Cleaning Sulphuric Acid

[javagamer]

Greetings,

After searching every store I could I finally came across a source for sulphuric acid in the form of drain cleaner. I was pleasantly surprised to discover (thanks to the online MSDS) that it's 94% sulphuric acid. Unfortunately the "12 buffers" added appear rather effective, making a few drops incapable of harming a cardboard box. Clearly I need to purify it, but I'm not entirely sure how.

 

After asking on the IRC (thanks UnintentionalChaos and Nitric) I learned that I should do something along the lines of adding activated charcoal to it, filtering it through fiberglass, and then concentrating to make up for any water gained in the above steps.

 

I do have some questions about the specifics though. First of all, how much charcoal should I add? Is it just a pinch, a spatula full, or is there no such thing as too much? Second, I've read concentrating it is as simple as boiling until thick white fumes emerge, is there a temperature I should aim for and how can I best judge how concentrated it is? Measuring the density?

 

Also, if it's alright to name sources I can post a link to the MSDS and website if that would help.

 

Thanks in advance,

Javagamer

 

(I'm not sure if this is the right place to put this so feel free to move it to where ever it belongs)

 

Edit: One of my main uses for this sulphuric acid is making nitric acid and nitrations. I've heard that you can use rather awful acid to make nitric acid, could I use unfiltered acid for this? If so would it also be good enough for nitrations?

Edited January 20, 2009 by javagamer

[Cap'n Refsmmat]

Incapable of harming a cardboard box? I've seen drain cleaner eat holes through the bottom of cardboard boxes. That stuff is stronger than you think.

[javagamer]

I took a drops and put about 5 drops on a cardboard box and it did nothing. That's how I determined the buffers are quite a problem.

[CaptainPanic]

Acid won't instantly explode the cardboard box away like you see in Hollywood movies. Give it a bit of time.

 

I'm more worried about somebody doing nitrations at home. Are you sure you know what you're doing? Tell us what you need it for (what nitrations do you want to do?)

 

I'm sure that posting references is ok, and you can most certainly post a link to any MSDS online. In fact, I'd encourage you to do that! MSDS are always a useful piece of info.

[javagamer]

I gave the cardboard box a few minutes and it didn't appear to do anything more than color it black (b/c the sulphuric acid is black, not from charring).

 

To start off I'm really interested in nitrocellulose and that is almost certainly what I hope to do first. I have a retort to make the nitric acid, all glass bottles to store it in, and I've read extensively on what to do, plus I have nitrile gloves, splash proof goggles, and an acid resistant apron.

 

It's Floweasy Drain Opener and the MSDS is available at http://floweasy.com/webadmin/doc_manager/uploads/123_Floweasy_MSDS.pdf.

[inuhbad]

First of all, you should be cautioned about using 'Over The Counter' chemicals & cleaners for the purposes of chemistry experimentation.

 

Over-the-counter chemicals, cleaners, and prep chemicals often STATE they have "X" for an active ingredient, at such a concentration, etc... Doesn't mean that's what ONLY in them.

 

If you need to use a chemical inorganic acid reagent, either buy LAB quality pure chemicals, or buy a decreased concentraion of a 'pure' chemical. Using some sort of 'Cleaner' or 'Draino' like substance or a 'Prep & Etch' surface treatment chemicals will screw up your results --> Sometimes BADLY.

 

They include, as you mentioned, buffers, and some other OTC chemicals include solvents, soaps, and other 'Impurities' which can cause problems for you... For my sulfuric acid needs, I can buy Sulfuric Acid from a Lab Supply place locally, or you could buy it at most Auto Parts Stores in 1 Liter Bottles. Auto Parts store acid is usually only 30% to 40% concentration, but it's PURE nitric acid, without additives, chemicals, cleaners/solvents added. You just need to boil out the water with a hot-plate & pyrex beaker (you'll need MORE stuff to do this safely, and follow a certain procedure, as it can be VERY dangerous - I don't recommend this indoors, nor outdoors when there's even remotely a chance of precipitation) to increase its concentration up above 90%. You will typically only get maybe 275 to 325 mL of ~96% Sulfuric Acid from a 1 Liter bottle though. That's not very much at all.

 

That's why I'll just buy it in KNOWN 96-97% concentration, but you also have to know how to handle it as it's EXTREMELY DANGEROUS! Do a Google Image Search for "Sulfuric Acid Accident" and you'll see what I'm referring to...

 

Its reaction with water is highly exothermic, and putting just ONE drop of water into sulfuric acid will cause it to splash, spitter, and boil, and quickly blind or disfigure you if it gets your face...

 

That said, you have to know how to HANDLE high-concentration sulfuric acid as well. Mishandling or lack of safety precautions & safety equipment (Especially during the Acid Concentrating Process) could get you severe chemical burns on your skin, it could make you go blind, burn & scar your lung tissue, and there's the ever-lovely possibility of DEATH... So I'd recommend not playing with high concentration sulfuric acid unless you know with 200% CERTAINTY that you know EXACTLY what you're doing, how to do it SAFELY, and what equipment you'll need.

 

That said, if you're going to use Sulfuric Acid to make Nitric Acid, I wish you the best of luck, because you're going to need a LOT of sulfuric acid, and a lot of a nitrate/salts because the Yields are absolutely PITIFUL. Contrary to what you might have read in the 'Poor Man's James Bond' or the 'Anarchist Cookbook' instructions on Nitrations, their recommended 'methods' are not only INCREDIBLY UNSAFE (and missing CRITICALLY important details), but they're also going to give you PATHETIC YIELDS for nitrations.

 

As for the Nitric Acid --> I highly recommend you AVOID doing any nitrations --> ESPECIALLY AT HOME.

 

Again, it's incredibly dangerous and there's a LOT more to doing nitrations (and especially the synthesis of creating Nitric Acid from Sulfuric Acid) than you may realize. And you likely won't learn what it is you're missing until you attempt a nitration without the proper knowledge/procedures/equipment, and by that point it may be too late as it's kind of hard to learn when you're dead or severely disfigured & blinded while a surgeon picks glass shards out of your body.

 

I was lucky enough to have learned the process in a University setting, in a proper lab, with THICK ballistic safety glass surrounding the lab table, an overhead fire hood & ventilation system, as well as an acid neutralizing sprinkler system and a chemical shower not more than 10 feet away just incase something got thru the glass or the gloves!

 

It's so dangerous, I wouldn't even THINK about trying to create nitric acid or do a nitration in my own home lab. I was nervous & scared as hell doing it in that incredibly 'safe' and 'controlled' environment, and the gasses produced in the process could blind/burn/kill you! I wouldn't DREAM of doing it in a home-lab!

 

If you need Nitric Acid for anything, save yourself from the dangers of nearly killing yourself trying to make the acid - just buy it.

 

Nitrations are incredibly dangerous, and not to mention, in Connecticut, where you state you are from --> CAN BE ILLEGAL! Not only do you have to abide by FEDERAL laws, but you should check your STATE, COUNTY, and MUNICIPAL/LOCAL laws to see what is or is not allowed for use in a home laboratory!

 

You also have to check, because many 'modern' laws to combat Methamphetamine Production could limit not only what CHEMICALS you can legally possess (in conjunction with a specific number of other chemicals), but you have to see what LAB EQUIPMENT is legal in your area as well!

 

Some states limit what kind of heating elements can be used in an in-home lab, and some limit what (and how much) chemicals you can have in the home as well.

 

For example, in my state, you have to fill out a form with the local County Sheriff just to be in POSSESSION of concentrated Sulfuric Acid, or Nitric Acid, and also the local Fire Marshall needs to be notified in writing of the presence of any such chemicals which might be in the house. That's state law that I have to abide by... Not to mention you can't have certain powdered metals or metal salts on hand unless you get an approved license for Pyrotechnics Manufacture on hand --> EVEN IF YOU'RE NOT DOING PYROTECHNICS --> You need it to possess the powders/salts!

 

You have to do more research on the legalities and SAFETY of what you're wanting to do. You could inadvertantly win yourself a new boyfriend named Tyrell or Bubba along with a lovely new 'pad' in ClubFed.

 

There are obviously a number of LEGAL uses for Sulfuric & Nitric Acids, but they're relatively limited, and certain Nitrations are a HUGE Federal No-No, and will get you more than just a simple slap on the wrist --> More like a new, violent, and unpleasant means to enflame some hemorrhoids for at least the next Decade.

 

So, after my 'warning' about how crazy this attempt is... I have to ask you two questions:

1.) What nitration are you hoping to try?

2.) Were you planning on doing anything regarding Azeotropic change?

[javagamer]

Inuhbad - I guess you missed this from my above post.

To start off I'm really interested in nitrocellulose and that is almost certainly what I hope to do first.

I am well aware of the dangers of sulphuric acid, that it dehydrates skin as it burns leading to more severe burns, and what to do in case of a burn. I wouldn't ever think of working with it without the proper safety gear and precautions.

I've already looked extensively into it and I am determined to make nitric acid so I think it is unlikely you will be able to persuade me otherwise. Chemistry is inherently dangerous if you don't take the necessary precautions, but your safety is always in your hands.

 

Also, I'm pretty sure that it's common knowledge (at least here) that the Anarchist's Cookbook contains less information than most cartoons. I can't imagine why anyone would endanger themselves by using such an obviously flawed source for anything. The only thing it's good for is a quick laugh.

 

I never did consider that my state might have laws regarding nitrations. I understand that certain chemicals like phosphorus are illegal, but I never thought a state could/would ban nitrations. I'd be interested to here where I can find out what laws my state has on amateur chemistry as google came up with nothing. I'm also surprised to hear that you have to report possible chemicals to the fire marshal as well as fill out a form. I don't think I have any chemicals that can't be bought OTC and I've never heard of anyone having to fill out a form to buy drain cleaner or reporting they have charcoal or denatured alcohol.

 

Also, here (SFN) it would appear from what I've read (I've been reading for months prior to posting this) many, if not most, people get their sulphuric acid from OTC sources. Besides, from what I understand even pathetic sulphuric acid will work for making nitric acid, though obviously yields wouldn't be as good.

 

Thanks for taking the time to write such a detailed response and your clear care for my safety.

 

Edit: I'm not sure I understand your second question.

Edited January 21, 2009 by javagamer
Adding more info

[inuhbad]

Inuhbad - I guess you missed this from my above post.

Greetings' date='

After searching every store I could I finally came across a source for sulphuric acid in the form of drain cleaner. I was pleasantly surprised to discover (thanks to the online MSDS) that it's 94% sulphuric acid. Unfortunately the "12 buffers" added appear rather effective, making a few drops incapable of harming a cardboard box. Clearly I need to purify it, but I'm not entirely sure how.

 

After asking on the IRC (thanks UnintentionalChaos and Nitric) I learned that I should do something along the lines of adding activated charcoal to it, filtering it through fiberglass, and then concentrating to make up for any water gained in the above steps.

 

I do have some questions about the specifics though. First of all, how much charcoal should I add? Is it just a pinch, a spatula full, or is there no such thing as too much? Second, I've read concentrating it is as simple as boiling until thick white fumes emerge, is there a temperature I should aim for and how can I best judge how concentrated it is? Measuring the density?

 

Also, if it's alright to name sources I can post a link to the MSDS and website if that would help.

 

Thanks in advance,

Javagamer

 

(I'm not sure if this is the right place to put this so feel free to move it to where ever it belongs)

 

Edit: One of my main uses for this sulphuric acid is making nitric acid and nitrations. I've heard that you can use rather awful acid to make nitric acid, could I use unfiltered acid for this? If so would it also be good enough for nitrations?[/quote']Sorry, I didn't read anything about nitrocellulose anywhere in there.

 

Anyway, I understand your eagerness to go about such a project, as it is rather fascinating from a chemist's perspective, but the legalities are just a bit 'tedious' to work around.

 

My particular state, if I recall correctly, classifies nitrocellulose as an explosive, and has no exemption for its purchase/possession for the use as a propellant in small arms ammunition. As you might know, there are various gunpowders of various forms that are made of nitrocellulose, and it has also been used in the past (in composite form with other compounds) as an explosive. You can still purchase, for the purposes of loading your own small arms ammunition, a variety of nitrocellulose based powders/propellants, and their possession is not illegal. However, the actual nitrocellulose itself, not a commercially produced propellant based on nitrocellulose, is a 'grey area' that varies from state to state in legality.

 

For my state, it's illegal, but in Connecticut, there appears to be a Grey Area:

See Section 29-343 of Connecticut Gen Assembly Chapter 541 on Explosives

Sec. 29-343. (Formerly Sec. 29-83). Explosives. Definition. "Explosive", as used in sections 29-344 to 29-349, inclusive, means any chemical compound or any mechanical mixture that contains oxidizing and combustible units or other ingredients in such proportions, quantities or packing that ignition by fire, friction, concussion, percussion or detonator may cause such a sudden generation of highly heated gases that the resultant gaseous pressure is capable of destroying life or limb or of producing destructive effects to contiguous objects, but not including colloided nitrocellulose in sheets or rods or grains not under one-eighth of an inch in diameter, wet nitrocellulose containing twenty per cent or more moisture and wet nitrostarch containing twenty per cent or more moisture; and manufactured articles shall not be held to be explosive when the individual units contain explosives in such limited quantity, of such nature or in such packing that it is impossible to produce a simultaneous or a destructive explosion of such units to the injury of life, limb or property by fire, friction, concussion, percussion or detonator, including fixed ammunition for small arms, firecrackers, safety fuses and matches. "Explosive", as used in said sections, shall not be deemed to include gasoline, kerosene, naphtha, turpentine or benzine.

 

Anyway, you should have your lawyer read over the above linked page regarding Chapter 541, and its sub sections to determine what, PRECISELY, is legal as the actual enforcement of such laws is often up to the interpretation of the officers doing the enforcing. That's how they base their decisions, and then it is left up to a judge to sort out the mess after a person is arrested & charged.

 

With a grey area, I'd be a little leery about the legalities if I were to attempt such an undertaking.

 

You also might want to search the Connecticut General Assembly website for more information regarding laws on pyrotechnics, proper storage, etc...

 

You might also want to search Drug/Methamphetamine lab related laws to see if your state bans certain lab-related equipment/items/chemicals for use/possession in your home. Some states do have such laws (California being the most draconian/controlling), and some states do not.

 

Just trying to look out for your safety & make sure you...

 

Kind of sad that my state now just blanket-bans many nitrated things, and you used to be able to buy sheets of dampened nitrocellulose at a magic shop just down the road 8 years ago... These days you can't find it anywhere.

 

You also might want to note that the law talks about it possibly being legal to possess nitrocellulose, but I'm not sure whether or not it's legal to manufacture your own.

 

I'm just saying with a grey area, I'd be hesitant, and it's also rather dangerous if you screw something up.

 

Making Nitric Acid isn't something I'd do indoors, but playing with concentrated sulfuric acid outdoors is also something I'd rather not do as well. Lots of safety concerns involved in the process.

 

I've found two local suppliers of nitric acid, so, after I get approval from the Sheriff & Fire Marshall, I'll probably buy some for my own purposes (experimenting with corrosion resistant finishes for steel alloys). Until then, I'm rather limited in what I can experiment with in my home due to some rather broad-stretching blanket-legislation in my state.

[jdurg]

I too am from CT and have read the laws on explosives quite extensively. What you have highlighted in the above quote just means "As long as what you have is an amount that can not possibly hurt you or property, it's okay to have".

 

So for nitrocellulouse, it means that if you have a small amount of it that is not confined and can not explode, it is legal to possess. Therefore, if your intentions were to just see how quickly that stuff burns, a small patch about 1 square inch would be okay to own. Again, however, the manufacturing of it probably involves quite a few other laws as well.

 

Your best bet is to call your local police department, or go there in person, and ask them. They may look at you as kind of odd, but more often than not if you show that you are responsible and not a lunatic, they'll be willing to explain the law to you.

[javagamer]

inhubad - There was a post in between my first one and your first one. Thanks for the help with the legal stuff.

 

jdurg- Thanks for your help and advice too.

 

Also, my original questions still haven't been answered.