| Pages:
1
2 |
Quince
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
Sulfuric, nitric, and peroxide from Rona
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).
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Quince
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
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?
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline
Mood: Chemistry: the subtle science.
|
|
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.
The single most important condition for a successful synthesis is good mixing - Nicodem
|
|
|
Joeychemist
Hazard to Others
Posts: 275
Registered: 16-9-2004
Location: Canada
Member Is Offline
Mood: Sedated
|
|
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
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
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! 
|
|
|
Quince
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
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]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Chris The Great
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
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
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
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]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Chris The Great
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
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
Hazard to Others
Posts: 275
Registered: 16-9-2004
Location: Canada
Member Is Offline
Mood: Sedated
|
|
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
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
How does extra water, if dilute acid is used, interfere with the process? Doesn't the nitration still happen, just slower?
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Joeychemist
Hazard to Others
Posts: 275
Registered: 16-9-2004
Location: Canada
Member Is Offline
Mood: Sedated
|
|
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!
|
|
|
chloric1
International Hazard
Posts: 1147
Registered: 8-10-2003
Location: GroupVII of the periodic table
Member Is Offline
Mood: Stoichiometrically Balanced
|
|
Drain cleaners
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 $35 at a photographic supply house! THere was no mention of permits or needing company
letterhead. It might be worth a try.
I think you can buy Red Phosphorus in Canada too! Is this true?
[Edited on 2/2/2005 by chloric1]
Fellow molecular manipulator
|
|
|
Quince
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
I remember an experiment I got from a book years ago (before public paranoia and ignorance made these things taboo), some kind of cyanide, and when
you put it in copper sulfate solution, it formed very interesting blobby brown shapes. Can anyone think of what exactly it would be? I had my
stepfather get me some from his lab, so it's probably not an uncommon chemical.
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
I have bought/used both technaflora's nitric and zonk plus. AS well I get almost all my solvents and HCl form there.
Chris, you got the conc. of technaflora's nitric the easy/smart way, I went through and did a titration of it. It worked out to be 1.93mol/L
Quince, what was the 35% peroxide sold as? And how much did it cost? I have never seen it at Rona before. I pay 14$/L at a hydroponics store.
|
|
|
Chris The Great
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
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
Harmless
Posts: 35
Registered: 10-4-2004
Member Is Offline
Mood: No Mood
|
|
http://www.napra.ca/pdfs/fedleg/021210precursor%20briefing.p...
This seems like a good quick summary of canadian precursor controls.
|
|
|
chloric1
International Hazard
Posts: 1147
Registered: 8-10-2003
Location: GroupVII of the periodic table
Member Is Offline
Mood: Stoichiometrically Balanced
|
|
Still strict but..
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! I think I can make but I will start with succeeding in hydrazine hydrate
first.
Fellow molecular manipulator
|
|
|
Mumbles
Hazard to Others
Posts: 436
Registered: 12-3-2003
Location: US
Member Is Offline
Mood: Procrastinating
|
|
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
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
| 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]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
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
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
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]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Chris The Great
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
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
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
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.
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
Quince
National Hazard
Posts: 773
Registered: 31-1-2005
Location: Vancouver, BC
Member Is Offline
Mood: No Mood
|
|
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.
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
