Lab notes - Making Oleum - 20% yield improvement - (May 4th - 2024)
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- čas přidán 3. 05. 2024
- 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: • Purification of Sulfur...
Lab notes - Making Oleum - Success (part 1): • Lab Notes - Making Ole...
Lab notes - Making Oleum - 20% yield improvement: This Video
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"Spicy flesh eating wax" 👍
That got me too.
Ditto, that got me too
those SO3 crystals forming at the condenser are beautiful... and hella scary
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.
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'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
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.
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.
👞👞💄💄💄😂💄🏣
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.
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.
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
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. ❤
💯
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.
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.
Great to see this lab note. Making oleum has drawn my attention recently.
Fantastic stuff man. Also really hyped to see you posting SOMETHING fairly regularly now. Keep it up!
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 had no idea sulfur trioxide polymerizes. I think that's so interesting, and very interesting that it's water dependent
Nothing I will ever attempt myself but it's interesting to watch someone else do it!
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
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 CZcams science content
I know its pedestrian but I love seeing distillation in action, excellent video.
It's like a nice walk in the park😁 (pun intended)
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 love your lab notes seasons, your sodium series was what got me to subscribe way back.
always love your work!
Loving the project!!
Love your channel. ❤
Keep us updated! this is fascinating!
Good progress!
Great stuff! Thank you for all your hard work!!
So glad youre back! 🤩
I love your process and these lab notes videos give a good view into what it takes to refine a work up
These lab notes are fascinating
Nice work ! :D
we use oleum itself to seal the glass connectors. (so no PTFE or silicon paste)
Highly informative!
Love your Lab Notes videos, and your others too, of course.
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'm always happy to see a new NurdRage video. Nice improvement on the oleum method.
Good work sir!
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.
Useful notes 👍👏
Informative 👍
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.
The corrosive potential of this product would make any heating wire instantly fail.
@@AlphasysNl i say use a high power laser.
I really like the work you are doing with this Oleum project it is very interesting.
Spankingly Marvellous !
jak zwykle niezwykłe:)
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!
Very nice! and Very Scary! Love it!
You exist. Congratulations!
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.
these crystals of sulfur trioxide are incredible
My dad works with SO3 sometimes. Rough, but can be done safely.
True OG of CZcams.
Wicked looking waxy solid.
I enjoyed this video as well as 99.9999% of your other content. Thank you
2 lab notes in as many weeks!? we're being spoiled! 😍
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!
awesome vid
I love these kinds of experiments that are far above what I dare doing.
I can't get hurt through a screen.
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.
Commenting for the CZcams 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).
Sure thing buddy!
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.
Maybe keep the SO3 in the collection flask liquid with a simple sand bath, that doesn't need to be heated much, but in a way that you can still observe it.
Then you should be able to see the difference with the liquids mixing due to the different refractive index.
You could also maybe try using (a polariscope) polarised light and polarising filter to see the difference in defraction.
Shine light through a polariser from the back through the receiving flask and view the flask through another polariser and adjust the angle/orientation of the viewing polariser until you find a view that works well. The change in density/defraction is much easier to see this way.
@@Killerhurtz Lasers. Chemistry needs more lasers.
I imagine you have some corrosion on board interconnect pins, or oxidized zif ribbon cables in that hotplate from the oleum fumes.
Awesome
I’m enjoying the danger goop videos.
Tremendous.
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.
Impressive video on some forms of sulfur trioxide and water vapour interactions. I haven’t seen the solid IRL.
Five words for valid comment
Love from India ❤❤❤
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,
Oleum synth is awesome! though not as awesome as having you back here!
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.
I could have written the exact same comment! This one definitely makes me anxious - don't think I'll be attempting this one.
nice.
I'm doing my part
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.
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.
Awsome
Commenting for proof of existing
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.
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...
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.
i have been watching your channel since i was a kid. i used to think that was your real voice
As you wish 😊
Oh no! You were trying to protect that hot plate too!
you could try using a fire blanket for insulation. they are made from woven glass fibres so shouldn't have the shedding problem
I comment to paise Al Gore's rhythm.
That's hilarious
That's hilarious
Perhaps attach a piece of ground glass or other porous material near the tip to provide nucleation sites. Might not have to reseed.
I like how you always encounter hotplate failure..
Use cheap $10 cooking plate, it can reach >500C without any problem and has normally 1KW power, just add cheap (but good) chinese triac thermostat with small thermocouple pressed to plate, if it will be destoyed by oleum it is not so expensive, about $25 for all
it may be viable to use a cooking hot plate as they get red hot on full power, theyre dime a dozen and precision is not necessary here so a simple thermocouple under the flask should be sufficient for control, good research as always
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.
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.
I can't help myself but notice that around the vacuum adapter it's fuming alot, maybe it's pulling water from the air and reducing the yield.
Maybe you also have to cool the receiving flask the reduce evaporation of SO3.
Edit:
You can even actually see something condesing at the adapter output
I am no alchemist, but I would try distillation into a round bottom flask on a heating mattle set just above the freezing point of whatever it is you are trying to collect.
Excelent video!
Do you have any plans on revisiting the electrobromine process for H2SO4? If I have the time i'm going to see a way to make Br2 using HNO3 catalitically.
I Made a test with NaClO3 and NaBr in acid medium to obtain bromine and using it to oxidize sulphur and it was succesfull. Sadly this adds Na ions to the reaction, but the overal process it's the next:
ClO3- + S + H2O => Cl- + 2H+ + SO4²-
This using the Br- as catalyst and at the end generating 2 H+
The HCl and HBr could be distilled and be left with a NaHSO4 solution.
I think the bromide can be collected oxidizing it to bromine and pipeting it before the distillation, but that's something that I'll probably do another day.
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.