Lab notes - Making Oleum - 20% yield improvement - (May 4th - 2024) 

"Spicy flesh eating wax" 👍

loleum. It´s great that you are still working on this method.

those SO3 crystals forming at the condenser are beautiful... and hella scary

I've been here with you since the first few videos. I was in middle school now I've graduated college. You're education has assisted me a lot.

i'm sorry for your loss. rip ceramic hotplate.

Great video! An idea I had for solving the problem with the clogging condenser, if you used a 2 neck receiver and had a rod or something held in the second neck set to have the product drip over, you could use that as an indicator and it could still work after initially clearing the condenser.

You're getting a lot of comments about the use of a common electric household burner and I wanted to come here to agree. I saw on your last video a flask bottom totally shattered, and while that's a painful thing, it shouldn't discourage you from exploring the idea further. The high temps and ease of replacement in case of failure are major advantages, while the coils cause glass to shatter. Use a sand bath. A simple pan from Goodwill can be filled with sand or salt, and heat that pan directly, and simply submerge the bottom of your glass in the hot sand. This should aid in uniform heating and I would expect it to entirely eliminate the problem you experienced. And, to echo several other commenters, the entire setup is very cheap and easy to replace.

When you said that you are just as inexperienced at this as we are: I can assure you sir that you could not be more incorrect.

Fantastic stuff man. Also really hyped to see you posting SOMETHING fairly regularly now. Keep it up!

Great to see this lab note. Making oleum has drawn my attention recently.

It feels like if you could attach a funnel or something to the output, then the crystal would grow on the funnel (allowing you to monitor progress) but would not clog the output as quickly.

This video is absolutely amazing. This is as OTC as it gets. Even a 20% yield is very useful. No one on the sciencemadness forums talked about this.

Something you might try: why not test 100% or greater sulfuric acid with the bisulfate instead of the usual 98%? Maybe water, even in small amounts, acts like a poison to this reaction. You could add a bit of the oleum from a previous run to the 98% acid and bisulfate to kill any residual water (kind of like the sodium/lithium jumpstart needed for your menthol-catalyzed sodium synthesis), and then distill like usual to find out!

Cool to see the process of making oleum, I've been watching your videos since around 12 years old, and now I'm in college learning about the chemistry behind it all. Thanks for all you do!

Nothing I will ever attempt myself but it's interesting to watch someone else do it!

When I was very little (can't remember exactly, but definitely before school) my father for some weird reason liked to tell me about different processes used in industry, in particular, how they dissolved sulfur trioxide in sulfuric acid inside special towers and got something called "oleum". I wasn't sure what it was, but from other description it seemed really scary. Many years later... well, little me was quite right about that last part

I've done a lot of work with molten salts. Frankly, I'm surprised the hotplate lasted as long as it did. Buy a cheap 120V kitchen style electric burner and use that. Much more rugged and you can reach much higher temps.if the element fails, they're only about 10-20 bucks to replace. Also, and I'm sure you know this, use kaowool. Aluminum is a poor insulator. Finally, I'd be nervous operating glass at these temps. Maybe there is no cheap substitute, you'd know better than me. But the danger risks here are high.

If you wanted to melt the SO3 plug on the inside of the flask, you could try using an infrared heat lamp. I believe SO3 has high absorption of thermal infrared, and the light should mostly pass right through the flask, like a little green house

I love your process and these lab notes videos give a good view into what it takes to refine a work up

i love your lab notes seasons, your sodium series was what got me to subscribe way back.

Heya NR, I'm not a Chemist in any way what-so-ever, but I've been watching you steadily since Dec 2014! I hope never to hear your real voice, I hope never to see your face because I love the Mystery behind the man; and your fantastic humor that inject here and there. Despite not being a chemist I've learned loads from you and several other Chem-Tubers (like Chemplayer) and it's amazing how often I actually recall the knowledge when I have to inform friends/family of Chemistry facts for whatever reason(s); and all from simply watching your videos casually. Stay awesome man.

I *love* your lab notes videos. So useful to hear you talk through the experimentation process, even if I never plan on making Oleum. Good luck upping your yield!

Thank you for making so many new videos! Welcome back NR!

I know its pedestrian but I love seeing distillation in action, excellent video.

I love your channel man. One of the best for practical with step by step and explanations of theory. I wouldn't change a thing. Keep the quality over quantity.

11:58 "Amateurs love their reproducibility and robustness, perhaps even more than professionals." Love this quote! And this is why I like to try out someone else's experiment procedure.

I didn’t realize you were back making videos. I missed a bunch I’ll have to go back over. You made the best early RU-vid science content

I'm always happy to see a new NurdRage video. Nice improvement on the oleum method.

I really like the work you are doing with this Oleum project it is very interesting.

That fuming nature reminds me a lot of the visual effects used in old films and TV shows, where something seemed to start fuming and melting, followed by bursting into flames or something, often used in Star Trek too, scary stuff really, but fun to see, via a computer screen, where it's safe... :P

Great stuff! Thank you for all your hard work!!

Loving the project!!

Thanks for this...I loved Chemistry at school, especially the lab work and watching demonstrations. It's like being back there, accompanied by the same sense of wonder

always love your work!

One of the main reasons I love and endorse your channel is that I am confident in your chemistry. I know it's going to be what you titled it. ❤

So glad youre back! 🤩

This is a great, well analysed video. It's hard to overstress just how dangerous SO3 is.

Love your Lab Notes videos, and your others too, of course.

I had no idea sulfur trioxide polymerizes. I think that's so interesting, and very interesting that it's water dependent

i love these method and efficiency progression videos. You really see the trial and error science brain come out

Keep us updated! this is fascinating!

Thank you for this video! It's very helpful!

I love these kinds of experiments that are far above what I dare doing. I can't get hurt through a screen.

True OG of RU-vid.

These lab notes are fascinating

I enjoyed this video as well as 99.9999% of your other content. Thank you

Regarding the determination of the endpoint: I noticed the vacuum takeoff barb on the tip of your condenser fumes quite a bit where it’s exposed to air, but the fumes above the liquid within the flask remain clear. This seems to suggest that you’ve got a decent vapor liquid equilibrium of SO3 vapor above the liquid distillate, and that maybe ‘wetting’ the pipette tip to check for crystallization at the vacuum takeoff barb would suffice, thus negating the need to take the apparatus apart to check? Been watching this series closely. Excellent work!

Good progress!

2 lab notes in as many weeks!? we're being spoiled! 😍

jak zwykle niezwykłe:)

Good work sir!

Love your channel. ❤

Spankingly Marvellous !

Very nice! and Very Scary! Love it!

Commenting for the RU-vid algorithm - and just to say I love your content. I'm a fellow Canadian chemistry nerd (BSc with specialization in chemistry from University of Alberta).

we use oleum itself to seal the glass connectors. (so no PTFE or silicon paste)

You exist. Congratulations!

Love all your videos.Especially the lab notes. You are a legend and the reason i have all my glassware. I would never do this because... Damn... Disting sulphuric acid is about my max threshold for for danger. So i will live vicariously through your videos.

Glass fiber rope makes a great insulator. No glass particles all over like with wool and you can rotate it around any object as needed. I have some lengths of about 1/2" and 1" rope. They make great insulators over round bottle mantles too, just rotate in spiral on over the bottle. Quick and easy. I also use carbon fiber sheets (like used as welding insulator). No sharp glass everywhere either and handles well high temperature too.

Once you achieve this goal, I'd love to see you explore the possibility of using the pyrosulfate to produce acetic anhydride, like you mentioned in the first video. I'm currently trying to explore this procedure myself based on some science madness posts and unconfirmed patents.

Wicked looking waxy solid.

Could you use one of the round bottom flasks with 2 necks at a receiver? you could use the second neck to run a small heating wire to the drip point to remove the solids. You could also use it as a safer access point to collect and test the condensate.

Highly informative!

Useful notes 👍👏

I’m enjoying the danger goop videos.

Impressive video on some forms of sulfur trioxide and water vapour interactions. I haven’t seen the solid IRL.

awesome vid

The youtube algorithm shure is hungry🤔 Keep up the good work, great contribution to the amature chemist community! I have personally been thinking about making some videos about my own expieriments, but don't have necessary lab and video equipment I would prefer.

My dad works with SO3 sometimes. Rough, but can be done safely.

Algorithm do not ignore this man's exploits! If trace water is enough to seed the polymerization, is some kind of very brief exposure of the collection flask to a puff of steam enough to get the seeding to happen on the walls of the flask? It would be really nifty to see that crystallization spreading across the entire surface of the flask.

Oleum synth is awesome! though not as awesome as having you back here!

Use a recirculator to run 37° water in the condenser.(Melting point of pyrosulfuric acid). I really enjoyed your characterization of sulfur trioxide solid as "Flash-eating wax."

Informative 👍

I've been following for many years and do my best to like every video I see. I'm sadly too poor to be able to give to a Patreon,

This reminds me of the making sodium video. Using oleum to pre dry the sulfuric acid seems like a logical step. I also think that a larger ratio of bisulfate should be used since the catalyst has a maximum water capacity.

The refractive index of sulfur trioxide is close to 1, whereas the refractive index of concentrated sulfuric acid is closer to 1.5. I'm assuming this significant difference could be used to determine when the distillate changes over to sulfuric acid. Borosilicate is also about 1.5, so if the fractions change sharply and are fairly pure individually, then you could tell when the distillate changes by when you can no longer see the glass-distillate interface on the drip tip.

Sure thing buddy!

I imagine you have some corrosion on board interconnect pins, or oxidized zif ribbon cables in that hotplate from the oleum fumes.

Hi NR, I have a few ideas for you to try: You can use the cheap coil hotplate if you use an appropriate heat spreader. Try using a heavy bottom stainless steel frying pan of the type used with induction hot plates. It will survive acid spills at the working temperature of this process. It will also help if you use a heat transfer fluid between the pan and the bottom of your flask. I would suggest a molten salt eutectic of 60:40 mixture of sodium nitrate and potassium nitrate, which is a liquid between 260-550 °C (500-1,022 °F). You won't need much. This is easy to make and pretty safe since you have no organic material nearby, and will survive acid spills with only a little release of HNO3 vapor at operating temp. Just don't let the salt freeze around your flask during cooling. Raise the flask or lower the pan. Your process is at the upper limit of silicone heat transfer fluids, so they are not very stable and may smoke or gel. There are previous suggestions of a sand bath, and while this could work, thermal conductivity and thus temperature controllability is poor. Use a fluidized bed system instead if you want to use this approach. In any case, use a stainless steel sheathed type K thermocouple in the molten salt or sand near the bottom of the reaction flask with an electronic PID controller like a REX-C100PID to closely regulate your temperature, the same as you could use with a Glas-Col mantle. The PID controller allows you to tune and compensate for the thermal mass of the heating system and is much better than the older SCR type heater controls. For your safety catch pan, use a kitty litter tray or steel tray half filled with dry clay type kitty litter. It will safely absorb a hot acid spill. I looked up the prep: Preparation of Sulfur Trioxide and Oleum, by GARAGE CHEMIST on ScienceMadness.org: He has some useful ideas. His use of Sodium Peroxydisulfate (Persulfate) is interesting. The advantage over Sodium Pyrosulfate is that it is non-hygroscopic, so it can be dried completely at low temperature. It decomposes at 180 °C to O2 and dry Pyrosulfate, so there is no water to distill off prior to SO3 production. If this release of O2 happens in solid phase, (I think this is the case) it would be a handling advantage. GC used a *small* amount of concentrated H2SO4 as a decomposition catalyst to lower the reaction temperature, much less Sulfuric than you are using, and this should improve yield. Distilled concentrated Sulfuric still has about 2% water due to high temp decomposition of vapor. This decomposes some pyrosulfate before SO3 is formed. This is why your use of 2x sulfuric acid gave lower yield. It looks like the Persulfate plus small amount of Sulfuric in the GC setup is a slightly damp powder, and remains so, which would eliminate any need for a stir bar. Your Erlenmeyer flask is a better idea than his RB flask for purpose of even heat transfer. Persulfate is commercially made from Bisulfate by electrolysis. I wonder if it could also be made by adding an appropriate amount of 30% H2O2 (or even 3%?) to the Bisulfate and gently heating to dryness? If so, this would be an easier route to Pyrosulfate even for regeneration of residual Na2SO4 for later batches. You might have to break up caked Persulfate. If it works out right, there will be no initial distillation of water before SO3 production, and no molten salt to deal with, so yield will improve. At worst, you might get some Piranha. There is no need to collect the water in a pre-distillation. You can just let your blanketed reaction flask vent to the air until it starts to fume, then you can install your short-path condenser. This keeps your glassware dry. Another observation is that it looks like there would be an advantage to adding some Sodium Bisulfate to a batch of Sulfuric acid when distilling the acid to obtain 98% concentrate. This might prevent bumping and eliminate need for stirring. How much? IDK, try empirical. Maybe a little, or maybe a lot. Erlenmeyer flask looks better than RB in this case too. Less trouble even if it does bump. I don't have an appropriate safe setup for this ATM or I would try it all myself. Regards... D

Great improvements! I think some way of infrared heating may work directly through glass and heat up crystallized oleum directly. Would be faster than heating the flask.

When you are done with this procedure, please try out the eecomposition of anhydrous copper sulfate. If done correctly, it can actually give quite good yields of SO3.

I comment to paise Al Gore's rhythm.

you could try using a fire blanket for insulation. they are made from woven glass fibres so shouldn't have the shedding problem

Love from India ❤❤❤

Awesome

I'm doing my part

these crystals of sulfur trioxide are incredible

Tremendous.

i have been watching your channel since i was a kid. i used to think that was your real voice

nice.

Maybe there is some way to melt the lump off the end of the tube using radiated heat, either IR or bright visible light. Having some sort of dark glass tip would help with the absorption of the radiated heat.

Perhaps attach a piece of ground glass or other porous material near the tip to provide nucleation sites. Might not have to reseed.

the goat

This is one of those "I'm so terrified of this that I'll never do this in a million years" sort of things that is on my "watch this space" bucket list...

Awsome

Fascinating! I have an idea or two to offer for consideration about condenser clogging. It sounds like the crystals form against a seed or water vapour. If you were to preheat the end of the condenser with the torch before fitting the receiver, you could remove any surface moisture. Also, the condenser opening is flat-side-down. What if you were to rotate the condenser near 180 degrees so the condensate could drip off the pointed tip? Would that be bad? Perhaps the SO3 might "stalactite" off the tip but without restricting the flow, and you'd still have your SO3 -> H2SO4 transition indicator.

If you have a laser with a wavelength the glassware won't block too much, maybe you could melt the polymer blockage with that? Also, if the condenser outlet pipe could be made into an inverse funnel, it might not block, as the seeding point seems to be somewhere at the lower edge.

"Spicy, flesh-eating wax" is the best description 😂

As you wish 😊

More nightmare fuel videos! Love it!