Extractions&Ire - 2017-11-06
We finally close the ring, finally put all our nitrogens in a row. This video follows the final pages of this writeup: http://www.sciencemadness.org/scipics/Engager/TzOTC/Synthetic%20routes%20to%20tetrazole%20compounds%20based%20on%20OTC%20materials.pdf Sorry if the video seems a bit disjointed, it was filmed over such a long period of time. Roast my results on twitter here: https://twitter.com/Explosions_Fire
sorry i edited this at 1am and forgot i put that last bit in, it is very poorly volume balanced and also not really funny oops
i'd like to recommend a book to you "'Ignition, An Informal History Of Liquid Rocket Propellants"
Nah man. That was brilliant
Suuuuuuurree lol
the cheeky accent makes chemistry videos watchable. good job I really enjoy these.
Yeesss! A new vid from Ex&F / Ex&I, the day is saved!
yay! another yellow chem ...
Congrats! Welcome to the exciting world of Tetrazoles! The supersaturation effect is neat. I do it with the recrystallising in hot water. Scratch the beaker inside with a rod to set it off. Yellow is fine! My batches were all yellow with this method. The NaN3 method got white product. It gets easier every time. Keep at it and you will get a decent amount!
AllChemystery how toxic are aminotetrazole anyway?
kan petyim not very. It is also used in some specific Anti inflammatory medications and some other niche medications.if i remember correctly.
Thanks mate! I finally finally joined, and am confident about the product. Yeah the beauty of this is I have all the precursors now, I can just keep making it... the limiting factor is probably the hydrazine sulfate but I have liters of conc. bleach, I just gotta put the time in
Cat … bedtime …
Dude, cats are active at night! Why do you think their eyes have reflectors in them? ^^
That is why one should not lock up a cat. At night. At day. Ever.
Pretty cool synthesis, glad to see you finally pulled it off!
Thank you brother!! Great series.
Cracked up at the pH paper.
Is it my imagination or is your tightly cropped camera work and self-depricating humour getting more and more like chemplayer?
That's quite a compliment, it's not intentional. I think there's something about expecting people to take your science seriously while also using rudimentary techniques and gear that brings out the self-deprecation. Glad you think things are getting more tightly cropped as well, i'm finding myself editing out more and more 'ummmms' each video I make
Congratz! You nailed it.
Whats this? A video?
I never thought id see the day
oi
what are u doing on youtube, go study
tha piece of litmus paper just cracked me up
What was the minora-looking thing on that "enema"?
TEST SPECIFICATION
APPEARANCE (COLOR) White to Light Yellow
APPEARANCE (FORM) Powder or Crystals or Granules or Chunks
TITRATION (NT) HCLO4 0.1M 96.5 - 103.5 %
PURITY (HPLC AREA %) ≥ 96.5 %
SOLUBILITY (COLOR) Colorless to Very Faint Yellow
According to Sigma. So the yellow seems to be normal
Mine looks exactly like yours and also bubbled like yours. I also think it's the bicarb
I used to do syntheses of a tetrazole and it was yellow in its deprotonated form. As soon as it got protonated it was colourless.
Did you see what happened to Cody's Lab?? He is on two strikes right now, and can't upload any videos. He just made an unlisted one public that has all of the current information in the description. I can't believe YouTube is now hitting him too. Is this truly the end for the truly epic science channels like his and yours?
A_Lonely Proton Yeah it's big news what happened to Cody. This doesn't really help YouTube's cause, Cody isn't really going to compromise just because YouTube tells him to, so he might have to set up elsewhere, and I'm happy to follow him wherever
Long live chemistry on the internet!
With all those nitrogens it would be neat if the yellow was some type of complex with an impurity. No real clue about what it is though.
The pH paper was yellow friend
Do you have a 1 mio USD NMR in your shack?
how much does each run of NMR cost? i assume the solvent is quite expensive, even if you can use the machine for free?
Kinda depends upon what solvent that you need to use. CDCl3 will cost you less than $1 assuming you use around 1 mL of solvent. D2O is a little more expensive, less than $2 per NMR tube. DMSO will cost you $3-4 to prep.
An NMR? That's not what I thought you said.
You have an NMR in your shed in the outback???
I wish :( bench top NMR one day!
bloody ripper mate!
thanks mate!
The second time I ran this synthesis after the 3hr reflux I had to add bicarbonate to get the ph to 4. Still managed to get 16.9g of 5-ATZ from 30g of the Aminoguanidine. The first time I got 17.8. I followed the publication to the letter. First time went exactly as it was supposed to. IDK what I did different.
Do you remember how the test for cyanamide turns it yellow?
conduit122 ammoniacal silver. Silver cyanamide is the yellow
Do you think there could have been any sort of contamination of that in your product?
conduit122 I don't think so, especially as it's a yellow solid, I don't think it's would've made it through the recryst stuff like it did. Interesting thought though, they are very similar yellows!
i like how you have failed experiments sitting around in a plastic bag labled "failure, unknown crap" for years. really makes you look professional, and like someone who shouldnt be party vanned before he accidentally creates a nerve gas and kills half his country.
I'd guess the yellow discoloration is from iron contamination
It could be, it could've picked up a lot of iron from that steel can used to make the Ca cyanamide, but it seems unlikely, especially the way it seems to stick with it after the recryst, but it makes about as much sense as any other theory really
What about that plant that had some explosive peroxide compound in it?
zubmit they're growing! Looking a lot bigger now, still a long way to go until I feel they have enough leaves though
@Extractions&Ire what about now
@Marcia Osullivan check the recent videos
I just finished my essay and could have an hour of sleep before college... Or I could have 44 minutes.
i'll try to make the next video shorter so i ruin your life less sorry
Extractions&Ire, I ruin my life just fine without your help thank you very much. Don't try to take credit for natural phenomenon. (Also, did you hear about Cody's lab? That's messed up.)
Yeah it's crazy. Totally unfair. A post about it made it to the front page of reddit (17,000 upvotes so far) so he'll probably do some good out of it in the long run but yeah, something has got to give. I'm happy to follow him wherever he goes, there's just not a good alternate platform....
Interesting how both times you picked it up and carried it about that crystallisation was induced. Why do you think that might be?
the motion causing the forming crystals to stick together,once they start sticking it's a chain reaction and they precipitate out
You seriously need a tripod.
thebestnumber1 ya I mean I have a tripod, it holds the DSLR for the shots like the one at 2:17 but I find with all the explaining it gets pretty boring having a still camera. It's also easier to explain things I find if I can just move the shot around freely. But I'm always open to suggestions, I have adapters put the phone camera on the tripod
Nah keep the moving camera. You're expressive and it reflects your personality.
Any updates on the other channel? Or is it totally gone? Saw Codyslab got strikes.
PacificWar1 The other channel is totally gone, but is planning on making a comeback! Either here or wherever Cody goes I guess
In obtaining aminotetrazole, an excess of nitric acid is needed? otherwise, tetraсene
The gas that was "bubbling off, and fucking off into the atmosphere" was probably dissolved CO2 from the neutralization. Some of it was done in a cooled solution right ?
A little bit of cooling, but it was a lot of bubbles, far more than I'd expect from that. The suggestion below is that solutions of bicarbonate give off CO2 when heated to form sodium carbonate in solution, and I think that's probably the cause. Dissolved CO2 likely contributes too. I definitely panicked and overthought it at the time didn't I
First viewer and first like
Extractions&Ire your welcome mate ☺. I don't have sodium nitrite so i need to make some by bubbling NO2 + NO into NaOH
Dollar Projects aw man, that looks like a tough reaction to pull off. Nitrite is one of those annoying chemicals I'd really recommend buying, as there's just no good and/or easy way of making them
Extractions&Ire i know.. But i don't have any source of money/funds for buying expensive lab grade chemicals but i can buy technical grade nitric acid for $3 / liter 68% which i can use for making NO2 and NO
well if you're determined, let me know how it goes because i'd be interested if you got it to work well, good luck!
Extractions&Ire thanks...... 😊
I know this is 2+ years old, and your filming is much better now, but holy jesus were you a terrible camera man... and editor... and producer, lol. But you were (and are) a great chemist, so that makes it bareable to watch. :-P
Your recent stuff is awesome qualuty though! Good job, mate!
P.S. regarding the crystals not forming readily, did you try scratching the inside of the beaker with your stir rod or spatula? That usually helps. (I know thats a novice level trick, but if merely carying it around was sufficient enough to triggered the crystallization process, then it seems that the scratch trick would work)
DeadGamer1030 - 2017-11-06
I think the bubbling is from heating the bicarbonate in water. Take a scoop of bicarbonate and put it in some very hot water, it will bubble and turn into sodium carbonate.
AllChemystery - 2017-11-06
DeadGamer1030 I think that’s right. The original synthesis called for sodium carbonate so there’s the extra CO2.
Extractions&Ire - 2017-11-06
Oh yes you're probably right, it is quite a concentrated bicarb solution too, thanks! I just assumed this synthesis wasn't going to work so every observation I made in my head turned into a reason things were failing...