Apoptosis - 2024-11-30
In this video I discuss the science and uses of nitrite compounds, and then test 7 different methods of making potassium nitrite. These methods are tested for purity and percent yield via an array of qualitative and quantitative tests, and the most promising methods scaled up to try and create a meaningful quantity of usable potassium nitrite. I also include a final purification step to clean any crude nitrite salt to 100% Purity. This is by far my longest video, and it kind of had to be given the complexity of the tests and analysis. I have heard though that many of you prefer longer videos in general, so leave a comment if you'd like to see more long chemistry videos like this one! NOTES: I also tried carbon and sulfur as reducing agents, but did not include them as they were both unreasonably difficult to clean up into a usable final product. This is because both carbon and sulfur are almost TOO good at reducing nitrate, and I ran into the same issue I did with the calcium formate where there was just a huge amount of byproduct and a violent decomposition. Additionally, ultrafine carbon requires celite filtration to remove completely. That said, both of these methods work (and are probably the cheapest per unit of mass) so definitely worth considering if the additional impurity isn't an issue. Also, I forgot to mention it in the video, but silver nitrite is a fantastic intermediate for the synthesis of any other nitrite salt. Simply react any chloride salt with the silver nitrite and you'll be left with insoluble silver chloride along with the nitrite salt of whatever cation held the chloride. Join this channel to get access to perks and support my work: https://www.youtube.com/channel/UCw8axYTp2BtinEmM_rdzUjQ/join CHAPTERS ____________________ 0:00 Intro 1:43 Why Make Nitrite? 4:30 Systematic Procedure 5:32 Running 7 Methods 12:57 Extracting Nitrite from Reaction Matrix 14:27 Titration for Quantitative Results 18:51 Qualitative Tests 20:55 Bulk Synthesis of Top Performers 28:16 Analysis of Final Potassium Nitrite 33:34 Purification to 100% 37:25 Future Ideas and Lab Notes ___________________________________________
"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... <.< tetrazoles anyone?
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!
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
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!
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.
Yes yes yes loving the longer video. This was a fascinating journey!
OMG THANK YOU so much it is so complicated to find nitrite, and I didn’t know where to start.
Loved the longer video!!! Content was very well made.
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! 😁
0:55 gotta chime in, nitrites can be used to make energetic compounds, my favorite being methyl nitrite (CH3ONO) (a sweet smelling, corrosive, gaseous compound with decently energetic tendencies depending on the concentration)
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" 😉😁
What kinda of starch
Thank you for this long-format video!
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!
i love how youtube cares more about you making the easily available chemical you can buy in 25kg bags more than a much less common nitrite
Love the long form. More please.
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!
Yes, seeing the failures is useful! No need to test alternatives, if I know they do not work.
Nicely done! And I for one prefer the "long form" approach.
Great systematic work, yes please more of this! Worth every minute of watch time. Good and real content is rare.
Nice.
Both long and short videos are useful.
Best is the long video that starts "with the short video" running thru the conclusions with all the notes needed to replicate the experiment.
This has the dual benefit to be actionable as well as it is a primer making it easier to follow the following process.
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 YouTube 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.
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.
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
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.
Dude, the amount of work here...legend.
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.
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.)
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
“Footage from future video:”. Shows forbidden lime jello. Yum yum. Anyway, YES. I like the longer form videos to see multiple ways and processes
Really big project and massive work, trenscendent!
Awesome thank you for your service to this community you are appreciated 🙏👍
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.
I much prefer seeing every step lol. I like longform videos.
Great video! Have been trying to get nitrites for a while
I love listening to you!! Thank you for your knowledge ❤🎉🎉
Very good video I must say. The length is not an issue if there is useful information shared .
Sodium Sulfite works as well except that the temperature must be controlled more carefully (around 500 ) so you don't get a runaway reaction . That will reduce the yield (normally within the 65-80% range) by probably 15-20 % .
Again, nice work 👍👍👍👍
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 🙂
Thank you so much! I really appreciate the feedback!
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
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.
Exelent work and production.
Amazing work !
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.
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.
Is there any significance to crystals forming at both the top and bottom of the beaker at 26:57 ?
who are you and why do i love hearing you talk about things that are currently beyond my brain............. carry on
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.
@NurdRage - 2024-12-01
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.
@TechGorilla1987 - 2024-12-01
Uh oh. You have summoned a YouTube God.
@integral_chemistry - 2024-12-01
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
@Techpriest1010 - 2024-12-01
Relax...... your smooth muscles
@seditt5146 - 2024-12-02
@@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.
@cezarcatalin1406 - 2024-12-03
@@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).