NurdRage - 2024-05-04
More lab notes on making sulfur trioxide and oleum. This time i was able to get up to 20%-25% yield with improved heating with better insulation. Also found out that precise temperature control is important and that the polymerization of the sulfur trioxide phases can be easily initiated by smearing it with a pipette on air. Previous videos: Purification of Sulfuric Acid by Distillation Revisited: https://youtu.be/0Gb9rM9BJ8I Lab notes - Making Oleum - Success (part 1): https://youtu.be/wB2zzm8VP9Y Lab notes - Making Oleum - 20% yield improvement: This Video Donate to NurdRage! Through Patreon (preferred): https://www.patreon.com/NurdRage Through Youtube Memberships: https://www.youtube.com/channel/UCIgKGGJkt1MrNmhq3vRibYA/join Twitter: https://twitter.com/NurdRage Reddit: https://www.reddit.com/r/NurdRage/ Instagram: https://www.instagram.com/nurdrageyoutube/
those SO3 crystals forming at the condenser are beautiful... and hella scary
Thanks for reminding me about the availability of sodium bisulfate!
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!
Good idea!
@@andersjjensen I actually chatted with NurdRage about this, and he said he tried, but the results weren't really notable (he basically got out all of the oleum he put in without any significant gains). Good to know though, I think he's planning to try other bisulfates soon as well, specifically potassium bisulfate, which shouldn't pyrolyze until a higher temp!
He said initially that 100% sulfuric acid is an equilibrium between water and free sulfur trioxide at high temperatures, making it not much different from oleum itself.
loleum. It´s great that you are still working on this method.
hopefully i'll hit my 30% goal!
@@NurdRage Good luck mate! I hope it works out
@@NurdRage I wonder how well reacting SO2 with Na2S2O8 in H2SO4 would work, it may be worth looking into.
@@NurdRageGiven that your process is a close cycle type with nothing thrown away - the yield % is not important anymore!
@@NurdRageyou could try wrapping up your glasswool in aluminum foil, so that you still have good insulating properties but the glass isn’t shedding everywhere it’s captured in the aluminum foil.
i'm sorry for your loss. rip ceramic hotplate.
Thanks! I think I can fix it.
@@NurdRage Let us know what was the reason of failure.
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.
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.
*your
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.
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.
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.
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
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!
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.
👞👞💄💄💄😂💄🏣
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.
True OG of YouTube.
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. ❤
💯
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
Maybe a laser pointer works well either
boro absorbs pretty much all IR light that tries to come through it. I have a beaker near an IR heater and it gets hot at the side close to the heater whereas the further remains at room temperature
i love your lab notes seasons, your sodium series was what got me to subscribe way back.
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!
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.
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.
I employ large-ish heatsinks on electric coils as a hot plate... 6 x 6 x 1/4 x 1" fins works great. Fins down, flat side acts exactly like a hot plate. Temp control isn't as great, and yeah it's aluminum, but definitely useful to have around. Nice even spreading of the heat and it captures a good majority of it from the coil.
Bonus, niche cases also find them useful to quickly dump modest amounts of heat without messing with water baths or whatever if one is kept in a freezer. Recrystallizations of various salts in stainless come to mind.
Dude, this is an awesome idea! its like the Turkish(I think) coffee.
I love your process and these lab notes videos give a good view into what it takes to refine a work up
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
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 YouTube science content
I'm always happy to see a new NurdRage video. Nice improvement on the oleum method.
I imagine you have some corrosion on board interconnect pins, or oxidized zif ribbon cables in that hotplate from the oleum fumes.
Loving the project!!
Rewards come with persistence, thanks and I find it very interesting. Take care.
Thank you for making so many new videos! Welcome back NR!
Very nice! and Very Scary! Love it!
My dad works with SO3 sometimes. Rough, but can be done safely.
Nothing I will ever attempt myself but it's interesting to watch someone else do it!
This is a great, well analysed video. It's hard to overstress just how dangerous SO3 is.
Great work it's fun to just see you work and learn a few things too.
These lab notes are fascinating
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!
I love these kinds of experiments that are far above what I dare doing.
I can't get hurt through a screen.
I really like the work you are doing with this Oleum project it is very interesting.
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.
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.
So glad youre back! 🤩
Keep us updated! this is fascinating!
Love your Lab Notes videos, and your others too, of course.
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.
i love these method and efficiency progression videos. You really see the trial and error science brain come out
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
2 lab notes in as many weeks!? we're being spoiled! 😍
I had no idea sulfur trioxide polymerizes. I think that's so interesting, and very interesting that it's water dependent
always love your work!
@SomeMorganSomewhere - 2024-05-03
"Spicy flesh eating wax" 👍
@briancox2721 - 2024-05-04
That got me too.
@erikhartwig6366 - 2024-05-04
Ditto, that got me too