Lab Notes - Making Oleum - Successful - (April 21-2024)

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:
Lab notes - Making Oleum - Success (part 1): This Video

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[NurdRage]

Update: I've been able to get the yield up to 22% in my latest experiments. So i'm still working on it.

[LabCoatz_Science]

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!

[dtrotteryt]

The donated hot plate comes to the rescue again! Yeah!! 🎉

[miketout]

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.

[andrews.]

You’re really pushing the limits with what can be done as a home chemist! Thank you for the inspiration NR ☺️

[jamesg]

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.

[gotnopee]

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

[Eero]

Great to see you making videos and well excplained!

+feeding the hungry algorithm

[parttime]

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"..

[mcdubstrizzle]

This is a huge breakthrough even with the yield. Great job as always, looking forward to seeing how far you can take it.

[waltonchan]

Sand bath with a blanket of glass wool should be fine enough to get temperatures up. Great and novel synthesis vids as always!

[shabushabu]

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.

[jonhu]

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)

[shrivanth]

Your video's are way more better than my chemistry class

[bedlaskybedla]

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.

[loganv]

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.

[AcoAegis]

this is awesome!

been watching your channel for maybe 16 years now, still my favorite chemistry youtuber

[MadMorgie]

Love seeing a new NurdRage video, especially when you are exploring new territory.

[syntactyx]

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!

[NormReitzel]

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.