Lab Notes - Making Oleum - Successful - (April 21-2024)
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- เผยแพร่เมื่อ 27 ส.ค. 2024
- These are my lab notes trying to make Oleum or Fuming Sulfuric Acid by amateur means.
Turns out it is possible to do it with just a ceramic hotplate, sulfuric acid, and sodium bisulfate. Along with standard laboratory glassware. But so far the yield is around 13%. I'm trying to optimize it.
The procedure is simply heat the sodium bisulfate on the ceramic hotplate and pyrolyze it until it becomes sodium pyrosulfate. Then let it cool and add in sulfuric acid. Distilling it again yields sulfur trioxide.
Previous methods require much higher temperatures to pyrolyze the sodium pyrosulfate directly.
Related videos:
Purification of Sulfuric Acid by Distillation Revisited: • Purification of Sulfur...
Lab notes - Making Oleum - Success (part 1): This Video
Lab notes - Making Oleum - 20% yield improvement (Part 2): • Lab notes - Making Ole...
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Update: I've been able to get the yield up to 22% in my latest experiments. So i'm still working on it.
Question: why are you making oleum? Some interesting syntheses coming up?
@@warmonger12z No special reason really, just wanted to take on the challenge. I didn't like the existing methods that were too hard, or too dangerous, or too expensive. Maybe i could contribute to the amateur literature and making it accessible with relatively modest equipment.
@@NurdRage fair do's
Not too shabby for doing it by ear, actually. I would be a bit concerned if Oleum concentrate is quite high as it's potentially possible to ignite anything organic like what fuming Nitric acid do. As for explosives like gun cotton, Oleum is basically like extra Sulfuric acid for free, so you won't need too much Sulfuric acid to make it workable. (And I definitely don't recommend doing so - I have done Nitroglycerin as it's stupid easy to make it so I knew the risks in making it, so again, don't do it unless you know safety rules, it's strict for a good reason - still it's kind of hilarious that this exact explosive is useful, even in medical settings - they are naturally desensitized, it's usually used for heart attack prevention).
man that stuff looks scary lol
Amateur chemistry always seems to take a healthy step forward when NurdRage uploads! Great work as usual, I'm gonna have to try this at some point once you've perfected the procedure!
Absolutely!
I think it's funny to watch NurdRage's dioxane video and hear him say "it's hard for the amateur to get elemental sodium" and think "you're wrong!"... When it is NurdRage that made it so much more accessible.
LabCoatz, I also need to start supporting you (and a few others) so I can have my name at the end of other videos that represent legitimate advancements in amateur chemistry like this one.
Hopefully one day I'll figure something out that is worth sharing, but thank you both for being gems in the wonderful ecosystem of TH-cam amateur chemists!
True.
Extractions&Ire ain't bad either
The donated hot plate comes to the rescue again! Yeah!! 🎉
What if you take e.g. frying pan, fill it with sand and put glassware on that....and continue with regular kitchen hotplate....then hotspots should not be an issue
@@great__successit works, but doesn’t have stirring and a lot of cooking hot plates and electric frying pans don’t give constant temperature. They turn on and off to stay within a temperature range.
@chemistryofquestionablequa6252 Induction cook tops, including the portable ones don't use PWM and offer a much more consistent temperature range. Or in some cases they do, but the on/off times are varied by milliseconds over the course of a second, like LED diming, which is essentially constant. But either way, if you have a lot of thermal mass from sand and a cast iron pan, the temperature fluctuations should be smoothed out
The tried and true amateur approach of using a gas torch can also be effective for reaching high temperatures
@@Spencergolde Induction most certainly DOES use PWM. I've got quite a few and at lower temperatures the on/off timing can be anywhere from 2 on 10 off to 5 on 2 off. It's only once you get up above a medium setting that they use amperage control to vary the output. They also can't regulate the temperature of the pan or contents by degree, only by the glass temperature where the pan is contacting it. Induction also has the same issue of not having magnetic stirring, which is necessary when dealing with solutions that are prone to bumping.
You’re really pushing the limits with what can be done as a home chemist! Thank you for the inspiration NR ☺️
An old friend of mines dad had a sulfuric acid plant next to this big oil refinery... we were taking and he said they made tanker cars of "Oleum".. He told me they had a leak of oleum gas one time and most of the workers cars in the parking lot got "Frosted"..
Oh no
There's trains full of this stuff? That's a bummer lol
Great to see you making videos and well excplained!
+feeding the hungry algorithm
Your video's are way more better than my chemistry class
i absolutely think you are just that good and worth the support. i just dont have the funds to hardly support myself or i would absolutely hand it over like fry from futurama much love bro thanks for helping me learn so much i wish i could somehow get into chemistry as a job. ive never even taken a chemistry class at any point in my life and i feel like i know so much thanks to you and a few other incredible chemist youtubers
A fun reaction I've used Oleum for was to brominate the bay carbons of perylene TCA, which forces a twist on the molecule. It resulted in a beautiful brightly fluorescent, dichromic solution in DCM and was the first step of a more interesting synthesis. It was a simple step using Oleum as a solvent and Aluminum Bromide as the brominating agent.
I hope nurdrage trys this. It sounds pretty cool ! 😎
You, sir, have a talent for filling voids in the common-chem knowledge-base. Thank You Very Much for this and all your work. Our knowledge is our greatest treasure.
If my 8 grade chemistry teacher was half as skilled at teaching as NerdRage I would probably followed that line of education and became a real chemistry lab worker.
This is a huge breakthrough even with the yield. Great job as always, looking forward to seeing how far you can take it.
I love your lab notes videos. I started watching your videos when I lost my lab after college about 14 years ago, and it made me feel like I was still in the lab doing what I loved. 14 years later, I'm almost financially ready to invest in equipment, and you're really putting a hotplate under my flask about it.
Just feeding the insatiable monster that must be fed. Amazing video as always.
I wish I'd had a teacher like you when I took my old chemistry course. Maybe I'd have pursued it as a career. Either way, love seeing how much effort you put into making them processes available outside professional labs (with proper safety measures in place)
this is awesome!
been watching your channel for maybe 16 years now, still my favorite chemistry youtuber
Same here. He didn't turn into a commercialized annoying parody of himself and I respect him for that.
Something many people were waiting for
these are my favorite kind of videos.
When I was an undergrad (late 70's) it was also "somewhat infamous in chemistry for being one of the key precursors" to a visit to the student health clinic. Even the cocky A+ folks obviously treated this stuff with great respect.
wonderful, love the update doc. thanks for this. i can't wait to see the optimized procedure you decide upon.
your series on nitric acid was phenomenal and indispensable to hobby chemists and professionals alike. i used your instruction to make WFNA to post a demonstration of the dangers of various chemicals versus various common forms of laboratory gloves/PPE. i've made chloroplatinic acid, azeotropic HBr, and sodium metal using your procedures and regularly utilize the products of those efforts in my own research.
you are the patron saint of hobby chemistry and one of the most brilliant, humble, honest (in critique of your work and your own errors, even though your errors are almost always ones any chemist would consider excusable), and never cease to keep the average hobby chemist in mind in all you do.
thanks for all you've given us over the years, doc. seriously. you are one of the reasons i'm now a professional degree-holding, not-enough-money making chemist today.
we love ya, NR!
Love seeing a new NurdRage video, especially when you are exploring new territory.
as always, ameture chemistry makes another massive step forwards, all thanks to this man
Thank you for this birthday present one day before my day
Good to C U back man.
Love the news
Ya sold me on building a Stainless steel fume hood as well as building in a scrubbing system so the trees around my lab don't get fried 👍
Sweet video!
terrifyingly fascinating
well done sir
You do great research-grade videos.
I'm thrilled! Keep us updated, this is interesting and innovative. Thanks!
You are so amazing, NurdRage!
Thanks for the chill videos
Always a pleasure to see your lab notes.
Dangerous stuff, but utterly fascinating. A catalytic process to separate water and sulphur trioxide.
Ive always wanted to see the old way of making sulfuric acid the destructive distalliation of iron sulfate. I know this isn't it but it would be a fun project to consider
Yery nice. This is (essentially) the method I've used since around 1990. I melt the bisulfate in a refractort dish used for moneral assay, then pout it out into a cold slab of aluminum (thick) to solidifym then break it up into chunks. From there, add to 98% H2SO4 and disyill as you did.
Adrian's lab (YT aka Plastic Raincoat) had a nice video on S03 quite a few years back, before his cool lab got destroyed by robbers, so sad. The video is still on his current channel Adrian's Chemistry Lab. He generated 02 (wet method) then passed the dried 02 over some burning sulfur then over heated platinized asbestos. If I recall the heating was only need to start the catalytic reaction. I would certainly want to make it a negative pressure draw through system with a sodium carbonate quench at the end of the line after the Oleum receiver (cooled).
Chromium oxide is a viable catalyst in place of platinum during oxidation steps. Ostwald nitration is one example of this, and a quick google search suggests that it also displays good activity against SO2.
You never dissappoint. Great stuff!
Thanks for good video
Great work as usual. Will follow and await further developments.
Boom ! Y'all Know when NurdRage is in da Room ! Oleum ! Hot Damn (literally) !
Superb work Nurdypants, as always :)
Somewhere in what i laughingly call "my mind" there's a thing about ferrous sulphate pyrolysis and oil of vitriol.
For a new procedure, any yield greater than 0% is a success
Really respect your channel. You are 100% the same as the beginning. You do what you love for the love of it. NileRed for example just makes stupid reactions in his super pompous useless lab. he became just a youtuber instead of a true chemist. you are a true chemist.
NurdRage, those synthesis videos are amazing and incredibly useful.
I feel much of the stuff you put on TH-cam would also deserve to be made into scientific papers. (Like your menthol-catalyzed sodium synthesis, for instance).
You would think all would be said and done about the preparation of such basic chemicals, even on a small scale. Yet you manage to significantly improve existing methods!
Acid videos are amazing. Yours is the best channel on TH-cam
YEARS AGO I SAW BATTERY ACID COULD BE CONCENTRATED BY BOILING. WHEN IT STARTED BUMPING I ADDED PYREX CHIPS IN A DRIVE BY FASHION. NICE VOLCANO, LEARNING THE HARD/WRONG WAY. I BUY DRAIN CLEANER NOW AND FOLLOW THE GOOD DOCTOR'S SAFTY ADVICE, OOPS.
*Abstract*
This video documents NurdRage's successful attempt to synthesize oleum (fuming sulfuric acid) using a modified pyrosulfate method. The experiment utilizes readily available materials such as sodium bisulfate, sulfuric acid, and a ceramic hotplate, eliminating the need for extremely high temperatures or exotic chemicals often associated with oleum production. While the achieved yield is around 13% [according to more recent comment 22%], the process demonstrates the feasibility of creating oleum through accessible means, opening avenues for further optimization and exploration within the amateur chemistry community.
*Summary*
*Safety Precautions and Introduction (**0:00**)*
* 0:04: Oleum is highly corrosive and carcinogenic; proper safety gear and a fume hood are essential.
* 0:29: This video explores making oleum with common chemicals and a ceramic hotplate.
* 0:50: The initial yield is approximately 13%, leaving room for improvement.
*Understanding Oleum (**1:08**)*
* 1:08: Oleum, also known as fuming sulfuric acid, is sulfuric acid with added sulfur trioxide.
* 1:17: Its fuming characteristic arises from the high vapor pressure of sulfur trioxide.
* 1:32: Oleum's potent dehydrating and sulfonating properties make it similar to boiling sulfuric acid at room temperature.
*Traditional Synthesis Methods (**2:25**)*
* 2:25: Common methods include the pyrosulfate, phosphoric acid, and tin sulfate methods.
* 2:34: The pyrosulfate method involves heating sodium bisulfate or persulfate to release sulfur trioxide, but it requires high temperatures exceeding 600°C.
* 3:06: The phosphoric acid method utilizes polyphosphoric acid's dehydrating properties but risks damaging glassware due to high-temperature reactions.
* 3:40: The tin sulfate method, while operable at moderate temperatures, involves tedious preparation and expensive materials.
*Modified Pyrosulfate Method (**4:29**)*
* 4:29: This experiment uses a modified pyrosulfate method to achieve oleum synthesis at lower temperatures.
* 4:53: Sodium bisulfate is heated on a ceramic hotplate to create sodium pyrosulfate.
* 5:16: A ceramic hotplate reaching 540°C is used due to the temperature limitations of standard hotplates.
*Sodium Pyrosulfate Production (**6:03**)*
* 6:03: Slow heating prevents thermal shock to the glassware.
* 6:25: Water is removed from sodium bisulfate, eventually leading to the formation of sodium pyrosulfate.
* 7:19: Stirring is avoided due to the potential breakdown of stir bars at high temperatures.
*Introducing Sulfuric Acid (**9:13**)*
* 9:13: Concentrated sulfuric acid is added to the cooled sodium pyrosulfate.
* 9:25: A PTFE stir bar is included to minimize bumping during heating.
* 9:52: At around 490°C, fuming indicates the distillation of oleum.
*Reaction Mechanism and Observations (**10:55**)*
* 10:55: The reaction between sodium pyrosulfate and sulfuric acid generates sodium bisulfate and oleum.
* 11:22: Oleum's volatility drives the reaction forward by releasing sulfur trioxide.
* 12:14: The sulfur trioxide content in the distillate decreases as the distillation progresses.
*Challenges and Yield (**16:05**)*
* 16:05: Accurately measuring the yield requires titration due to the fuming nature of oleum.
* 17:15: The oleum concentration is determined to be 112% sulfuric acid equivalent, translating to 53% free sulfur trioxide.
* 17:49: The final yield is around 13%.
*Future Optimizations (**18:01**)*
* 18:01: Potential improvements include better heating methods and adding oleum to the next run for increased purity.
* 18:33: Fractional distillation of oleum could potentially yield purer sulfur trioxide.
*Oleum Properties and Handling (**18:44**)*
* 18:44: Oleum demonstrates its corrosive nature by charring a tissue and damaging nitrile gloves.
* 19:10: Proper handling in a fume hood is crucial due to the hazardous fumes.
*Conclusion (**19:50**)*
* 19:50: While the current method shows promise, further refinement is needed before widespread amateur application.
* 20:18: Safe storage and disposal procedures are essential for handling oleum.
gemini 1.5 pro Token count
7,218 / 1,048,576
Best chemical channel!
Sand bath with a blanket of glass wool should be fine enough to get temperatures up. Great and novel synthesis vids as always!
I appreciate very much chemistry done by an actual chemist and not some tyro.
Thank you so much!
Thank you for the tutorial on making some really scary stuff ! I will pass on DIY for now.
I recently made some oleum by electrolyzing conc sulfuric acid drain cleaner. I used Pt on Ti electrodes for the anode and cathode, but interestingly the cathode got destroyed much quicker than the anode. It took about a week and I had to cut off the cathode every couple of days to get fresh Pt in the solution (the titanium did not conduct in the conc acid), but I managed to get a decent amount of oleum. I didn’t titrate it, but it fumes a good amount in air. I put the cell inside another jar to protect it from atmospheric moisture, but I suspect the maximum concentration you can achieve depends on how well you exclude outside air from the cell.
you’re just that good
Wow. Just wow. This is impressive.
Good god I was not expecting a video like this. This is amazing. I really can't say anything lol you are wild.
As for the inert dielectric constant measuring device, I think you can get away with a straight vacuum take-off adapter. Male and female joints, 5-10cm of straight glass tube and a hose adapter on the side. Then through the opening you put in 2 glass tubes with metal plates on the inside and all you have to monitor is capacitance on a multimeter. The only problem is the plates have to be small and close together, plus submerged. If the gap was small enough the capillary action could keep a sample sucked up into the gap which would be with some diffivulties. But it can very well be done.
Very interesting! If you want some interesting experiment with oleum, try to dissolve sulfur in it. It form blue S8(2+) cation. Se and Te also behave similarly, but they react even with regular conc. H2SO4 - Te needs mild heating, Se needs cca 200 °C. They form magenta Te4(2+) and green Se8(2+). Se8(2+) can be oxidized to yellow Se4(2+) by SeO2. Iodine also dissolves in oleum to green I2(+). Polycations of Br and Cl are also known, but idk if they can be made from oleum and Br2 or Cl2.
Cannot wait to see how this turns out!
Spooky fuming stuff, grant me more spooky fuming stuff oh algorithm of the youtube. Thanks for demonstrating reactions that are far to scary for me to ever want to attempt on my own, it's really neat chemistry.
love these chem videos!
I find it an amazing coincidence that you uploaded a video about oleum in the same day my procrastination made read about a class of compounds called borosulfates which analogues to silicates, but with boron relacing silicon. Oleum is one of the main reagents used in their synhtesis.
Congrats to fixing this method on video👍
Looks like a breakthrough in chemistry to me
Do love a bit of chem even if I may never get round to doing any myself.
Been subbed for years bro
Making the trioxide is something I've been planning for decades. There is a textbook experiment that uses a huge apparatus producing dioxide and oxygen, leading them into a chamber with platinized asbestos, but I'm sure that produces only tiny amounts since the amount of platinum is so small and would get wrecked by impurities rather fast.
I was actually thinking about using the industrial route with vanadium pentoxide, scaled down. Trioxide is not my priority at the moment, but I'd really like to do this while I'm alive. :D
I would use bottled oxygen. As for sulfur, purified, pharmaceutical one would be the best. Agricultural sulfur that comes in bags looks very pure but it has some crap in it visible when it's melted.
I'm glad you're still making videos as I've been following you for a really long time and you haven't succumbed to sensationalistic crap like some other people.
The real question i have with that is, what do you make the reaction vessels out of?
Then again, i guess you pretty much have to to go with fuzed quartz.
Sweet.
Thanks Nurdrage for your interesting and informative videos. This is a great one but it uses Sulphuric acid to make Sulphur trioxide, I was thinking of trying the pyrosulphate method using a modified pottery kiln and using an old gas bottle with malleable iron pipework as the apparatus. I undestand iron/steel has a reasonable resistance to dry sulphur trioxide which it should be once heated to 600c plus and its cheap enough to easily replace. If I can get that to work all I'll need after that is a small Ostwald plant to burn ammonia to NO2 and I'll be self sufficient.
Did'nt you forget the Iron Sulphate method to produce S03/Sulphuric acid
The Boss❤
Pretty successful and affordable for a first attempt, it seems c
Thats fantastic, the only thing fuming more than your product are the safety rangers, i look forward to see you perfect this, goood work & i am relieved you are still uploading, i was worried when i had not seen anything for a while.
Thanks again for a really interesting video!
Thanks for the great video. It’s interesting to know a potential way of a 3rd nitration
Of a certain hexagonal molecule?
For a moment I thought you were making Oleic acid
- and hoping you're planning on making Ferro Fluid in an upcoming video.
Love learning about chemistry, it's amazing how elements can/will interact - Thanks for all your great work and wonderful teachings 🥰
Thanks!
Thank you!
Awesome method!
I have been watching you, for what feels like a decade, produce the best content youtube could ask for. Please talk to Nilered and lets see another vision come to life 🙏
Grab a coffee, thanks! Love to watch; to dumb (&/| smart ;) to try! :)
Thank you so much!
Seems so simple! Surprised that this isn't done more often (aside from the risk of burning your face off of course).
Fantastic stuff!
Excellent video!
I've been making oleum this way for decades. I used the bisulfate method described in VOgel - Fuse bisulfare in nickel crucible and heat melt until it fumes. POur out melt, break it up inTo flaskes. Dissolve in Conc sulfuric acid and distill. I have never been interestyed in separating SO3 per se (Way too dangfeous foir me), 30% oleum if fairly easy and as safe as boiling sulfuric acid can be.
Comment for the insatiable monster as mentioned. Keep up the great work brother.
Love this!
How about polyethylene gloves such as people use for kitchen tasks? They're pretty resistant to a LOT of stuff, and they are quite cheap. Down side, they're not elastic in any useful sense, so they're a bit of a loose fit.
Incredible!
❤thank you Nur❤
My procedure came from a 1944 "Qualatative Analysis" book on making "Fused Sodium bisulfate (A commercially available product) by melting sodium bisulfate in an evaporating dish and heating until it starts to fume. The melt is then poured out onto a glazed ceramic tile - whish often fractures. The solidified pyrosulfate is then broken up ijto flakes.. I have carried out this procedure many times (heavy gloves, perchlorate hood (which was in the geochemistry lab and mostly unused). To make oleum, just distill sulfuric acid over the fused bisulfate. A note: solid SO3 is Extremely Dangerous - much more so than the liquid. If one tries to melt it, at the melting point, the solid alpha form transforms into the liquid beta form and the vapor pressure triples All At Once. In an open dish, it's scary. In closed glass apparatus it could be catastrophic. My yields - based on NaHSO4 were around 20%, which was enough for my purposes. Good luck, thank you, and BE CAREFUL!!
Great work, dude!
Fuming death vapor is fun to watch...on TH-cam :) I have no need for Oleum, but this synthesis was very cool.
Not sure if you ever considered using a trash metal burner, but you could submerge it in sand to even out the heat but be careful with its electronics, maybe tape around the sides to a plastic dish with the bottom cut out for cooling, maybe a cooling fan too… just an idea for you
An expensive option would be using a solder pot, ones for lead free should be able to match brain temperatures from 200-450C. A nice blanket of molten solder will keep you heat hood and even. Size is going to be a little limited.
Watching this video is a throwback to my summer research projects at uni where I used oleum to do nitrations.
Scariest nitration mix I've used (which didn't nitrate my substrate btw) was 70/30 oleum/WFNA at 160 °C.
I have the utmost respect for the acid. However, my supervisor got a drop on his hand when he was training me how to use it and showed me that even oleum on the skin can be fine if you wash it off quickly enough.
What kind of compounds were you nitrating? I’d expect that whatever you tried to nitrate at 160c° would carbonize pretty quickly.
@@chemistryofquestionablequa6252 Nitroterephthalic acid to dinitro according to a literature procedure (that was a load of shit). Called for 50/50 oleum, WFNA reflux at 160°C or something like that.
I never got the dinitro compound, only starting material. Surprisingly, nothing got carbonised.
@@r9341-tss1 that must have been nerve wracking, a nitration bath that hot is scary!
@@r9341-tss1 it's just astonishing what makes it into "the literature." Did no one so much as attempt to replicate the procedure before giving it the thumbs-up peer review? And don't get me started on "yields" sections, which often range from "best we ever got, weighed wet" to "pure fantasy."
Had a Oleum leak once at the plant i worked at. We were stuck at the lab, and the highway next to the plant was closed down for all trafic.
Glad I have P2O5. That looks very involved.
Love from India ❤
4:53 Ahh, the old "hopeful 2-second delay so I can escape" polypropylene tub trick. Yep, I've danced at this rodeo before.
18:15 maybe a sand bath would help with those hot spots
I use dnail PTFE joint protectors for sealing my joints, they aren't cheap but they are reusable depending on the chemicals they come in contact with. You can also use crystal boiling chips or crystal bearings, i have no suggestions for your low temp plate, possibly using a heated oil bath with the flask bottom submerged.
As a suggestion, don't put the magnetic stir retriever in the solution itself. This can contaminate your solution. Put the retriever on the outside and work the magnetic stir rod up the side. Normally we just use a second magnetic stir rod.
Try putting the shiny side of the foil facing inwards, it will raise the heat level
Awesome. Thanks! Feeding the monster...
Testing nitrile glove resistance to oleum while wearing the same kind of glove was a powermove :D
You should try the catalytic oxidation route. I've seen people pull off the ostwald process at lab scale, so SO3 should be doable.
Quarz tubes are also surprisingly easy to get. They're used in some types of radiative electric heaters to contain the nichrome coils. I got two from my old microwave's "grill". V2O5 can be bought for pottery and Pt catalysts on ceramic wool are surprisingly easy to make.