Sciencemadness Discussion Board - Sulfuric acid dye

Sulfuric acid dye

cobrasniper555 - 5-6-2008 at 22:06

ScienceMadness,
I understand what it means to spoonfeed and individual idiot and I'm asking that if this looks like a spoonfeeding request, please delete the topic and not my account...it's all I ask.

With that out of the way, I would like to say that I've been doing reactions and synthesizing different chemicals (not just energetic or pyrotechnic) using concentrated battery acid (the electrolyte) as sulfuric acid in my synths. Lately, I found out that my local hardware store has started selling sulfuric acid drain openers (I knew they were acidic when I saw the plastic wrapping over them and finally looked at the contents). When I decided to buy some and "check" it out by pouring a small amount in a container, I noticed it had a dye to it. It was a dark, dark reddish (maybe?) dye.

My question is, would this dye interfere with future reactions and become a liability? I worry, because if I can get sulfuric acid a lot easier through drain openers, I'm ready to switch sources. I also searched the forum and didn't find anything as well as the internet with other people using dyed sulfuric acid.

Thank you!
Cobra

P.S - I apolegize if this is in the wrong forum.

[Edited on 6/5/2008 by cobrasniper555]

12AX7 - 6-6-2008 at 04:02

- Move to reagents.

The contents vary, others here have reported golden color ranging to black foaming stuff. Dyes, buffers and who knows what else might be used. What brand is it?

Tim

Nick F - 6-6-2008 at 04:54

I use the purple "One Shot" brand without problems. As long as the dye doesn't interfere with your reaction, which in most cases it almost certainly won't, then recrystalisaton or distillation can be used to remove any impurities introduced by it (and these purifiction procedures should be used anyway).
Any sort of foaming agent could be a pain in the arse though if there's any gas production in your reactions...

gregxy - 6-6-2008 at 08:23

I bought some Roto which has a yellow color probably due impurities rather than dye. Before I use it for nitrations, I add a pinch of NH4NO3 and then heat it to boiling in an open beaker with a propane torch. (I boil off about 10% of the volume). This seems to oxidize whatever is giving it the yellow color since I end up with clear acid. It also helps concentrate the acid by boiling off most of the remaining water.

There is no telling what is in these drain openers, for nitrating things the impurities don't seem to matter.
I would think that they would be free of toxic metals since the EPA would not want them being thrown down the drain but there could be almost anything else.

garage chemist - 6-6-2008 at 09:31

Funny thing so many people here use drain opener as their H2SO4.

In Europe, there are no H2SO4 based drain openers. Due to this, people who want to nitrate things (or do serious chemistry) actually have to order some chemicals instead of being able to use some OTC crap from the hardware store.

I have never bought any H2SO4 that was not crystal clear and 98%.
How about buying some of that instead of drain cleaner?

cobrasniper555 - 6-6-2008 at 10:10

For the drain cleaner, it's: Marc Heavy Duty. I've been thinking about it. What if it's hydrochloric acid? Isn't it used as a drain opener as well or does it react too much with pipes/draines/etc.?

-Cobra

Nerro - 6-6-2008 at 11:16

Quote:

Originally posted by garage chemist
In Europe, there are no H2SO4 based drain openers.

Yes there are.

woelen - 6-6-2008 at 11:43

Quote:

Originally posted by garage chemist
In Europe, there are no H2SO4 based drain openers.

I think you should write "In Germany, there are no H2SO4 based drain openers.".

In NL there are H2SO4 based drain openers, I actually have 1 liter of this stuff. The bottle tells that it is 98% H2SO4.

http://www.onlinebouwmarkt.nl/winkel/view_product.php?produc...

This stuff is fairly good. It has a pale brown color, when viewed through several cm's of liquid. I use this stuff for quite a few of my experiments and it works fine. Only for critical stuff (e.g. metal coordination chemistry experiments) I use real lab-grade H2SO4.

cobrasniper555 - 6-6-2008 at 12:18

I took another look at it and it is of the same type of color. A pale brown/dark-dark red kind of color. On another note, because everyone here is a chemist (in a way) by not only synthesizing explosives for joy and not destruction, this link might be quite enjoyable for you: http://chemistry.hsc.edu/cavebook/chsaltpeter3.html. It's an activity for creating sulfuric acid (extremely diluted but still interesting). I understand some of you may have a vessel similiar to the lead-chamber and don't want to use this procedure but it is still a nice little activity for the family or friends.

Enjoy and thanks!
-Cobra

garage chemist - 7-6-2008 at 04:56

Very interesting, thanks for the correction.
In Germany and France there are no OTC H2SO4-based drain openers.
I was unaware that the situation was different in NL and possibly other european countries.

Zinc - 7-6-2008 at 05:42

The link doesn't work.

chloric1 - 7-6-2008 at 06:03

Quote:

Originally posted by garage chemist
have never bought any H2SO4 that was not crystal clear and 98%.
How about buying some of that instead of drain cleaner?

Quaility lab grade H2SO4 is not terribly expensive in the USA if you do your homework and price compare but its a matter of convenience and priority. First off, the hazmat charges are unreal and frequently more expensive than the acid itself. One supplier I know of sells 93% technical grade for $20 per gallon but the hazmat is $35! So the only economic option is to order a case for $60. Or I can stop in ACE and pick up some Rooto for $15 or $20 with no hazmat. That is especially appealing when you only need to dry gases or generate HCl.

not_important - 7-6-2008 at 06:27

Remove the 'dot' at the end of the link. You should always place several spaces after a URL you paste into a message to avoid any text punctuation being treated as part of the URL. Complex URLs are best put on a line by themselves.

Warming (80-120 C) several ml of the acid, and cautiously and slowly adding H2O2 drop by drop might destroy the colour, similar to adding nitrates but without adding metal ions. Remember you'd be adding water to acid, so take precautions regarding splattering and waiting 20 or 30 seconds between drops. If that does clean up the colour you can work out how to do it safely on a larger scale.

cobrasniper555 - 7-6-2008 at 19:27

Thank you not_important, I'll try that tomorrow! About the link, I noticed the period this morning but someone already posted so I couldn't edit.

MagicJigPipe - 7-6-2008 at 20:14

Quote:

How about buying some of that instead of drain cleaner?

Using that for drying and distillations would be a huge waste, IMO. The only reason I would "waste" $20-$50 on HAZMAT for H2SO4 is for sensitive reactions. For reactions that are sensitive but don't require extremely pure acid I just use "boiled down" battery acid.

The very expensive H2SO4 (because of HAZMAT) should be reserved for the most sensitive reactions, IMO. I think using a retort would be an excellent way to produce extremely pure H2SO4 from drain cleaner (and even purer from battery acid). Has anyone done that? I really don't want to risk my glassware again trying to distill H2SO4 with normal jointed glass.

cobrasniper555 - 7-6-2008 at 21:01

Thanks for the advice. Another quick question is how do you convert Molarity to a "percentage"? Are you using Mass-Mass or what? This is for future notation because I've just stayed with Molarity in the past. For me to communicate with logs of data in my notebook, I would have to convert to percentage of acids (H2SO4 for example) and what not.

Thank you,
Cobra

not_important - 8-6-2008 at 02:56

Problem is that percentage can be weight/weight (w/w), weight/volume (w/v), or volume/volume (v/v) in terms of solute vs solvent. In manufacturing you can see all three, w/w being convenient when dealing with larger amounts especially when temperature control is an issue. On a small scale lab setting dealing with liquid reagents, v/v is the easiest in many cases.

This looks like a quick reference on theory
http://people.clarkson.edu/~skeelsmc/solutions.pdf

Many handbooks such as Lange's or CRC, especially older editions, frequently have tables that allow you to easily convert between measurement types for more common chemicals.

Klute - 8-6-2008 at 13:49

GarageChemist I have to deisagree with you, there are H2SO4 drain cleaners in France

I usually use this kind for most reactions, because it's very cheap (4E a liter) and never seems to pose a problem. It's dark brown colour, but over 97% content. The cheapest lab-grade I can get is 17E a liter, so it's worth a while to get the hardware store grade!
When adding a little 30% H2O2 it clears up entirely so it must be some kind of organic dye.

grndpndr - 3-4-2009 at 03:50

Certain chem supply online has technical grade 93% Sulfuric Acid in 5 gallon carboys @approx $65 with ground shipping and the $25 hazmat a little less than $100.Not great the hazmat hurts but with the cost of the drain cleaner being what it is I much prefer the 93% tech grade sulfuric acid over the unkown quantity that is drain cleaner.With gas,I have to drive 80 miles round trip for the best drain cleaner Ive found.
(Liquid Fire) I cannot recall its exact price but I think Im losing money buying the drain cleaner IIRC some $8-$9 quart
plus gas!

On the other hand to be really economical you need to get the whole 5 gal carboy to compensate for the hazmat.take up a collection w/like minded friends If nothing else.
Bulk tech grade sod nitrate, 25lb sacks @$35 less than $3 lb plus shipping and hazmat if it applies,again a known quantity pretty clean nitric acid, or nitrations.
6.95 lb asa pure powdered vet supplys,diabetic sweeteners
erithrytol $24/5lbs all plus shipping. Some of the basics can still be relatively inexpensive if shopping CAREFULLY!!

[Edited on 3-4-2009 by grndpndr]

Gamal - 3-4-2009 at 16:13

I have been searching all over for this info

The only H2SO4 I can get in Sweden is brown colored teknical grade 96 %. I want to remove the impurities from it.
Are you telling me that I can just warm it and put some H2O2 in?
Isn't it anything else then organic impuritys in the teknical grade H2SO4?
Is there any other ways to get rid of other impuritys in that stuff?

Gamal

DJF90 - 3-4-2009 at 17:14

I suspect in technical grade there will be varying amounts of metal ion contamination. The best way to purify it would be distillation, although you might want to do this under reduced pressure as sulfuric acid boils at 338C at atmospheric pressure IIRC. However the metal ion contamination shouldn't cause you any major problems unless you try using it as an analytical reagent...

grndpndr - 4-4-2009 at 10:51

Ive used old battery electyrolyte boiled down to +/- 93%
w/o issue as well as very iffy draincleaner again w/o issue in many nitrations,and nitric acid distillation.Technical grade would be a huge step up for my purposes.

Few things I can imagine where it wouldnt be adequate OT distilling over 93% nitric acid w/o concentrating the SA
first.The 93% tech grade should take care of the majority of needs successfully.

16MillionEyes - 12-4-2009 at 19:18

I've treated my drain opener sulfuric acid with 12% H2O2 and it only turns the color from brown to yellow, plus you get dilution. The stuff, however, has proved to be useless for a lot of things, but good for others.

Some people here seem to concerned about the color, but I think the important thing is the chemical inside that causes the color. Even if the color dissappears, the organic or whatever it is, still remains in some unknown way (unless you get the stuff to cleanly oxidize to CO2 and H2O assuming no other elements present) which I think is a potential screw up for organic synthesis. It is also surprising that, whatever it is that they add, is still a mystery even for the members of this board. I myself got tired of looking up for the "secret formula" but I got no success.

hissingnoise - 13-4-2009 at 04:52

If the contamination was purely organic it should be oxidised by prolonged heating and driven off as CO2/H2O.
It's frustrating not to know what's in it, and it seems a very well-kept secret. . .
If it was metallic electrolysis might plate it out, but you'd need an inert anode like Pt or PbO2.
I don't have either, unfortunately. . .

Sedit - 13-4-2009 at 08:37

Prolong heating of H2SO4 has always caused it to form small dark clumps that take a large percent of the color with them leaving a yellowish acid. I presume its carbonized organics and they can be filtered off later on with some effort.
Still for the crystal clear acid nothing works like oxidizer added to the mixture.
I don't think its really as much of a secret as much as they just dont really know whats in the drain opener so they don't bother to mention the fact that it comes as waste from other industrial process so the contents can vary widely. I would think that the best way to find the contamination would be to research where your supplier gets there H2SO4 from.

nitric - 13-4-2009 at 10:58

Just switch to reagant grade, in the end it may save your life if you mess up using battery with possible lead sulfate contaminates. To purify H2SO4 requires a vacuum distillation setup and that is extremely risky, not to mention expensive, or try to filter the H2SO4 through glass wool(clean, no plastic coated stuff, the kind that is stringy and brittle) in a glass funnel. as a note, i get my H2SO4 of of ebay from a biodesiel store that sells it for the two-step procces of making biodesiel, its 95-98% reagant grade.

[Edited on 13-4-2009 by nitric]

grndpndr - 14-4-2009 at 10:35

IIRC that may be be the most expensive source of H2SO4 Ive seen and are you sure its reagent grade?Ill check and Edit /repost if the ad claims its a reagent grade.Quick check revealed a 98% SA nothing said about it being a reagent grade but at the $54 gallon base price and $25 shipping
(hazmat wasnt mentioned)Thats very pricey sulfuric acid.
W/o assurances its a reagent grade and I would take anything e-bay adverstisers say with a grain of salt.

[Edited on 14-4-2009 by grndpndr]

nitric - 14-4-2009 at 11:16

i must add that its not shipped hazmat so order at your own risk. ill post the link when i find it.

Sedit - 21-4-2009 at 20:14

Has anyone else ever experianced this while cleaning there H2SO4 with H2O2, I did as I always do and added a few caps to a flask of dark H2SO4 to make it clear. Problem was I had the heat to high and walked away from it and when I came back to it there was the normal thick 'smoke' comming off when its concentrated all the way. The H2O2 boiled out of the solution before it had time to work and I was left with a concentrated H2SO4. Yes I screwed it up by walking away but no matter I just thought I would add a little more H2O2 and put it on the correct setting this time. The second that the H2O2 hit the now cooled down acid it started fizzing greatly and what struck me by suprize was the very strong smell of Ozone comming off the mixture. Has anyone else experianced this? I have never heard of O3 being generated by these means and it struck me as odd. I am very formilar with the smell of ozone from working with High voltage since I was very young and there is no mistaking that this was O3 bubbling out of the concentrated H2SO4/H2O2 solution.
Is this normal or what?

Formatik - 21-4-2009 at 21:09

It's normal alright. The source is the decomposing H2SO5. Bach in Ber. 33 [1900] 3117 had already noted the evolution of O3 by decomposition of H2SO5 in conc. H2SO4. And then Arnold in Ber. 35 [1902] 2903, 2906 describes evolution of rich amounts of O3 through H2O2 and H2SO4.

Sedit - 21-4-2009 at 21:32

Thank you Formatik, I assumed someone else had noted it at one time or another but Iv never heard referance to it till today. Rich amounts of O3 sounds about right. Iv worked around tesla coils quite abit and the concentration I smelled just now was stronger then anything before.
Thanks for the referances Im going to have to go look them up.

~Sedit

Formatik - 22-4-2009 at 13:55

Arnold's paper is here. He gives a procedure which he says at room temp. gives an abundant amount of ozone. Namely: in a 1 to 2 L glass flask, 15-20 ccm H2SO4 containing 5-10 g sea sand is cooled, after which 1-2 ccm of 10 to 30% H2O2 is added. The other Ber. paper is here and just describes some of the decomposition of H2SO5.

Sedit - 22-4-2009 at 15:22

Err... Aside from a few chemical names my german leaves alot to be desired. But I have no reason to doubt the man given the intensity of the Ozone I smelled last night. Its kind of strange when it catches you off guard because I was in no way expecting a blast of ozone to come off of this, I was just attempting to clear up some H2SO4 to clean any organics out. Its the first time I have synthesised Ozone from anything but High frequency electricity.

~Sedit

Elawr - 23-4-2009 at 06:46

Have any of you guys noticed no more H2SO4 drain cleaners at many of the hardware stores where it used to be sold? At Home Depot and Marvin's in my area, all I can find are solutions of sodium and potassium hydroxide in various proportions. Last place I saw any was at Lowe's.

grndpndr - 14-5-2009 at 04:16

Not yet SA drain cleaner but the local ace quit selling nitrate of soda although I do see it on the ace main web page for sale.I was BSed that store doesnt handle it others likely do.
Im so far out in the sticks its very uneconomical to drive 200miles Rt to buy 8-12 lbs of Nitrates and I hate to buy online though I suppose a few lbs of nitrates for the garden shouldnt arouse supiscion.Not like being a member of the site anyway.

Still i much prefer non -e transactions.

entropy51 - 30-5-2009 at 11:33

Please excuse any hiccups as I try my first post.

I have had good luck buying Rooto in the past; it was never very discolored and has worked well for my purposes.

I just bought a new bottle and have made two surprising observations. The first is that this bottle is very nearly colorless. It has only the very slightest brownish tint, almost identical to reagent grade sulfuric.

The more surprising thing is that when a 1 mL sample was diluted 1:100 and an aliquot titrated with 0.095 N NaOH, it appears that the Rooto is about 97% H2SO4. Since this seemed rather high (titrations of previous bottles were about 93%), I made a 1:00 dilution of reagent grade acid and titrated with the same NaOH, obtaining a very similar result as the Rooto titration.

I realize that many impurities may be lurking in this material, but judging by color and concentration it appears to be significantly better than any Rooto I've used in the past.

I'm curious as to whether others have noticed similar changes in the material sold in Root bottles?

1281371269 - 30-5-2009 at 17:23

Not a response to Entropy, but:
I heated up 250ml of One Shot drain cleaner in a flask in an oil bath over a low flame
The solution expanded significantly - Surfactants?
At first grey fumes were given off, then later white fumes - H2O / SO3 respectively
After perhaps 15minutes, most traces of the purple dye were gone, when placed in an 100ml clear glass bottle a sample of the stuff seemed almost colourless
It remained very hot for a long time, the flask of it managed to warm up three seperate pans of water before seeming any cooler - The acid maintaining the heat, or some reaction?
It also fumed for a long time - possibly I overboiled and produced Oleum?
The outsides of the flask near the top had bits of brownish material on them, as if they had been burnt - the dyes maybe?

I wonder if anyone can provide an explanation? - The expansion is most likely surfactants, and the fumes H2O / SO3 respectively
If not, it's interesting info anyhow because the drain cleaner is easily available in the UK at £7 or so / L

entropy51 - 2-6-2009 at 15:08

Mossydie,
The MSDS for One Shot (http://www.frontiersd.mb.ca/safety/MSDS/Imperial%20Soap/One%...) says that it contains 5-10% 1,2-dichlorobenzene. This might explain the foaming and brownish residue formed by heating.

The fumes are just the fog of condensed H2SO4 vapor that occurs when you heat H2SO4, I think. Heating H2SO4, even to boiling, does not produce Oleum. (We wish!)

You might want to find a drain cleaner without so much organic contaminant. Look to see what's available and check the MSDS to see what they contain, although the MSDS is no guarantee. But in the case of One Shot, it does tell you something!

grndpndr - 3-6-2009 at 22:34

It almost seems a roll of the dice despite the MSDS as far as H2SO4 Drain cleaners are concerned.Ive bought a fair quantitity over the years mainly for a quirky drain but also for use as a precursor and frankly it appears the companys sell whatever there able to buy at the time.I used to buy Rooto, perfectly aceptable for many nitrations, had an amber tint and moderate viscosity.Some months later i bought the same brand at the same store and it was heavily dyed black and when a nitration was attempted it foamed heavily as was described and resulted in a failed synthesis.

In any event i stumbled across liquid lightning in a neighboring town about 6months ago and it too was amber colored,with a viscosity similar to light motor oil.But on another thread (NG) I just read a gent bought liquid lightning and it appeared as the heavily dyed rooto I bought some years back?I gotta assume theres little consistency between batches.The suppliers buy whatevers available in bulk that meets VERY lenient specs with concentration likely to be the only one there concerned with
and its really a crap shoot.

The only answer ive found around the tech grade route(and $25 hazmat/possible flags) is using the local garage to order unused batt electrolyte (35%) and concentrate it,no hazmat and in the end I believe it to be cheaper and a far better product(ive read tech grade) though a bit more efforts required its definetly worth it as you can actually observe the nitration watching for indicators.

Cant get proper paragraphs?Resorted to breaks,Sorry.

[Edited on 4-6-2009 by grndpndr]

[Edited on 4-6-2009 by grndpndr]

[Edited on 4-6-2009 by grndpndr]

[Edited on 4-6-2009 by grndpndr]

1281371269 - 4-6-2009 at 04:41

I ordered three 1l bottles of unused battery electrolyte, I'm going to boil them down as soon as I have the time. It think they are pretty pure - but for doing things such as making HCl or HNO3 the drain cleaners will work perfectly. The electrolyte is very expensive...

grndpndr - 8-6-2009 at 17:56

Ive always bought larger amounts of electrolyte closer to 1-1/2 /2gallons approx.Its much cheaper in bulk. Besides i dont think batterys would tolerate many impurities OT the obvious lead contamination.Used battery electyrolyte contained large amounts of undissolved materials I assumed to Be
lead sulfates? Given a few hours time would settle and the clear acid could easily be decanted and the remainder properly disposed of.The concentrated used acid never giving any problems/contamination in nitrations of picric acid
one synthesis in particular where lead impurities would lead to obvious problems?!Having used both used and new electrolytes no obvious differences were ever noted though safety sake Id still prefer the unused electrolyte.Fingers ,hands ,arms or life cant be purchased for a few bucks,chump change compared even to a single 10 min DR office call.

grndpndr - 9-6-2009 at 14:55

In went to a neighboring town on a Dr visit/shopping trip.
To my utter dismay Liquid lightning was very close to $10
a liter with tax.$40 a gallon and 200ml for an unknown quantity H2SO4 and god knows what else.Thats far more expensive than bulk tech grade.
93% tech grade H2SO4 is avaiable at $70case of 6gallons,
with $59 shipping and the $25 hazmat.Unless Im missing something thats $154/case of 6gallons or $25-$26 a gallon
delivered.If thats to excessive and you dont have a partner to share costs, battery electrolyte is available from the local auto repair /auto supply in 1.5-5qallon quantitys of approx 35% H2SO4./Ive purchased it before and the result was a highly concentrated H2SO4 w/o coloration or obvious contaminations at much better prices and product.Im done with drain cleaner.$10 more would buy a gallon of 93% tech grade H2SO4 or a good quantity of a similar if not better grade acid , batt electrolyte. :mad:

[Edited on 9-6-2009 by grndpndr]

1281371269 - 9-6-2009 at 15:00

It annoys me that it costs so much for a hobbyist when it's the chemical made most in the world :mad:

Then again, how much do you use?

grndpndr - 9-6-2009 at 15:58

Obviously an order of a complete case of 6 gallons or 5gallons bulk would last the average hobbyist a lifetime and more. Realistically
though if partnered up the 5gallon bulk 35% electrolyte when concentrated to 98% should =approx.875 gall each considering a bit of loss or even if for personal use 1.75 gall
98% H2SO4 shouldnt be considered excessive particularly with the rapid dissapearance of the most common chemicals
including the nitrate salts..Speaking of dissapearing chems I was suprised to see Pyrotek i believe offereing hexamine powder @$14 lb!Peroxides over a certain % IIRC 8% + is also on a hit list of osha/ATF.Due to a rapid increase in deaths and seriuos injury resulting from peroxide accidents, FWIW.

[Edited on 10-6-2009 by grndpndr]

[Edited on 10-6-2009 by grndpndr]

1281371269 - 9-6-2009 at 16:22

The hexamine tablets can be bought pretty easily - I have some in my watched list on ebay, 8 for £4. Although I'm a bit :/ about ordering them considering I recently bought citric acid and am definitely going to buy 1l H2O2 pretty soon. It works out cheapest from ebay too - £13/l whereas a chemicals site would be cheaper but shipping would raise the total insanely, unless one were to buy it as part of a large order.

Edit: Also, is the percentage of acid in the battery electrolyte measure by weight or volume?

[Edited on 10-6-2009 by Mossydie]

grndpndr - 10-6-2009 at 06:38

HV chem. has the tech grade 93% < $20 individual gallons
5gall. $65,case of 6 (I think 6) $70
E-bay does seem relatively inexpensive for many items that otherwise would be shipped hazmat.Strange and unsettling experience inquiring about hazmat from an online batt electrolyte supplier.1.5gall-5gall carboys.Used the site to figure cost and shipping and called to confirm hazmat. it seemed as if he and I were from diff planets looking at different sites basically priced me so far out of reality it was an outright refusal to sell.

Battery electrolytes of all things?
Meth manufacture fears again?I was under the impression the pseudophed laws were the answer to all the meth man. problems!Obviously that was simply a beginning slide down the slippery slope.

I see electrolytes are measured in SP gravity now at least on the sites i visited.I imagine it helps eliminate confusion .

[Edited on 10-6-2009 by grndpndr]

[Edited on 10-6-2009 by grndpndr]

grndpndr - 15-6-2009 at 10:58

Had some leftover ROOTO brand in the house I just rented.Just a slight amber color however on heating to remove as much remaining water as possible I heated the SA in a water bath?Dont know what possesed me a water bath of all things?In an event the old ROOTO H2SO4 turned pitch black on heating at which point I killed the heat.After cooling to room temp I added approx 50ml of 8% H2O2 and let sit overnight.Next AM i again began heating the SA and a gentle bubbling began apparently oxidizing out the color/impurities leaving a water white acid.?SA remaining clear but with some loss of
its water clear appearance.As the color of the Rooto had gone so bad i had intended to use it for nitric acid production
as it stands now its the clearest H2SO4 ive ever used for nitrations save battery electrolyte?

grndpndr - 15-6-2009 at 10:59

Had some leftover ROOTO brand in the house I just rented.Just a slight amber color however on heating to remove as much remaining water as possible I heated the SA in a water bath?Dont know what possesed me a water bath of all things?In an event the old ROOTO H2SO4 turned pitch black on heating at which point I killed the heat.After cooling to room temp I added approx 50ml of 8% H2O2 and let sit overnight.Next AM i again began heating the SA and a gentle bubbling began apparently oxidizing out the color/impurities leaving a water white acid.?SA remaining clear but with some loss of
its water clear appearance.As the color of the Rooto had gone so bad i had intended to use it for nitric acid production
as it stands now its the clearest H2SO4 ive ever used for nitrations save battery electrolyte?

1281371269 - 15-6-2009 at 11:23

Oh H2O2, I might try that - and on heating it should turn to water right?
So I can just add it to drain cleaner and get clear acid, although clear acid is not necessarily pure acid...

hissingnoise - 15-6-2009 at 12:14

If you heat the H2O2 before adding the draincleaner it will turn into water.
Heating it after adding the draincleaner will oxidise some of the contaminents normally present in such acid. . .

entropy51 - 15-6-2009 at 15:39

Mossy, H2O2 + H2SO4 makes piranha acid, a ferocious acid. Use the search engine. This is not something to be attempted by the inexperienced. If you try it you should be VERY careful.

Black H2SO4 seems to work fine for making HNO3 or HCl. Decolorizing it doesn't get rid of many things likely to be in there, like the dichlorobenzene that the MSDS says in yours.

Piranha + dichlorobenzene may run away!

1281371269 - 15-6-2009 at 15:40

Oh that was silly, I knew that. My apologies. I will try a very small amount in a very large beaker.

benzylchloride1 - 19-6-2009 at 12:56

I recently purchased a bottle of Drano brand sulfuric acid. The acid looked almost like the acid in my bottle of ACS grade sulfuric acid. The acid has a very slight yellow tinge due to the paper liner on the cap of the bottle. The warning label on the bottle states that it contains concentrated sulfuric acid. Some bottles I have seen specify the ingredient as specially inhibited sulfuric acid. I have used this acid for most of my chemistry experiments and it seems to work fine.

entropy51 - 19-6-2009 at 14:15

benzylchloride1, did you mean Drano? All the Drano entries at http://www.householdproducts.nlm.nih.gov/ indicate that Drano products contain NaOH.

The reason I ask is that I recently hit the jackpot with a bottle of Rooto. It looked like ACS reagent SA and was about the same concentration, as I reported upthread. I'm wondering if Rooto put out a really good batch!

einstein(not) - 19-6-2009 at 15:28

Recently I concentrated some liquid fire drain cleaner and find myself confused with the results of the specific grafity test.

Liquid fire before boiling is a very dark reddish brown and not very viscous. Specific gravity 1.825
After boiling it becomes transparent light reddsh and quite a bit thicker. Specific gravity 1.800
After bubbling in SO3 from 500gr. of sodium bisulfate dehydrated to sodium pyrosulfate with some H2SO4 as catalyst into 250ml of boiled liquid fire it was almost clear. Specific gravity 1.700

The msds list sulfuric acid specific gravity 1.835 and rodine specific gravity 1.3-1.5

I'm wondering if I might not have dehydrated the bisulfate enough and got some dilution from steam passing over that caused the specific gravity to decrease. Shouldn't it increase with concentration?

Rodine 85 msds here: http://www.telfordindustries.com.au/Uploads/Images/HENKEL%20...

[Edited on 19-6-2009 by einstein(not)]

grndpndr - 29-6-2009 at 12:48

There is very obviously a hit and miss aspect to what youll get in regards to H2SO4 drain cleaners depending perhaps on geographic as well as time differentials..Ive seen what appears to be near reagent grade with a slight yellow tint and then the same brand some time later Ink black producing a great amount of foam during a lab,In fact ruining
the entire synthesis.

crazyboy - 29-6-2009 at 13:10

Quote: Originally posted by entropy51

Mossy, H2O2 + H2SO4 makes piranha acid, a ferocious acid. Use the search engine. This is not something to be attempted by the inexperienced. If you try it you should be VERY careful.

This is true but I have done it effectively. I was using "Flush-Out" to produce Acetic acid with sodium acetate however when I used the regular Flush-out the product refused to freeze even in a freezer while acetic acid made with reagent grade would freeze in the fridge.

Well the cleanup went very well. The acid was named "Flush Out" it came in a gallon jug and cost about $16. The acid looks like motor oil or brown cough syrup.

"

100ml of the acid were added to a 600ml beaker. Slow additions of 30% hydrogen peroxide were added and the mixture heated up and produced O₂ (decomposition of H₂O₂). About 40ml hydrogen peroxide were required to make the acid almost clear but still tinged slightly yellow.

The mixture was heated for several minutes the mixture boiled and produced dense white fumes but didn't darken. The mixture was heated for about 10-15 minutes until large plumes of fumes came over and the volume was back to about 100ml.

The result was 100ml of almost water clear sulfuric acid.

grndpndr - 29-6-2009 at 13:28

Ive had almost Identical results with 500ml of slightly less discolored H2SO4 from a very old bottle of Rooto in a rental

Liquid fire in my area is slightly discolored a yellow tint with a viscosity of approx 20wgt motor oil not a reddish tint at all.
I suppose to assure what you bought last wk is similar to whats on the shelf this week is if thers a lot #.Find a good lot
stock up.Or find a garage/auto supply/e-company willing to sell bulk H2SO4 batt electrolyte.Best way in my limited experience to get good quality concentrated H2SO4.And at $9-$11 liter drain cleaner ,cost for a superior product isnt excessive.

grndpndr - 2-7-2009 at 07:06

Wish i had some friends who ejjoyed chemistry.phoned the nearest chem and janitorial supply asking for a gallon of tech grade H2SO4,turns out they had it but it was $118 gallon

Explanation was breaking 15gallon carboys down the cost skyrockets.i asked how much then the 15gallon carboy of 93% H2SO4 would cost delivered as im on thier truck route.
No shipping charges,$151/15 gallons delivered.

1281371269 - 2-7-2009 at 12:11

15 gallons :O that's quite a lot of H2SO4...are you going to buy that much?

I tried out the H2O2 cleanup, it did leave me with nice clear acid but then I poured this into an old olive oil bottle for storage which I thought was clean...it made the acid go a strange light yellow colour, so I diluted it and poured it away which was a bit of a waste and I regret doing it.
There are several companies online that will sell reagent grade acid at reasonable prices and ship to home addresses, providing the rest of the order is not suspicious, one is lpchemicals.com

Sedit - 2-7-2009 at 12:28

I think I would if it came down to it and it was good acid.

@crazyboy

You can even get the acid much much clearer then that. If you heat it one a hot water bath for sometime until the minor fizzing of the H2O2 stops and then leave it to sit overnight or longer before boiling it down it will become water clear.
I have gotten into the habit of as soon as I get a new bottle of H2SO4 I add a couple caps of H2O2 and leave it sit for a couple days till its about the color of your pictures there. Then I heat it for about 2-3 hours on a water bath and leave it sit again. It normaly clears up completely overnight which I boil down till the thick fumes come over. At that point its ready to be rebottled in smaller containers so that I don't contaminate it with water every time I open the bottle.

Little excessive I know but I like the looks of the perfectly clear, high concentration acid I get from it because it lets me gadge the colors of reactions better for different things.

Question: I have some cheep Liquid Lightning H2SO4 around here that says "Virgin sulfuric acid with 12 buffers"

Any idea what the 12 buffers maybe and there effects on reactions. The MSDS was less then helpful and only stated 45% H2SO4 and H2O.

grndpndr - 2-7-2009 at 21:00

I wouldn hate to buy that much but everwher ive checked
with cost which is minimal,$65 /5gallons with S+h+hazmat its near the $151! if i lived in a city i could quite easily rid myself of the majority OT than a few gallons for personal use
but 500 people has few chemists or much need for diluted electrolyte.Liquid lightning is $9+tax a liter plus a 80 mile drive.So far have found no outlets for bulk(2.5 gall.) batt electrolyte.Chances are real slim id buy 15 gallon carboy w/o a solid plan to rid myself of at least 12 gallons but as I cannot find electrolyte for sale on the internet, local garages or auto supply anymore andTech grade 93% is outrageous, Im wondering what youall are gonna do when H2SO4 Drain cleaner dissapears.Scrounge used batterys?Which ive done with successful labs

Ive just tried the H202 cleanup in the last few days with a very old Rooto brand that wasnt to badly discolored until it was heated, then it turned a dark brown.Organics?Anyway i added weak 6% H2O2 to the cold
drain cleaner thyat eveninmg heated in the morning with a mild fizzing and a resulting water clear H2SO4! 500ml H2SO4
approx 5oml 6%+ H2O2.I 0nly had 3% H2O2 I froze more than 1/2 of water from resulting in approx 6% I assume.

benzylchloride1 - 3-7-2009 at 21:56

Sorry for taking so long, the sulfuric acid was Rooto brand and works well for synthesis.