that was yellow before, in my school lab. But I'm not sure about this. As I recall, the solution was not yellow (and this is a faded yellow, more clear than yellow, but it has the tint) until the mercury was exposed to it.

I guess I should just dump it. But fuck, so much time, such a waste. It's very upsetting.

Right after I do something stupid like this I feel, "you know, if you just wouldn't have fucked with it, you'd be fine, you'd have your thermometer AND your perfect pure acid" but NOOO, I'm too curious for that and careless. Well, we all learn from our mistakes.

Excuse the length of this, and possible spelling/grammatical errors, I am quite drunk/on MDMA. Soooo,...

Thanks a lot for your input though, you guys rock.

Z-Row - 8-4-2004 at 13:28

Quote:

And BTW, how do you dispose of it? I know I'm supposed to neutralize it first, but I wasted like half of my sodium hydroxide trying to neutralize the used battery acid I had retrieved directly from the battery, and it stil wasn't neutralized. I ended up dumpoing it directly into the sewer. I know that this shouldn't be done, but reagents aren't cheap.

Why not dump it into the sewer? It is sold as drain cleaner after all, right? You don't have to neutralize it, just dilute it first (and remember, add acid to water, not water to acid). And there are other cheap bases out there to neutralize acids with, you don't HAVE to use NaOH. NaHCO3 and Na2CO3 can be found in a grocery store as "baking soda" and "washing soda" respectively (although the sodium carbonate would be better than the sodium bicarbonate for neutralizing acid) and they are both dirt cheap ( about $.85 US / lb. )

Mendeleev - 8-4-2004 at 13:44

Mercury is not very toxic in terms of dying, so much as it accumulates in the body, because it is not metabolized and causes brain damage. I don't think such a small amount will affect you too adversely unless you drink it. I've actually heard a story, I am not sure if it is true, but in some third world country a poor street performer ritually chugged a liter of mercury and did a belly dance which looked weird because the heavy mercury in his stomach lagged behind the rest of his body while he danced, and then barfed it back into its vessel. I wonder how long he will live, if he exists. Also, why do you use mercury, I ordered red alcohol thermometer, they are about $3 each, and when I broke one during a nitro synthesis, it was no problem.

tom haggen - 8-4-2004 at 15:39

silly medeleev, you can't use red alcohol thermometers for high temperature applications. Back in the old days they used to use mercury as a potion in the non stop search for everlasting life. Ironically these potions brought death. Thunder you have almost motivated me to start a thread about fail experiments. If you only knew some of experiments that have gone wrong for me...

[Edited on 8-4-2004 by tom haggen]

BromicAcid - 8-4-2004 at 18:55

You can take some sulfur powder and put it on your floor and sweep it around a bit. This should make the sulfide which is relatively inert and lacks the inhalation hazard in that it does not volitize easily.

thunderfvck - 9-4-2004 at 01:06

That's a nice piece of information, BromicAcid. Although I doubt that I'm in any serious risk, it seems as though most/all of the mercury fell into my acid. But in the future, if it ever happens again I'll be doing that, seeing as how I DO have sulfur (ah, the excitement!).

As for neutralizing the acid before disposal, using any carbonate will produce that damned CO2. And you could imagine the mess my impatience would make trying to neutralize all of the acid.

So, should I really waste all of my acid? I could always set this acid aside for showy experiments that I could demonstrate to my friends. But primarily, at the moment, I want to make some acetic acid/nitric acid. These acids will be distilled, so I'm guessing it would be okay to use an acid that is contaminated SLIGHTLY?

Mumbles - 9-4-2004 at 09:16

You could bubble in some H2S to precipitate the HgS. The only unknown is how fast/if the concentrated acid will react to just form more HgS and Mercury Sulfate.

The MSDS says its incompatable with Strong acids. I'm assuming this means it does react. Perhaps rediluting will allow more time to filter out. This should get more out than with the concentrated. This does of course mean another concentration.

If you're distilling the acids off, I think the mercury contamination should be ok. The mercury should theoretically stay in the distilling flask.

Mendeleev - 9-4-2004 at 10:41

What is the difference between a partial and full immersion thermometer, is it that one can be fully emerged and the other one can't, or is it that one has to be fully emerged to measure properly, and the other one only a certain amount?

ech310n - 9-4-2004 at 18:48

Quote:
Originally posted by Mendeleev
What is the difference between a partial and full immersion thermometer, is it that one can be fully emerged and the other one can't, or is it that one has to be fully emerged to measure properly, and the other one only a certain amount?


I'm sure a Google search would had given the answer you are looking for but here is a link to a page I had in my bookmarks that will explain the difference: General info on thermometers

thunderfvck - 18-4-2004 at 00:34

Well, I finally did it! My hotplate was out for repairs over the past week or two, and I haven't been able to concentrate my acid. First thing I did when I got it back was buy a 1 L measuring cup that I felt would make a more efficient container. And so it does! Problem is, I changed stirrers when I added the acid to this measuring cup, and the solution turned PURPLE. It was very nice but left me slightly unhappy (this was the contaminated Hg stuff anyway). So I dumped that into my 6L flask and added some activated carbon. A few days later the color's cleared and it looks like this will be my nitric acid producing batch.

ANYWAY! So I put some fresh acid in the 1 L measuring cup and heated it...Took a few hours to boil down to the point where it started to smoke, but it smoked. Oh man did it ever. My basement was FILLED with this vile, throat-itching, smoke. It was terrible. Even with the window open...I guess I really need a fume hood! Anyway, the smoke was enough to set the fire alarm off and that was unpleasant. So now I am currently doing it outside, and it's quite beautiful really, the thick smokey whiteness that would gag me if given the chance.

Thanks to everyone for their replies!

Mendeleev - 25-5-2004 at 19:22

I had a bad run of luck myself today with sulfuric acid. It all started when I walked into NAPA today to replenish my suppy of acid which I had very recently depleted. Normally they give me the huge 5 gallon containers but today there was a different lady and she gave me a 1 liter container. That's about 18 times less and it cost me 5 bloody dollars. It you get roughly 200 mL from that that will cost $100 per 4 L of concentrated acid. At that rate it would be cheaper to buy 4L of concentrated ACS grade acid for $60 from http://www.sciencelab.com and a lot less hassle, thus my frustration. I wasn't about to start a riot over not enough acid so I just paid and left. Tom Haggen, I believe you said you bought acid at NAPA, do they sell it to you in 5 gallon or 1 quart containers? Maybe they have both and it just depends on the clerk what you get? Anyway that was the least of the bad luck. I thought maybe I was in luck and this was concentrated 98% acid that you have to dilute yourself. Not so, I tested it, density=1.245, corresponding to 33% acid. I proceeded to boil it down. The 1 liter took 6 hours to boild down to 98% in a 1L beaker. I take the beaker off the hot plate and proceed to carry it further away from the hot plate for cooling. When I took the acid off it was at 225C, There was no noticable thumping from uneven boiling but when I took it off, the agitation must have awakened some feral spirit in the acid for it went "thump". It got onto my hands causing me to tilt the conainer slightly. Enough for another thump which sent about 100 mL of 225 degree C, >90% sulfuric acid to spill onto my leg. My leg turned black and I now have second degree burns on it and several enourmous burn blisters. My status as "hazard to self" is most befitting. This has never happened before, usually the thumping is not nearly as violent. I am not so sorry about the leg as it will heal in time, but I lost a good 200 mL of concentrated acid which stook 6 goddamn hours to boil down. Any one want pictures of the scars ;)?

[Edited on 26-5-2004 by Mendeleev]

Saerynide - 25-5-2004 at 20:07

owwieeee.... :o

Theoretic - 26-5-2004 at 03:27

Pics?
POST 'EM!

ShadowStalker - 3-6-2004 at 13:37

uhh i this this topic is kinda old but anyways

iv noticed with some of(ok most of them) that when its blak is hell if you let it sit for a week or two the lead and trash falles to the bottem and the acid shude be about 65% pure (hopefully)...

why make it so hard?

Magpie - 7-6-2004 at 19:40

I can understand the problems of the poor folks who live where sulfuric acid is illegal to buy, but why would anyone in the US boil down 35% battery acid? That seems like a very hazardous and boring activity. After a little internet searching I'm having a 2.5L bottle of ACS grade delivered to my doorstep. Of course this presumes you have a credit card and don't mind using it.

Mendeleev - 8-6-2004 at 11:11

Sorry I took a while posting the picture, but anyway, this was taken 48 hours after getting burned. A 2.5 L 98% bottle ACS grade acid costs $70. Up until recently I've been buying 5 gallons of 35% for 20$ AFter boiling down that leaves about 4 L of 98% pure sulfuric acid. That's 4 L for $20 or 2.5 L for $70 plus those bastardly hazardous shipping fees. That's $5/L vs $30/L. Hmmmm, which to get, which to get... Besides if you're going to order everything online why don't you just order whatever it is you're trying to make. The novelty of recreational chemistry is to able to turn complete crap: yuppy house hold cleaners, batteries, and paint chemicals, into something good: formamide, TNT, nitroglycerine, meth, etc.

[Edited on 8-6-2004 by Mendeleev]

[Edited on 8-6-2004 by Mendeleev]

Burnt Knee.jpg - 16kB

Eliteforum - 8-6-2004 at 15:33

Oooch! Looks painful!

If that were mine I couldn't wait for it to scab! Am I alone in liking the picking of scabs?!

tom haggen - 8-6-2004 at 15:55

mendeleev, I just bought a five gallon container of H2SO4 33% for like $17. But I've also purchased the 1.5gallon containers. The 1.5 gallon packages come in a plastic pouch contained in a cardboard box, they are like $7, I scammed them down to $5 one time:D. My old material science teacher had one of those 1liter containers you bought. But yes, NAPA carries all three options, sometimes they run out of the big 5 gallon jugs though. You just have to be presistant with those dumbasses. Oh ya, your fucking crazy for picking up a hot beaker filled with hot sulphuric acid. I always let my glassware cool down on the hot plate. No matter what the chemical, your damm lucky the glass didn't crack. At high temperatures glassware is very sensitive to temperature change!!! Did it feel strange when you got burned by the hot H2SO4? The hottest H2SO4 I've ever gotten on my hand was probably 50C and it did some damage to my skin, yet it was relatively painless. It was bizarre, I don't want it to happen again.

magpie, unless your a college professor or a licensed pyrotech, I wouldn't be buying chemicals off of the internet.

[Edited on 9-6-2004 by tom haggen]

[Edited on 9-6-2004 by tom haggen]

make vs buy

Magpie - 8-6-2004 at 17:40

Mendeleev,

I checked with NAPA before I ordered the ACS grade. I would pay $40 for what I would pay NAPA $20 for in the 5-gallon container. I don't know what the shipping costs will be but I will let the forum know. Saving the hassle, hazards, and getting ACS grade made it a no-brainer for me. I also will be getting "Readily Available Chemicals" and purifying as required, but H2SO4 is not one I want to tangle with.

Tom Haggen,

I am neither a college professor, licensed pyrotech, or have a business license. My credo is that I'm not doing anything illegal. Why shouldn't I buy chemicals over the internet? Sincerely, please let me know.

Magpie

Mendeleev - 8-6-2004 at 22:12

Pyrex beakers are made to be placed directly on the hot plate or flame, the company says so, so if it cracks while being used in its standard application and you get injured as a result, you sue for lots of money. Its a completely legit cause to sue if the beaker brakes under 250 C, if the company says they can be placed directly on a flame. As far as picking it up, I used tongs and gloves, that's why my hands didn't get killed, just the few splashes on my knee. However I will heed you're advice and leave it on the hotplate to cool next time, because I don't need something like this to happen to me again :). It never thumps that much, I don't know what the hell happened. It didn't feel weird when I got it on me, it just felt like any other hot corrosive chemical feels to the skin, burning a hole in you. That's a pretty awesome deal you're getting magpie, ACS sulfuric acid for $40/2.5 L. I am considering buying a 750 pound (190 L) drum of technical grade 93% sulfuric acid for $115 from Gallade Chemical, because it is such an awesome deal. It works out to about 60 cents a liter. I think they sell to individuals.



[Edited on 9-6-2004 by Mendeleev]

Esplosivo - 8-6-2004 at 23:02

Quote:

Pyrex beakers are made to be placed directly on the hot plate or flame, the company says so, so if it cracks while being used in its standard application and you get injured as a result, you sue for lots of money. Its a completely legit cause to sue if the beaker brakes under 250 C, if the company says they can be placed directly on a flame.


Of course they can resist 250 deg Celcius, but they will withstand only a small amount of thermal stress. I once placed a pyrex beaker, which had been, heated on cork to let it cool. It happened that a drop of water was present on this cork and viola, a fine thread streaked through the glass.

Forgot to mention that in my case the beaker of capacity 250cm3, contained only approx 25cm3 of solution in it. I don't know if this small volume of solution would have affected the cracking, since a small volume cannot 'absorb' as much heat as in the case of larger volumes. In other words the cooling due to the drop of water occured too rapidly and therefore thermal stress would have occured to a larger extent.

[Edited on 9-6-2004 by Esplosivo]

tom haggen - 9-6-2004 at 10:40

Sure there are probably applications where you need to transfer scolding hot chemicals from one container to another. But since my equipment is so primative I always make a point of letting my glassware cool down on the hot plate. It's not going to go anywhere:D.
Magpie, I really don't have a reason for not buying chemicals off of the internet. I just like to keep my name off government lists.

Magpie - 9-6-2004 at 11:27

Mendeleev,

I have to eat a little crow on my order for the 2.5L bottle of ACS acid. They are not filling my order as they do not ship to individuals.

So I went back to Google and found 2 suppliers who look like they will ship to individuals. You don't know for sure until the order is completed.

One reason I wanted to bring this issue up for discussion is that I'm concerned about all the forum members who seem to be boiling down sulfuric acid - it just seems so risky. At one place I used to work a fellow employee was burned badly by room temperature 93% sulfuric acid spraying all over his leg - very painful, several weeks in the hospital, permanent scars and pain. And he was quite close to a safety shower and used it. I really hope everyone can find a good supplier (like you have) so they don't have to do this anymore. This is a case where John Ashcroft's policies are really backfiring on the people he is trying to protect.

Tom Haggen,

I understand how you feel and debated this issue with my self for many months. I finally decided to take a stand that my activities are legal and proceed accordingly.

This is the other reason I wanted a discussion. I want to know what the concerns and liabilities are with ordering chemicals and equipment with full documentation, i.e., over the internet with a credit card.

tom haggen - 9-6-2004 at 14:24

Oh ya magpie, I actually hate concentrating my own H2SO4, releasing large amounts of sulfur oxides into the atmosphere is not my idea of a good time. If I didn't care about being anonymous I would definitely order chemicals off of the internet.

hodges - 9-6-2004 at 15:03

I order chemicals online all the time (USA). I'm not doing anything illegal, and if someone is watching what I order I doubt my orders for 2oz of Mg or 4oz of Fe2O3 or even things like 70% HNO3 and KI are going to look that suspicious. Certainly not enough quantities to make much of a bomb out of - there would be far easier alternatives I'm sure. The closest thing I have to anything organic is denatured ethyl alcohol and sodium acetate, so if someone thinks I might be making drugs then they must not know too much.

Living in an apartment, I'm far more corncened what my neighbors might think vs. what authorities might think. I know that I have never had a serious accident and that my chemicals are not likely to pose even as much of a hazard as (say) a gas grill that I see people storing on their patios. I know that, but if I were to get a package labeled "DANGER - EXTREMELY HAZARDOUS" my neighbors might (rightfully) feel a bit of concern. Fortunately, almost every chemical I have ordered has been delivered in "plain" packaging. I get a ton of science and electronics stuff through the mail, and those packages tend to be well labeled, so hopefully that is everyone's first guess as to what the other packages contain.

S.C. Wack - 9-6-2004 at 15:15

Risky? Chemistry? Good! Killing or maiming themselves is a good way get those who don't belong in this field out of it before they can do more harm. Some people cannot accept the fact that they don't plan well enough to do chemistry. These words are not directed at the picture poster, shit happens to everyone.

Accidents happen. So when handling things like sulfuric acid, you have to be more careful. After doing this chemistry thing for a while, and have various bad experiences, you learn from your errors. You see some accidents as errors, because many of them are preventable to a degree. At least the ones I've had.

But I'm not so careful either, using the battery acid and pyrex "not for stovetop or broiler use" to 500F in the oven. I can't imagine doing this on the stovetop in visionware, the fuming in air is horrible if the oven door is opened while the acid is hot. But I do take precautions, the bowl is in a deep, heavy cast-iron skillet. The heat is raised very gradually. No problems, yet.

Advice for what its worth for those in the US:
Some chemicals are better bought than made, and auctions, well...Red P is very much a controlled substance, yet people sell and buy it on ebay. There was just listed a very freaky auction, a grab bag of some very freaky chems. And I doubt that there will be any problems, except the cost of shipping. BTW, on that huge Gallade order, exactly how much is the shipping on that item? So, people are buying these. Email them in a couple months, and see what they say, if they respond, if you really want to know.

Buy all the chemicals you can, using your credit card, while you can. Because the buying situation is not going to improve, in person or online. Shop around, prices are incredibly variable. Better yet, start your own chemical business, selling to individuals.

Just look at all the crap they put in slx and sunnyside alcohol, for profit or otherwise. Almost chemically useless. The other OTC chems are next, and many have been taken off the shelves in some states already. I do not care if people use, make, or sell meth, but I am very pissed at the cooks and the media for the chemical controls. P cpds. are so organically useful. I guess if it wasn't for the meth hysteria, we'd have the environmental hysteria that the EU does.

If no one buys from the retail sellers due to paranoia, they won't have enough incentive to continue selling to individuals. They will not have any incentive to fight proposed legislation. Then what? Will we be pissing on wood ash/mulch piles for KNO3 like in the old days?

BromicAcid - 9-6-2004 at 16:43

I buy my H2SO4 from the hardware store for cleaning drains, it says industrial strength right on the bottle and says not for sale to individuals but I've never had a problem purchasing it. 1 L bottles, $16, on the back it says, guaranteed 99% H2SO4, works very well.

But I used to boil down my own acid, I would boil it down in of all things, a metal pan. Those ones with the really thin layer of ceramic on them. It worked fine several times but on one attempt a piece of it must have flaked off because the acid looked like it was boiling all the sudden really localized and it went straight though the pan and into my cheap heating element, took that sucker out quick but one odd thing, I had a portion of this boiled down acid sitting around all winter and it was nearly clear when I put it away, come summer it was still clear but a large amount of yellow precipitate was on the bottom of the container, looked like sulfur but I didn't test it.

However I do buy many of my chemicals, but there is a hazmat fee on any high concentration >45% that I've seen. Strange considering I've bout benzene by the liter with no hazmat. Must be just corrosives and explosives that require hazmat.

tom haggen - 9-6-2004 at 17:33

Ya the only thing is that drain cleaner crap is contaminated with some type of dye. I noticed some strange variations between 2 different jugs of sulfuric acid I bought. They were both clear at 33%, but when I concentrated one it would turn a much darker yellow color while the other would stay almost clear when concentrated. Both were from NAPA I don't really understand it.

[Edited on 10-6-2004 by tom haggen]

[Edited on 10-6-2004 by tom haggen]

Saerynide - 9-6-2004 at 17:53

The one that turns dark yellow/brown has trace amounts of contaminants in it. I posted links in this thread which mentions this.
All the H2SO4 Ive made looks like that when it gets more concentrated too.

Someone suggested that the acid be passed through carbon filters if i remember correctly.

[Edit]: I havent tried the carbon filter thing yet though.

[Edited on 10-6-2004 by Saerynide]

OTC's becoming rare?

Magpie - 9-6-2004 at 18:52

I have read S. C. Wack's post and agree on many points. I too feel that the OTC's will likely become less available and/or more crapped up with useless additives.

I'm stocking up agressively now on reagent chemicals and generic glassware. I'm buying basic reagents like oxalic acid, methanol, sodium hydroxide, etc. Just today I searched on the internet for lye and couldn't find a supply! Many soapmakers on the internet said they couldn't find it anymore due to all the meth making in their area. I was so concerned I went right out to see if I could find some. Much to my pleasant surprise I found Red Devil lye in two different chain grocery stores. I bought a 1lb container.

I found a good supply of Drygas methanol at a chain drugstore and bought 2 bottles. The Heet methanol is being phased over to IsoHeet isopropyl alcohol.

I have already mentioned that I no longer see toluene in Home Depot or Lowe's. I think this may be another casualty of the drug war. They have apparently substituted xylene.

Mendeleev - 9-6-2004 at 20:55

Yea, the DEA sucks ass. I don't see toluene at Home Depot or Lowes anymore, but Ace Hardware still has it. Heet gas line antifreeze methanol is found everywhere even wal mart, and red devil pure lye is also found at any grocery store, hardware store, and Wal-Mart. I have not seen any evidence to indicate them dissapearing, but knowing the DEA they just might. I've attached a pdf file about the DEA's actions, which shows just what dicks they are. I don't think they will be able to take away sulfuric acid though, it is the most produced chemical in the United States, and at the very least it will be found in batteries.

All the hardware stores I've been to also sell concentrated sulfuric acid, but it is dyed black, and when attempting to distinguish the layer of nitroglycerine from the layer of mixed acids, the fact that everything is pitch black doesn't help, the same goes for TNT nitration. I generally use the hardware store acid for distilling nitric because the black crap does not distill over, but if the acid is actually physically present in the reaction mixture, I boil down the clear battery acid. I bought more sulfuric acid at NAPA today, this time I told the lady I wanted the 5 gallon container and it was all good. She showed me all three sized that you mentioned tom haggen, and I got my pick, thanks :).

As I mentioned before I am considering ordering that 200 L drum of sulfuric acid for around $115 from Gallade Chemical. Now I wouldn't be concerned about ordering even red phosphorus or hydroiodic acid in 4 oz quantities but 200 L of sulfuric acid means I am up to something, and the truth is, its just the most useful chemical in the lab and having 200 L of it makes me feel comfortable. It's used to produce any acid from its salt, catalyze nitrations through water removal, purify iodine, make phosphorus, its just extremely usefull. I am almost positive if I order such a large drum I will get either a call or a personal visit from the DEA, and I will tell them that it is my personal business and they can kiss my ass. Luckily this country has not become Nazi yet and a purchase is not enough to justify a search warrant. The web site I want to order the drum from is http://www.galladechem.com/ . I am almost sure they sell to individuals because in their line of questions they ask you in the check out order form, they ask what you what will you be using the chemical for and one of the answer options is household, and also they ask if the delivery will be to a residential or business address.

[Edited on 10-6-2004 by Mendeleev]

[Edited on 10-6-2004 by Mendeleev]

Attachment: dea.pdf (85kB)
This file has been downloaded 767 times

Cyrus - 10-6-2004 at 14:43

Quote:
Originally posted by BromicAcid
I buy my H2SO4 from the hardware store for cleaning drains, it says industrial strength right on the bottle and says not for sale to individuals but I've never had a problem purchasing it. 1 L bottles, $16, on the back it says, guaranteed 99% H2SO4, works very well.

hazmat.


Ouch!! Home Depot had a discount on sulfuric acid when I got my acid, so I got mine for about $2 a L!:P No dyes at all that I can see, however, I dropped a piece of the paper inner liner in there by accident when trying to remove it, so now one of the bottles of acid is all brown:mad:

[Edited on 10-6-2004 by Cyrus]

Mendeleev - 10-6-2004 at 17:04

It's clear?! What brand is it?

Quantum - 11-6-2004 at 03:34

Please...Please tell us the brand;)

Cyrus - 11-6-2004 at 16:53

The label says;


instant
POWER GUARANTEED (to the right a picture of an orange sun, to the left a picture of a p-trap (plumbing))

PRO lIQUID
DRAIN OPENER (in large slanted bright orange letters)


below this,

DANGER POISON (to the right a skull and
crossbones, and a test
tube pouring acid on
someone's hand:D)

below this,

(to the left) Concentrated
Sulfuric Acid

(on the right) CAUSES SEVERE IMMEDIATE BURNS: hmm, duh, its H2SO4

MAY BE FATAL IF SWALLOWED no, really, I can't use it as an antacid?

KEEP OUT OF CHILDREN'S REACH (mine is stored at ground level:P)

below this, on the left,

CONTENTS 1LITER
( 33.8 Fl. OZ. US)

to the right
Before use, read all directions, cautions & first aid on the label.

sorry I can't get a digital pic. :mad:

On the back, among many stupid things such as "if you squeeze this bottle hard while it is open, acid may come out the top" (not a direct quote) it says,

Distributed by
SCOTCH CORPORATION
P.O. BOX 4466
DALLAS, TX 75208
214-9434605
5/02 - yes I got this a while ago.

Contains:
93% Sulfuric Acid
CAS# 7664-93-9

If this is not enough information, I can give more, but the bright orange lettering is pretty distictive- I should note that it had a faint yellow color last time I checked, but that could be because of my contaminations, nothing like the blackish purple crap in the other bottles!

EDIT-sorry guys I said earlier that the acid was all brown, it is just very slightly yellow. Must have been my evil clone...

[Edited on 12-6-2004 by Cyrus]

S.C. Wack - 11-6-2004 at 17:26

Yeah, thats the crap. Note the smell of anything you make with it. Note the way the inside of the container has been turned black. Not good enough for certain uses.

drain cleaner comparison

Magpie - 11-6-2004 at 20:39

I surveyed the stores in my area for sulfuric acid drain cleaners today and found three: Lightning, MCC, and Roebic. I haven't tried them so can't say which are any good. But based on the label the Lightning is probably no good as it has "twelve buffers." How in the fuck do you buffer sulfuric acid?

I checked Lightning's website and found an interesting comparison chart for drain cleaners:
http://www.liquidlightning.net/ll/Compare.html

Based on this chart the good ones look like Ramout and Instant Power. But according to above posts Instant Power may not be good for all applications.

Magpie - 11-6-2004 at 20:56

S.C. Wack says
Quote:

Yeah, thats the crap. Note the smell of anything you make with it. Note the way the inside of the container has been turned black. Not good enough for certain uses.


That could very well be carbon particles from the deterioration of the inside of the container. I don't know of any cheap plastics that can stand up to sulfuric acid for any length of time, especially if it gets too hot.

Mendeleev - 11-6-2004 at 22:27

Yea, the infamous instant power. I have the lightning stuff as well as roebic, san-teen, and liquid fire, and all are black. I can't believe my home depot doesn't have the instant power stuff, what state do you live in Cyrus?

Cyrus - 12-6-2004 at 17:56

Well now, that's a pretty big assumption!

Who says I live in a state of the United States at all?

Actually, I am the famous Cyrus from ancient Persia, yes, thats right, the very one who diverted the course of the Tigris, well, its been several thousand years, so I can't remember if it was the Tigris or the Euphrates, but then I sacked Babylon!

So currently I am living in a mansion deep in the hidden recesses of Persia, (with broadband internet access from Persia On Line), but I visit Washington a lot.

That's where the acid was purchased.

sc wack, I didn't say the acid was perfect. All I said, basically, is that this brand is better than the purple crap.
:P
If you want to do some delicate reactions, buy your acid from Flinn, Frey, etc. if you want to do general stuff- ie dissolve the metal off of a light bulb/make boric trimethylether/dehydrate things/react with bases/etc...
This stuff is fine.
It never makes black stuff- presumably carbon, unless it is heated a lot, and even then, the reaction went fine. And I don't even know if the black stuff was the acid's fault.

[Edited on 13-6-2004 by Cyrus]

Mendeleev - 12-6-2004 at 19:12

They let you carry acid on a plane?

[Edited on 13-6-2004 by Mendeleev]

Cyrus - 12-6-2004 at 21:10

All I'll say is; "it is good to be the king."

finding a good H2SO4 drain cleaner

Magpie - 15-6-2004 at 08:49

The sulfuric acid drain cleaners I find in the hardware stores seem to be loaded with bullshit additives to make them "safe." However, the chart link I posted earlier listed a promising candidate, i.e., Clobber by Hercules. A plumbing supplier carries it but will not sell it to anyone but plumbers. I might be able to work around this. Does anyone have any experience with Clobber?

Since you are in the USA

Polverone - 15-6-2004 at 09:38

I will recommend "ROOTO" brand sulfuric acid drain opener, if you can find it. The acid is strong and has just a light yellow color to it. There's nothing but H2SO4 and some small percentage of water present.

Battery Acid

newby - 23-6-2004 at 04:19

Hi, Just came accross this thread, so thought I would add my experience of this somewhat theoretical idea. First I got some battery acid as far as I am aware it is around 35% concentration, I then set up for simple distillation and distilled around two thirds of water from the solution, checking and emptying the collection flask periodically until what was coming over began to undicate acid to litmus paper. The temperature of the hotplate was kept around 150c, Next I did a rough calculation of the density and assumed a density of 1586, that is 1586 grams per litre. Knowing concentrated H2S04 to be 1850 grams per litre, I was some way off of my target. The next problem was my hotplate, with a max temp for liquids of 250c this would not do, I needed to get the temp up to at least 290c but keep it below 340c less my acid began to break up. I decided to use a heating mantle with a max temp of 450c. The acid was boiled in this and I used several condensers one on top of each other as a sort of glass exhaust to vent the noxious fumes, I began boiling with a thermometer in the solution, however some of the fumes began to drift down around the flask so I kept my distance, I did to runs boiling the contents until dense white smoke began to issue from my makeshift exhaust and then kept it going for about 10 minutes. Cracking was heard from the flask and I assumed this to be water molecules being forced out of solution by the heat. After letting the solution cool, I wondered if I had breached the upper temperature limit of 340c as I had not checked the thermometer temp due to the fumes. The resulting solution indicated strong acid to litmus paper, practically dissolving my strip of litmus, but the acid was not clear, it had turned to a golden colour not unlike brake fluid maybe slightly darker, possibly I had breached it's upper temp limit, it should be clear, or possibly there is something else in there that has caused discolouration. Theoretically I think lesser concentrations could be concentrated by this method but a good heating mantle with a thermostat or boiling the acid in a bath of oil of a known boiling point temp which does not exceed around 300c would be needed. I hav'nt worked out the sp of this golden acid so I cant tell you what it's concentration is but working back from how much water has been removed it must be almost there. If anyone out there is thinking of trying this, do so with extreme caution, first and foremost on my mind was safety, I also used quality labglass, lab stands and hotplates.

Re Battery Acid

newby - 23-6-2004 at 06:51

It seems you can clean this acid if coloured with contaminants by using the easily available Hydrogen Peroxide

Hydrogen peroxide (H2O2) is effective in removing colour from Sulphuric acid and the rate at which hydrogen peroxide clears up the acid varies with the acid temperature, the quantity of SO2 dissolved in the acid and the strength of H2O2.

Bench scale test should be performed to determine the amount of hydrogen peroxide to be added, the temperature and residence required to produce a product acid of acceptable quality

For a small sample I would think we are talking in the few drops range at a temperature of 80c, If anyone has tried this I would be interested in how it turned out :cool:

Reverend Necroticus Rex - 23-6-2004 at 10:14

Adding hydrogen peroxide would produce caro's acid aka peroxymonosulfuric acid, which is unstable I think, and certainly quite mean (I speak from personal experience here) Caro's acid is known as piranha bath, for obvious reasons, as it is one hell of a strong acid.

newby - 23-6-2004 at 10:42

The h202 used is a 50% solution, it is not a concentrated solution being added to S03, your starting with H2S04, The amount used to clean discoloured sulphuric acid for a given quantity is whatever is found in bench testing or roughly 1.5kg h202 to the ton H2S04, so I am assuming a small sample would require dropwise amounts. I understand this to be the process used in industry if they, for whatever reason end up with a batch of discoloured concentrated sulphuric acid, trying to lighten this by diluting with large amounts of pure clean acid is'nt very effective. I assume this process of cleaning discoloured acid works by bleaching the contaminants while having no reaction with the H2S04 which is relatively stable. If industry use this process to add 'Value' to there acid, I would think this to mean they can sell there acid for applications which require a higher grade instead of selling it for drain cleaner or the like. I am not talking about adding h202 to free S03:cool:

Reverend Necroticus Rex - 23-6-2004 at 11:20

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]

newby - 24-6-2004 at 01:45

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:cool:

Mendeleev - 24-6-2004 at 07:02

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.

Drain Cleaner

Zac - 28-6-2004 at 13:43

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:o 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:(

BromicAcid - 28-6-2004 at 18:13

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.

tom haggen - 30-7-2004 at 21:22

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.

tom haggen - 31-7-2004 at 08:12

Anyone?

The_Davster - 31-7-2004 at 10:08

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.

tom haggen - 31-7-2004 at 12:00

Ya I guess i'm just over cautious.

BromicAcid - 31-7-2004 at 17:34

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.

The_Davster - 31-7-2004 at 18:47

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?

BromicAcid - 31-7-2004 at 18:53

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.

Rooto

MadHatter - 1-8-2004 at 07:59

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 !

HankeyPoo - 4-8-2004 at 17:10

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 :P

BromicAcid - 8-8-2004 at 17:53

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! :D

[Edited on 8/9/2004 by BromicAcid]

FrankRizzo - 8-8-2004 at 21:37

Bromic,

Are you sure that it was sulfuric acid that you were distilling over? IIRC, 98% sulfuric acid boils at over 300C.

BromicAcid - 9-8-2004 at 14:09

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.

Interesting thead

Quantum - 9-8-2004 at 19:36

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.

battery acid

mick - 13-8-2004 at 10:04

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

FrankRizzo - 22-9-2004 at 14:14

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.

rift valley - 22-9-2004 at 14:23

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

thunderfvck - 24-9-2004 at 12:36

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...

Glass

MadHatter - 25-9-2004 at 10:53

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.

acx01b - 6-11-2004 at 07:29

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)

chloric1 - 20-8-2005 at 18:17

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!
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