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PoWEr
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Sulfuric Acid from Sulfamic Acid
Ever since the Ammonium Persulfate post, I have been considering if this is actually worth it, as woelen said it's cheaper to just distill sulfuric acid. However
in my country the highest concentration I could find is 10% 1L (kinda convienent isn't it) for 28PLN (7,47USD). So for that I could get ~100ml's of
concentrated sulfuric acid. So 280PLN (74,74USD) for 1 liter of conc. sulfuric acid is quite a lot of money and therefore I decided to start my
research again.
Then I found about this reaction:
HNO2 + H3NSO3 → H2SO4 + N2 + H2O
Now Sulfamic acid in my country costs 71PLN (18,95USD) for one liter and this is all nice and good but HNO2. According to reaction I found:
3 HX + 3 MNO2 → 3 MX + HNO2 + NO + NO2 + H2O
All I need is a strong and diluted acid, as that page says and a nitrite salt. An obvious choice would be HCl, since It's cheap and not regulated, 31%
1L costs 19PLN (5,07USD) and sodium nitrite, which is apparently a food additive. 1kg of it costs 18PLN (4,80USD).
Then I added everything up and the total cost would be about 90PLN (24,02USD), which is about 68% cheaper! This is only the start though as a new
problem arises with HNO2, which is the funny property that causes it to not liking to exist and so it must be done in freezing temperatures and it
must be used as fast as possible, since the breakdown produces NO (it literally tells you do not). Luckily the byproduct is also HNO3, which also
reacts with sulfamic acid and makes the same products but instead of nitrogen, there is N2O, so in the end everything cancels out, N2O is less toxic
than N2, but then you have to handle with NO, just like chemistry should be!
So the reactions should be in theory assuming no HNO3:
1. 3HCl + 3NaNO2 → 3NaCl + HNO2 + NO + NO2 + H2O
2. HNO2 + H3NSO3 → H2SO4 + N2 + H2O
Of course doing this outside and then distilling.
So If I were to turn 1kg of sulfamic acid into sulfuric acid, it would be about 10M of sulfamic acid, which would need 10M of HNO2, which needs 30M of
HCl and NaNO2. For NaNO2 it would be 2070g, which is about ~36PLN (9,61USD) and for HCl, since a 31% 1L solution should contain ~8M, it would be
~76PLN (20,29USD). In total it would be 183PLN (48,85USD), which is 35% cheaper! Now I can finally get some high quality salt for my french fries!
This procedure seems fairly simple and mostly free of any unwanted substances since nitrogen compounds shouldn't react much with sulfuric acid, but
there could be problem with NaCl? It's still first drafts and oh well maybe I missed something very important that will make this entire thing
actually more expensive than just distilling it, but that's the fun part of chemistry!
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Keras
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I’m not sure why you (and other people) try to find fancy ways to get sulphuric acid when NurdRage demonstrated how well the oxalic acid + copper
sulphate way worked, given your patient enough to filter out the ultrafine particles of copper oxalate. Neither of the reactants are regulated and
their price is low (copper sulphate might be a bit more expensive, but you can replace it by ferrous sulphate, albeit with loss of yield).
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AdamE
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Quote: Originally posted by Keras  | | I’m not sure why you (and other people) try to find fancy ways to get sulphuric acid when NurdRage demonstrated how well the oxalic acid + copper
sulphate way worked, given your patient enough to filter out the ultrafine particles of copper oxalate. Neither of the reactants are regulated and
their price is low (copper sulphate might be a bit more expensive, but you can replace it by ferrous sulphate, albeit with loss of yield).
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Let him test the yield.
Update us on your findings.
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PoWEr
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| Quote: Originally posted by Keras | | I’m not sure why you (and other people) try to find fancy ways to get sulphuric acid when NurdRage demonstrated how well the oxalic acid + copper
sulphate way worked, given your patient enough to filter out the ultrafine particles of copper oxalate. Neither of the reactants are regulated and
their price is low (copper sulphate might be a bit more expensive, but you can replace it by ferrous sulphate, albeit with loss of yield).
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At this point finding ways to make sulfuric acid became a thing I enjoy to do for some reason, also because I want a cheap and high yielding way to
make sulfuric acid.
He showed in his video that it didn't work well at the end, and with iron sulphate the maximum yield he achieved was 67% assuming Its sunny for 8
hours, and in my country Its currently uncommon, so without the sun the maximum yield he achieved was 57% which to be honest, is actually good, but
why stop here?
Also apparently this post actually made it with copper sulphate and the yield was 91%, Im not so sure about it.
[Edited on 24-5-2025 by PoWEr]
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Keras
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| Quote: Originally posted by PoWEr |
He showed in his video that it didn't work well at the end, and with iron sulphate the maximum yield he achieved was 67% assuming Its sunny for 8
hours, and in my country Its currently uncommon, so without the sun the maximum yield he achieved was 57% which to be honest, is actually good, but
why stop here?
Also apparently this post actually made it with copper sulphate and the yield was 91%, Im not so sure about it.
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I’m currently purifying sulphuric acid made from copper sulphate and oxalic acid. I didn't really measure the yield, but the concentrated acid is
surprisingly easy to get. Most of the water seems to be gone at about 120 °C, which means you don’t have to push your glassware very high. You just
collect what's left in the boiling flask.
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MrDoctor
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for nitrous acid couldnt you just load up a Birkeland-Eyde's water with sulfamic acid?
Also from what i understand, nitric acid wont react with sulfamic acid at low concentration, i dont know where it becomes strong enough, or what the
curve is for reactivity, but i have a feeling that nitric acid byproduct wont be an issue.
Lastly, why not try making sulfuric acid by thermally decomposing sulfamic acid instead? there might be some merit to tweaking the decomposition by
slipping a little oxygen in there somehow, to get only SO3 instead of SO3+SO2, i believe it breaks down into NH3+SO3, so then if you can burn that
ammonia away at the same time in an oxidizing environment, that should afford you only SO3. incidentally, vanadium pentoxide is a candidate there,
though i could imagine something like a mixture of silica, copper oxide and maybe some iron oxide, would work too. vanadium at least yeilds some NO
from the oxidation. But im getting ahead of myself here, because these reactions need to be like 400-700C, and you could pretty much just feed sulfur
in to get the same output. actually dont nitric oxides quite famously oxidize sulfur up all the way?
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bnull
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| Quote: Originally posted by Keras | | I’m not sure why you (and other people) try to find fancy ways to get sulphuric acid when NurdRage demonstrated how well the oxalic acid + copper
sulphate way worked, given your patient enough to filter out the ultrafine particles of copper oxalate. Neither of the reactants are regulated and
their price is low (copper sulphate might be a bit more expensive, but you can replace it by ferrous sulphate, albeit with loss of yield).
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Too late for the party, I guess, but there's one thing you forgot. Oxalic acid is banned or restricted in some places because it is a poison. UK, if
I'm not mistaken, had that issue.
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chloric1
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Why does it have to be nitrous acid? Option one could be just reducing nitric acid with a metal or reducing agent and leading brown NO2 fumes into
solution of sulfamic acid. Or oxidation of sulfamic acid with aqua regia that has a 1:1 HNO3 and HCl mix. Fumes could be a problem.
Fellow molecular manipulator
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Keras
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| Quote: Originally posted by bnull | | Too late for the party, I guess, but there's one thing you forgot. Oxalic acid is banned or restricted in some places because it is a poison. UK, if
I'm not mistaken, had that issue. |
Yeah, I didn't know that. Stupidity is world's most shared attribute. I wonder how complicated it is to get a licence in the UK.
Otherwise, you can make sulphuric acid from nitric acid and sulphamic acid, but I doubt this is of any value.
As a get-round you can use methanesulphonic acid. Not regulated, as strong as sulphuric acid, and with many advantages (e.g. non oxidising).
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MrDoctor
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are you sure its oxalic not formic acid?
oxalates are like, everywhere. parsey by weight is almost 2% oxalic acid or oxalate. spinach, chives and amaranth are 1%
sucrose also can be oxidized to oxalic acid using nitric acid, i think catalytically if oxygen is added somehow. supposedly it can also be made by
alkaline hydrolysis of wood or cellulose, and i know a bunch of other oxidizers like permanganate work too just not yielding as much.
Not to dissuade you but the real breakthrough will pretty much always just be a novel way of running the contact process (oxidizing
S>SO2>SO3>Oleum) in a manner that is intrinsically safe and compatible with standard glassware, or minimal engineering, with a catalyst that
can regenerate in situ preventing poisoning, the big challenge at the end is that youll generally end up with a dilute SO2 stream, leading to a dilute
SO3 stream, that is difficult to totally dissolve into your oleum, if you burn the sulfur, and unburnt sulfur tends to poison the recommended
non-platinized catalysts.
Elemental sulfur gets the greatest possible yield out of any precursor too, by weight its about 300% since you are just sticking water and oxygen to
it with no reason any should be lost. comparatively while sulfamic might be conveniently close to sulfuric already, and cheap in bulk depending where
you are, the gains arent exactly great for the mass processed.
IMO where the answer is at, is either reacting sulfuric/oleum with sulfur to produce pure SO2 to re-oxidize over and over, multiplying your acid, by
either direct oxidation or electrolysis of the resulting sulfurous acid in a simple split cell, either way, letting you use either pure undiluted SO2,
or, an exactly controlled quantity of air, whatever works, your choice.
The other is a stack of mixed simple catalysts (iron, copper, vanadium and molybdenum, maybe some silica or celite too) poured into a quartz test tube
or carefully loaded borosilicate one, where sulfur and air are added very slowly such that pretty much just SO3 (and excess air) leaves the test tube,
but its only one gaseous stage and its freely regulated to match whatever means is used to hydrolyze the SO3, which people struggle to do at a sulfur
candles flow rate.
one last thing; given that sulfamic acids decomposition-rearrangement seems to work out as, SO3 frequently forming unsuccessfully and oxidizing some
ammonia, its possible the introduction of ozone could drive the reaction more cleanly to form SO3, as ozone by default will oxidize sulfamic acid, but
at a high temperature i think it would rather oxidize the free ammonia that is trying to form. assuming it works that way, you would also subsequently
get nitric oxides that go on to do even more work again on the molten sulfamic acid. its possible the addition of an output from a small pumped ozone
generator could help out quite a bit, constantly adding radicals that get used over and over before being consumed, with or without a catalyst to keep
the reaction temperature quite low. this is just speculation however. it is clear that any SO2 formed would oxidize, and if in the decomposition
process the SO2 is due to SO3 having an oxygen stolen then ozone with a greater potential would potentially be able to join in, and hopefully then go
on to be used completely rather than just donating a single molecular oxygen, leading to nitric oxide formation.
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Keras
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I mean, if you have a quartz test tube, the best way is to pyrolyse sodium bisulphate at 600 °C to directly produce SO₃ which you can then lead
into a chilled receiving flask, before dilution into (pre-made) concentrated sulphuric acid.
[EDIT: Picture]
[Edited on 27-5-2025 by Keras]
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MrDoctor
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this seems like it would still be rather taxing on the valuable quartz glassware compared to what it would ultimately yield. but very useful sure, for
quickly producing some SO3 or a little oleum to restore some wet sulfuric acid back to 98% without distilling. Best way is subjective. convenient and
cleanest? probably, but the yield will be awful per batch.
i would argue that continuously adding in molten sulfur and air into a less intensely heated test tube is superior, electric heating would not be too
difficult, in theory it might also be possible to heat inductively
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bnull
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| Quote: Originally posted by MrDoctor | are you sure its oxalic not formic acid?
oxalates are like, everywhere. parsey by weight is almost 2% oxalic acid or oxalate. spinach, chives and amaranth are 1%
sucrose also can be oxidized to oxalic acid using nitric acid, i think catalytically if oxygen is added somehow. supposedly it can also be made by
alkaline hydrolysis of wood or cellulose, and i know a bunch of other oxidizers like permanganate work too just not yielding as much.
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Yes. See Licensing for home users of poisons and explosive precursors, item 15 under Regulated poisons. Oxalic acid content exceeding 10% w/w needs a
license.
Oxalic acid is rapidly decomposed by permanganate, by the way.
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woelen
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All of this still looks to me like a lot of hassle to get your sulfuric acid. Getting pure acid will be hard, you have to get rid of all kinds of
impurities. You NO/NO2 from the nitrite will not be pure if you use HCl for making it. It also will contain some ONCl (nitrosyl chloride), the higher
the concentration of acid, the more you get of this unwanted by-product.
Another issue: How fast is the reaction between NO/NO2 and sulfamic acid? How do you deal with unreacted remains of sulfamic acid in your solution? it
will not simply boil away. And another thing is, nitric acid only reacts with sulfamic acid at high concentration of the nitric acid (I know from
personal experimenting with mixes of these two chemicals), so you also may have nitrate impurities.
The cost of chemicals is one thing, but you also need suitable equipment to do this. So, if you try it, I really am interested in the final result,
and each new method for making H2SO4, which one finds, is welcome. But I do not have high expectations from this method.
A good alternative may be methanesulfonic acid: https://www.laboratoriumdiscounter.nl/nl/methaansulfonzuur-7...
A 5 liter jerrycan of this will cost you around 80 euros if you add shipping from NL to Poland. This acid is nearly as strong as sulfuric acid.
At the same company you can buy 15% sulfuric acid, 5 liters for 25 euros: https://www.laboratoriumdiscounter.nl/nl/zwavelzuur.html
If you combine this with the methanesulfonic acid, then I expect the shipping costs still to be the same. You need to give a declaration of how you
use the sulfuric acid (telling that it is used for home chemistry expriments is OK), but you can buy it.
So, summarizing, there are alternatives for making it yourself, but if you try to make it according to your process, I am interested and willing to
think with you about optimizing this, but due to practical issues my expectations are not high.
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MrDoctor
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you wont have nitrate impurity, since it wont exist outside of as an acid which can distill off, but you will certainly have ammonium salts at very
least, in there if your combined oxides and decomp products arent led away from the sulfamic acid. sulfamic hydrolyzes and decomposes above 200C so i
would assume that by the time you boil it down, you wont have it present at least. i feel like by the time you reach 80% conc most of the problems
will have solved themselves. any sulfate will become bisulfate, im not sure but i think something happens to that once you reach 285C
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PoWEr
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In my country it seems like Its the opposite, high concentration of formic acid (85%) is very cheap and nothing has to be filled and on the other
hand, I could only find 5% oxalic acid, which costs even more than formic acid.
Speaking of formic acid, If oxalic works on copper sulfate to yield sulfuric acid, why not use formic acid? The pka and structure is almost the same.
Also instead of copper sulfate which can cost a lot, why not use some cheap sodium sulfate?
| Quote: Originally posted by MrDoctor | | its possible the introduction of ozone could drive the reaction more cleanly to form SO3, as ozone by default will oxidize sulfamic acid
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This gave me an idea, that maybe after all you could just use ozone to directly convert sulfur to SO3? Even if not directly, first to SO2 and then SO3
at a hopefully lower temperature? Perhaps the contact process could be modified to use ozone with a catalyst.
Birkeland-Eyde's Water? I only know the process and couldn't find anything about water. I actually considered this process once but then I realized
the electricity bill could be... well, not a nice thing to see.
Never heard of this before, do you have any paper on that?
| Quote: Originally posted by woelen | | It also will contain some ONCl (nitrosyl chloride), the higher the concentration of acid, the more you get of this unwanted by-product.
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Oh well, I didn't know this forms, it seems like Its a corrosive gas, so doing this outside could fix this issue.
From what I have read, they should not react a lot and generally stay inert, since the process I found should be done under cold conditions (to make
sure nitrous acid stays for as long as possible) they shouldn't react and even if, create tiny impurities that don't matter.
Well, I thought of just filtering it off.
| Quote: Originally posted by woelen | | And another thing is, nitric acid only reacts with sulfamic acid at high concentration of the nitric acid (I know from personal experimenting with
mixes of these two chemicals), so you also may have nitrate impurities. |
Sciencemadness wiki didn't say anything about only high concentrations reacting, it will be also nitrous acid. I never found anything about this
reaction on internet so it may or may not work actually.
| Quote: Originally posted by woelen | | I am interested and willing to think with you about optimizing this, but due to practical issues my expectations are not high. |
Yeah... I belive the main problem is nitric/nitrous acid. I have no idea what else could be used that would react and yield sulfuric acid. People
already pointed out the idea of just burning it in oxygen/ozone to get SO3. MrDoctor also said that nitric oxide apparently can oxidize sulfur, so
maybe you don't need ozone after all?
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chempyre235
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| Quote: Originally posted by PoWEr |
This gave me an idea, that maybe after all you could just use ozone to directly convert sulfur to SO3? Even if not directly, first to SO2 and then SO3
at a hopefully lower temperature? Perhaps the contact process could be modified to use ozone with a catalyst. |
I've been working on an apparatus to do just that. However, I planned to carry out the reaction as a suspension in water, which has been acidified
with some sulfuric acid, to aid in dissolving more ozone. By using a suspension, I shouldn't have to worry about SO3 vapors, because it
would hydrate to sulfuric acid directly. Performing the reaction in water should also help to regulate the temperature.
To my knowledge, ozone is a powerful enough oxidizer to oxidize sulfur to SO3 directly, without the use of a catalyst. Moreover, ozone has
the potential to oxidize metals to their highest oxidation states, and chloride to chlorate and even perchlorate (depending on reaction conditions).
[Edited on 5/29/2025 by chempyre235]
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MrDoctor
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sorry, id use quotes but i guess the forum is still getting attacked by bots or whatever.
to clarify; the context of nitric oxides oxidizing sulfur to SO3 is when included in combustion, so essentially its just a gas phase catalyst, though
it being famous, im not sure why i said that, i might have been linking some thoughts incorrectly.
As for the water of a birkland eyde reactor, im reffering to the whole aparatus not the reactor chamber itself, so pretty much just setting up a BE
nitric acid generator but using sulfamic acid solution instead of pure water.
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PoWEr
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| Quote: Originally posted by chempyre235 |
To my knowledge, ozone is a powerful enough oxidizer to oxidize sulfur to SO3 directly, without the use of a catalyst. Moreover, ozone has
the potential to oxidize metals to their highest oxidation states, and chloride to chlorate and even perchlorate (depending on reaction conditions).
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How do you plan on generating ozone? This seems like a very efficient and pollutant free method of sulfuric acid as long as you keep the inside filled
with inert gas (so no nitrogen reacts).
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davidfetter
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| Quote: Originally posted by PoWEr | | Quote: Originally posted by chempyre235 |
To my knowledge, ozone is a powerful enough oxidizer to oxidize sulfur to SO3 directly, without the use of a catalyst. Moreover, ozone has
the potential to oxidize metals to their highest oxidation states, and chloride to chlorate and even perchlorate (depending on reaction conditions).
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How do you plan on generating ozone? This seems like a very efficient and pollutant free method of sulfuric acid as long as you keep the inside filled
with inert gas (so no nitrogen reacts). |
Oxygen concentrators, which can be had for relatively cheap, serve as good-enough inputs to ozone generators.
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bnull
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| Quote: Originally posted by PoWEr | | Speaking of formic acid, If oxalic works on copper sulfate to yield sulfuric acid, why not use formic acid? The pka and structure is almost the same.
Also instead of copper sulfate which can cost a lot, why not use some cheap sodium sulfate? |
One word: solubility. Having similar structure and pKa is not important. Copper(ii) oxalate is insoluble in water, while the formate is soluble (125
g/L at 25 °C, according to Lange's Handbook 16th). Sodium oxalate and formate are soluble. If you can find a substance whose sulfate is soluble but
the formate isn't, that would be the one.
As pointed out, you can use iron sulfate with oxalic acid, if copper sulfate is too expensive.
One thing I forgot to mention: let the copper oxalate sludge rest for a day or two. You get a nice clear liquid and a compact mud.
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chempyre235
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| Quote: Originally posted by davidfetter | | Quote: Originally posted by PoWEr | | Quote: Originally posted by chempyre235 |
To my knowledge, ozone is a powerful enough oxidizer to oxidize sulfur to SO3 directly, without the use of a catalyst. Moreover, ozone has
the potential to oxidize metals to their highest oxidation states, and chloride to chlorate and even perchlorate (depending on reaction conditions).
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How do you plan on generating ozone? This seems like a very efficient and pollutant free method of sulfuric acid as long as you keep the inside filled
with inert gas (so no nitrogen reacts). |
Oxygen concentrators, which can be had for relatively cheap, serve as good-enough inputs to ozone generators. |
Correct. I've already purchased one for this purpose. To answer @PoWer, there are a couple of methods of ozone generation. The most common method is
through electrical discharge. There are small, fairly inexpensive ozone generators for home fumigation that use this technique.
Another method is irradiation of oxygen with UV-C. Some fluorescent bulbs are capable of this. There are also some industrial LEDs and other bulb
types that are made for ozone production, but they're spendy.
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PoWEr
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| Quote: Originally posted by chempyre235 |
Correct. I've already purchased one for this purpose. To answer @PoWer, there are a couple of methods of ozone generation. The most common method is
through electrical discharge. There are small, fairly inexpensive ozone generators for home fumigation that use this technique.
Another method is irradiation of oxygen with UV-C. Some fluorescent bulbs are capable of this. There are also some industrial LEDs and other bulb
types that are made for ozone production, but they're spendy. |
Don't ozone generators have the problem of also making some compounds with nitrogen? This would contaminate the final product. As far as I know, there
are no ozone generators (at least ones that don't cost a thousand dollars) that have a port to insert an oxygen tank or something similar (or like
david said - oxygen concentrator).
[Edited on 30-5-2025 by PoWEr]
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Lionel Spanner
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And yet, oxalate salts - from which it's very easy to make oxalic acid - are not regulated in the same way.
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chempyre235
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@PoWer:
Yes. NOx contamination is an issue with discharge ozonators, and the devices typically don't have a way to connect to a tank or a
concentrator. For this reason, I've been looking at trying the UV-C method. However, gutting and rehousing a cheap ozonator could work, too.
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