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[*] posted on 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.

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tom haggen
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[*] posted on 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]




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[*] posted on 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.




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[*] posted on 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. )
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[*] posted on 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.
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[*] posted on 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]




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[*] posted on 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.



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[*] posted on 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?




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[*] posted on 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.
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[*] posted on 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?



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[*] posted on 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
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[*] posted on 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!




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[*] posted on 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]




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[*] posted on 25-5-2004 at 20:07


owwieeee.... :o



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wink.gif posted on 26-5-2004 at 03:27


Pics?
POST 'EM!
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[*] posted on 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)...
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[*] posted on 7-6-2004 at 19:40
why make it so hard?


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.
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[*] posted on 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




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[*] posted on 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?!




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[*] posted on 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]




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[*] posted on 8-6-2004 at 17:40
make vs buy


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.

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[*] posted on 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]




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[*] posted on 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]




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[*] posted on 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.




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[*] posted on 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.




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