Sciencemadness Discussion Board - Sulfuric, nitric, and peroxide from Rona

Sulfuric, nitric, and peroxide from Rona

Quince - 1-2-2005 at 19:43

Vancouver, BC -- just went to Rona, a hardware chain. They had the 35% peroxide (though very expensive), and a pH Down from Technaflora (nitric acid for hydroponics), as well as Zonk Plus Drain Opener from SIPCO Industries LTD (sulfuric acid).

My question is, how can I tell the concentrations, and if there are any other ingredients? Labels do not say, and I have searched but couldn't find datasheets, even on the manufacturer websites. Is there any way to estimate acid concentration, and increase it? (yes, I'm a newbie, it's been a while since highschool chemistry).

Quince - 1-2-2005 at 20:10

Well I'll be damned. I thought the acids were probably dilute, but when I put the cotton in, the mixture started boiling and the cotton dissolved completely, with the usual orange fumes starting to come out. I had to add lots more cotton. But when I added the bicarbonate solution to neutralize the acid a few mintues later, all the cotton completely fell apart. WTF am I doing wrong here?

Magpie - 1-2-2005 at 20:24

For estimating the concentrations of liquids I like to use a hydrometer as it is quick and easy. I bought a universal type with range of 0.8 to 1.2. The sp gr of many common chemicals such as sulfuric acid, nitric acid, etc are readily available in handbooks such as CRC, Perry's Chemical Engineers. Or you can probably get it from Google. As a last resort there are the International Critical Tables.

Oh, to use the hydrometer you need a tall, skinny glass vessel. A 250 mL graduated cylinder is perfect.

Joeychemist - 1-2-2005 at 20:36

Quince,

The drain cleaner should be no less than 90% H2SO4, the rest should be water. (The drain cleaner I buy is 96% conc.) The HNO3 is more than likely less than 65%, you can determine the concentration buy measuring the density/volume of the acid. 100% pure HNO3 is 1.58 g/cm³

If you wish to purify you’re acid I suggest using the search button, as it has been covered here before many times.

The “orange” fumes were un-doubtable NOx gas, and it is *NOT* good to be breathing the stuff in.

Chris The Great - 1-2-2005 at 20:58

Technoflora nitric is 13%, I checked as I saw the stuff in a Rona as well. So basically, it's useless! But the other chems should be fine. It was mentioned on their website, on the customer support forums.

I'm interested in the drain cleaner though, I haven't seen that in a hardware store before! Looks like I have some shopping to do! :cool:

Quince - 1-2-2005 at 22:49

Chris, is this nitric too weak to concentrate? Or is there any other source of nitric acid?

Joeychemist, I did try searching about concentrating nitric acid, and I didn't find anything around these forums.

[Edited on 2-2-2005 by Quince]

Chris The Great - 1-2-2005 at 23:33

It could be concentrated however it wouldn't be worth it as more concentrated versions are supposably sold at hydroponics stores as the same product. However, it won't mention that it is more dilute, as the technoflora product says on the label. I have not looked in hydroponics stores, but that is what the product is for. Just find one that doesn't mention that's it 'extra safe' or even better, one that's concentrated, and contains nitric acid. Sometimes they contain other acids.

Hmm, you could probably nuetralize it by nuetralizing with sodium hydroxide/ bicarbonate to give sodium nitrate, which can be extracted by boiling off the water. You can then use this in nitrations, or mix with sulfuric and distill out the nitric or if you have glass filter paper, filter out the NaHSO4/Na2SO4 and be left with ~90% red nitric acid.
Doing that would save alot of sulfuric, as distilling nitric out of 13% concentration by mixing with H2SO4 and distilling as it usually is done simply will use way to much sulfuric to be worth it. Potassium hydroxide could also work.
But if you can buy much more concentrated acid, maybe even 65%, then it's not worth the effort in my opinion, unless of course you already bought the 13% acid.

Also, unless you have an all glass still, you can't distill it (it destroys rubber etc) so that might be your only option.

Quince - 1-2-2005 at 23:46

I went to one hydroponics store before Rona, and the pH Down there, other than the Technaflora one, was either phosphoric acid, or some solid stuff.

Um, the Technaflora one doesn't say how dilute it is on the label. Maybe you were looking at a different package.

What I wanted the nitric for is to try making a bit of blasting gel (nitroglycerin dissolved in nitrocellulose colloidion). You say I can use sodium nitrate in nitrations -- will this work for nitroglycerin and nitrocellulose? Or what's the best approach, given what I have/can-reasonably-find?

[Edited on 2-2-2005 by Quince]

Chris The Great - 1-2-2005 at 23:56

Yes, you can use nitrate salts, as they react with sulfuric acid to produce nitric acid as per:

H2SO4 + NaNO3 --> NaHSO4 + HNO3

Yeilds are apparently a bit lower, and the NaHSO4 will stay in the mixture as a solid, but it does work.
Someone else can probably supply much better information on doing this than me, I just know it works, calculate out how much NaNO3 to add to so much sulfuric to get whatever mix you want, and go from there. The reaction releases alot of heat however, so be careful to let it cool down again before beginning nitration.

The concentration was listed on their customer support boards, under the topic pH down if a remember...
http://www.technaflora.com/phpBB2/viewforum.php?f=3
However there is a problem with their site right now, none of the topics open properly. But that's where I found the 13% figure.
Hmm, I always figured the more concentrated stuff could be found at hydroponics stores, I guess not

Joeychemist - 2-2-2005 at 00:05

Quince, if you do not have any glassware you can make HNO3 the easy way, although yields are shitty and it is a waste of perfectly good nitrate salts, it is effective. Look at Brainfever’s site here;
http://brainfever.2ya.com/

Also, you don’t necessarily need HNO3 to make nitro, you can also use nitrate salts like KNO3.

Quince,please check you're U2U mail box.

[Edited on 2-2-2005 by Joeychemist]

Quince - 2-2-2005 at 00:23

How does extra water, if dilute acid is used, interfere with the process? Doesn't the nitration still happen, just slower?

Joeychemist - 2-2-2005 at 00:47

To try and nitrate something with weak HNO3 like that you would need to add 10X the sulfuric acid just to suck up the water and again, the yeilds will be a shitty hafl nitratred product.

Quince, check you're U2U mail box!

Drain cleaners

chloric1 - 2-2-2005 at 03:51

I found out that sulfuric acid darain cleaners where taken out of hardware stores in America sometime in 2004

. I wanted to buy some as it is concentrated but not very pure. I wanted to use it in a chlorine gas generator to remove water vapor. It seems Canadians are more chemically liberated than Americans nowadays. I even saw a pound of sodium cyanide for $35 at a photographic supply house! THere was no mention of permits or needing company letterhead. It might be worth a try.

I think you can buy Red Phosphorus in Canada too! Is this true?

[Edited on 2/2/2005 by chloric1]

Quince - 2-2-2005 at 04:38

I remember an experiment I got from a book years ago (before public paranoia and ignorance made these things taboo), some kind of cyanide, and when you put it in copper sulfate solution, it formed very interesting blobby brown shapes. Can anyone think of what exactly it would be? I had my stepfather get me some from his lab, so it's probably not an uncommon chemical.

The_Davster - 2-2-2005 at 06:09

I have bought/used both technaflora's nitric and zonk plus. AS well I get almost all my solvents and HCl form there.

Chris, you got the conc. of technaflora's nitric the easy/smart way, I went through and did a titration of it. It worked out to be 1.93mol/L

Quince, what was the 35% peroxide sold as? And how much did it cost? I have never seen it at Rona before. I pay 14$/L at a hydroponics store.

Chris The Great - 2-2-2005 at 07:09

Well, it's sold as 'Liquid Oxygen', 35% in big numbers on an atom symbol. Below the 35% it says hydrogen peroxide. The colour is light blue and white, in a clear plastic bottle. Same price though, so it's not really saving you money. IIRC is was $15/ 1L at my Rona.
It also comes in 4L jugs but I haven't seen that.

I'll try Rona maybe next weekend, since everyone seems to be having so much success there, and I have about 50mL of my H2O2 left.
The last time I was there was very quick, I didn't have time to look around. I was looking for nitrate fertilizers, so went straight to the gardening section. Looks like I may have missed out on quite a bit!

Yes, I've noticed that I can find some chems here in Canada that others have a hard time finding. The exception being KNO3 and H2SO4, as I haven't found a source for either other than old car batteries.
I'm not sure about the red P, I'll have to check it. I know it's in 8 shot caps, and can be easily removed with hot water if you're desperate

Does Canada have a banned/restricted list such as the States? I haven't actually seen a Canadian one, though I haven't really looked that hard.

skippy - 2-2-2005 at 08:07

http://www.napra.ca/pdfs/fedleg/021210precursor%20briefing.p...
This seems like a good quick summary of canadian precursor controls.

Still strict but..

chloric1 - 2-2-2005 at 10:13

Good Grief! Thats what it was like here in the US in 1990 or so when I first got into the hobby!! Guess if I am too paranoid to have something shipped from a Canadian dealer I can always drive to Windsor or Toronto if I get too hard up for stuff. Now it seems I can no longer order sodium azide! :mad:

I think I can make but I will start with succeeding in hydrazine hydrate first.

Mumbles - 2-2-2005 at 17:44

I can still get sulfuric acid drain cleaner around here. Perhaps they chain just stopped carrying them around there, or it was a state regulation.

I know which photography place you mention and they seem to be alright. Prices are a tad high, but oh well. I got some permanganate a few years ago. Actually, if you look you can get Sodium Cyanide cheaper in the US, also needing no licences or anything. Just hazmat shipping and you are on your way.

Quince - 2-2-2005 at 19:54

Quote:

Originally posted by rogue chemist
I have bought/used both technaflora's nitric and zonk plus.

What did you do with the nitric? Did you find a way to concentrate it?

Isn't there any substance that will not react with the nitric, but will absorb the water from it, and can be separated out?

Chris, if I do the neutralization with bicarbonate, you say it can be mixed with sulfuric acid and the solid filtered out using glass filter paper. Will this solid not fall to the bottom or float to the top, so a separation could be done without such paper? Or does something remain dissolved and I must distill? You also say the result is red nitric acid. I thought that's bad, because it means it has gas dissolved. I've read that vacuum distillation is needed to get clear acid, but I don't have a setup.

If the weak nitric is mixed with sulfuric and strong nitric distilled, can't the weak sulfuric that's left be concentrated by heating and evaporating water?

Another question: what are Canadian sources for thermite material (powdered aluminum, iron oxide)? I don't have any way to make fine powder.

[Edited on 3-2-2005 by Quince]

The_Davster - 2-2-2005 at 20:05

I tested the nitric for use in making HDN, as expected, a terrible yield was recieved. Now it is used for washing glassware

. I may distill it one day....

You can make iron oxide quite easily. Dissolve steel wool in HCl, filter out insoluble particles. Precipitate iron hydroxide by addition of NaOH. Decant a few times. Add a bit of 35% peroxide and the iron hydroxide reacts to form iron(III) oxide. Filter and dry.

Chris: My peroxide from the hydroponics store has the same name. What section of Rona did you find the peroxide in anyway? I swear I have wandered those isles long enough to have seen all the good stuff(and read almost all lables

)

[Edited on 3-2-2005 by rogue chemist]

Quince - 2-2-2005 at 20:13

Yeah, but I don't have a source for NaOH. Dishwasher detergent contains it, but I don't have any way to separate it from the other crap. The garden store sells some lime, but it doesn't seem to be NaOH.

Where can I get aluminum powder? Doing it manually gave terrible results.

BTW, is it possible to vacuum distill nitric acid without a pump, by using weight of water (the same way that a siphon provides suction)? Or does the suction need to be continuous, instead of just achieving reduced pressure in the beginning?

[EDIT] Using baking soda to neutralize some of the Technaflora nitric acid, it took maybe half the volume of baking soda (loose) vs the acid before CO2 stopped fizzing out. Does this fit the percentage concentration given above?

The drain cleaner sulfuric acid, however, started giving white fumes immediately in the microwave, before even boiling.

I boiled the water away in the microwave from the neutralized nitric acid, and there was a hard white mass left at the bottom. I added about twice the original nitric acid volume of the sulfuric acid. Since the thing was still quite hot, as well as the sulfuric (which I had heated to fuming), there was quite a bit of boiling. Most of the crystal mass dissolved with some stirring, and now the liquid is pale yellow in color, with something floating around it, either small particulate matter or tiny bubbles, I can't tell.

I cooled it and added some cotton, but the cotton dissolved completely. Maybe there's too much sulfuric acid.

[Edited on 3-2-2005 by Quince]

Chris The Great - 2-2-2005 at 22:40

Ok, why did you heat the sulfuric acid? Heat is bad for this reaction as heat destroys nitric acid! You probably had a mixture of sodium bisulphate and sulfuric acid as if the mixture was boiling, then it would probably be around 250 degrees, hence no nitric is going to stay for very long.

Hmm, also with baking soda there will be starch as well, so it will be a mixture of sodium nitrate and starch. A fire hazard, to say the least. Probably good to invest in some lye (NaOH). They should sell that at Rona.

And yes, red nitric acid is bad, as it has dissolved NO2 gas. However, it would take alot of cooling to keep the temperature down low enough to prevent NO2 formation, so generally it's easier to let it turn red (cool it though! Just don't be crying if it turns reddish) and buble air through it, or add a small amount of urea to nuetralize.

A vacuum distilliation works as long as there is a vacuum. If you can maintain a vacuum because there are no leaks, then it will work. But this probably isn't easy.

Check roguesci.org for several great threads on aluminum powder made easy, in the pyrotechnics forum.

I thought electrolizing steel nails = iron oxide? That would save expensive hydrogen peroxide. I think there was a thread on it somewhere.

I found mine in the garden section. There was a huge amount of it, next to a huge amount of the nitric. It was really hard to miss, but your Rona may be layed out differently. It was next to all sorts of plant nuetrients and such, not fertilizer, but the weird stuff people add to it.

Quince - 3-2-2005 at 00:05

I did another neutralization of some more dilute nitric acid and added the evaporated white solid (which by the way seems to stain brown both my fingers and especially paper when wetted) to the sulfuric/crystals mixture left over from last time, after it had cooled. The mixture warmed a bit, but I cooled it again in the freezer. It was basically a slush of partially dissolved white stuff. I put the cotton in, but again it started to fall apart within three minutes -- I really don't understand why the cotton keeps dissolving. I dumped the whole thing in cold water and washed and neutralized it. This time there was some left over that I dissolved in acetone and let the acetone to evaporate. The result was extremely contaminated with crystals, but at least the part around the vessel walls would burn OK. So the overall yield was a few percent of the original cotton...

I have to figure out a better way, or to somehow remove the contaminating salt before I add the cotton.

It says on this site that you can mix 15:10 sulfuric acid with saltpeter and use that to make nitrocellulose. I wonder if this would also work for nitrating glycerin.

Quince - 3-2-2005 at 18:08

I went to the local gardening store (David Hunter's), and they had no nitrate fertilizers whatsoever. All nitrogen was in other forms (urea, etc.). Should I expect this from all stores across the province? Perhaps nitrates were pulled from Canadian retail fertilizers due to their use in explosives.

The_Davster - 3-2-2005 at 19:30

That store, David Hunter's, does it cater to the general public or for agrarian uses? Very few, if any gardening stores that sell to the public carry pure nitrate fertilizers.

Quince - 4-2-2005 at 07:53

General public. Will the others sell non-wholesale?

BTW, for those in Canada, is it possible to buy nitrocellulose/guncotton/smokeless powder, or do I need a license? It's too hard to get a uniform amount of nitration when DIY. What sort of place would sell it?

[Edited on 4-2-2005 by Quince]

Chris The Great - 5-2-2005 at 03:03

Hmm, go to bigger Rona's when shopping, I stopped by a smaller but cloaser Rona and they lacked both sulfuric and H2O2. Luckily I found a large amount of calcium hypochlorite which I needed, but this means I still have no H2O2.

I need to check the bigger Rona where I found my H2O2 before, but it's a fair distance away from me.

Quince - 5-2-2005 at 03:24

Mine had both 35% H2O2 and 90%+ H2SO4, but only 12% HN03. This hypochlorite, is this the stuff sold as pool chlorinator?

So, does any Canadian know about the smokeless powder/nitrocellulose/guncotton/pyroxilin? Can this be bought OTC?

My main question: what's the cheapest source of lab equipment in Canada (I want to get an aspirator and stuff for distillation)?

[Edited on 5-2-2005 by Quince]

Chris The Great - 17-3-2005 at 18:02

Went back to my small Rona, found the Zonk plus drain cleaner. $16/900mL.
But later I found a drain opener labeled 'Proffessional Liquid Drain Opener' at a small local Home Hardware I had never gone in before, for $8/900mL. The also had less concentrated stuff for home use, for $7.5/900mL, but of course who wants that?

So, I'm definatly keeping the $8 stuff, but I'm wondering how pure the Zonk stuff is, ie is it worth it to keep it as it's more concentrated etc? Otherwise I'll take it back and get another 900mL of the HH stuff.

EDIT
Looked through the bottles with a bright light, the stuff from Rona is clear, while the cheaper HH stuff is coloured heavily (can't see through it at all). I might just have to keep both of them to figure out what works the best, so I can save cash if fairly pure sulfuric acid is not needed. No point in using $16 H2SO4 to dry some gas when I can get $8 that will work just as well.

[Edited on 18-3-2005 by Chris The Great]

The_Davster - 17-3-2005 at 18:30

Zonk plus was the first sulfuric acid I ever had. Nostalgia

. It is quite concentrated but it is on the expensive side for some reason(you are actually getting it 2$ cheaper than when I bought it). It worked for me to make picric acid with a long time ago. I also know I used it in another nitration but I forget what it was.

EDIT: "the stuff from Rona is clear" Are you speaking of the Zonk Plus???... Mine was completly black and opaque. Another sulfuric acid source from Rona is "clear line drain opener". It is a bright red colour, and is cheaper than the zonk, 11$/L. I have not used it for anything other than distilling nitric from so far, however it worked quite well for this purpose.

[Edited on 18-3-2005 by rogue chemist]

Quince - 17-3-2005 at 20:20

The Zonk Plus I bought is transparent with a slight dirty yellow tinge, that's all. When I poured it out of the bottle, it had a tiny bit of gunk near the bottom, but other than this it seems good.

Also, I found KNO3 at Rona, sold as stump remover (about $9 Canadian for 500 g).

I just used both of these sources to vacuum distill HNO3 and it looks good. I had to add water to dissolve all the KNO3, but the end result was HNO3 with density about 1.45 and just the lightest yellowish tint (I heated too fast). I can't believe the amount of water going through the aspirator to distill 20 mL...I'm thinking that's the most expensive thing in the procedure.

[Edited on 18-3-2005 by Quince]

The_Davster - 17-3-2005 at 20:22

I guess mine was just quite old and had reacted with the plastic bottle that it was in, I remember reading somewhere that this happens to sulfuric acid if stored in plastic for long periods of time.

Chris The Great - 17-3-2005 at 21:30

Perhaps they changed their product, after all it seems you got this acid quite some time ago (at least that's what I get from reading your post). Maybe they realized it was cheaper and worked better to just use the barrels of sulfuric acid they buy in bulk instead of diluting and adding other stuff to it.

The other stuff is a nice pink colour, appearing red when in any sort of quantity (ie drops of it are pink, but the stuff inside looks deep red). It's very pretty. I'll have to do a bunch of experimenting with them on spring break to see if one has any advantage over the other.

Darkblade48 - 28-3-2005 at 19:48

Quote:

Originally posted by rogue chemist
EDIT: Another sulfuric acid source from Rona is "clear line drain opener". It is a bright red colour, and is cheaper than the zonk, 11$/L.

[Edited on 18-3-2005 by rogue chemist]

Didn't want to start a new thread, so I'm digging up a semi-old thread here.

I was just curious if there was any reason why the sulfuric acid was red, and if it had any negative effects (maybe there are contaminants?)

12AX7 - 28-3-2005 at 20:23

I think he means the bottle, I have the same stuff, liquid fire is the brand. I seem to recall a store(-ish) brand as well, I forget which was cheaper.

Tim

Darkblade48 - 28-3-2005 at 20:30

Weird, the liquid I have is some "Professional Grade Drain Opener" and it's labelled as containing H2SO4, but it's definitely red/reddish in colour.

12AX7 - 28-3-2005 at 21:17

Huh, stuff I have is a light yellow color, thick and dense (as it ought to be). Doesn't smell like anything either, I was expecting it to?? Maybe yours has excess SO3 in it, I always imagine things like that coloring it dark and evil... even though that would be fuming sulfuric and probably still colorless anyway...(ah, imagination...one can only hope

).

Tim

Darkblade48 - 29-3-2005 at 20:52

This might be a bit hazy, but I think it gets the point across

http://www.cpindustries.ca/products-services.php

The picture on the right hand side shows a few bottles of chemicals, two of the bottles have a reddish liquid on the inside. That's essentially what I have for my H2SO4 (I just happened to buy a different brand, but the colouring looks exactly the same)

I asked some of my profs at university and they said it's possible that they put in something to make it look "nasty and scary" so that you don't drink it (on the contrary, I think it kinda looks like red Kool-Aid

)

Chris The Great - 31-3-2005 at 22:11

It's a dye, probably added for the above reasons.

It dissappears when I make Caro's acid, so I would think it's most likely organic and destroyed by the oxygen (some bubbling was noticed, but very very little, as the colour went away).

Considering it isn't being attacked by the sulfuric acid, I would think it would be realively inert in most reactions. Very little would be added anyway so it shouldn't affect the results that much even if it did react.

I also noticed my Zonk acid is slightly murky white, and not completely clear as I previously thought.