The formation temperature of sodium nitrite is very nearby to its decomposition temperature. So I think your end product will be a mixture of sodium nitrite, unreacted nitrate and hydroxide from decompostion. If it was pure nitrite, the reaction with sulfuric acid would have been even more vigorous then that which was shown here. I would recomment doing a recrystallisation and/or a quantitative analysis via titration to determine the real purity and yield. It's better to heat mixtures of solids in crucibles than in beakers, because they are much more heat resistent and especially made for this purpose. But nevertheless It's an interesting pathway (never seen it before) and really worth a try. A very effective method is the reduction of potassium nitrate with calcium formate by heating the stoechiometric and thoroughly mixed/grinded solids, which I have shown on my channel: 1. The conversion proceeds visible quickly and nearly quantitative. 2. Potassium nitrite is a little more heat resistant than sodium nitrite. 3. Calcium carbonate as the second product is filtrable, too. 4. You get a much purer product in a relatively high yield. Unfortunately the highest loss in the synthesis of alkali nitrites always occurs in the necessary purification step by crystallisation, because it's an extremely soluble salt. So the product always is to be found in the supernatent, not in the crystal mass!
Yeah there was definitely some sodium peroxide formed (the solution was fairly alkaline when I diluted it, and there was a small but visible reaction). There's also definitely some nitrate left for the reasons you stated.. I will say I got better results doing this in an oven at max temp like I mentioned (I didn't show it because it didn't look particularly interesting), but this is a process I wasn't sure would work and definitely would like to improve upon, and using potassium nitrate as a starting point is a fantastic idea! I'll also definitely try the formate method as I do have some formic acid now.
@@integral_chemistry Hydroxide, not peroxide. And an normal oven is not hot enough for the reduction (and not recommendable at all then if you still use it for making food). With the potassium salt, heating of the mixture by the bunsen burner is really less problematic, because the nitrite cannot be destroyed before it has formed. The sudden end of the reaction is clearly visible (stop of smoking). If you then take away the burner immediately most of the formed nitrite will survive...
@@experimental_chemistry Hello, did you delete your video showing the reduction of potassium nitrate with calcium formate? I would like to see that but I really cannot find the video on your channel.
I have made about 7 attempts to make sodium nitrite by reducing nitrate, and depending on what the container's made from, the purity varies from 60% to non-existent, as it is extremely easy to destroy the intended product by reducing it all the way to ammonia the easiest way to make it by far is bubbling nitric oxide gas into a solution of caustic soda, but if you can get hold of nitric oxide you'll have no trouble finding OTC sodium nitrite
that's a good idea! I do believe the dissolution of copper in dilute nitric acid yields nitric oxide (while the dissolution in 67% nitric acid yields nitrogen dioxide). Might be worth a try. What were you using as a reducing agent? With the method I do here I believe the decomposition products would be nitrogen oxides and sodium oxides.
@@integral_chemistry I first tried graphite with calcium hydroxide, as per a 1905 patent (US792515), with mixed results, 37% purity at best due to the product reoxidising to nitrate at the reaction temperature, and in aluminium containers, no product at all due to decomposition to ammonia the best results, though poor, were in tin cans previously used for food (coconut milk, to be precise) that had some kind of coating on them the greatest success I had was adding sodium sulphide in portions to molten nitrate, under an argon atmosphere; when I'd added about 60% I started getting small deflagrations (due to the nitrite product reducing the sulphide, forming elemental sulphur and this reacting with the remaining nitrate), stopped at that point, and got a 60% pure product however, when I added all of the sulphide, it destroyed the nitrite and the end product I got was most likely ammonium sulphate it was at this point that I felt it was a better use of my time to order 1 kg of it from Poland, where it's readily available
As you mostly do dye/pigment chemistry, here's a suggestion for the sodium nitrite: potassium hexanitrocobaltate (III), a beautiful bright yellow dye. I have made a detailed write-up on the preparation of it, which I could provide if necessary
Yeah I'd love to check that out! I tried that one once before but wasn't able to get any precipitation. My suspicion was that potassium nitrite rather than sodium nitrite was required but I'm not actually sure.
The nitrite test with sulfuric acid will produce some nitrosylsulfuric acid. When mixed in cold, the nitrosylsulfuric acid will be stable. It will fume in moist air and decompose in water above 50 oC into sulfuric and 1:1 mixture of nitric oxide and nitrogen dioxide. This is one convenient way of producing dinitrogen trioxide and/or nitrous gases - absorbing these in cold dilute alkali metal solution will regenerate the nitrite. Nitrosylsulfuric acid make also a useful indicator called the Liebermann reagent.
Nitrites release nitrogen oxides even with acetic acid when gently warm, while nitrates not. I think is better use that as indicator of nitrites than concentrates sulphuric acid.
I think it is easier to melt potassium nitrate and decompose it by some more heat to potassium nitrite and oxygen. Unless you exactly need sodium nitrite.
hi, do you think companies who need large amounts of nitrite do this to avoid the problem of buying large quantities of the hard to find nitrite?? Do you have any info on how the major producers of nitrite related cleaners make large batches of their product??
Seems easy but the pain is its purity. Nevertheless it was kinda easy and tidy way to make Alkali nitrites. Will you please try out a diazotisation with it ? Hope to see more from you !
What is your source of calcium sulfite? Did you buy it from a chemical company, make it, or is it availible as a consumer product? I saw it is used as a food additive and for water treatment, but i didn't find a "OTC" way of buying it in my quick search.
Yeah I just made it myself. I have a video filmed months ago where I made it, I just wasn't sure it was interesting enough to post. I'll go ahead and do it since it seems a few people are interested :)
interesting but while less messy than other methods I've seen on youtube, it's still complicated. I feel like it should be as easy as to add couple of grams of ascorbic acid or some over the counter reducing agent into the solution and boil it for couple of minutes with 100% yield and purity
@@integral_chemistry I've quickly found two patents. One is doing it in alkaline solution, oxidizing ammonia with nitrogen-oxygen gases and the other uses zinc electrode in saturated nitrate solution producing zinc oxide and nitrites. Other one nitrates alcohols to form amyl nitrite but it makes sense only if this is your desired end-product. Sounds like funny projects but I bought a bottle of poppers instead LOL. It's expensive AF tho
@@trollmcclure1884 Despite of using them for making alkyl nitrites alkali nitrites are very useful reagents, for example for the sythesis of azo dyes. Yes, I think the electrolytical method might work, but like with almost all lab scale electrolyses it takes a long time and the yield and purity is often not very high. I can't imagine how it should be possible to oxidize ammonia with nitrous oxides in alkaline environment. Introducing NOx into alkaline solution itself already results in the formation of nitrite, additional ammonia might destroy the just formed nitrite! I guess ammonia will be oxidized catalytically beforehand and the resulting NOx are introduced into alkali hydroxide solutions afterwards.
I Don't Really Understand Why Chemistry Channels Try To Hide (Yes, HIDE,Not Saying Something That You Know When You Know It's Important) The Hazards Of The Substances They Make, Like, You Should Have Added A Health Warning At the Begining Of Your Video, Imagine If Someone Tried To Make The Substance Just like You Did Without Knowing It's Hazards (Espically When Comparing It To The Much Safe Sodium Nitrate)
That's true, and I do try to add warnings, especially more recently as my audience has expanded. I feel though this process is so difficult and obscure that nobody without a clear understanding of what sodium nitrite is and it's associated hazards would even click on this video to begin with (much less try and make it). But yeah generally I agree with you
I did this in an oven, heating the calcium sulfite and sodium nitrate to 250C for an hour, packed down in the glass container and covered with 2 layers of foil to slow down the oxidation of my product. Once complete, I did the sulfuric acid test on the unprocesses product and it spontaneously produced the NO2 gas. However once I removed the sulfate/sulfite and recrystallized the product from water it doesnt pass the sulfuric acid test unless heated, implying its nitrate. My final product is a very slightly yellow crystalline powder, which could be nitrite but without evolving the NO2 from reaction with H2SO4 at room temperature I'm thinking its nitrate. Any suggestions as to why I passed the H2SO4 test before purifying the product, but not after?
Would this work with Barium Nitrate and Calcium Sulfite to yield Barium Nitrite? Planning to give it a shot because Barium Nitrite is unobtanium and the only other option I can find is creating lead sponge to do a messy and crude, low yield reduction
@@integral_chemistry I FINALLY got around to locating my sodium sulfite and made some Calcium salt. I plan to try the reduction of BaNO3 in the next day or so. I will post the results as promised 6 months ago. LOL... Life got in the way of the hobby. Anyway, thought you might be interested. I think BaNO2 may provide a novel one pot path to a pure form of the ammonium salt of NitroTetrazole. More to come.
Does the sentence (~0:20) "reduce the nitrate to nitrite and oxidize the sulfite to sulfate" kinda sound like rap music on purpose or is it accidental or is my brain just being weird? I find the sentence's rythm and alliterations to match the background music really well.
its kinda tough honestly. I'm trying to develop a better method for this right now but you basically just want to get it as hot as you can without it getting so hot that it starts producing NOx gasses.. its delicate and imprecise without a calibrated oven.
Just tried this, and my product did not pass the qualitative test. My product only reacted with conc. sulfuric acid once heat was applied 😭 I used a toaster oven (rather then the one I use for my food). I didn't observe any NO2 gas forming during heating. I left it in the toaster oven at 230 C for at least an hour. What did I do wrong? Perhaps my toaster oven doesn't get as hot as it claims to be? Did I leave it in too long? I also used 100 grams of sodium nitrate which is quite a larger scale, could this have affected the results?
Not really.. I just mixed sodium metabisulfite and calcium chloride and adjusted the pH up a bit. It's not the most useful chemical so I haven't been able to really find it
@@Wavy_Gravy not paranoid at all, I don't like paying for shipping since I live in the middle of nowhere. Ended up just making my own as suggested. I honestly kinda doubt there are watchlists related to this that I'm not already on anyway.
@chemistryofquestionablequa6252 Idt they exist, anymore at least. Even when it did, it wasn't "watched." More an after the fact thing. Any who, pool supply places carry it. Water conditioner. Idk which products, but I'm pretty sure I've seen it pure(ish) at my old job. Spa places have an odd assortment of chems, too.
@@integral_chemistrystrangely enough my shower head water filter has a layer of calcium sulfite as an anti-Chlorine. Manufacturer probably thought having an insoluble antioxidant to reduce free chlorine was optimal
I made it! I've got a video on how I did it that I plan on putting out soon but tldr you just react metabisulfite with calcium hydroxide or sodium sulfite with calcium chloride.
"How to cure Depression"
Google: Talk with a therapist, do sports
Bing:
Oh my God.. Now, there is a reason it's impossible to buy sodium nitrite.. and it's somewhat related to Bing 🙄
@@integral_chemistry Sodium Nitrite was illegalized in my country some weeks ago and police went to the houses of people who bought it
@@NoUser376I bought 2kg of sodium nitrite and anti emetics without any problems
How does sodium nitrite poison? Does it leave you breathless?
(bing might have led me here)
i expect we’re all here for the same reason lol. buh bye guys
❤
Wonderful, your channel is full of gems,
The formation temperature of sodium nitrite is very nearby to its decomposition temperature.
So I think your end product will be a mixture of sodium nitrite, unreacted nitrate and hydroxide from decompostion. If it was pure nitrite, the reaction with sulfuric acid would have been even more vigorous then that which was shown here.
I would recomment doing a recrystallisation and/or a quantitative analysis via titration to determine the real purity and yield.
It's better to heat mixtures of solids in crucibles than in beakers, because they are much more heat resistent and especially made for this purpose.
But nevertheless It's an interesting pathway (never seen it before) and really worth a try.
A very effective method is the reduction of potassium nitrate with calcium formate by heating the stoechiometric and thoroughly mixed/grinded solids, which I have shown on my channel:
1. The conversion proceeds visible quickly and nearly quantitative.
2. Potassium nitrite is a little more heat resistant than sodium nitrite.
3. Calcium carbonate as the second product is filtrable, too.
4. You get a much purer product in a relatively high yield.
Unfortunately the highest loss in the synthesis of alkali nitrites always occurs in the necessary purification step by crystallisation, because it's an extremely soluble salt. So the product always is to be found in the supernatent, not in the crystal mass!
Yeah there was definitely some sodium peroxide formed (the solution was fairly alkaline when I diluted it, and there was a small but visible reaction). There's also definitely some nitrate left for the reasons you stated..
I will say I got better results doing this in an oven at max temp like I mentioned (I didn't show it because it didn't look particularly interesting), but this is a process I wasn't sure would work and definitely would like to improve upon, and using potassium nitrate as a starting point is a fantastic idea! I'll also definitely try the formate method as I do have some formic acid now.
@@integral_chemistry
Hydroxide, not peroxide.
And an normal oven is not hot enough for the reduction (and not recommendable at all then if you still use it for making food).
With the potassium salt, heating of the mixture by the bunsen burner is really less problematic, because the nitrite cannot be destroyed before it has formed. The sudden end of the reaction is clearly visible (stop of smoking). If you then take away the burner immediately most of the formed nitrite will survive...
@@experimental_chemistry
Hello, did you delete your video showing the reduction of potassium nitrate with calcium formate? I would like to see that but I really cannot find the video on your channel.
@@ysch4110 ua-cam.com/video/BhBxDkU7AmI/v-deo.html
Great video!
Thank you 😊
I have made about 7 attempts to make sodium nitrite by reducing nitrate, and depending on what the container's made from, the purity varies from 60% to non-existent, as it is extremely easy to destroy the intended product by reducing it all the way to ammonia
the easiest way to make it by far is bubbling nitric oxide gas into a solution of caustic soda, but if you can get hold of nitric oxide you'll have no trouble finding OTC sodium nitrite
that's a good idea! I do believe the dissolution of copper in dilute nitric acid yields nitric oxide (while the dissolution in 67% nitric acid yields nitrogen dioxide). Might be worth a try. What were you using as a reducing agent? With the method I do here I believe the decomposition products would be nitrogen oxides and sodium oxides.
@@integral_chemistry I first tried graphite with calcium hydroxide, as per a 1905 patent (US792515), with mixed results, 37% purity at best due to the product reoxidising to nitrate at the reaction temperature, and in aluminium containers, no product at all due to decomposition to ammonia
the best results, though poor, were in tin cans previously used for food (coconut milk, to be precise) that had some kind of coating on them
the greatest success I had was adding sodium sulphide in portions to molten nitrate, under an argon atmosphere; when I'd added about 60% I started getting small deflagrations (due to the nitrite product reducing the sulphide, forming elemental sulphur and this reacting with the remaining nitrate), stopped at that point, and got a 60% pure product
however, when I added all of the sulphide, it destroyed the nitrite and the end product I got was most likely ammonium sulphate
it was at this point that I felt it was a better use of my time to order 1 kg of it from Poland, where it's readily available
As you mostly do dye/pigment chemistry, here's a suggestion for the sodium nitrite: potassium hexanitrocobaltate (III), a beautiful bright yellow dye.
I have made a detailed write-up on the preparation of it, which I could provide if necessary
Yeah I'd love to check that out! I tried that one once before but wasn't able to get any precipitation. My suspicion was that potassium nitrite rather than sodium nitrite was required but I'm not actually sure.
@@integral_chemistry Mine worked just alright with Sodium Nitrite, check your pending comments on youtube, it filtered the link I've sent you
@@ar-l How do you check those? there are tons of comments that have been filtered out that I'd really like to actually see lol
@@integral_chemistry Under the Comments menu option in UA-cam Studio app/website
The nitrite test with sulfuric acid will produce some nitrosylsulfuric acid. When mixed in cold, the nitrosylsulfuric acid will be stable.
It will fume in moist air and decompose in water above 50 oC into sulfuric and 1:1 mixture of nitric oxide and nitrogen dioxide. This is one convenient way of producing dinitrogen trioxide and/or nitrous gases - absorbing these in cold dilute alkali metal solution will regenerate the nitrite.
Nitrosylsulfuric acid make also a useful indicator called the Liebermann reagent.
Huh.. I'm actually trying to Remake this project right now so I'll see if I can work and of that into the vid. Thanks for the info!
Mix it with urea and heat gently in the presence of iron oxide. When the bubbling stops the reaction is complete.
Wouldn't do it, nitrite + urea is a mix that can actually detonate (not deflagrate like black powder, actually detonate like a high explosive)
Nitrites release nitrogen oxides even with acetic acid when gently warm, while nitrates not. I think is better use that as indicator of nitrites than concentrates sulphuric acid.
What is the best antacid to use to keep sodium nitrite from breaking down into nitrate after being in the elements very long?
I think it is easier to melt potassium nitrate and decompose it by some more heat to potassium nitrite and oxygen.
Unless you exactly need sodium nitrite.
hi, do you think companies who need large amounts of nitrite do this to avoid the problem of buying large quantities of the hard to find nitrite?? Do you have any info on how the major producers of nitrite related cleaners make large batches of their product??
Average sodium nitrite dealer:
Thank you for the informative video. Is it possible to make an experiment for the synthesis of sodium manganese oxide?
Seems easy but the pain is its purity. Nevertheless it was kinda easy and tidy way to make Alkali nitrites.
Will you please try out a diazotisation with it ?
Hope to see more from you !
For people that Cant buy nitrites its a really good OTC way to NaNO2 imo.
@@Energetics_Testing agreed
@@SciGuy700 Also i will make a batch of NaNO2 and see if its viable to make P-DDNP
Maybe you could do a thermal decomposition video of sodiumnitrate into sodiumnitrite.
What is your source of calcium sulfite? Did you buy it from a chemical company, make it, or is it availible as a consumer product? I saw it is used as a food additive and for water treatment, but i didn't find a "OTC" way of buying it in my quick search.
Yeah I just made it myself. I have a video filmed months ago where I made it, I just wasn't sure it was interesting enough to post. I'll go ahead and do it since it seems a few people are interested :)
interesting but while less messy than other methods I've seen on youtube,
it's still complicated. I feel like it should be as easy as to add couple of grams of ascorbic acid or some over the counter reducing agent into the solution and boil it for couple of minutes with 100% yield and purity
Things should be made as easy as possible, but not more easy than this.
Ascorbic acid in aqueous solution wouldn't work.
You'd be surprised how tough it is to effectively reduce 😅 I haven't had any luck doing this in solution with any reducing agent (so far)
@@integral_chemistry Nascent hydrogen is able to reduce nitrates and nitrites in alkaline solution - but unfortunately already to far: to ammonia...
@@integral_chemistry I've quickly found two patents. One is doing it in alkaline solution, oxidizing ammonia with nitrogen-oxygen gases and the other uses zinc electrode in saturated nitrate solution producing zinc oxide and nitrites. Other one nitrates alcohols to form amyl nitrite but it makes sense only if this is your desired end-product.
Sounds like funny projects but I bought a bottle of poppers instead LOL. It's expensive AF tho
@@trollmcclure1884
Despite of using them for making alkyl nitrites alkali nitrites are very useful reagents, for example for the sythesis of azo dyes.
Yes, I think the electrolytical method might work, but like with almost all lab scale electrolyses it takes a long time and the yield and purity is often not very high.
I can't imagine how it should be possible to oxidize ammonia with nitrous oxides in alkaline environment. Introducing NOx into alkaline solution itself already results in the formation of nitrite, additional ammonia might destroy the just formed nitrite!
I guess ammonia will be oxidized catalytically beforehand and the resulting NOx are introduced into alkali hydroxide solutions afterwards.
I Don't Really Understand Why Chemistry Channels Try To Hide (Yes, HIDE,Not Saying Something That You Know When You Know It's Important) The Hazards Of The Substances They Make, Like, You Should Have Added A Health Warning At the Begining Of Your Video, Imagine If Someone Tried To Make The Substance Just like You Did Without Knowing It's Hazards (Espically When Comparing It To The Much Safe Sodium Nitrate)
That's true, and I do try to add warnings, especially more recently as my audience has expanded. I feel though this process is so difficult and obscure that nobody without a clear understanding of what sodium nitrite is and it's associated hazards would even click on this video to begin with (much less try and make it).
But yeah generally I agree with you
I did this in an oven, heating the calcium sulfite and sodium nitrate to 250C for an hour, packed down in the glass container and covered with 2 layers of foil to slow down the oxidation of my product.
Once complete, I did the sulfuric acid test on the unprocesses product and it spontaneously produced the NO2 gas. However once I removed the sulfate/sulfite and recrystallized the product from water it doesnt pass the sulfuric acid test unless heated, implying its nitrate.
My final product is a very slightly yellow crystalline powder, which could be nitrite but without evolving the NO2 from reaction with H2SO4 at room temperature I'm thinking its nitrate.
Any suggestions as to why I passed the H2SO4 test before purifying the product, but not after?
Very cool but yeh CaSO3 is a sus chemical, I'd liké to see how to make it as well 🧐✨
Calcium hydroxide and Sodium Metabisulfite.
@@EddieTheH thank you very much ,I even have both !
You can also just mix any soluble sulfite salt with calcium chloride :)
Would this work with Barium Nitrate and Calcium Sulfite to yield Barium Nitrite? Planning to give it a shot because Barium Nitrite is unobtanium and the only other option I can find is creating lead sponge to do a messy and crude, low yield reduction
It should yeah! And I feel you, I tried the lead sponge method and it was a total nightmare, definitely don't recommend
@@integral_chemistry I FINALLY got around to locating my sodium sulfite and made some Calcium salt. I plan to try the reduction of BaNO3 in the next day or so. I will post the results as promised 6 months ago. LOL... Life got in the way of the hobby. Anyway, thought you might be interested. I think BaNO2 may provide a novel one pot path to a pure form of the ammonium salt of NitroTetrazole. More to come.
Does the sentence (~0:20) "reduce the nitrate to nitrite and oxidize the sulfite to sulfate" kinda sound like rap music on purpose or is it accidental or is my brain just being weird?
I find the sentence's rythm and alliterations to match the background music really well.
what is the theoretical yield heating the 2 components to 310c?
How do you know when its at the correct temperature?
its kinda tough honestly. I'm trying to develop a better method for this right now but you basically just want to get it as hot as you can without it getting so hot that it starts producing NOx gasses.. its delicate and imprecise without a calibrated oven.
Just tried this, and my product did not pass the qualitative test. My product only reacted with conc. sulfuric acid once heat was applied 😭
I used a toaster oven (rather then the one I use for my food). I didn't observe any NO2 gas forming during heating. I left it in the toaster oven at 230 C for at least an hour.
What did I do wrong? Perhaps my toaster oven doesn't get as hot as it claims to be?
Did I leave it in too long?
I also used 100 grams of sodium nitrate which is quite a larger scale, could this have affected the results?
good
Does this same process work with potassium nitrate for making potassium nitrite? And if it does, are the same temperatures used?
Do you have an otc source of calcium sulfite without having to order it?
Not really.. I just mixed sodium metabisulfite and calcium chloride and adjusted the pH up a bit. It's not the most useful chemical so I haven't been able to really find it
Why so paranoid?
@@Wavy_Gravy not paranoid at all, I don't like paying for shipping since I live in the middle of nowhere. Ended up just making my own as suggested. I honestly kinda doubt there are watchlists related to this that I'm not already on anyway.
@chemistryofquestionablequa6252 Idt they exist, anymore at least. Even when it did, it wasn't "watched." More an after the fact thing. Any who, pool supply places carry it. Water conditioner. Idk which products, but I'm pretty sure I've seen it pure(ish) at my old job. Spa places have an odd assortment of chems, too.
@@Wavy_Gravy gotta love pool stores, everything from oxone to peroxide, HCl, bisulfate, carbonate, bromides, etc.
I don't have calcium sulphite, what should i use instead ?
I didn't have it either (its not a very useful chemical) but its pretty easy to make from sodium sulfite or sodium metabisulfite
@@integral_chemistrystrangely enough my shower head water filter has a layer of calcium sulfite as an anti-Chlorine. Manufacturer probably thought having an insoluble antioxidant to reduce free chlorine was optimal
Where did you source you calcium sulfite
I made it! I've got a video on how I did it that I plan on putting out soon but tldr you just react metabisulfite with calcium hydroxide or sodium sulfite with calcium chloride.
@@integral_chemistry thank so much I was thinking about making some
@@integral_chemistry also I love your channels
ua-cam.com/video/Yu1gXbmQ4a8/v-deo.html
Can you make me one? (100G & above 96% purity) I can pay
U want to ctb ???.
@@Ronak-ob3yc are you a SancS member?
I am not a member
@@Ronak-ob3yc Alright but to answer your question, no i don't, i just need it for a company.
@@johnmachenzie1613 and 100 grams is your requirement that's kinda sus 😳