Thanks man! Yeah the purification was quite a headache to figure out but at least it finally came together. Also thanks again for the permanganate titration idea. Always love a quantitative tie-in where possible
@@integral_chemistry Yeah thanks for the Titration and quantitative test. I always just melted a pool of Lead and chucked in Nitrate until Litharge and bubbles stopped forming. Huge excess of Lead which ya might want to give a try.
@@integral_chemistry You made nitrite from nitrate but did you know there is a very obscure way of making pure nitrite from ammonia and oxygen? Fill a flask with a saturated solution of Schweizer's reagent at room temperature, put an oxygen filled balloon on top and let the solution on strong stirring for a few days. As the oxygen is consumed you need to either refill the balloon from time to time or have a pressure valve maintain the gas pressure at a few dozen millibars above ambient. At the end of this process you will end up with purple-indigo crystals of copper amino nitrite complex. Because the nitrite is covalently bound in a complex, oxygen cannot oxidise it to nitrate. Liberate the nitrite with sodium or potassium hydroxide which will release copper hydroxide and ammonia then you can further purify it with silver nitrate if you feel it’s not pure enough. The most nitrite you can make with this method is 1.25 nitrite per one copper but it takes forever because the second oxidation is fairly slow (weeks). However, getting one nitrite per one copper is considerably faster (1-5 days depending on room temperature, oxygen purity, stirring speed and the concentration of the solution).
Absolutely phenomenal work! Working from small scale to large scale, multiple runs, qualitative tests and titration? I'm not sure when was the last time I've seen someone be so careful and diligent in actually getting reliable numbers for their results. Keep it up!
Great video! Very thorough and easy to follow. Thanks for sharing! Also, I really like the longer video showing the whole process and would like to see more of it in the future. Keep up the great work!
I'm pleased that you took up my method, which I found in an earlier German forum. Unfortunately, here in the EU, calcium and magnesium nitrates are now also monitored, as are alkaline nitrates. Purchasing and possession are not prohibited, but the seller must report suspicious orders so that you can quickly be affected by a house search. Pure ammonium nitrate is completely prohibited. Only heavy metal nitrates and barium nitrates are unrestricted in the EU. They are also difficult to get in Germany itself, so you have to resort to sellers in other EU countries. Calcium nitrate can be made from calcium hydroxide and ammonium sulfate saltpeter, which is not monitored. Overall, it is safer to buy nitrite than nitrate here in the EU. Reduction methods are easier to carry out in porcelain crucibles than in narrow glasses. The relatively lively implementation with formate is not a problem if the experiment is carried out outside or in a hood. The reaction usually starts after just under a minute and actually produces some smoke - but that's all. If the heating is stopped beforehand, the reaction remains incomplete. However, if you heat unnecessarily for longer, decomposition will begin. Nitrite solutions are also sensitive to air. It helps to let the mixture of calcium nitrate and potassium carbonate solution sit overnight. This ensures that no potassium carbonate is left unreacted. Recrystallization of the end product helps to achieve higher purity, but comes at a great cost to the yield. It is probably hardly possible to produce analytically pure nitrite using amateur methods, but in the end any method is better than none at all.
As always thank you so much for the great info! I did figure the issue with the formate run was a matter of temperature control, I think in both cases I heated it too long considering the relatively high level of decomposition compared to the other methods.. same thing when I tried reduction by sulfur/carbon. And yeah the test tubes sucked for the reduction, only really used them for visual clarity but they were a pain especially with the formate/oxalates that put off gasses during the reaction. Also makes sense in the EU that nitrite would be easier to get than nitrite.. makes me wonder though, wouldn't a good source of nitrate in the EU be the oxidation of nitrite? The stuff certainly oxidizes far easier than nitrate reduces.
Its very valuable to see all of the "failures" here. While they failed to efficiently produce nitrite, there's a lot of things that happened that might be useful or useful to avoid for people trying other reactions. Also, silver again. Its always silver. It would be nice if you could get from silver nitrate to nitrite in one step since they're so easy to separate, but probably not (without already having a nitrite salt, I mean).
loved this longer video. It honestly is something I'm going to use in the future as a chemist for reference videos on how to make these things and how to do it well.
Great work! Just to say, iodine reacts with the iodide ion in aqueous solution to form the triiodide ion, which is orange. That is likely the orange color you were seeing.
Looks like hammerth beat me to it but yeah that's why I didn't claim triiodide (although yeah it was almost certainly triiodide lol) I just came across some literature on how nitrite can also complex to iodine and i wasn't exactly sure how favorable that complex was relative to triiodide (sounds like not very) Thanks for the info Reguardless! 😁
Cool always knew the CaSO3 method was the best, Wish you gave tips and trick for filtering the calcium sulfate. Love the longer video and the method for purification with silver nitrate. Also i think(i may be wrong) that solubility of sodium nitrite/nitrate is not the same in alcohol(they are almost the same in water) so alcohol can be used for making the sodium salt. edit: heating a strong oxydent with a combustible(alcohol) is probably not a good idea.
What a pleasure to watch man! Thank you for all the hard work, I would love to see more! For me this longer format was superior, I very much enjoyed the journey through all of the processes to finally end at a resolution. Just great man.
Hey, if you want an easy, fast way to get nitrite from nitrate that is pure enough to make alkyl nitrites (at least that), 1:1 sulfur to KNO3 ratio BY VOLUME, burned on a surface you don't care much about. Of course, you could do it stoichiometrically correct and get the pure product. I've got an eye for the nitrite via this method, and the best part is you can separate the waste from the product with water. It works. It stinks during burn, but it works. I was very surprised the first time. Nice video, as per usual. It's always fun to watch a contest. ❤
Hm ill have to give that a try. I actually did try a sulfur reduction but I cut it from the final video because it just made a big mess lol. I figured by burning the mixture I'd basically just have gunpowder and therefore reduce the nitrate all the way to nitrogen. Instead I tried indirect heating which just sorta melted it together into a rock-solid mass 😅 I'll update on how it goes!
@integral_chemistry it burns a lot like gunpowder, yes, but what happens is this puddle drips out and gets onto the surface of where you burn it (hence where you don't care what happens to the surface!) And when it cools it looks a lot like toothpaste, with weird colors in it: pinks, yellows even greens sometimes and of course where bubbles had been and burst little pock marks and craters. This will prove to be very hard like rock, but you can use a hammer and rather lightly tapping it to break off pieces AND will prove to be at least mostly nitrite. Works for any alkali nitrate, probably just as well for calcium, strontium and barium though I never tried. First time I made nitrite was accidental. I thought firecrackers were filled with blackpowder and I didn't have any idea at 15 years old that chemists go by weight, not volume. I had put 6:1:1(nitrate, sulfur, charcoal respectively) just like "Pyrotechnics" had said were in "Chinese firecrackers" , ending up with this grey powder that looked very much like what I saw in black cats. Lol was I wrong! My parents' driveway had a bunch of little stains all over it from me back then (we've moved, stains haven't). That was the first time I encountered those puddles that become seemingly as hard as cement. I didn't know chemistry yet, hadn't taken it in school (I was 9th grade then, turned 15 middle of that year) until 11th grade and then again in college. But frankly i learned so much more through hands on experimenting. I was scared away from organic Chem due to falling grades but have learned a decent amount through hands-on and RUclips as well. Anyways... You can use plain old carbon if you don't have the sulfur on hand. Just remember to keep the ratio way off from blackpowder. With a 6:1:1 ratio BY weight, the nitrate is a smaller pile than the sulfur and even smaller than the charcoal, just for reference against my first pyrotechnical mistake, 30 years ago... your work on this was really inciteful. I like learning ways to do things.
@SetTheCurve absolutely, just need excess nitrate to charcoal, even by volume. 1:1 by volume will work, but you might burn off some of the nitrate like gunpowder burns. It's cheap anyways, so if you test it it will do exactly as I described. I didn't have a scale back then, we'll, I had a balance beam and I was underage to buy a scale and we didn't have cellphones (rich people did, and business people). Texting sucked, bc every number has three letters on it, so a text was super rare. It's one if the reasons older people don't like texting. Sorry, I digressed. I'm suggesting strongly to burn the two on a surface you don't care about. It looks like a burn stain looks when done, once you break up the toothpaste-looking cement-like nitrite puddle. Drop a piece into some vinegar, small piece, but bug enough so you can see the gas coming off. In a test tube you will see the orangy, rusty brown gas that is NO2 being made from the NO produced from nitrite reacting with acetic acid. Btw, if you only had a super small piece and can't see the gas, is the piece fizzing in the liquid at all? If so, then you got it. If not, then it's still nitrate. That easy, for real. All from a happy accident ☺️
In my quest to get Barium Nitrite, I settled on using Silver Nitrite as the intermediate as well for very pure product. I've had near 100% recovery of the silver after doing the double displacement to Barium Nitrite. I've also been using the CaSO3 route to reduce Barium Nitrate to Barium Nitrite via your reduction. I recently use a muffle to slowly ramp the temp with a close fitting lightly vented lid, which has resulted in much better yield. THat said, my use for the Barium Nitrite is not sensetive to Barium Nitrate contamination and it's acidified with HNO3 anyway. Great video! And if I didn't say it, thank you for the starting point you shared with CaNO3!
Thank you so much, I'm glad the video helped! The initial cost sucks but I do love silver salts for Displacement reactions because it really is so easy to recover the silver at near 100% yields.. as you said i do think barium is just a better choice overall for this process than calcium for a variety of reasons. It's unfortunately very toxic and less avaliable so I did skip it for this video but it's just so much cleaner than calcium for these replacement reactions.. might try your muffle idea at some point too
@@integral_chemistry I'm going to noodle the idea of using Barium Sulfite to reduce the Barium Nitrate. The point you made about it's lower decomp temp was the ah-ha moment. I will try to update you once I give it a shot. What's your view of the best path to Barium Sulfite? Are you starting with NaCO3 or CaSO3.
This is great stuff man! You've just elevated your value as a chem youtuber with this addition. Also longer vids are cool. Nile red does them and as long ad they have a decent pace they don't bore. You balanced the information with process good too.
Video is great but I am not satisfied. You didnt test reducing with starch. I made my nitrie in this way. I burned 400g of potassium nitrate with 80-100g of starch in a pan, then dissolved in minimal amount of boiling water, hot filtered. Evaporated filtrate to volume of 200ml and cooled. Obtained nice slightly dark crystalls, vaccuum filtered and dried in dessicator bag over CaCl2. Yeild was around 30-35%. Purity is questionable but I succesfully used this for diazotation. Maybe you can test this method too? I want to know the purity of nitrite obtained by this method.
Absolutely, and cheap charcoal if done right is even better, superior actually. Sometimes im getting filling that such videos are to make it feel like its impossible to synthesize like his video about TNT for example... Anyway for -NO2 use charcoal, for TNT just type "Dug TNT" in youtube search and you will be satisfied. NBothing is complicated.
Great example of analytical work. This was a fantastic video. (Although it looked like a lot of work.) That looked like a praseodymium salt at the end.)
I like the long video format very much, also because it adds a lot of educational value to your content. I wouldn't want shorter videos to completely go away though. Maybe you can switch back and forth, depending on the project? That would be the best of both worlds.
Very happy to hear you liked the longer format! Tbh I don't think I'd even be able to make videos this long but once every few months so no worry about the shorter ones going away. Do love the idea of making these videos that capture the actual process like this one more often as well, sure I'll eventually strike a balance
Enjoyed the longer video!! After the preliminary testing I started supporting calcium sulfite like it was sports team lol Its nice to see it won in the end
@@integral_chemistryAmazon doesn't care at all about the regulations, as long as nobody calls them out. They can't go after Jeff Bezos as he's basically a dystopian deity above any mortal law. You can still find 90% sulfuric acid on amazon while is banned everywhere else in the EU. I've seen substances that I won't name that can be used as extremely toxic chemical warfare agents being openly sold on amazon. Stuff is crazy.
Excellent work. Very very scientific approach, really appreciate the work! Just a quick note - silver salts (or any heavy atoms) have a tendency to explode with some organic compounds (fulminates, acetilids, picrates, etc...). I am not so sure if you cannot run into trouble with using AgNO2 in diazotation...? I have not checked lit I am just thinking out loud. there is HCl, so in theory all will crash out as chloride and should be safe. But then again that could also take down your product and you might lose yield? I always did diazotation with sodium salt and then converted the diazonium salt to BF4- for stability... Also on a different note, I don`t know how this is in US, but here you can buy so called "butcher`s Salt" for meat curing. It contains 0.6 % of NaNO2 - it is not much, but then again, 1 kg costs less than a dollar. so in theory purifying 25 kg (costs 11 dollars here) of this could give you like 125 g of nitrite. there is also no KNO3 so the only impurity would be NaCl, but that should be easy to rid off.
Really useful information here for those of us needing nitrites for synthesis! Love the longer videos bro. Sorry to hear bout the Patreon what happened? Hope it gets resolved and everything works out! 💯🤞🏼
Thanks a ton man! I had felt it'd been a while since I made a video on a practical process, and very happy to hear lots of people seem to have gotten at least something from the video. And yeah Patreon thing really sucks, definitely helped having a steady stream of revenue for misc lab supplies and such. Definitely update when I hear back
Thank you for this! I'm going the CaSO3 route, and made a bunch of Ca(OH)2 via CaCl and NaOH to start, but thanks for pointing out i could have just been a little smarter and done it in one step with the Na2S2O5.
Glad you found it helpful, and lemme know how it goes! Another quick tip: you can buy calcium hydroxide from nearly any grocery store and it's a lot cheaper than sodium hydroxide or calcium chloride. It's sold as "Pickling Lime" usually near canning supplies
Hi! Nice video! I have an idea. When I was student, they gave us to make some complexes in inorganic chemistry lab classes. I got to make potassium hexanitrocobaltate(III). Procedure was simple, just take some Co(NO3)2 disolve in water and add six time more (in mols) KNO2. After that, I bubbled oxygen through solution and precipitate of potassium hexanitrocobaltate(III) started to form. Also, you can speed up the process by using hydrogen peroxide. After some bubbling, I filtered the suspension and I got nice yellow powder. I remember that I got almost quantitative yield. Here one cobalt binds with six nitrites (via nitrogen atoms), much more than silver in silver nitrite. Also cobalt nitrate is cheaper than silver nitrate. I think that you can somehow destroy this complex and get potassium nitrite in solution. I had an idea to use hydrogen sulfide for this. In suspension of potassium hexanitrocobaltate add three times more potassium hydroxide (in mols) and bubble excess of hydrogen sulfide. Cobalt should prcipitate as CoS and there will be some elemental sulfur from oxidation of H2S by Co(III). In solution will remain only potassium nitrite. After, just separate precipitates from solution. I think this could work. Only downside of this potential method is toxicity of H2S and cobalt salts. Anyways, I hope you will succeed! Greetings from Serbia!
Very interesting. Thank you for your diligence and patience. I wasn't aware of the federal ban on nitrite since I was able relatively recently (about 1.5 years ago) to purchase a considerable amount of it from a well-known OTC chemical supplier. But it looks like it happened soon after that... In any case if I ever run out of it (which will likely not happen) now I know how to make my own, and I am grateful to you for that.
Very impressive once again. I was wondering if part of the nitrite doesn’t reoxide to nitrate at high temperature, making the process less effective. Why not try heating under inert atmosphere? Also why not try sodium hydrosulfite as the reducing agent? EDIT: I’m dumb. It would be impossible to separate from the product. Oh and BTW, I recently found out how to make methylene blue. No really complicated, provided you have N,N-dimethylaniline that you can make from aniline and methyl iodide (or buy). EDIT: On second thought, maybe you should’ve activated zinc by immersing it in hydrochloric acid for a short while. I’m going to test that tomorrow at microscale in aqueous medium. As far as I remember, all reductions with zinc begin either by washing the powder in HCl or adding a catalytic amount of copper sulphate, which must have the same effect. EDIT 2: Reduction of potassium nitrate by zinc in water works. The zinc has to be clean (powder, rinsed in hydrochloric acid and washed). Mix the nitrate in solution with the zinc → nothing much happens. Add a catalytic (in my case, a few crystals are enough on a ~100 mg scale) amount of copper sulphate and bingo! There is instant formation of a white layer of zinc oxide and the solution definitely contains nitrite as it turns a potassium permanganate solution colourless.
The “dumb” method mentioned first may not be as stupid as advertised if the source of NOx is a birkeland eyde reactor. The purity of product and simplicity of the process may make it worthwhile.
That's a good point^ I do think the complexity is building the reactor to begin with. Seems a prohibitive process (although I've never tried myself) If you could get it to work though yeah 1000% that would be the best method, basically infinite free nitrite or nitrate at that point. Worth looking into for sure
silver nitrite in itself useful for victor meyer reactions to form nitroalkanes, or for halide substitutions in general. i would reserve it for that purpose alone considering how expensive silver is, which makes sense since the organic syntheses that require pure nitrite usually convert it to isopropyl nitrite instead (thereby purifying it). inorganic chemists might be out of luck though. i doubt i would appreciate nitrate or silver contamination in my nice metal complex crystals 😅
With regards to the formate method: I think the violent reaction is required. I did try lower heats (just above melting point of KNO3 like 330 degrees) with longer times and there was no nitrite. Once the reaction kicks off, an air quality monitor shows a small amount of carbon monoxide being released but not a dangerous amount. There is a strange odor and a lot of smoke so do it outside. The temperature when the reaction starts is probably around 350-400 if I had to guess. I did many small runs (35g KNO3) using porcelain crucibles on an electric stove with foil insulation which worked fine. The reagents do not need to be especially well mixed or dry for the reaction to work. pH of diluted extracts is alkaline so some over reduction is certainly occurring. For the lead method, SM members say tin can be substituted for lead.
Very good video interesting methods for producing the potassium nitrite just 2 comments here first I think you meant to say iodine precipitate not gas the second is potassium nitrate according to Wikipedia is NOT very hygroscopic! I think if that does occur is because of small amounts or traces of sodium nitrate which is extremely hygroscopic in the same way pure sodium chloride doesn't cake only because of impurities like magnesium chloride in commercial salt.😮😅
Thank you very much! And yeah I did kinda misspeak there, I meant to say triiodide forms along with solid iodine which is partly vaporized by the very exothermic reaction 😅 and really not hygroscopic? I'd actually not heard of this phenomenon. Is it kind of similar to a eutectic mixture? Come to think of it, it was honestly just all the potassium hydroxide byproduct lol Edit: just re-read your comment and I might have misspoken in the video 😅 i meant to say Nitrite is hygroscopic, nitrate isn't (which is partly why it's so useful)
@integral_chemistry you're very welcome I am just so amazed you have difficulties there getting the nitrites? Here in Australia not so hard as our Government agencies not cracking down on that.Except of course on Ammonium nitrate! Which you can't buy here. Ever since the 911 attacks there.Is it just the potassium nitrites? I bought 2 packs on eBay of sodium nitrite 500 g each 99.95% purity. I am jealous as you can get so many things there! We can't get Here 😞🥺perhaps we can exchange ideas?
I’m wondering if another way to purify it would be to use the crude nitrite to make an alkyl nitrite and purify that and then convert it back to an alkali nitrite
I think you're onto something. Isopropyl Nitrite production is not sensetive to Nitrate contamination in my understanding. The only hitch I see is the low-ish yield of Isopropyl Nitrite and the resultant losses related in the conversion back to an alkali metal salt.
I might be totally wrong here but I think NurdRage gave this exact process a try a while back and I think I remember it failing somehow. I'll have to try and find the video but what you're describing sounds oddly familiar (and should work on paper i feel)
@@integral_chemistry I've got a procedure that states that mixing ethyl nitrite and NaOH in ethanol and leaving it be for two days gives somewhat 90+% NaNO2. No quantities are mentioned but something worth looking into. Secondary alcohols like NR tried may not work great
Longer content showing the learning process you went through sets more realistic expectations for what someone should expect in real world chemistry, as opposed to textbook lab experiments that “should” work every time. Seeing your persistence makes it easier to deal with setbacks instead of giving up. A 15 minute video wouldn’t have done this research justice.
Possibly, another route would be the copper II catalyzed, electrolytic oxidation of ammonia. Depending on the voltage and reaction conditions (anode material used, temperature), the process can be tweaked to make nitrate or nitrite. I have yet to get it to work though. Such a route would be welcome for European folks due to the strict regulations making it difficult to buy compounds containing those two anions.
I believe there is a patent out there for membrane assisted electrolysis as a method of oxidizing nitrate to nitrite with high purity. I’m a little surprised it hasn’t been attempted on RUclips yet.
Apoptosis (Some day before): Too busy to watch videos longer than 3 mins. Also Apoptosis: A 42 minutes video🤣 Got to bookmark this and watch it on TV later.
LMAO yeah that is a literal quote of mine 😅 I do struggle with the ole' attention span in front of a screen.. I think making this video took years off of my life tbh. Lemme know what you think when you get around to watching!
@@integral_chemistry This video is indeed very informative and it took me another day to finish it! I am not a big fan of solid-solid reactions, but the one with calcium sulfite seems solid! (No pun intended), so I guess I will employ that method as well when making nitrite. The purification part is also very nice, and I would prefer this kind of longer format.
Would it be possible to react the final silver nitrite with sodium or potassium chloride to obtain extremely pure sodium or potassium nitrite while precipitating extremely insoluble silver chloride?
Yeah residual sulfite would definitely react with permanganate. I doubt any would survive the heat, though, even if it didn't react with the nitrate. Can always precipitate residual sulfite/sulfate with barium nitrate just to be sure
@ my first thought when the sulfite performed significantly better than other agents was that some of it made it through. It might be a good idea to cook sulfite without the nitrate just to see how even/consistent/complete the decomposition was. That said, you’ve obviously thought about it a lot more than me 😅
Appreciate the detailed breakdown! A bit off-topic, but I wanted to ask: I have a SafePal wallet with USDT, and I have the seed phrase. (alarm fetch churn bridge exercise tape speak race clerk couch crater letter). Could you explain how to move them to Binance?
when i was into salt water fish tanks back in the day the negative byproduct of living biomass in a small closed system was nitrites & nitrates....a build up of these would result in a die off in the system. i wonder if that is an option for obtaining nitrites?
I used to have a reef tank too. If I remember correctly, nitrite was even more toxic than nitrate. I'm guessing it's not a suitable way to produce them because they were measured in ppm.
The concentration is way too low to be useful while still being high enough to be toxic. There's a concept to use the buildup of nitrite and nitrate from aquaculture to fertilize plants, but I don't think that was ever developed beyond early experimentation.
I was never able to get it to work without a big unworkable mess or huge impurities (like it the formate run but worse). I think it may be a matter of tighter temp control, certainly feasible but so far not much luck on my end
Would the reaction also work, if you would heat up KNO3 with a formaldehyde solution to form the nitrite and formic acid ? Or even just heating a KNO3 ad ethanol solution although the solubility is low of he crystals.
I do certainly think that could be feasible, whether by some divided cell or a deviation of the partial electrochemical oxidation of ammonia. Either way I haven't tried it but I'd love to in the future!
@integral_chemistry yes but I'm making potassium nitrate This method Potassium carbonate add in nitric acid After that add water and freez it You can get a crystal purest potassium nitrate.
Thank you good sir. I have been looking for a source of this reagent for awhile. I suffer from government the same way you do so buying it isn't an option.
Please make a similar vid about iodine. I have 2 pounds of sodium iodide and I wanna make myself elemental iodine and tincture I can use. Here's the problem: we cant buy 30% hydrogen peroxide in the EU. I can buy potassium nitrate tho and HCl. How do I react those to be able to get iodine out of a solution? It didn't work the last time so I added a pool oxidizing tablets. What I ended up with is a brown mixture of HCl and possibly nitric acid. Total waste of my iodide.
That could be a cool video! Although it might take me a while. If you wanna get started sooner I do know how you could get pure iodine with what you have. Simply set up a chlorine generator by dripping the HCl onto the chlorine tablets (obviously dangerous) and feed the gas into a solution of iodide. The chlorine is more reactive than iodide so it'll displace elemental iodide. Alternatively a safer option would be to use persulfate which can easily oxidize iodide to iodine and should be available in most countries. Also 3% peroxide will do a fine job in a pinch, 30% is honestly overkill
@integral_chemistry Yes persulfate tablet it was. But it didnt precipitate as I expected so I was not able to filter it out. And then there's unbeknown to me sulfur contamination. Maybe it was too acidic or something like that. It seems simple in videos and then it doesnt work out. I'll try the weak, 10 times more expensive peroxide thanks.
@@trollmcclure1884 Hm, surprising the persulfate didn't work.. Perhaps the tablet itself was impure. You could also try dissolving it and filtering any solids before reacting it with the iodide. Another thing is that iodine will react with excess iodide to form soluble triiodide, so you might just not have used enough persulfate to get a sufficient oxidation. And yeah.. peroxide is somewhat expensive, but because a mole of peroxide is so lightweight compared to iodide it shouldn't take much. One final thought: See if percarbonate is available to buy where you are. Very cheap and generates peroxide when it dissolves in water.
I'm confused how in the beginning of the video when you started talking about nitrite salts, you said something about how nitrites can cause methemoglobinemia, which is usually rapidly fatal, but then you also said that in specific forms, the nitrite ion is also useful in blood pressure medications. Huh?
NitrAte ions NO₃- are strong oxidants which transforms the ferrous (Fe²⁺) ions present in haemoglobin into ferric (Fe³⁺ ) ions which are incapable of fixing oxygen, given that they are in their maximal oxidation state (methaemoglobin). NitrIte ions (NO₂-) are metabolised into nitrogen oxides which act as strong vasodilatation agents (they relax veinous wall tissues) which leads to reduction of blood pressure. This is also why azides are poisonous (inter alia).
I suppose you could, thing is though curing salt is 0.5-5% sodium nitrite and I'm not really sure how you could selectively extract it from all the sodium chloride. Guess you could remove most of the chloride using lead nitrate
@integral_chemistry on a long enough timeline, all actions become illegal. Even life would be illegal as possible threats are "removed." For example, murder is illegal. Has been for some time. How many other laws have been created to attempt to curb the already illegal activity. Eventually, taking a breath could endanger the O2 for someone else. It's a vicious, self consuming circuit... or network, which is possibly a more accurate description.
RUclips: Posting videos of Ukraine war and various improvised drone drop loads IS OK ALSOl RUclips: Absolutely NO Chemistry you can learn on one Page of wiki. HUMANS: Dafuhk?
@@7hunderstorm242 I have experience with Pb, -SO3 and C method. Highest quality is from Pb, -SO3 is low quality because contact will never be intimate enough, and -SO3 are not so cheap per unit mass, carbon, if done right has acceptable quality and is cheapest of them all, so easiest and cheapest method
Awesome work! i'll probably be making my nitrite this way, the purification is what really sets this apart from all the other procedures i've seen.
Uh oh. You have summoned a RUclips God.
Thanks man! Yeah the purification was quite a headache to figure out but at least it finally came together. Also thanks again for the permanganate titration idea. Always love a quantitative tie-in where possible
Relax...... your smooth muscles
@@integral_chemistry Yeah thanks for the Titration and quantitative test. I always just melted a pool of Lead and chucked in Nitrate until Litharge and bubbles stopped forming. Huge excess of Lead which ya might want to give a try.
@@integral_chemistry
You made nitrite from nitrate but did you know there is a very obscure way of making pure nitrite from ammonia and oxygen?
Fill a flask with a saturated solution of Schweizer's reagent at room temperature, put an oxygen filled balloon on top and let the solution on strong stirring for a few days. As the oxygen is consumed you need to either refill the balloon from time to time or have a pressure valve maintain the gas pressure at a few dozen millibars above ambient. At the end of this process you will end up with purple-indigo crystals of copper amino nitrite complex. Because the nitrite is covalently bound in a complex, oxygen cannot oxidise it to nitrate.
Liberate the nitrite with sodium or potassium hydroxide which will release copper hydroxide and ammonia then you can further purify it with silver nitrate if you feel it’s not pure enough.
The most nitrite you can make with this method is 1.25 nitrite per one copper but it takes forever because the second oxidation is fairly slow (weeks). However, getting one nitrite per one copper is considerably faster (1-5 days depending on room temperature, oxygen purity, stirring speed and the concentration of the solution).
"youtube, I am not making potassium niTRATE, im making Nitrite"
"So anyways, I bought Potassium nitrate on amazon for $20"
I chuckled at the comment that Nitrites are not used for energetics... Heh Heh...
When guns are legal, nitrates are the least of the problem I feel.
@@jianjieyap2010keep politics out of this bud.
@derekturner3272 shhh YT will hear you 😅
I laughed sooooooo hard
Re: longer format, love it. A+. Woild absolutely watch more in the future.
Thanks for the feedback, love to hear it!
Absolutely phenomenal work! Working from small scale to large scale, multiple runs, qualitative tests and titration? I'm not sure when was the last time I've seen someone be so careful and diligent in actually getting reliable numbers for their results. Keep it up!
Great video! Very thorough and easy to follow. Thanks for sharing! Also, I really like the longer video showing the whole process and would like to see more of it in the future. Keep up the great work!
What shakin' my brother?!
Thank you so much man! Love the feedback, always happy to hear that people are genuinely interested in the nuts and bolts of it all
Yes yes yes loving the longer video. This was a fascinating journey!
I'm pleased that you took up my method, which I found in an earlier German forum.
Unfortunately, here in the EU, calcium and magnesium nitrates are now also monitored, as are alkaline nitrates. Purchasing and possession are not prohibited, but the seller must report suspicious orders so that you can quickly be affected by a house search. Pure ammonium nitrate is completely prohibited.
Only heavy metal nitrates and barium nitrates are unrestricted in the EU. They are also difficult to get in Germany itself, so you have to resort to sellers in other EU countries.
Calcium nitrate can be made from calcium hydroxide and ammonium sulfate saltpeter, which is not monitored.
Overall, it is safer to buy nitrite than nitrate here in the EU.
Reduction methods are easier to carry out in porcelain crucibles than in narrow glasses.
The relatively lively implementation with formate is not a problem if the experiment is carried out outside or in a hood. The reaction usually starts after just under a minute and actually produces some smoke - but that's all. If the heating is stopped beforehand, the reaction remains incomplete. However, if you heat unnecessarily for longer, decomposition will begin. Nitrite solutions are also sensitive to air.
It helps to let the mixture of calcium nitrate and potassium carbonate solution sit overnight. This ensures that no potassium carbonate is left unreacted.
Recrystallization of the end product helps to achieve higher purity, but comes at a great cost to the yield.
It is probably hardly possible to produce analytically pure nitrite using amateur methods, but in the end any method is better than none at all.
As always thank you so much for the great info! I did figure the issue with the formate run was a matter of temperature control, I think in both cases I heated it too long considering the relatively high level of decomposition compared to the other methods.. same thing when I tried reduction by sulfur/carbon.
And yeah the test tubes sucked for the reduction, only really used them for visual clarity but they were a pain especially with the formate/oxalates that put off gasses during the reaction.
Also makes sense in the EU that nitrite would be easier to get than nitrite.. makes me wonder though, wouldn't a good source of nitrate in the EU be the oxidation of nitrite? The stuff certainly oxidizes far easier than nitrate reduces.
@@integral_chemistry
Yes, indeed... 😉
Its very valuable to see all of the "failures" here. While they failed to efficiently produce nitrite, there's a lot of things that happened that might be useful or useful to avoid for people trying other reactions.
Also, silver again. Its always silver. It would be nice if you could get from silver nitrate to nitrite in one step since they're so easy to separate, but probably not (without already having a nitrite salt, I mean).
loved this longer video. It honestly is something I'm going to use in the future as a chemist for reference videos on how to make these things and how to do it well.
Great work! Just to say, iodine reacts with the iodide ion in aqueous solution to form the triiodide ion, which is orange. That is likely the orange color you were seeing.
It can also do the same thing with pseudohalogen anions like nitrite, although the formation constants of such complexes are much lower.
Looks like hammerth beat me to it but yeah that's why I didn't claim triiodide (although yeah it was almost certainly triiodide lol) I just came across some literature on how nitrite can also complex to iodine and i wasn't exactly sure how favorable that complex was relative to triiodide (sounds like not very) Thanks for the info Reguardless! 😁
Loved the longer video!!! Content was very well made.
Cool always knew the CaSO3 method was the best, Wish you gave tips and trick for filtering the calcium sulfate. Love the longer video and the method for purification with silver nitrate.
Also i think(i may be wrong) that solubility of sodium nitrite/nitrate is not the same in alcohol(they are almost the same in water) so alcohol can be used for making the sodium salt.
edit: heating a strong oxydent with a combustible(alcohol) is probably not a good idea.
Yes, seeing the failures is useful! No need to test alternatives, if I know they do not work.
What a pleasure to watch man! Thank you for all the hard work, I would love to see more! For me this longer format was superior, I very much enjoyed the journey through all of the processes to finally end at a resolution. Just great man.
Hey, if you want an easy, fast way to get nitrite from nitrate that is pure enough to make alkyl nitrites (at least that), 1:1 sulfur to KNO3 ratio BY VOLUME, burned on a surface you don't care much about. Of course, you could do it stoichiometrically correct and get the pure product. I've got an eye for the nitrite via this method, and the best part is you can separate the waste from the product with water. It works. It stinks during burn, but it works. I was very surprised the first time. Nice video, as per usual. It's always fun to watch a contest. ❤
Hm ill have to give that a try. I actually did try a sulfur reduction but I cut it from the final video because it just made a big mess lol. I figured by burning the mixture I'd basically just have gunpowder and therefore reduce the nitrate all the way to nitrogen. Instead I tried indirect heating which just sorta melted it together into a rock-solid mass 😅
I'll update on how it goes!
@integral_chemistry it burns a lot like gunpowder, yes, but what happens is this puddle drips out and gets onto the surface of where you burn it (hence where you don't care what happens to the surface!) And when it cools it looks a lot like toothpaste, with weird colors in it: pinks, yellows even greens sometimes and of course where bubbles had been and burst little pock marks and craters. This will prove to be very hard like rock, but you can use a hammer and rather lightly tapping it to break off pieces AND will prove to be at least mostly nitrite. Works for any alkali nitrate, probably just as well for calcium, strontium and barium though I never tried. First time I made nitrite was accidental. I thought firecrackers were filled with blackpowder and I didn't have any idea at 15 years old that chemists go by weight, not volume. I had put 6:1:1(nitrate, sulfur, charcoal respectively) just like "Pyrotechnics" had said were in "Chinese firecrackers" , ending up with this grey powder that looked very much like what I saw in black cats. Lol was I wrong! My parents' driveway had a bunch of little stains all over it from me back then (we've moved, stains haven't). That was the first time I encountered those puddles that become seemingly as hard as cement. I didn't know chemistry yet, hadn't taken it in school (I was 9th grade then, turned 15 middle of that year) until 11th grade and then again in college. But frankly i learned so much more through hands on experimenting. I was scared away from organic Chem due to falling grades but have learned a decent amount through hands-on and RUclips as well. Anyways...
You can use plain old carbon if you don't have the sulfur on hand. Just remember to keep the ratio way off from blackpowder. With a 6:1:1 ratio BY weight, the nitrate is a smaller pile than the sulfur and even smaller than the charcoal, just for reference against my first pyrotechnical mistake, 30 years ago... your work on this was really inciteful. I like learning ways to do things.
I would love to see a follow up trying out these. That would be awesome if carbon alone works, if that’s what you’re implying.
@SetTheCurve absolutely, just need excess nitrate to charcoal, even by volume. 1:1 by volume will work, but you might burn off some of the nitrate like gunpowder burns. It's cheap anyways, so if you test it it will do exactly as I described. I didn't have a scale back then, we'll, I had a balance beam and I was underage to buy a scale and we didn't have cellphones (rich people did, and business people). Texting sucked, bc every number has three letters on it, so a text was super rare. It's one if the reasons older people don't like texting. Sorry, I digressed. I'm suggesting strongly to burn the two on a surface you don't care about. It looks like a burn stain looks when done, once you break up the toothpaste-looking cement-like nitrite puddle. Drop a piece into some vinegar, small piece, but bug enough so you can see the gas coming off. In a test tube you will see the orangy, rusty brown gas that is NO2 being made from the NO produced from nitrite reacting with acetic acid. Btw, if you only had a super small piece and can't see the gas, is the piece fizzing in the liquid at all? If so, then you got it. If not, then it's still nitrate. That easy, for real. All from a happy accident ☺️
In my quest to get Barium Nitrite, I settled on using Silver Nitrite as the intermediate as well for very pure product. I've had near 100% recovery of the silver after doing the double displacement to Barium Nitrite. I've also been using the CaSO3 route to reduce Barium Nitrate to Barium Nitrite via your reduction. I recently use a muffle to slowly ramp the temp with a close fitting lightly vented lid, which has resulted in much better yield. THat said, my use for the Barium Nitrite is not sensetive to Barium Nitrate contamination and it's acidified with HNO3 anyway. Great video! And if I didn't say it, thank you for the starting point you shared with CaNO3!
Thank you so much, I'm glad the video helped! The initial cost sucks but I do love silver salts for Displacement reactions because it really is so easy to recover the silver at near 100% yields.. as you said i do think barium is just a better choice overall for this process than calcium for a variety of reasons. It's unfortunately very toxic and less avaliable so I did skip it for this video but it's just so much cleaner than calcium for these replacement reactions.. might try your muffle idea at some point too
@@integral_chemistry I'm going to noodle the idea of using Barium Sulfite to reduce the Barium Nitrate. The point you made about it's lower decomp temp was the ah-ha moment. I will try to update you once I give it a shot. What's your view of the best path to Barium Sulfite? Are you starting with NaCO3 or CaSO3.
Nicely done! And I for one prefer the "long form" approach.
Good long video wasn't boring at all. A couple of these won't hurt anybody, just a couple of beakers, maybe. Thanks for the class!
Thank you for this long-format video!
This is great stuff man! You've just elevated your value as a chem youtuber with this addition. Also longer vids are cool. Nile red does them and as long ad they have a decent pace they don't bore. You balanced the information with process good too.
Great systematic work, yes please more of this! Worth every minute of watch time. Good and real content is rare.
Video is great but I am not satisfied. You didnt test reducing with starch. I made my nitrie in this way. I burned 400g of potassium nitrate with 80-100g of starch in a pan, then dissolved in minimal amount of boiling water, hot filtered. Evaporated filtrate to volume of 200ml and cooled. Obtained nice slightly dark crystalls, vaccuum filtered and dried in dessicator bag over CaCl2. Yeild was around 30-35%. Purity is questionable but I succesfully used this for diazotation. Maybe you can test this method too? I want to know the purity of nitrite obtained by this method.
Absolutely, and cheap charcoal if done right is even better, superior actually. Sometimes im getting filling that such videos are to make it feel like its impossible to synthesize like his video about TNT for example... Anyway for -NO2 use charcoal, for TNT just type "Dug TNT" in youtube search and you will be satisfied. NBothing is complicated.
"that's what she said" 😉😁
Great example of analytical work.
This was a fantastic video.
(Although it looked like a lot of work.)
That looked like a praseodymium salt at the end.)
I like the long video format very much, also because it adds a lot of educational value to your content. I wouldn't want shorter videos to completely go away though. Maybe you can switch back and forth, depending on the project? That would be the best of both worlds.
Very happy to hear you liked the longer format! Tbh I don't think I'd even be able to make videos this long but once every few months so no worry about the shorter ones going away. Do love the idea of making these videos that capture the actual process like this one more often as well, sure I'll eventually strike a balance
Enjoyed the longer video!!
After the preliminary testing I started supporting calcium sulfite like it was sports team lol
Its nice to see it won in the end
Dude, the amount of work here...legend.
Amazing work !
Really big project and massive work, trenscendent!
“Footage from future video:”. Shows forbidden lime jello. Yum yum. Anyway, YES. I like the longer form videos to see multiple ways and processes
Awesome work. It's getting harder to find NaNO2 in a lot of places.
Tell me about it.. although someone in the comments here was able to find a 500g jar on Amazon which is wild to me. Might grab it while I can
@@integral_chemistryAmazon doesn't care at all about the regulations, as long as nobody calls them out. They can't go after Jeff Bezos as he's basically a dystopian deity above any mortal law. You can still find 90% sulfuric acid on amazon while is banned everywhere else in the EU. I've seen substances that I won't name that can be used as extremely toxic chemical warfare agents being openly sold on amazon. Stuff is crazy.
Awesome thank you for your service to this community you are appreciated 🙏👍
Did your ferric oxide filter nicely or was it a pain? Amazing video, best you've uploaded so far, please keep up the good work.
OMG THANK YOU so much it is so complicated to find nitrite, and I didn’t know where to start.
Excellent work. Very very scientific approach, really appreciate the work! Just a quick note - silver salts (or any heavy atoms) have a tendency to explode with some organic compounds (fulminates, acetilids, picrates, etc...). I am not so sure if you cannot run into trouble with using AgNO2 in diazotation...? I have not checked lit I am just thinking out loud. there is HCl, so in theory all will crash out as chloride and should be safe. But then again that could also take down your product and you might lose yield? I always did diazotation with sodium salt and then converted the diazonium salt to BF4- for stability...
Also on a different note, I don`t know how this is in US, but here you can buy so called "butcher`s Salt" for meat curing. It contains 0.6 % of NaNO2 - it is not much, but then again, 1 kg costs less than a dollar. so in theory purifying 25 kg (costs 11 dollars here) of this could give you like 125 g of nitrite. there is also no KNO3 so the only impurity would be NaCl, but that should be easy to rid off.
Really useful information here for those of us needing nitrites for synthesis! Love the longer videos bro. Sorry to hear bout the Patreon what happened? Hope it gets resolved and everything works out! 💯🤞🏼
Thanks a ton man! I had felt it'd been a while since I made a video on a practical process, and very happy to hear lots of people seem to have gotten at least something from the video. And yeah Patreon thing really sucks, definitely helped having a steady stream of revenue for misc lab supplies and such. Definitely update when I hear back
Thank you for this! I'm going the CaSO3 route, and made a bunch of Ca(OH)2 via CaCl and NaOH to start, but thanks for pointing out i could have just been a little smarter and done it in one step with the Na2S2O5.
Glad you found it helpful, and lemme know how it goes! Another quick tip: you can buy calcium hydroxide from nearly any grocery store and it's a lot cheaper than sodium hydroxide or calcium chloride. It's sold as "Pickling Lime" usually near canning supplies
That was a cool video I appreciated it ! More video like that would not be too much 🙂
Hi! Nice video! I have an idea. When I was student, they gave us to make some complexes in inorganic chemistry lab classes. I got to make potassium hexanitrocobaltate(III). Procedure was simple, just take some Co(NO3)2 disolve in water and add six time more (in mols) KNO2. After that, I bubbled oxygen through solution and precipitate of potassium hexanitrocobaltate(III) started to form. Also, you can speed up the process by using hydrogen peroxide. After some bubbling, I filtered the suspension and I got nice yellow powder. I remember that I got almost quantitative yield. Here one cobalt binds with six nitrites (via nitrogen atoms), much more than silver in silver nitrite. Also cobalt nitrate is cheaper than silver nitrate. I think that you can somehow destroy this complex and get potassium nitrite in solution. I had an idea to use hydrogen sulfide for this. In suspension of potassium hexanitrocobaltate add three times more potassium hydroxide (in mols) and bubble excess of hydrogen sulfide. Cobalt should prcipitate as CoS and there will be some elemental sulfur from oxidation of H2S by Co(III). In solution will remain only potassium nitrite. After, just separate precipitates from solution. I think this could work. Only downside of this potential method is toxicity of H2S and cobalt salts. Anyways, I hope you will succeed! Greetings from Serbia!
Very interesting. Thank you for your diligence and patience. I wasn't aware of the federal ban on nitrite since I was able relatively recently (about 1.5 years ago) to purchase a considerable amount of it from a well-known OTC chemical supplier. But it looks like it happened soon after that... In any case if I ever run out of it (which will likely not happen) now I know how to make my own, and I am grateful to you for that.
Exelent work and production.
Very impressive once again. I was wondering if part of the nitrite doesn’t reoxide to nitrate at high temperature, making the process less effective. Why not try heating under inert atmosphere? Also why not try sodium hydrosulfite as the reducing agent? EDIT: I’m dumb. It would be impossible to separate from the product.
Oh and BTW, I recently found out how to make methylene blue. No really complicated, provided you have N,N-dimethylaniline that you can make from aniline and methyl iodide (or buy).
EDIT: On second thought, maybe you should’ve activated zinc by immersing it in hydrochloric acid for a short while. I’m going to test that tomorrow at microscale in aqueous medium. As far as I remember, all reductions with zinc begin either by washing the powder in HCl or adding a catalytic amount of copper sulphate, which must have the same effect.
EDIT 2: Reduction of potassium nitrate by zinc in water works. The zinc has to be clean (powder, rinsed in hydrochloric acid and washed). Mix the nitrate in solution with the zinc → nothing much happens. Add a catalytic (in my case, a few crystals are enough on a ~100 mg scale) amount of copper sulphate and bingo! There is instant formation of a white layer of zinc oxide and the solution definitely contains nitrite as it turns a potassium permanganate solution colourless.
The “dumb” method mentioned first may not be as stupid as advertised if the source of NOx is a birkeland eyde reactor. The purity of product and simplicity of the process may make it worthwhile.
That's a good point^ I do think the complexity is building the reactor to begin with. Seems a prohibitive process (although I've never tried myself)
If you could get it to work though yeah 1000% that would be the best method, basically infinite free nitrite or nitrate at that point.
Worth looking into for sure
@ Great job on this video, btw! This has to be the most informative one so far on an essential lab chemical.
silver nitrite in itself useful for victor meyer reactions to form nitroalkanes, or for halide substitutions in general. i would reserve it for that purpose alone considering how expensive silver is, which makes sense since the organic syntheses that require pure nitrite usually convert it to isopropyl nitrite instead (thereby purifying it).
inorganic chemists might be out of luck though. i doubt i would appreciate nitrate or silver contamination in my nice metal complex crystals 😅
With regards to the formate method: I think the violent reaction is required. I did try lower heats (just above melting point of KNO3 like 330 degrees) with longer times and there was no nitrite.
Once the reaction kicks off, an air quality monitor shows a small amount of carbon monoxide being released but not a dangerous amount. There is a strange odor and a lot of smoke so do it outside. The temperature when the reaction starts is probably around 350-400 if I had to guess. I did many small runs (35g KNO3) using porcelain crucibles on an electric stove with foil insulation which worked fine. The reagents do not need to be especially well mixed or dry for the reaction to work. pH of diluted extracts is alkaline so some over reduction is certainly occurring.
For the lead method, SM members say tin can be substituted for lead.
Very good video interesting methods for producing the potassium nitrite just 2 comments here first I think you meant to say iodine precipitate not gas the second is potassium nitrate according to Wikipedia is NOT very hygroscopic! I think if that does occur is because of small amounts or traces of sodium nitrate which is extremely hygroscopic in the same way pure sodium chloride doesn't cake only because of impurities like magnesium chloride in commercial salt.😮😅
Thank you very much! And yeah I did kinda misspeak there, I meant to say triiodide forms along with solid iodine which is partly vaporized by the very exothermic reaction 😅 and really not hygroscopic? I'd actually not heard of this phenomenon. Is it kind of similar to a eutectic mixture? Come to think of it, it was honestly just all the potassium hydroxide byproduct lol
Edit: just re-read your comment and I might have misspoken in the video 😅 i meant to say Nitrite is hygroscopic, nitrate isn't (which is partly why it's so useful)
@integral_chemistry you're very welcome I am just so amazed you have difficulties there getting the nitrites? Here in Australia not so hard as our Government agencies not cracking down on that.Except of course on Ammonium nitrate! Which you can't buy here. Ever since the 911 attacks there.Is it just the potassium nitrites? I bought 2 packs on eBay of sodium nitrite 500 g each 99.95% purity. I am jealous as you can get so many things there! We can't get Here 😞🥺perhaps we can exchange ideas?
I’m wondering if another way to purify it would be to use the crude nitrite to make an alkyl nitrite and purify that and then convert it back to an alkali nitrite
I think you're onto something. Isopropyl Nitrite production is not sensetive to Nitrate contamination in my understanding. The only hitch I see is the low-ish yield of Isopropyl Nitrite and the resultant losses related in the conversion back to an alkali metal salt.
@@derekturner3272 well that is bound to happen when performing a purification but in this case it might be too much to be worth it
I might be totally wrong here but I think NurdRage gave this exact process a try a while back and I think I remember it failing somehow. I'll have to try and find the video but what you're describing sounds oddly familiar (and should work on paper i feel)
@@integral_chemistry I've got a procedure that states that mixing ethyl nitrite and NaOH in ethanol and leaving it be for two days gives somewhat 90+% NaNO2. No quantities are mentioned but something worth looking into. Secondary alcohols like NR tried may not work great
@@integral_chemistry yea I thought I vaguely remembered someone either trying it or at least proposing it as an option but I didn’t remember who
I like the long-format video, but it really depends on how much free time I have. I think a mix of video lengths would be decent.
Longer content showing the learning process you went through sets more realistic expectations for what someone should expect in real world chemistry, as opposed to textbook lab experiments that “should” work every time.
Seeing your persistence makes it easier to deal with setbacks instead of giving up. A 15 minute video wouldn’t have done this research justice.
Possibly, another route would be the copper II catalyzed, electrolytic oxidation of ammonia. Depending on the voltage and reaction conditions (anode material used, temperature), the process can be tweaked to make nitrate or nitrite. I have yet to get it to work though. Such a route would be welcome for European folks due to the strict regulations making it difficult to buy compounds containing those two anions.
I believe there is a patent out there for membrane assisted electrolysis as a method of oxidizing nitrate to nitrite with high purity. I’m a little surprised it hasn’t been attempted on RUclips yet.
Scrap Science tried the electrolytic nitrate synth and it worked, but was low yielding.
@@chemistryofquestionablequa6252 oh, right- I saw that. Apparently there’s a way to make nitrite from nitrate, however. I haven’t seen that done yet
@atari7001 I hadn't heard of that, I'll have to look it up. Thanks for the heads up about it!
Apoptosis (Some day before): Too busy to watch videos longer than 3 mins.
Also Apoptosis: A 42 minutes video🤣
Got to bookmark this and watch it on TV later.
LMAO yeah that is a literal quote of mine 😅 I do struggle with the ole' attention span in front of a screen.. I think making this video took years off of my life tbh.
Lemme know what you think when you get around to watching!
@@integral_chemistry This video is indeed very informative and it took me another day to finish it!
I am not a big fan of solid-solid reactions, but the one with calcium sulfite seems solid! (No pun intended), so I guess I will employ that method as well when making nitrite.
The purification part is also very nice, and I would prefer this kind of longer format.
Late to the party but happy to be here. Lets go
Is there any significance to crystals forming at both the top and bottom of the beaker at 26:57 ?
Longer is great
Is the Forbidden Baja Blast caffeine free?
Would it be possible to react the final silver nitrite with sodium or potassium chloride to obtain extremely pure sodium or potassium nitrite while precipitating extremely insoluble silver chloride?
3:48 wait. Is this why I can’t find this on the grocery store anymore ?
I used it all the time for jerky back in the day
Does residual sulfite affect the permanganate titration?
Yeah residual sulfite would definitely react with permanganate. I doubt any would survive the heat, though, even if it didn't react with the nitrate. Can always precipitate residual sulfite/sulfate with barium nitrate just to be sure
@ my first thought when the sulfite performed significantly better than other agents was that some of it made it through. It might be a good idea to cook sulfite without the nitrate just to see how even/consistent/complete the decomposition was. That said, you’ve obviously thought about it a lot more than me 😅
Appreciate the detailed breakdown! A bit off-topic, but I wanted to ask: I have a SafePal wallet with USDT, and I have the seed phrase. (alarm fetch churn bridge exercise tape speak race clerk couch crater letter). Could you explain how to move them to Binance?
Can i use this for sugar rockets?
when i was into salt water fish tanks back in the day the negative byproduct of living biomass in a small closed system was nitrites & nitrates....a build up of these would result in a die off in the system. i wonder if that is an option for obtaining nitrites?
I used to have a reef tank too. If I remember correctly, nitrite was even more toxic than nitrate. I'm guessing it's not a suitable way to produce them because they were measured in ppm.
The concentration is way too low to be useful while still being high enough to be toxic. There's a concept to use the buildup of nitrite and nitrate from aquaculture to fertilize plants, but I don't think that was ever developed beyond early experimentation.
Why do not use sulfur as reducing agent ?
I was never able to get it to work without a big unworkable mess or huge impurities (like it the formate run but worse).
I think it may be a matter of tighter temp control, certainly feasible but so far not much luck on my end
3:45 Nitrate or Nitrite?
It should say nitrite.. only pic I could find to illustrate the difference lol
There is also the aqueous reduction of nitrate with freshly precipitated lead sponge, i thing poor man's chemist made a video about it.
0:52 I'm getting my coat 😆😆😆
Would the reaction also work, if you would heat up KNO3 with a formaldehyde solution to form the nitrite and formic acid ? Or even just heating a KNO3 ad ethanol solution although the solubility is low of he crystals.
No.
IMO, errors and failures are just as important and educational as successes.
@1:11 - What are they going to do next - take down my videos about processed meats and gout? For frog snack!
Probably. Nothing would surprise me at this point 😅
Is this not a decent target for an electrochemical process?
I do certainly think that could be feasible, whether by some divided cell or a deviation of the partial electrochemical oxidation of ammonia. Either way I haven't tried it but I'd love to in the future!
Please make a video on
Making potassium nitrate kno3 pure 99%
I can try, only worry is youtube taking it down.. they don't like nitrates lately
@integral_chemistry yes but I'm making potassium nitrate
This method
Potassium carbonate add in nitric acid
After that add water and freez it
You can get a crystal purest potassium nitrate.
Thank you good sir. I have been looking for a source of this reagent for awhile. I suffer from government the same way you do so buying it isn't an option.
How about bubbling CO2 to convert the hydroxide to the bicarbonate and then precipitate it?
+1 on the long form content
Apoptosis OF in bio when?
You should mess with fluoroantimonic acid or hydrofluoric acid next
Please make a similar vid about iodine. I have 2 pounds of sodium iodide and I wanna make myself elemental iodine and tincture I can use. Here's the problem: we cant buy 30% hydrogen peroxide in the EU. I can buy potassium nitrate tho and HCl. How do I react those to be able to get iodine out of a solution? It didn't work the last time so I added a pool oxidizing tablets. What I ended up with is a brown mixture of HCl and possibly nitric acid. Total waste of my iodide.
That could be a cool video! Although it might take me a while. If you wanna get started sooner I do know how you could get pure iodine with what you have. Simply set up a chlorine generator by dripping the HCl onto the chlorine tablets (obviously dangerous) and feed the gas into a solution of iodide. The chlorine is more reactive than iodide so it'll displace elemental iodide. Alternatively a safer option would be to use persulfate which can easily oxidize iodide to iodine and should be available in most countries. Also 3% peroxide will do a fine job in a pinch, 30% is honestly overkill
@integral_chemistry Yes persulfate tablet it was. But it didnt precipitate as I expected so I was not able to filter it out. And then there's unbeknown to me sulfur contamination. Maybe it was too acidic or something like that. It seems simple in videos and then it doesnt work out. I'll try the weak, 10 times more expensive peroxide thanks.
@@trollmcclure1884 Hm, surprising the persulfate didn't work.. Perhaps the tablet itself was impure. You could also try dissolving it and filtering any solids before reacting it with the iodide. Another thing is that iodine will react with excess iodide to form soluble triiodide, so you might just not have used enough persulfate to get a sufficient oxidation.
And yeah.. peroxide is somewhat expensive, but because a mole of peroxide is so lightweight compared to iodide it shouldn't take much. One final thought: See if percarbonate is available to buy where you are. Very cheap and generates peroxide when it dissolves in water.
@@integral_chemistry percarbonate sounds good. Thanks!
@@trollmcclure1884 You could always just buy iodine. I don't know where you get your peroxide but you should be able to get 10 L 12% for 25 €
Super
With the lead method I keep envisioning molten nitrate over a puddle of lead. Or maybe tin as a substitute. And just like, stir it somehow.
I watched the whole thing. It was longer than expected.
Yeah, low concentrations of Iodine in water look orange-ish. Higher ones look brown. I2 dissolves as I3- in the presence of additional iodide.
Second
Organic Chemistry is amazing and is also political unfortunately. ❤
Very unfortunate :/
I'm confused how in the beginning of the video when you started talking about nitrite salts, you said something about how nitrites can cause methemoglobinemia, which is usually rapidly fatal, but then you also said that in specific forms, the nitrite ion is also useful in blood pressure medications. Huh?
NitrAte ions NO₃- are strong oxidants which transforms the ferrous (Fe²⁺) ions present in haemoglobin into ferric (Fe³⁺ ) ions which are incapable of fixing oxygen, given that they are in their maximal oxidation state (methaemoglobin). NitrIte ions (NO₂-) are metabolised into nitrogen oxides which act as strong vasodilatation agents (they relax veinous wall tissues) which leads to reduction of blood pressure. This is also why azides are poisonous (inter alia).
Yknow, I don't think amyl nitrites are primarily used for the their intended medical function
I think you may be onto something there 👀
im sorry for contributing to the ban of nitrite
Why don’t you just purify curing salt ?
I suppose you could, thing is though curing salt is 0.5-5% sodium nitrite and I'm not really sure how you could selectively extract it from all the sodium chloride.
Guess you could remove most of the chloride using lead nitrate
Since when can you not get Nitrite in the US? Pretty sure you can get 99% from some online bait shops
Nicshe
Its not even a thing you can use to wake you from the computer simulated world.
You and "your" dangerous content are not welcome on patreon... apparently.
I say "your" because chemistry belongs to noone, it simply is what it is.😊
Yep that's always been my point! Certainly the only field of science that we as a culture routinely criminalize
@integral_chemistry on a long enough timeline, all actions become illegal. Even life would be illegal as possible threats are "removed."
For example, murder is illegal. Has been for some time. How many other laws have been created to attempt to curb the already illegal activity. Eventually, taking a breath could endanger the O2 for someone else. It's a vicious, self consuming circuit... or network, which is possibly a more accurate description.
RUclips: Posting videos of Ukraine war and various improvised drone drop loads
IS OK
ALSOl RUclips: Absolutely NO Chemistry you can learn on one Page of wiki.
HUMANS: Dafuhk?
First
You are unnecessary complicate it. Carbon is superior in every aspect.
CaSO3 method is purer and better yield, but I would have liked testing carbon method as well
@@7hunderstorm242 I have experience with Pb, -SO3 and C method. Highest quality is from Pb, -SO3 is low quality because contact will never be intimate enough, and -SO3 are not so cheap per unit mass, carbon, if done right has acceptable quality and is cheapest of them all, so easiest and cheapest method
I would appreciate longer videos
Easy way: Go buy a bag of 11-0-44. Done!
Good for surface hardening in the molten salt but.. en.wikipedia.org/wiki/Potassium_nitrite