Sciencemadness Discussion Board - Hardware store chemicals - questions

Hardware store chemicals - questions

freddurgan - 29-9-2006 at 19:06

I went to my local hardware store and was pleased to find very accessible and useful chemicals.

I can get:
Toluene (bottle says 100% pure) for like 5 bucks
Xylene (unknown concentration)
VM & P Naptha (?? random alkanes?)
"Concentrated sulfuric acid" (I don't know the concentration)
Hydrochloric acid in like 20% concentration

I'm confused about sodium hydroxide. I found many products with sodium hydroxide in it, but at questionable concentration and other chemicals.

Do any of these not function well as lab chemicals? And why? Solutions?

Thanks!

Magpie - 29-9-2006 at 19:53

Look for the one that says 100% lye.

not_important - 29-9-2006 at 20:27

All of these will ahve some impurities in them, how important they are depends of the use.

Xylene should be pretty pure, maybe some ethylbenzene. But as it's an ortho/meta/para mix, generally it's just used as a solvent and the other compounds that might be in it won't affect that use.

VM & P is just hydrocarbons, mostly saturated. There's a set of specifications on boiling range and what not, again it's a solvent.

Concentrated sulfuric acid seems to run from 80 to 95 percent. Sometimes it has other ingredients in it but they should be listed or implied with statements like "improved anti-corrosion formula", these are likely a lot less useful.

Typically it is brownish to almost black, this is generally traces of hydrocarbons and elemental carbon. That can be removed to some extent by heating the acid to boiling, and usually occurs during concentration if you need to do that.

Concentration to 98 percent is done by distilling off the water until the constant boiling temperature of 330 C is reached. For weaker acids just a simple open flask or dish will do, but once the concentration hits 80% or so then the vapour will contain acid as well and some sort of simple fractionation is wanted.

Concentrated sulfuric acid likes to bump when boiled, boiling stones and bits of broken pyrex help reduce this problem. But it means that you shouldn't heat the concentrated acid to near bolling in a open/wide-mouthed container, because it is going burp acid at you.

Hydrochloric acid typically has traces of iron in it, giving it a yellow-green tint. The 20% concentration is slightly less than constant-boiling, and doesn't fume nearly as much as the other common 30 to 36 percent acid. You can distill the 20% acid to remove impurities; if you do this with the stronger acid it will lose HCl gas until the strength drops to the constant boiling range. You can put distilled water in the receiver to absorb the HCl gas, if you measure it correctly you'' end up with the 20-21% acid.

Drain-cleaning sodium hydroxide will show up as everything from a water solution with potassium hydroxide, to nearly pure NaOH with small amounts of the carbonate and calcium or NaCl in it, to mixtures that are sold as being better at cleaning out drains. For most purposes small amount of carbonate, calcium, or chloride aren't going to matter, often this will be labled as 100% lye. The mixes are another story, usually aren't that useful.

Quince - 1-10-2006 at 01:06

Regarding the sulfuric acid from drain cleaner, I suggest heating the stuff until a temperature that is likely to deactivate any buffers they have added, plus that will evaporate some of the water. The solvents can have their purity improved by distillation, especially if you have a Vigreux of fractioning column.

not_important - 1-10-2006 at 02:02

The sulfuric acid drain openers do not have buffers in them. They may have corrosion inhibitors to protect the pipes, and surface agents to speed penentration of the plugging material by the acid. They also seem to have dyes and possibly other agents in them to make them look like something other than water, to make them look like stuff you don't want to touch.

The corrosion inhibitors may include inorganics like phosphates, these would not be affected by heating. Organic inhibitors are likely to be oxidised by heating the acid to near boiling, as are dyes and surfacants; these are not 'inactivated', they are oxidised to CO2 and water with SO2 being produced.

One MSDS listed 0,5% thiourea as the corrosion inhibitor., this would seem that it might release some H2S during heating.

Polyethylene oxide seems to be a common surfacant, 0,2 to maybe 1,0 percent; the higher concentrations will thicken the acid even though the surface tension and this 'wetness' is lowered.

US patent 5429764 is for a sulfuric acid based drain opener, and lists possible additives. Amount those are perfluoroalkyl sulfonates, which are not going to be easy to break down just by heating the acid; various other fluoronated additives are listed.

If you actually distill the acid, not just concentrate it, most inorganics will remain behind. If you can do that, and there seem to be much organics in the acid, adding some potassium persulfate to the acid before distilling (but after a preliminary boil) will oxidise the organics so that none carry over into the diistilled acid. However distilling sulfuric acid is not to be undertaken lightly, you need all-glass apperatus and can not use hydrocarbon grease on any joints. And it will be _hot_, 330 C boiling point.

Those in the US counting on getting their sulfuric acid from drain opener should read this. It appears that the request was turned down, but another may be in the works - I'm not sure if what I saw on the request refusal applied to this or a previous one.

http://cpsc.gov/pr/sado_moore.pdf#search=%22sulfuric%20drain...

Quince - 1-10-2006 at 02:54

Quote:

Originally posted by not_important
adding some potassium persulfate

Uh, I think anyone needing to use drain cleaner as a source for H2SO4 will have even more trouble obtaining K2S2O8. If you're living in the US, someone on eBay does sell it. Elsewhere like Canada, good luck. You might as well tell us to make H2SO4 by diluting oleum.

[Edited on 1-10-2006 by Quince]

Nicodem - 1-10-2006 at 03:23

I would assume his notion included Oxone as a potassium persulfate equivalent as well. But generally a little H2O2 is added (very carefully!) to the dirty H2SO4 if the only goal is to decolorize it and then concentrate it by heating only.

Quince - 1-10-2006 at 03:39

Actually I tried a bit of 35% H2O2, but the original slight yellow tint was unchanged.

Nicodem - 1-10-2006 at 03:43

Yellow? What's wrong with yellow? I was talking about the carbon and other black stuff in some hardware store H2SO4. A yellow tint says not much about the purity of a compound. If it only has a yellow tinge then you can even assume that it is quite pure and better don't mess with it unless you know it is not pure.

Quince - 1-10-2006 at 04:24

So if not carbon etc., what's the yellow from? It's gotta be from something.

Vacuum Distillation

MadHatter - 1-10-2006 at 07:43

I've used this for some of the more shitty H2SO4 drain cleaners like Roebic but
find it unnecessary for Rooto. Rooto does a great job on its own and doesn't have the
severe discoloration I've noticed in others. My next purchase of H2SO4 drain
cleaner will be the "Misty" brand. Supposedly it's as high as 93%. I'm currently searching
local janitorial supply houses for this one.

evil_lurker - 1-10-2006 at 14:05

Sometime in the near future I'm going to attempt to get a 750lb drum of 96-98%concentrated technical grade. Should be much better than the stuff sold as drain cleaner.

My plan is to repackage it and sell it by the liter with a minium order of a 4L case. I could sell larger quantities, but then it would have to go Hazmat which would eliminate any potential savings.

I'm going to try to keep the cost below $10 per liter.

My question is would anyone be interested?

Quince - 1-10-2006 at 16:58

Can you ship to Canada?

not_important - 1-10-2006 at 17:20

Quote:

Originally posted by Quince
So if not carbon etc., what's the yellow from? It's gotta be from something.

In general it is traces of carbon or carbon compounds, and/or iron. You can do a test for iron to if your particular source has iron or not. Larger amounts of carbon tend to go orange-brown, brown, brown-black, or used-automotive-oil black as the amount of carbon and carbon compounds goes up.

not_important - 1-10-2006 at 17:27

Quote:

Originally posted by Nicodem
I would assume his notion included Oxone as a potassium persulfate equivalent as well. But generally a little H2O2 is added (very carefully!) to the dirty H2SO4 if the only goal is to decolorize it and then concentrate it by heating only.

The persulfate is what the more recent purification of reagents texts suggest. I've always used H2O2 myself, adding it drop by drop to the hot acid until it seems to have no more effect, then boiling for a bit to decompose any excess H2O2.

I think that H2O2 is no longer suggested because of the possibilty of explosion if too much is added at once, or added to cool acid which is then heated. With the organics they put in some drain cleaner acid, I would be careful using H2O2, get the acid hot first, keep the addition rate down and in small portions.

Adding H2O2+water to concentrated sulfuric acid is going to splatter and spit, best to do it in a flask.

Note the the stablisers in the peroxide are going to end up in the acid.

evil_lurker - 1-10-2006 at 18:25

Quote:

Originally posted by Quince
Can you ship to Canada?

Shouldn't be too much of a problem.

I can send it anywhere UPS ground can go.

Quince - 1-10-2006 at 18:45

Uh oh... UPS over the border is a no-no. They charge a ludicrous brokerage fee (separate from the customs charge itself). US Postal Service is the way to go...

evil_lurker - 1-10-2006 at 20:32

See that'd be the catch right there. You can't ship concentrated sulfuric acid via USPS.

If they caught me mailing that my ass would be grass.

Quince - 2-10-2006 at 00:51

What about FedEx or Purolator?

UPS may be worth it for say 10 L and up.

[Edited on 2-10-2006 by Quince]

Thermal - 2-10-2006 at 11:34

DHL used to be pretty good about chems - dunno about now.

indigofuzzy - 7-10-2006 at 00:54

Kinda curious, Is there an easy way to get ahold of dilute sulfuric acid, aside from buying the concentrated stuff and diluting it? I've heard that there's some special way to dilute strong acids without hurting yourself, and doing it the wrong way = bad things happen. So I'd prefer, if i can, to find a source of more dilute (say 20-50%) H2SO4, that's still relatively pure (that is, just H2S04 and water).

But maybe I ask WAY too much...

Quince - 7-10-2006 at 03:43

Automotive electrolytic battery.

ethan_c - 7-10-2006 at 09:12

Some drain cleaners. Many have at least a significant amount of H2SO4, and there are several that are essentially the concentrated acid, maybe with a few surfactants.

Quince - 7-10-2006 at 09:35

His point was he didn't want to spend on concentrated acid. H2SO4 is only useful for a drain cleaner when it's concentrated, so any drain cleaner he'll find will not be dilute.

Baphomet - 21-11-2006 at 04:50

If you need to dilute it indigofuzzy just remember to add the acid to water rather than the other way around, and try not to breathe any fumes.
Where I live it's easier to obtain a semiautomatic weapon than to get pure H2SO4. The drain cleaner is mixed with copious amounts of 'morning fresh' or similar

I'm not above emptying an old car battery to get sulphuric.

grndpndr - 9-11-2009 at 04:59

Quote: Originally posted by Quince

Automotive electrolytic battery.

Ive found used battery electrolyte more useful than any of the reccomended brands of drain cleaner.Bit more work,questions,but the result is water clear concentrated H2SO4 likely some lead contamination.Fresh Battery electrolyte
<$15 6x950 ml/$30 2.5gallons IIRC? 1.265 SG. Around 2L+ 98% per 6qts my ciphering?Concentrated Electrolyte Far cheaper than even a local PU of tech grade H2SO4 93% sans shipping unless I wanted to buy 5gallons.I considered the same reselling as the other poster but decided against the additional hassle possibly w/LEO,sales tax,license etc.Im on thier shipping route so no hazmat/or shipping charges period.Chem+Jan.supply very handy as would be the 'lowly' school janitor and his unquestioned access to useful chemicals.
batt.electrolyte needs to be pretty clean of contaminants or the battery will be("poisoned") short lived ,lead contaminats of course being the exception in used elecrolyte,being no problem given its usual intended use.And most auto shops are eager to rid themselves of dead batt.Rather than pay a premium to have them picked up,only problem being the new
sealed batterys however simply drillin a hole in the individual cells will give access to the electrolyte.
I could be way of base here but the information I run into is the waste acid from steel mills,H2SO4 used to remove the scale from rolled steel plate etc is reused in drain cleaners.
Any drain cleaner i had left would be used for Nitric acid production/cleaning my clogged drain, which was $9 L! for Liq Lightning/worse,Black Rooto.FWIW

[Edited on 9-11-2009 by grndpndr]

hissingnoise - 9-11-2009 at 06:09

I've found the red shit and the clear acid on the same shelf in hardware---if there are two brands I open the top and have a peek under a light (and sometimes the containers are translucent); if anyone asks, I just say (something like) I wondered why the bottle was so friggin' heavy and had to have a quick look. . .

grndpndr - 9-11-2009 at 06:26

Good Idea,always have a preplanned (not rehearsed) reply
to any questions your likely to encounter.The cleanest Ive encountered (visually)is the Liq lightning,Rooto,IME sometimes varies between midnight black and a light wt clean motor oil coloring like the lot # Liq lightning Ive found.But even the electrolyte can be difficult to get unless your known or you find the right counter person.An individual can order the 5gall -15 gall lots of 93% SA locally but A well though out reason for its need best be ready and the 15gall obviously excessive.The recent use of 98% H2SO4 for use in recycling used veg oil to diesel fuel etc .99% NaNO3 is also available for the same use as is 100% lye etc.Tighter control of SA's inevitable.
IMHO

[Edited on 9-11-2009 by grndpndr]

hissingnoise - 9-11-2009 at 06:40

I've never seen black stuff this side of the pond; the darkest was a bit darker than Rosé!
At 9 Euro for half a litre, it's not cheap. . .

[Edited on 9-11-2009 by hissingnoise]

grndpndr - 9-11-2009 at 06:53

Rose Odonnel?Oh you mean wine!The only wine Im familiar with would be Ripple,MD20/20/Cabernet Suavignon.Closer to a MD20/20 w/o the purplish hue.So maybe a bit of exageration but very dark in fact I had no changes in coloration at all during the lab even during sulfonation.

Seriously,same store,only brand they carry, I was in fact very suprised myself.

At $9 euro a half liter its not cheap". To what do you refer?

[Edited on 9-11-2009 by grndpndr]

hissingnoise - 9-11-2009 at 07:06

Both grndpndr, but the acid is never more than 9 Euro---not yet anyway!
Rosie O'Donnell---now she is dark, and more than a match for Larry David!

[Edited on 9-11-2009 by hissingnoise]

hissingnoise - 9-11-2009 at 15:20

I wonder why those posts deserved such summary deletion?
Seems a bit over-cautious. . .

Polverone - 9-11-2009 at 15:38

The whole series of responses was based around a now-deleted spammer's post. They cluttered the thread and didn't even make sense after the spam-post was removed.

entropy51 - 9-11-2009 at 17:29

You should look around some more!

Quote: Originally posted by entropy51

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 1:100 dilution of reagent grade acid and titrated with the same NaOH, obtaining a very similar result as the Rooto titration.

grndpndr - 9-11-2009 at 21:17

Thanks for the sage advice.When i need better/cheaper than
'the concentrated elecrolyte Ill run right out 200 miles round trip to pay more for a product of an unknown quality/content.Or order tech grade 93% H2SO4 $19.95 gallon add shipping/hazmat and pay $70+ gallon.The Liq. light. Ive seen lately does have a light motor oil color and viscosity and may work fine for most uses.The Rooto I no longer buy due to the experience I had with the product being very dark for whatever reason which may only have occurred with that lot#.Eectrolyte I know is made to standards w/o contaminants that would "poison a battery" and is cheaper.I need look no further than a friendly auto supply store, thanks.

Its a personal preference based on the fact Im aware of whats in a battery electrolyte and its cheaper after concentrating to 93% than drain cleaner which I havent a clue where it came from and what it was used for prior to bottling as well as what additives are used to protect the pipes?That should be an acceptable personal decision with valid reasoning.NO?Besides the fact its much easier to observe labs w.water clear H2SO4 and anything that might or might not be occuring than with a darker substitute.Im glad your happy with your choice.I am happy with mine,my wallets a bit healthier and it serves its purpose quite well

[Edited on 10-11-2009 by grndpndr]

entropy51 - 10-11-2009 at 07:06

Quote:

I havent a clue where it came from and what it was used for prior to bottling as well as what additives are used to protect the pipes?

According to the Rooto company, it's drain opener contains no additives, but not true of many other brands. Apparently some lots were not used for anything prior to bottling. But to each his own.

grndpndr - 10-11-2009 at 18:49

I have bought rooto before and it was perfectly satisfactory.
For all I know the current lot on the shelves is exactly as you describe.As I said the Liq.Light. seems to be a perfectly fine product OT the moderate discoloration and of course the price.It may be cheaper in your area but it is $9 L out here and 85 miles RT
but then again theres 3 hardware stores within 42 miles one way. After the single experience with what I still believe to be Rooto has made me gunshy.

Anyone have this experience of 'clarifying' H2SO4 of the discoloration with H202 only to have the discoloration return
after reheating the H2S04 to Rid the SA of any accumulated water?The acid became near crystal clear after a small addition of H202 but returned to its orginal if not a darker color opon reheating? Im afraid I keep horrid notes of my labs so thats no help as far as the exact order/temp involved.

I agree Entropy if it works for you great I have no bone to pick w/anyone,as you say to each his own.

Respectfully,grndpndr

[Edited on 11-11-2009 by grndpndr]

entropy51 - 10-11-2009 at 18:56

Thanks, grndpndr! I think it's good for people to put their different experiences out there for people to consider. Proximity of the supplier is definitely a consideration. I'm sure I'll get burned on Rooto eventually, as you once said buying it is a crap shoot.

Formatik - 10-11-2009 at 21:28

Quote: Originally posted by grndpndr

Anyone have this experience of 'clarifying' H2SO4 of the discoloration with H202 only to have the discoloration return
after reheating the H2S04 to Rid the SA of any accumulated water?The acid became near crystal clear after a small addition of H202 but returned to its orginal if not a darker color opon reheating?

That might be a ferric sulfate contaminant.

bbartlog - 10-11-2009 at 22:07

Quote:

Had this happen with my homemade H2SO4. I think it's likely some organic compound that's quite resistant to oxidation. Ferric sulfate seems like it should usually be reddish, but for all I know that changes once the pH drops to zero.

hissingnoise - 11-11-2009 at 02:15

Oxidisable contaminents are oxidised fairly quickly by hot concentrated H2SO4 so H2O2 treatment isn't neccessary. . .

Quote: Originally posted by bbartlog

Had this happen with my homemade H2SO4.

Homemade bbartlog---pray tell?

Formatik - 11-11-2009 at 12:01

Common impurites of sulfuric acid known to older chemists and depending on the process used, include: HNO2, HNO3, hyponitric acid, sulfurous acid, arsenous-, arsenic acids (this from arsenic-containing sulfur or ores), lead sulfate from lead chamber or lead pans, small amounts of iron oxide, copper oxide, calcium, or alkali partially from the water. Selenium from selenium-containing sulfur and ores. Hydrochloric acid from KCl. Antimony oxide, thallium oxide, mercury oxide (from sulfur or sulfur ores). In addition we know the brownish discoloration imparted on sulfuric acid by organic bodies. The charr and suspension of carbon. But also the brown and black humic compounds e.g. humic acid and humin formed when sugar is boiled with sulfuric acid. Unless a deliberate impurity is added to the drain cleaner like a dye or foam agent, I doubt the kinds of impurities encountered are going to have changed much since then. But suspect a better modern management of impurities like arsenic.

Simple distillation of impure sulfuric acid which isn't done too long leaves behind non-volatiles like Pb, Fe, Ca, K salts, etc. That could at least rule those inorganics out. Iron contamination from iron oxide comes from fuming sulfuric acid process. To see if copper or iron are present, precipitation with H2S or ammonium sulfide would show if they are. According to Justus Liebig, lead can be separated nearly entierly by diluting with water and allowing to settle.

To test for lead one test was (described in Handwörterbuch der reinen und angewandten Chemie by Liebig), to conc. sulfuric acid: 1 to 2 drops hydrochloric acid was added. In the presence of lead - at the point of contact - there is immediately white cloudiness and on shaking a white turbidity results which disappears on further addition of hydrochloric acid. The most sure and accurate way to do this is said to be done by using sulfuric acid which has at the most 1 volume percent strong hydrochloric acid added.

[Edited on 11-11-2009 by Formatik]

bbartlog - 11-11-2009 at 12:52

Quote: Originally posted by hissingnoise

Homemade bbartlog---pray tell?

Nothing practical, I'm afraid. I electrolyzed an MgSO4 solution with a terra cotta (flowerpot) membrane placed in an HDPE bucket. Stainless steel cathode in the flowerpot, lead anode outside the flowerpot in the bucket. Ran it for several days using a battery charger (6V). Accumulated Mg(OH)2 inside the flowerpot and on the cathode was removed daily. Then I boiled down the acid portion until I had a rather concentrated solution, and added ethanol[1], causing the remaining MgSO4 and water to separate from (most of) the H2SO4 and alcohol. Then I distilled the H2SO4/alcohol, adding dilute H2O2 a couple of times (both to oxidize organics and to provide water, which allows more alcohol to be driven off before the H2SO4 gets so concentrated that it starts turning the ethanol into other things).
Net result was about 120g of fairly concentrated H2SO4 (though I have yet to titrate it). Impure though; dark even after adding H2O2 and reconcentrating. And not worth the effort if you have access to any commercial source. I actually have both a 1 gallon and a 1 liter container of Rooto H2SO4; this was just done as an exercise.

[1] I also used IPA on one occasion. Though this does separate, I find that it ends up making a weird slushy mixture with the MGSO4/water portion if there is a lot of MGSO4, and this is harder to separate than the analogous (EtOH+H2SO4)-(MGSO4+H2O) mixture. The ethanol doesn't seem to 'stick' to the MGSO4 crystals as much, for example you can filter it off of them without vacuum. I also think the IPA is more likely than the ethanol to be responsible for any remaining organic gunk.

grndpndr - 11-11-2009 at 13:37

Wouldnt ferric sulfate be assosciated with the use of H2SO4
to remove scale from rolled steel/iron plate.One of the uses I had heard the H2SO4 was used for pior to it being used as an acceptable waste acid in drain cleaner?Ergo the darker color upon heating

The H2O2 was added to cold H2SO4 and slowly heated the following day,not added to hot SA.The acid cleared but returned to the original color upon boiling to remove any introduced water.

Formatik,you mentioned diluted SA contaminated with lead
would precipitate out according to a source I cant recall.
To take this further then would lead sulfate also precipitate out of used lead /acid electrolyte which could be removed by careful decanting?Using this method Ive had very good results concenrating the electrolyte to a water clear concentrate but metals content particularly lead is a concern.
although I suspect other metal contamination in electrolyte is low
the concern being possible 'poisoning' of the battery.

[Edited on 11-11-2009 by grndpndr]

[Edited on 11-11-2009 by grndpndr]

Formatik - 2-12-2009 at 00:32

Quote: Originally posted by grndpndr

Formatik,you mentioned diluted SA contaminated with lead
would precipitate out according to a source I cant recall.
To take this further then would lead sulfate also precipitate out of used lead /acid electrolyte which could be removed by careful decanting?Using this method Ive had very good results concenrating the electrolyte to a water clear concentrate but metals content particularly lead is a concern.
although I suspect other metal contamination in electrolyte is low
the concern being possible 'poisoning' of the battery.

Sorry, I didn't see your question until now, grndpndr. With lead contaminated acid, expect sol. PbSO4 content even as high as 1.1%, esp. when conc. Although H2SO4 concentration increases solubility of PbSO4 a lot, traces of the acid have been found to actually decrease solubility in several experiments done by Sehnal (Compt. rend. 1909, 148, 1395), so a 0.049% H2SO4 solution only solubilized 0.0006g PbSO4 per 100cc solution equivalent. If it's true, then it is close to as good as ACS grade. ACS grade sulfuric acid has 0.0001% heavy metals (Pb). Decantation or siphoning should work if settled sediment from around the bottom of the liquid does not come over. But there also is always distillation. Distill it enough and you have trace metal grade.

Picric-A - 3-12-2009 at 11:46

Try bubbling a bit of H2S through the PbSO4/H2SO4, then chill to Ppt PbS.
Filter though glass and you have much purer acid.

Formatik - 4-12-2009 at 16:40

Conc. H2SO4 would probably solubilize PbS forming PbSO4, in that case I'd suggest dilute acid also. But generating H2S can have its own issues. I would rather chose to separate as mentioned in the post above.

grndpndr - 18-12-2009 at 04:03

Belated thanks for the responses.The dacantation worked well but as to lead content I did no testing at the time but the result was a water clear H2SO4 from OLD battery acid w/o filtering,high temp distillation.That it was clear is no indication of contaminants or lack there off I only know the acid was perfectly satisfactory for my uses and was free though somewhat laborious but did I mention free and successful synthesis.

OT but did anyone happen to see a show concerned with a barge salvage operation. Im sure this was following Katrina?
The cargo was H2SO4 filling a 4000 ton river barge

No specifics as to the H2SO4 concentration etc.Destined to become Rooto/LL maybe

[Edited on 18-12-2009 by grndpndr]

entropy51 - 18-12-2009 at 06:31

Quote:

Destined to become Rooto/LL maybe

More likely to a Gulf coast oil refinery. I believe they still use H2SO4 by the bargeload.

grndpndr - 18-4-2010 at 14:20

Im afraid had I been on the job they never would have missed a few 5gallon HDPE containers.Lightn the load dont ya know.Helpin out!

Maybe akin in some way to its use in biodiesel!??
Anyway I could likely have put it to good use!

[Edited on 18-4-2010 by grndpndr]

[Edited on 19-4-2010 by grndpndr]

The WiZard is In - 19-4-2010 at 10:42

Quote: Originally posted by freddurgan

I went to my local hardware store and was pleased to find very accessible and useful chemicals.

I can get:

Thanks!

Copper and aluminium sulphate
Calcium, potassium and magnesium chloride
Sodium tetraborate
Sodium silicate solution

Calcium hypochlorite - useful in making chloroform.
Which speak of — was discovered not far from the
current Schloss Zauberer [Hexenmeister] where in
The Bibliothek WiZardæ (the finest collection
of arcane publications and nudist magazines in the
free world) just off the grand ballroom I find shelved :—

Linda Stratmann
Chloroform : The Quest for Oblivion
Sutton Publishing 2003

Not strong on chemistry, but interesting.

What may be more interesting is what you can
no longer easily buy OTC —

Carbon tetrachloride
Trichlorethlene
1,1,1 Trichloroethane
Oxalic acid
Tri-sodium phosphate (TSP)
&c., &c.

[djh/
-------
Do you believe that the sciences would ever had
arisen and became great if there had not beforehand
been magicians, alchemists, astrologers and WiZards,
who thirsted and hungered after abscondite and
forbidden powers?

Friedrich Nietzsche
Die fröhliche Wissenschaft, IV, 1886

bbartlog - 19-4-2010 at 12:09

Quote:

Oxalic acid
Tri-sodium phosphate (TSP)

I was able to buy both of these at a hardware store about a year ago. I do sometimes wonder whether some of the chemicals I buy are old stock that will not be replaced (I bought a gallon of sulfuric acid at an old hardware store that I strongly suspect will not be restocked) but the Na3PO4 and oxalic acid appeared to be regular items of trade with multiple boxes/tubs on the shelf, not dusty or anything.
Dichloromethane is something I can't seem to find OTC in these parts... there is a five-gallon pail of some parts degreaser at the local auto parts store that appears to be mostly DCM, but all the smaller containers of superficially similar solvents appear to be petroleum distillate based. And I don't need nor want to pay for five gallons of solvent.

grndpndr - 22-4-2010 at 21:07

I recently noticed TSP at a hardware store some Distance away.
New I shoulda bought some but its a source of very good drain
cleaner (liquid fire) works well Ill be back but given the chance I buy batt. electrolyte $14 6 L 34%.Much cheaper and no additives.Local ACE
Is no longer the place! Close stores no longer stock the stuff that was useful. Gotta get creative and spend gas money.

chief - 23-4-2010 at 05:15

Has anyone a suggestion for finding toluene or benzene in germany, from hardware-stores ?

hissingnoise - 23-4-2010 at 05:32

Companies specialising in industrial paints/coatings should still carry toluene (toluol) but the last time I looked in my local hardware I could see only xylene. . .

gnitseretni - 23-4-2010 at 08:55

Walmart carries a paint thinner that has a high percentage DCM in it, for those who are looking for it. This one http://www.wmbarr.com/product.aspx?catid=72&prodid=117

None of the hardware stores around here carry toluene anymore and xylene seems to be slowly disappearing as well.

grndpndr - 23-4-2010 at 19:23

i BELIEVE IVE SEEN TOLUENE RECENTLY BUT THATS THE EXCEPTION.
iF YOU INTEND TO GET SOME OF THESE DISSAPEARING SOLVENTS ETC
BETTER DO SO POST HASTE.ACETONE,TOLUENE ALMOST NONEXISTENT,MEKP'S GETTING THERE.UNFORTUNATELY THERS QUITE ALOT DISSAPEARING FASTER THAN i CAN BECOME AWARE OR AFFORD.

aonomus - 25-4-2010 at 21:28

I have found that quite a few of the chemicals being removed from OTC sources but not restricted by law may be due to environmental issues. Chlorinated compounds, DCM (paint stripper), perchloroethylene/tetrachloroethylene (dry cleaning) are less available due to health concerns, improper disposal, and better options (such as CO2 based supercritical extractions). Trisodium phosphate was a concern as a phosphate source for eutrophication of water bodies, such as Lake Erie which was totally eutrophic for a while but managed to turn around and become productive again.

Other chemicals are harder to find/get due to lack of popular demand, not everyone needs copper sulfate root killers anymore, with all the suburban cookie cutter houses, few people actually have to deal with old-growth hardwood trees that work their way into old piping/sewer pipes.

On the bright side in Toronto, a local commercial plastics shop carries chemicals such as MEK, toluene, acetone, GAA, and DCM in usable amounts with reasonable prices, straight from a local chemical supplier in metal tins with the original labeling.

watson.fawkes - 27-4-2010 at 05:27

Quote: Originally posted by aonomus

I have found that quite a few of the chemicals being removed from OTC sources but not restricted by law may be due to environmental issues. [...] On the bright side in Toronto, a local commercial plastics shop carries chemicals such as MEK, toluene, acetone, GAA, and DCM in usable amounts with reasonable prices, straight from a local chemical supplier in metal tins with the original labeling.

I can second this. As far as solvents go, the phasing-out of oil-based paints came about because of concerns about air pollution from VOC (volatile organic compounds, i.e. solvents) concerns. There's less use of solvents now, and it's not economical to stock them at some point, so the item disappears off the shelf.

I'll also second the point about industrial availability. Much of what's disappearing from ordinary retail (big box home store) is still available from trade suppliers. For example, the BBHS's around here no longer stock toluene (they dropped it fairly recently), but it's still available at paint suppliers and other suppliers to tradesmen.

SWilkin676 - 10-5-2010 at 11:00

Ace Hardware still carries TSP. Some things you have to go out into the rural stores for.

Stores that sell epoxy supply still have pretty decent solvents.

I found this link on another forum - nice data for flammables.
Ignitable Liquids Database

The WiZard is In - 10-5-2010 at 13:54

Quote: Originally posted by SWilkin676

I found this link on another forum - nice data for flammables.
Ignitable Liquids Database

------
Ignitable Liquids Database - No. Must be Obama Admin. at work
again. Search failed to find two of the most flammable liquids
that come to my mind — carbon disulphide and ether [ethyl/sulphuric].

For serious fun I reference : —

RDTR No. 144
Handbook of Selected Properties of Air-and Water-Reactive Materials.
U.S. Naval Ammunition Depot Crane, Indiana
March 1969

I own a library bound - what appears to be an NTIS copy. I would be
A- Astounded and B- Amazed if it couldn't be DL'd. It lacks an index.
Once again I would be A & B...

By da — page 145 is not totally readable in either versions.

watson.fawkes - 10-5-2010 at 14:59

Quote: Originally posted by The WiZard is In

No. Must be Obama Admin. at work
again. Search failed to find two of the most flammable liquids
that come to my mind — carbon disulphide and ether [ethyl/sulphuric].

Given that it's a database of consumer products, this is hardly surprising. It takes all of a minute to figure this out. Incidentally, "SRN" stands for "sample reference number", which takes about another minute with Google to figure out.

I'll just chalk up arbitrary political defamation as another attribute of your activity here.

The WiZard is In - 10-5-2010 at 16:28

Quote: Originally posted by watson.fawkes

Silly me. I would have though that a data base prepared by the
National Center for Forensic Science would be more complete.
Apparently they like O's admin. refusal to use the word terrorist —
are only concerned with amateur arsonists.

djh
----
You get a lot more co-operation with a
kind word and a gun — than with a kind
word alone.

Al Capone

not_important - 10-5-2010 at 17:44

Quote: Originally posted by The WiZard is In

Ignitable Liquids Database - No. Must be Obama Admin. at work
again.

From that site

Quote:

The Ignitable Liquids Reference Collection (ILRC) was developed by the ILRC Committee of the Technical Working Group for Fire and Explosives (TWGFEX). This reference collection stems from the pioneering work of the Illinois State Police Crime Laboratory System under the leadership of Bruce VanderKolk and Susan Johns, and the Pinellas County (Florida) Crime Laboratory under the direction of Reta Newman and Kevin Lothridge.

Committee Members

Sharee Wells (Committee Chair) Alabama Department of Forensic Sciences

Craig Bryant (Committee Chair) Centre of Forensic Sciences

Steve Allen National Center for Forensic Sciences - UCF

Mary Williams National Center for Forensic Sciences - UCF

Michael Sigman National Center for Forensic Sciences - UCF

Doug Byron FAST

Carol Clemmons US Army Criminal Investigation Laboratory

Jess Dunn Iowa DCI Crime Laboratory

Sherrie Thomas Bureau of Alcohol, Tobacco, and Firearms

Karen Fleisher Miami-Dade Police Department

Tracey Ray Charlotte-Mecklenburg Police Department

Ruth Henk Wisconsin State Crime Laboratory

Judi Hoffmann Montana Forensic Science Division

Copyright © 2006 University of Central Florida. All Rights Reserved.

Someone seriously needs to get that time machine away from that dude, 1st was posting bogus birth announcements in the Honolulu papers, now it's creating defective database before he was elected.

Might it possibly that nowadays hardware stores rarely stock CS2 or Et2O, and thus they are very rarely used in arson?

The WiZard is In - 10-5-2010 at 18:48

Quote: Originally posted by not_important

Might it possibly that nowadays hardware stores rarely stock CS2 or Et2O, and thus they are very rarely used in arson?

Which would be a good reason to use them... no one would look for them.

General JH Binford Peay, commander of the US Central Command, on the bombing in Saudi Arabia.

"You would not see this in the normal types of terrorism."

Professional soldiers are predictable, but the world is full of amateurs.
Murphy's Laws of Combat

regarding CH2Cl2

Formatik - 29-6-2010 at 20:17

The dichloromethane obtained by distilling hardware store paint stripper will typically contain methanol (sometimes other volatiles also). These two form an azeotrope that boils at 37.8C and has 92.7% by mass dichloromethane, the rest methanol. I've distilled before such a paint stripper just trying to distill out dichloromethane and the density of the distillate was measured, 1.26g/cc. This is also the density one estimates of the azeotrope. H2O also forms a more minor azeotrope.

Methanol forms addition compounds with a number of salts. Like with CaCl2 it forms CaCl2.3 CH4O and CaCl2.4 CH4O (Ann. 19, 168; Z. a. Ch. 52, 15, etc). (CuSO4)3.CuO.4 CH4O forms from cupric sulfate and a lot of methanol (C.r. 142, 1272), green needles, that decompose easy at 110 deg., and lose methanol in moist air under decomposition. MgCl2 + 6CH4O are deliquescent crystals (J. pr. [2] 20, 376), etc. EtOH also forms similar addition compounds.

This is apparently one way of removing the methanol. Several others have been talked about (UTFSE). I've been meaning to distill the CH2Cl2 with CaCl2, then measure the density of the distillate, but haven't got the time right now.

quicksilver - 16-12-2010 at 10:08

A very quick little note about tri-sodium phosphate (TSP): a Bill has past some moths back and 14 Sates in the USA have banned TSP from use in
DISH WASHING DETERGENTS. This now pretty much voids all soaps and detergents from the addition of phosphates. The run on the sale of TSP has been mentioned in the local news. It seems that certain dishwashers demand tri-sodium phosphate due to highly calcified water which when run through small outlet jets: clog. Dishwasher service calls are becoming overwhelming and the standard method of oxalic acid flushes using a commercially sold item run into a $7 washed set of dishes. Result is a run on industrial TSP, which in-turn is getting environmental types screamingly angry.
News-radio item was owner of store stating tri-sodium phosphate (TSP) will no longer be sold.

Those who had predicted that certain OTC chemicals will be lost are apparently correct; especially if they have an environmental impact that has either sudden or observable repercussions.

The other issue is ammonium nitrate. I live in a rural state (for the most part) and we were able to obtain ammonium nitrate via truck. The bagged ammonium nitrate was stopped via agreement with fertilizer manufacturers on a quasi-casual basis. But delivery via commercial truck was acceptable with certain provisos. This is no longer the case. The "Be Aware For America" campaign (Google it, if interested) is no longer considered effective and through commercial agreement with a Norwegian firm pure ammonium nitrate will no longer be sold in the USA. Bagged and truck-level Calcium nitrate mixed with ammonium nitrate will only be available if it meets specific elements. Norwegian firm YARA has captured bagged market. Large scale farming will now have to "register" to obtain ammonium nitrate. Thus since really only acidic soil tobacco farmers REALLY need it; the commercial sales are pretty mush lost. Nitrate/nitric acid chemical companies which produce fertilizers are now selling off those structures with "prill towers", pretty much nation wide. The "big boys" (DuPont, etc) are now basically going to own the small market for US made ammonium nitrate. Basically, it's gone.

k2976 - 16-12-2010 at 12:29

DCM is available as spray gun cleaner also. Needs to be fractionally distilled before using.

Magpie - 16-12-2010 at 14:23

Quote: Originally posted by SWilkin676

Ace Hardware still carries TSP.

Have you read the label on Ace's "TSP?" It may not actually contain any. I had to go to a paint store to get real TSP.

cnidocyte - 18-12-2010 at 23:57

I wonder how well activated carbon can be used to clean hardware store chems. I tested it out on this purple coloured methylated spirit product I found and it removed the purple colourant so I'd assume it would have removed other crap is present in trace amounts.

Trisodium Phosphate

franklyn - 2-2-2011 at 20:17

Not as cheap as the supermarket dishwashing products but it is 100 %

http://www.nationalchemicals.com/store/template/product_deta...
http://www.nationalchemicals.com/store/template/product_deta...

.

grndpndr - 3-2-2011 at 14:46

IIRC ACE's TSP is/was Savogran Brand TSP 75-80% TSP/20-25% Na sesquicebicate.1/2lb boxes.
Also @ ACE

Savogran oxalic acid IS 100%

Rooto Lye is also 100%

Ace discontinued 4lb boxes Bonide Nitrate of Soda 15-0-0 Fert. Good to go most uses.OTOH, 'Hi Yield' brand Nitrate of Soda 16-0-0(4lb sacks) is full of clay etc MUST be purified to yield decent NaNO3.

Formatik - 4-2-2011 at 12:19

Follow up comment on my note above. Has anyone gotten demethanolization of DCM to work, and verified by density? I have mixed the DCM azeotrope with methanol with a lot of CaCl2 pellets, mixed it, let it stand for some time. Then after distillation the density was the exact same as the azeotrope.

On a separate note, I'm going to warn against using drain cleaner sulfuric acid in any kind of synthesis. I have used a drain cleaner in an attempt to make dimethyl sulfide. The drain cleaner had an odor to it, but it looked like technical grade brown acid. Sulfuric acid should always be odorless! I suspect this acid may have formed an unknown highly potent lung poison which potentially almost put me out for good, a few indirect whiffs of this impurity was enough to cause severe respiratory effects.

Magpie - 4-2-2011 at 13:15

Quote: Originally posted by Formatik

Has anyone gotten demethanolization of DCM to work, and verified by density?

http://www.sciencemadness.org/talk/viewthread.php?tid=9270#p...

entropy51 - 4-2-2011 at 17:11

Quote: Originally posted by Formatik

On a separate note, I'm going to warn against using drain cleaner sulfuric acid in any kind of synthesis. I have used a drain cleaner in an attempt to make dimethyl sulfide. The drain cleaner had an odor to it, but it looked like technical grade brown acid. Sulfuric acid should always be odorless! I suspect this acid may have formed an unknown highly potent lung poison which potentially almost put me out for good, a few indirect whiffs of this impurity was enough to cause severe respiratory effects.

Might it be a little rash to recommend against using any drain cleaner sulfuric for any synthesis based on your experience with one drain cleaner in one synthesis?

Perhaps better advice would be not to use what you described as "cheap" drain cleaner with a foul odor.

From your thread it is far from clear that the sulfuric was the cause of your reported symptoms.

In this video, Robert Thompson shows a bottle of Rooto that is crystal clear and titrates to 18 molar. Rooto is typically an excellent source of sulfuric for the home chemist and you have not presented any evidence to the contrary.

Formatik - 4-2-2011 at 20:32

Quote: Originally posted by Magpie

http://www.sciencemadness.org/talk/viewthread.php?tid=9270#p...

Thank you. This site is pretty big! I trust your results. Looks like some more work was needed for me.

Quote: Originally posted by entropy51

Might it be a little rash to recommend against using any drain cleaner sulfuric for any synthesis based on your experience with one drain cleaner in one synthesis?

Another bad experience I've had is with the quality of another drain cleaner which was light brown and yellow, and even clear. I have attempted to get rid of the yellow brown tinge by boiling the same drain cleaner amount with conc. H2O2, several times! It got clear, but boiling further the color just reverted to light brown again, this suggests an inorganic impurity.

Quote:

Perhaps better advice would be not to use what you described as "cheap" drain cleaner with a foul odor.

Certainly. That's a good warning indicator of an impurity I would have been better off paying attention to in the first place. The odor of the acid wasn't too strong though, the scent smelled something like used motor oil. I have reagent grade conc. H2SO4 which is entirely colorless and odorless, which I should have used. But figured the drain cleaner would have done the job as good.

Quote:

From your thread it is far from clear that the sulfuric was the cause of your reported symptoms.

H2S poisoning was the most I could gather at the time. But now I'm entirely convinced it had only a small, if any role. The respiratory effects were, yes, similar and the smell very foul which hints at a sulfur toxin. The reason I'm convinced it was the acid, is because I had to get rid of my distillate. Some of it was destroyed with oxidants, but with distillate amount of 1mL impure dimethyl sulfide, working outside with a chemical respirator I felt strong but less severe effects again for several days. This strongly suggests it was the acid impurity. This impurity is the most wicked compound I've ever encountered, extremely foul smelling and travels distances rapidly.

Quote:

In this video, Robert Thompson shows a bottle of Rooto that is crystal clear and titrates to 18 molar. Rooto is typically an excellent source of sulfuric for the home chemist and you have not presented any evidence to the contrary.

18 M would tell you the acid content itself, but does not rule out other impurities. Use at your own risk. My experiment was supposed to be entirely harmless. I suggest to look for warning indicators of impurities in your acid (color, smell, foam, etc.) before and if you do use it.

MrHomeScientist - 5-2-2011 at 07:33

After hearing many of you talk about how hard to find some of these chemicals are, I was pretty surprised to find that my local Home Depot stocks a lot of them. All in the same section I found xylene, acetone, MEK, TSP, toluene, and phosphoric acid (Klean Strip Phosphoric Prep & Etch, whose <a href="http://www.wmbarr.com/ProductFiles/KS%20Phosphoric%20Prep%20and%20Etch.pdf">MSDS</a> claims 34 - 35% with no other ingredients, although it does have colorants).

All of them look like regular products, and not the "last item on the shelf, won't be restocked" type that was talked about earlier. I'm not sure if Florida hasn't gotten around to removing them yet, but for the time being things seem pretty easy to come by.

I went ahead and bought some TSP because it was cheap and sounded like the most likely to disappear soon, but I don't really have any good experiments to use it for. Any suggestions?

Magpie - 5-2-2011 at 09:32

I recently polished off my 1 gallon supply of Rooto sulfuric acid, which I bought probably 5 years ago. This had a slight orange tint, but never gave me any problems. I just bought a new half gallon jug of Rooto acid and it is completely clear.

I noticed recently that my local brewers supply is now carrying one gallon jugs of regular full strength phosphoric acid.

Jimmi_P - 6-3-2011 at 10:21

I agree with entropy51, rooto drain cleaner is a really good source for sulfuric acid. I use it all the time. It is crystal clear and I've never had a problem.

Magpie - 29-3-2011 at 13:05

During some recent assays of oleum I began to suspect the strength of the "98% sulfuric acid" that I bought from Elemental Scientific. I bought this specifically for its high strength, intending to use it for sulfonations.

I was first suspicious that it wasn't very strong just due to its relatively low viscosity, but never assayed it. Then when I used it to make up an oleum the oleum assayed much lower than I had calculated. Therefore, I decided to assay the Elemental Scientific sulfuric acid, and the Rooto that I had recently bought.

The Elemental Scientific acid titrated out as 89.3%. And to my surprise, the Rooto was titrated as 88.4%. In both cases I titrated with 1.04N NaOH, standardized with 0.1N KH phthalate.

Has anyone else tested the strength of their con sulfuric acid?

[Edited on 29-3-2011 by Magpie]

smaerd - 29-3-2011 at 13:16

I did a very basic titration of Rooto H2SO4 and I believe it came out to be 18.4 molar? Though the accuracy of this isn't trust-worthy, the NaOH it was titrated with was not standardized.

Magpie - 29-3-2011 at 13:27

Quote: Originally posted by smaerd

I did a very basic titration of Rooto H2SO4 and I believe it came out to be 18.4 molar?

My handbook says that this would be just over 98%.

smaerd - 29-3-2011 at 14:01

It must be incorrect. Sorry for posting.

entropy51 - 29-3-2011 at 15:18

Quote: Originally posted by Magpie

The Elemental Scientific acid titrated out as 89.3%.

Weigh 100 mL in a volumetric flask to check the density as a check on the titration.

Bot0nist - 29-3-2011 at 15:32

A liter of H<sub>2</sub>SO<sub>4</sub> bought from dudadeisel claims 98% with an MSDS that list contaminate as <0.01% Fe. Titration with NaHO to around 95%

Orange colored liquid lightning "virgin sulfuric acid" drain cleaner titrated at 96%~97% though heavy contamination is apparent.

No Rooto acid can be found in my local area. Only their NaHO/KHO type.

[Edited on 29-3-2011 by Bot0nist]

Magpie - 30-3-2011 at 08:23

Quote: Originally posted by entropy51

Quote: Originally posted by Magpie

The Elemental Scientific acid titrated out as 89.3%.

Weigh 100 mL in a volumetric flask to check the density as a check on the titration.

The density of the Elemental Scientific acid was measured by this method at 1.832 @16C. For acid at 20C my handbook says this is 93.7%.

For 89.3% acid the density should be 1.81.

e14 - 5-2-2018 at 19:08

If not already said, synthesises just have side reactions anyways.

WangleSpong5000 - 16-2-2018 at 20:48

Yeah that's very true. It's easy in the beginning to think that chemistry is very black and white. A perfect science even... the more experiments you do (and some are real give sways) you realise that side reactions are pretty much inevitable as the products 'on the side' where all a part of the process of electrons playing musical chairs so to speak and they play a part deep within the black box that they occupy the speculative and the theoretical aspects of chemistry.... A + B may = C but no-one ever said that A or B was absolute values... we just always saw them that way.

Omniquist - 28-2-2018 at 16:11

Hi everyone. I didn't read all the post, just page one and this last page. I can't recall seeing rooto in my area, but "liquid lightning" has two varieties at the lowes store near me. One is a nasty black waste product that someone had the sense to bottle and sell, but I wouldn't touch this out of respect for my equipment. The other one labeled "professional strength", is nearly clear, boasts 93 percent, worked with phenol sulfonation (firsthand) but did not work in production of chromic acid. The damn chromate went green/blue on me so it's heavily corrupted in use there. I treated this acid to flame w broken Pyrex subbing for boiling chips. This helped bring the concentration up but the same issue with chromic acid persisted. Adding drop wise h2o2 finished the job. I don't recommend this though as Caro's acid can form.. Hope this helps anyone