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Author: Subject: Sulfuric acid dye
nitric
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[*] posted on 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. :D

[Edited on 13-4-2009 by nitric]
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grndpndr
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[*] posted on 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.:o



[Edited on 14-4-2009 by grndpndr]
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nitric
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[*] posted on 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.
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[*] posted on 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?





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[*] posted on 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.
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[*] posted on 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





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[*] posted on 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.
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[*] posted on 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





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[*] posted on 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.



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[*] posted on 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.:oStill i much prefer non -e transactions.
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[*] posted on 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?
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[*] posted on 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
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[*] posted on 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!
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[*] posted on 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]
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Mossydie
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[*] posted on 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...
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[*] posted on 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.
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[*] posted on 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]
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Mossydie
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[*] posted on 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?
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[*] posted on 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]
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[*] posted on 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]
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[*] posted on 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.:oBattery 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]
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[*] posted on 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?
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[*] posted on 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?
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[*] posted on 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...
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[*] posted on 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. . .
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