Making a Rare and Very Unstable Chemical (and also Potassium Iodate)

In this video I first show my new method for making and purifying potassium iodate from any chlorate or bromate salt. I then use the potassium iodate to make a rare and very unstable heteropentahalide interhalogen salt with the formula KICl4; or potassium tetrachloroiodide.
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As a side note, using a potassium salt as an oxidizer would probably work better than a sodium salt for making iodate. I do like however that using a sodium salt really emphasized how effective my purification process was.
PS: You need STRONG hydrochloric acid for the interhalogen salt solution to be strong enough to crystallize. I tried first with 25% and no matter what I did it would not crystallize.
#chemistry #science #hydrogen #gas #elements #fire #chemical #industury #color

[@LabCoatz_Science]

Now I'm kinda curious what the KICl4 converted the acetone to...chloroacetone? Mesityl oxide? Mesitylene? Mesityl chloride? The dark color kinda makes me think it's polymerizing, which does potentially point to a self-Aldol reaction. Regardless, KICl4 seems like a potentially useful chlorinating agent! I wonder if using HF would give a more stable KIF4 salt...

[@integral_chemistry]

Huh I actually hadn't considered this idea until you and I think one other person brought it up. I simply attributed the darkening to free iodine, but now I think it's certainly worthy of further testing. Obviously my concern was really only to make a weird salt, love that you've got me now thinking of uses for this stuff. I'll check the chat and see if anyone can come up with some sort of qualitative test to confirm if it can indeed act as a chlorination agent

[@rogermorrison2968]

"Mesityls" - не варианты. В такой среде ни одна двойная связь не выживет. Несомненно, образовывались хлорзамещённые ацетона.

[@TheFalseJared]

@@integral_chemistry Isnt chloro acetone a potent lachrymator? If so it might be easy to cross that off if your eyes weren't waterin while you were cleaning everything up

[@LordProtectorPepper]

This the type of nerdy ass comment that just makes yt a better place

[@aidanclarke6106]

Methyl acetate is also an option

[@ChemicalForce]

Oh yes how it infuriates me to set the light so that there is no f*сking reflection on the test tubes when I take macro shots

[@integral_chemistry]

I've borderline given up 😅 macro shots are so finicky as it is with the 1mm depth of field you get, lighting and reflections on top of that I've driven myself nuts trying to get it right. Oh and lint. I always get lint in my Beakers from drying them off. Usually it's invisible but with macro shots it's so distracting

[@ChemicalForce]

@@integral_chemistry I know that feel bro 🫂

[@DangerousLab]

@@integral_chemistry I use cross polarization to minimize the reflection on glassware, but that's very difficult to set.

[@oxoniumgirl]

Try lighting from behind and aside the tubes with narrow field lights while the camera is in the dark field areas. If you light from behind the camera there will always be a reflection on the tube because of the FoV of the macro lens interacting with the curvature of the test tube. When I was doing chem videos I used a LED flashlight in a retort clamp on a stand set deeper into the fume hood and off to the side.

[@ChemicalForce]

​@@oxoniumgirl Yes, unlike filming in a studio, shooting inside a fume hood imposes limitations on lighting. Keep in mind that much depends on the specific reactions you are filming!

[@aqua-op]

Pick one for all reactions for the rest of your life. 1. Final product always low single digit yield but always very high purity 2. Final product always over 3 digit yield, ie always highly contaminated.

[@integral_chemistry]

Oh christ that's awful 😅 uhh assuming I'm allowed to purify after the fact I'll choose triple digit impure trash. If not I'll take the pure single digit yield and run at 10x scale. Both suck lol

[@nerd1000ify]

As a biochemist, one 'synthesis' I do (recombinant protein expression) has a yield of less than 10 mg from 100g of cell paste. And it's contaminated with all the other stuff that is in living cells. The suffering is real.

[@natekloepfer1571]

The red-brown acetone solution likely contains iodine monochloride and possibly from elemental iodine.

[@integral_chemistry]

I honestly hadn't thought that the acetone had been chlorinated here until you and a few others brought it up. Definitely gives me some ideas for future projects!

[@philouzlouis2042]

@@integral_chemistry Beware that I2 or Cl2 (or HCl in oxydizing environment like H2O2) are quite potent laccrymators probably due to tiny amounts of CH3-CO-CH2-X (X being Cl or I) PHZ

[@ligmasack9038]

Beautiful Crystals.

[@ishzarkklyon9590]

I can hear Tom from Explosions&Fire breathing heavily at that bright yellow

[@pjbth]

Crazy how the crystals just kind of pop into existence

[@jimmyc3238]

Beautiful! The chemistry seems pretty basic, but is actually quite complex. If I may make a suggestion: the font makes this hard to understand, especially around <a href="#" class="seekto" data-time="456">7:36</a>. The "I" (upper case i) and "l" (lower case l) are virtually identical. As a grad student, I worked with cobalt carbonyl compounds, so I know how annoying writing this stuff can be.

[@integral_chemistry]

Thank you so much! I will say I do my best to make complex ideas as simple and straightforward as possible, and I appreciate you found that to be the case here. And yeah the font is an issue here, and it will be again with a couple videos I'm working on now. I've found so many of the fonts that make a clear distinction between the lowercase "L" and uppercase "I" to look pretty goofy, but given it's going to continue to be an issue I should probably take a deeper look pretty soon..

[@1HeartCell]

when you said "if you dont like crystals" I was like why the fuck would such a person watch a video like this

[@integral_chemistry]

LMAO you'd be surprised, I've gotten complaints on the Crystallization clips. I love them too much to stop though

[@jackingwads7513]

​@@integral_chemistry bruh no way how can you like chemistry and not love crystallization That's half the reason to like chemistry

[@lucazsy]

I was like "who doesn't like crystals?"

[@redmadness265]

​@@integral_chemistry Why?? What lameos don't like looking at crystals?

[@afrog2666]

Because "Making a Rare and Very Unstable Chemical" doesn`t mention crystals? A better question is "who tf has a problem with crystals" lol. "DAMN CRYSTALS Took Ur juuurrrbs!"

[@j_sum1]

Genius. So much clever stuff in there. And the crystallisation shot was gorgeous. I thoroughly enjoyed that.

[@imikla]

Super interesting synthesis and I love the beautiful crystals!

[@integral_chemistry]

Glad you liked it! I wish this was easier to scale up because they are some of the most beautiful crystals I've seen

[@Psychx_]

I would have used K2SO4 instead of K2CO3 because that's what I got at hand (and CaSO4 being even less soluble than the carbonate), but what ever works, works. Great idea!

[@integral_chemistry]

Thanks man! And yeah that's true you could go the calcium sulfate route, I honestly just hate filtering the crap. It seems every time I try to pull a vacuum on calcium sulfate I get an unworkable sludge

[@oxoniumgirl]

@@integral_chemistry there's a trick to filtering it btw; you place filter paper on top of the glass frit, and then use a thin rod to poke holes in the sludge in a grid pattern without piercing or breaking the papers below, the gypsum clumps up and the holes allow fluids to be indirectly pulled into the vac by venturi forces acting around the holes. The sludge will be dried slowly without the vacuum system being blocked off this way, and as it dries the gypsum mass will shrink in size forming cracks which allows more fluid to be pulled from the hardening mass. This also allows easy removal because it will pull away from the sides of the filter funnel. I used to make nitric acid in bulk via the gypsum method.

[@rogermorrison2968]

Вы ошибаетесь. РастворимостьCaSO₄ значительно выше, чем у CaCO₃. В то же время он плохо фильтруется и удерживает много воды и растворенных в ней веществ.

[@philouzlouis2042]

@@rogermorrison2968 From memory of lixiviation tests in our environemental lab analysis, it is over 10 000 mg CaSO4 what highly supprised our French customers (Plaster of Paris ;o) ) because over the treshold limits for SO4(2-) of soil destined to inert garbages. It also makes a cake of fine intricated needles. PHZ

[@jncojoke]

Your thumbnail had me in the typical scrolling, Ooh pretty crystals, who doesn't like pretty crystals. I had books in the 80s that my grandfather gave me that were filled with pictures of natural crystals, I'd look at them for hours as I didn't understand how these objects even existed.

[@integral_chemistry]

Same! I used to have a book of different crystals under polarized magnification, it was absolutely one of my favorites

[@philouzlouis2042]

Hi Apoptosis, Nice video and experimentation. Just as a side note from my basic knowledge of chemistry (we are always students into that field of wonders ;o)), If chlorate are very potent oxidizers, more so than bromate or iodate (from pyrotechnic and uncompatibilities understanding); it follows the rule of electronegativity; so Cl > Br > I. Note that they are ready to "give their oxygen easier and thus to "scavenge" it easier the other way arround. For that reason hypohalite are hell good oxydisers (somehow unstable) and the ease of disproportionation goes into the order I > Br > Cl; for that reason IO(-) froms nearly spontaneously IO3(-), while BrO3(-) requires some more energy and ClO3(-) some heat to "deteriorate" Javel-Bleach water. 3 OCl(-) -heat-> OClO2(-) + 2 Cl(-) (take some time below 30°C but the warmer the weather the faster commercial bleach isn't efficient anymore) 3 OBr(-) --> OBrO2(-) + 2 Br(-) 3 OI(-) --> OIO2(-) + 2 I(-) Then as oxydation comes into consideration; oxydation up to perchlorate takes quite some energy but is acheivable; oxydation up to perbromate is hell difficult (for that reason despite perchlorates are amongst the stabler into the sequence of OCl(-), OClO(-), OClO2(-) and OClO3(-)) one may consider bromate to be a nearly endpoint for conventional OTC chemistry and the resulting perbromate is an utterly powerful oxidizer (read unstable towards reducers - thus low activation energy); on the contrary iodate is absolutely no endpoint and leaves access behind to some periodate quite easily. Periodates are also powerful oxydizers (known for ages - in early begin of the 20th century - so more than 100 years ago) into organic chemistry) able to cut geminal diols into aldehydes) but somehow stable and useable from that "ancient time" because easily accessible. To my feeling, you excess wheight-yield might also come from periodate of sodium or potassium; because as chemistry logic follows some "not-so-obscure" rules; if iodates are less soluble; periodates are even less soluble and precipitates thus even more readily. As a complication periodic acid (yeah an acid that shows off often - periodically ;o) ) has not always a simple formula HIO4 (metaperidoic acid) but also orthoperiodic acid (H5IO6) what must provide also some solubility constants troubles and hydratation troubles (H5IO6 = 2 H2O + HIO4, after all). To finish; oxydation may happen dry like what you did, maybe with the help of fusion into the water of crystallization (?) of chlorate and iodide to lead to chloride and iodate (and maybe periodate?); it can also happen into solution: Cl2 is indeed also a strong oxydizer and can dillute into water to generate the nascent powerful oxydant hydrogen hypochlorite (hypochlorous acid). Cl2(g) + H2O --> HOCl + HCl So: HOCl + I(-) --> Cl(-) + HOI OCl(-) + HOI --> Cl(-) + HOIO OCl(-) + HOIO --> Cl(-) + HOIO2 (iodic acid and iodate) OCl(-) + HOIO2 --> Cl(-) + HOIO3 (periodic acid and periodate) Meaning bleach can do the job too ;o). Hoping it gives you some wood for your fire. Regards, PHZ (PHILOU Zrealone from the Science Madness forum and other alt. engr. newsgroups on old A.O.L.)

[@MadScientist267]

I'm only an amateur hobbyist but the group 1/2 carbonate swap is my (currently) favorite magic trick 👍

[@integral_chemistry]

Tbh I've been doing this for ages and only now am I really appreciating the wonderful carbonate swap 😅 I used to be really into the sulfate swap but this is way cleaner

[@MadScientist267]

​@@integral_chemistryHaha yeah my only gripe is the filter after. My first run with it was to pull the strontium out of a road flare, ended as the chloride for methanol. People also told me I'd never get the sodium out... that flame is *clean* haha just takes patience at the filter. Ever since I've kept it in mind and done a few of them... handy indeed

[@tomasfrybert]

oh my god your channel is gem

[@integral_chemistry]

Awe thank you! 😄

[@christopherleubner6633]

Reminds me of rutilated quartz. Very nice crystals.

[@KeepAnimeDegenerate]

Apparently CsICl4 is more stable than the potassium salt, and can be precipitated from the yellow solution upon addition of a cesium salt

[@jasonpatterson8091]

Because it's text, please note that the following is not intended to be negative, just trying help clarify some confusion. Your theory of why the yield was over 100% doesn't make sense to me. We are assuming that KI + NaBrO3 --> KBr + NaIO3 due to solubilities, right? If it's a <a href="#" class="seekto" data-time="61">1:1</a>:<a href="#" class="seekto" data-time="61">1:1</a> reaction, then any unreacted bromate that might precipitate out represents iodate that was never formed. Since the molar mass of KBrO3 is less than NaIO3, that should hurt your yield rather than improve it. However, sodium iodate does appear to be a hydrate (wiki says that pentahydrate exists). My honest guess is that your yield was significantly lower and you've got a bunch of water of hydration. When you purified using calcium carbonate (good idea, by the way) you lost some impurities and probably some product as well, bringing your hydrated mass down enough to make it under 100%.

[@integral_chemistry]

Oh damn yeah no I think you are 100% correct. Interestingly enough, my initial script did blame water of hydration until I went back and took that bit out after I couldn't find any literature regarding potassium iodate forming hydrates. I actually didn't catch the fact that it was the sodium salt that formed in the first reaction until I had already finished my recording, and so my sloppy last minute decision to hurry up and get the video finished was to blame the bromate, and I didn't even think to check if sodium iodate formed hydrates. In any case yeah a pentahydrate would add considerable mass, so I'm pretty certain the yield was close to 100% with the extra 16% being water of hydration. Good catch.

[@flyingshards595]

Very clever, much appreciated

[@oxoniumgirl]

Oooh very excited for your TLC video! I never got to get instructed on modern analytical chem, when I learned chemistry in my youth we were learning from a 1920's chem book and I don't think chromatography was even invented yet.

[@Disrup7or]

You have a criminally low number of subscribers. Thank you for doing what you do ❤

[@sobertillnoon]

Me: How well does this hotplate work? Sales person: eh? Wellish.

[@integral_chemistry]

Lol got a chuckle out of me, mostly because that brand name never ceases to be weird to me

[@devin6159]

I don’t know how I got here or what a single word meant but I enjoyed the video lol thanks for the rad video!

[@integral_chemistry]

Ha! No problem at all dude! Happy to hear you enjoyed it

[@OtherWorldExplorers]

In the future could you describe what these chemicals are used for. I mean it was completely fascinating especially when it precipitated out as a crystal. It was like a cactus was shedding. But as a lay person like myself I think knowing what this stuff is used for even if it's just to test a theory. Would bring a form of closure to the video. Thanks for posting.

[@experimental_chemistry]

Very interesting! Only knew the synthesis before based on the oxidation of iodide by chlorate in a hydrochloric acidic solution, followed by the addition of potassium hydroxide. Unfortunately chlorate is restricted here meanwhile and bromate is carcinogenic. So I am glad about knowing a Polish seller where I can get iodate easily and not too expensive. The polyhalide salt is indeed very nice - got this idea from woelen homescience again? 😉

[@DangerousLab]

Woelen's resources are awesome, I have been referencing his experiments since 2009, unfortunately his experiments don't usually associate with any videos.

[@experimental_chemistry]

​​@@DangerousLab There are many short videos about the reactions, but only on his page.

[@DangerousLab]

@@experimental_chemistry Oh ya, some of them have clips for the reaction but mostly are just photos and text.

[@integral_chemistry]

Glad you liked it! Iodate salts are always obnoxiously expensive so I definitely have spent a good amount of time thinking about the best way to make them. And yes! I do need to go back and credit him in the video description at least. I came across his site a few months ago and after going through most of it I pulled this idea, the tetraperoxochromate+phosphorus, and a third idea I'll probably have a video out on in around a month. The third is the one he did on the fluorescent copper iodide pyridine complex, but to get to that video I still need to put one out on making the copper chromite decarboxylation catalyst, and another on making the pyridine itself. Basically my next month's lineup lol

[@experimental_chemistry]

​​@@integral_chemistry Since iodide got much more expensive recently, it's not cheaper than iodate anymore. Therefore the effort to make it myself is not really worthwhile, but it got more difficult to do: chlorate is restricted and permanganate hard to get.

[@StoneWaterGlass]

The first, neat reaction with can be done in water solution instead I believe, you dont need that much heat

[@LightPhoenix7000]

I recognize the song playing over the crystal montage from the LoFi Girl stream!

[@StoneWaterGlass]

I think you can bubble ozon through a solution of an iodide salt in water to generate the iodate, or even periodate.

[@oxoniumgirl]

KICl4 is only stable in solutions or environments where there is an excess or equilibrium of free Cl, much like copper tetraamine sulfate is only stable in solutions or environments where there is an excess or equilibrium of ammonia, so you can't dry it in air without decomposition. If you set up an environment with Cl gas, such as a schlenk line and schlenk filter flask with Cl atmosphere, you should be able to vacuum filter it and eventually ampoule it for permanent storage and display.

[@mgdurandolo]

Thanks!

[@energytv3536]

Didn't know iodate is a strong oxidizer

[@NguyênKhoaCôngTy]

Hey Apoptosis , you can make a yellow crystals of tetrachloroiodic acid by the reaction : ICL3 + HCL = HICL4 or I2 + 3 Cl2 + 2 HCl + 4 H2O → 2 HICl4 Lets try it!

[@chemicalvamp]

Yeah! Yellow chemistry 🙃

[@lucazsy]

Those crystals are gorgeous! Btw, do you know a safe proccess to make soluble fluorine compunds from fluorite crystals?

[@Psychx_]

I see you are using a break hand vacuum pump aswell :D Since the summer holiday has started, I've been spending a lot of time experimenting purifying various anorganic substances and growing crystals. When going through liters of solution and/or you got a very fine participate, that pump definitely substitutes for a forearm workout. My veins pop out now, but only on my dominant arm. Gotta process even more solution and make it symmetrical xD

[@integral_chemistry]

Glad you noticed that! I honestly prefer it to the vacuum pump in some situations as you get a more careful control over how strong a vacuum you pull.. I've had issues in the past pulling too strong a vacuum on vacuum distillations and making a huge mess.. And yeah it definitely becomes a forearm workout! Thank God tbh, forearms are the worst thing to hit in the gym

[@VoidHalo]

Oh man, growing crystals is great fun. I got some really weird curved crystals that looked like claws from sodium or calcium acetate, I forget which. They were creeping up the sides of the container, as crystals do, and as they grew out of the side, I guess gravity pulled them down and made them curve right back into the container with these beautiful ridges running along it. It's weird the way the crystals can creep up and over the side of the container like that. Even creeping all the way to the table and sticking your container to it.

[@Psychx_]

@@VoidHalo AFAIK there's always a few molecules thick water layer (i.e. from moisture in the air, from the solution inside, etc.) covering the surface of the glassware. This also allows ions to travel and helps the crystal climb the side as evaporation does its thing. That teeny tiny amount of water can also be enough to disturb water-sensitive chemical reactions, which is why the glassware has to be dried before some experiments.

[@rogermorrison2968]

@@VoidHalo Возможно, вы были в шаге от великого открытия.

[@tomzwinkels6940]

Very cool many can you maybe give some exotische reaction with KICl4

[@highlandlab1924]

Does it burn sugar like other oxidizers? Imagine a purple smoke rocket.

[@officermeowmeowfuzzyface4408]

Should change that to: *DOES NOT WANT TO EXIST*

[@jayc2469]

I have a pot of Potassium Iodide Tablets with all this threat of Nuclear War and Pootin mouthing off! Any good? They're bloody expensive lately too! Scarce in Poland as to be expected

[@christiannorf1680]

What kind of monster would skip the crystal part?

[@RiehlScience]

Do you think potassium chlorate and iodide would work? It would get around the problem of sodium being present, and it’s much easier to get for most people.

[@experimental_chemistry]

Alkalines chlorate are restricted here in the EU while the bromates still aren't.

[@zenongranatnik8370]

Looking at half potentials, theoretically it works in acidic solutions

[@Exotic_Chem_Lab]

Cool

[@Caberbalschnit]

Soooo, you made it just to make it decompose? I love the chemistry videos here on youtube. Just wish there were more uses for the products made in videos like this, that we could see, other than decomposition. I mean watching solids and liquids change color or ignite are cool and all from a scientific standpoint. But eventually get boring. Im prolly the only one on youtube that thinks like that, but still lol.

[@freakwilly3559]

What lofi song did you use during the crystal montage?

[@CatboyChemicalSociety]

Cursed idea but can you use this instable salt as a chlorinating agent in place of SOCl2

[@integral_chemistry]

I hadn't even thought of this cursed idea but I love it! I'll definitely look into it and see if anything comes out of it

[@lharsay]

What's the decomposition reaction of the salt? Is it like: KICl4->KCl+I2Cl6

[@jimsvideos7201]

Yellow chemistry, partially redeemed? 😅

[@200-b8k]

amazing video

[@brettmoore3194]

I asked chemdelic but no response. So i was asking if GABA could be hydroxylated by hydrogen peroxide to form the gamma hydroxy butyric? I know the gbl pathway but i like to find different starting material than, what is published🎉

[@Yakkityyak248]

If we don't like crystals? Heaven forfend

[@FK-ng2gf]

crazy

[@rogermorrison2968]

Надо было отфильтровать и высушить в атмосфере Cl₂.

[@Satori-d6y]

Lyophylize.

[@gimplekin3629]

when you say it shouldn't exist, and yet it does. that leads me to think you don't know what you're talking about.

[@integral_chemistry]

Lol just a way to get people who wouldn't normally click on it to give it a shot. Technically it's not a lie because "should not exist" is vague and subjective.. like you could make the argument cars should not exist

[@williambradley611]

Like this comment

[@createvideo561]

Nah I'd win

[@VoidHalo]

Dislike your comment? Okay. Not that it matters for anything. Doesn't decrease your likes, you can't even see how many dislikes there are. I guess Google doesn't care about marketing psychologically addictive products to children who are too young to agree to the terms of use. But they do care if their feelings get hurt.

[@integral_chemistry]

Yeah I really miss the dislike button.. you can add it back with a plugin but it was pretty important for getting accurate feedback at the very least

[@williambradley611]

I also miss the time when you could see the dislike count

[@createvideo561]

@@williambradley611 then from the heavens I summon myself to create a new platform with nothing but dislike buttons

[@taktsing4969]

I don't think therefore I am not

[@amandahugankiss4110]

i should not exist..

[@DangerousLab]

Getting >100% yield because you are not a Chemist🧪, you are a Chemagician🪄 (Always sad to see when yield went wrong...)

[@integral_chemistry]

LMAO I think that's gonna be my go-to explanation when I exceed the 100% mark in the future

[@nzcym]

It may become a great way to carry out haloform reaction. **************************************************** en.wikipedia.org/wiki/Haloform_reaction

[@philouzlouis2042]

Reminds me of the iodoform reaction in organic chemistry that allows solid CHI3 yellow to precipitate out of methylketons, acetaldehyde or origin alcohols subsequently oxydized into ketons or aldehydes (Me-CHOH-R with R = H or hydrocarbon moeity) CH3-CH2-OH + OI(-) --> CH3-CH=O + H2O + I(-) (ethanol case - pimary alcohol) CH3-CH=O + NaOI --> CHI3(s) + HCO2Na + NaI + NaOH (CH3-)2CHOH + OI(-) --> CH3-CO-CH3 + H2O + I(-) (isopropanol case - or secondary alcohols) PHZ