@@ExtractionsAndIre Sounds like you're saying "antinomy"! ^^ think "anti-money" instead. (In french it's called "antimoine", litteraly "anti-monk"! Some say it might actually be the origin of the element's name, as quite a few monks were versed into alchemy, and might have poisoned themselves with it.
Great vid. Massive color changes. Distillation of a metal salt at less than hellish temperatures. Rarely seen metalloid chemistry. Success. What more could we want? Thanks Tom!
Thanks for the comment! I thought this was going to be pretty boring when I first started so I'm pleased at how nice and interesting the video turned out
That color change is possibly due to a peroxo-metal complex. I know titanium likes to do that. It dissolves at an ungodly slow speed in HCl forming a purple solution; and, when you add hydrogen peroxide, it suddenly goes a very intense and bright orange color as it forms peroxo-titanium chloride.
I remember working in an analytical chemistry lab and being super careful with mg/L solutions of this stuff because it was toxic... here you are grinding up the raw product in your back yard 😄 I wish you a long and prosperous life.
We can make Anti Money, but only with great difficulty and much energy expenditure, as the coinage has to be crashed together in the light, at practically _the speed of dark._ ;)
Nah he wouldn't be able to have any of that here on Earth because the matter that makes up our air would react very violently with the antimatter that makes up the anti-cloth that the anti-people use to make their anti-money.
Good result. Antimony butter fumes are extremely (fatally) toxic when hot, so the outlet tube shouldn't be left open but connected to bubblers of water or ammonia, or at the very least silicon tubing that runs any fumes far away from you. Luckily no one died in the making of this video.
I wonder if the solids left over from the distillation aren't primarily antimony oxides (and whatever other impurities, but that Sb looked very nice and crystalline in the beginning. Arsenic halides are also volatile, so be careful). Mellor, Vol 9 , p. 469 (sciencemadness library) has some information on the preparation of the trichloride. Peroxide probably wasn't the best oxidizer due to antimony's tendency to form oxyhalides. Nitric acid in small amounts would probably be better. Since the trichloride decomposes on distillation, you can probably recover more by dissolving the residues in HCl under reflux and distilling again. I guess distilling it in a current of dry HCl or even Cl2 may prevent decomposition. Awesome video as always, love the style mate!
Probably didn’t need to pump any water through your short path. But I’ve tried that as well before. Just using an aquarium air pump works pretty well. The air cools it enough. But not too much. Cool synth tho
Good thought, I just didn't know how it would do with the short-path. The SbCl3 was still coming through real hot, like 100C, which was fine but without the water cooling it might have been 150C which is pretty high... Probably still fine though. Also, I don't yet have a air pump I could use here. I've got to build one for the ozone project so maybe this will be a solution I could do in future
This is the most jank yet through and interesting chemistry’s video I’ve seen. I love the old stuff and really appreciate how far you have come as a creator, great job!
THANK YOU for this video!!!!! I was soaking some smd components (ie resistors, diodes capacitors etc) in hcl to get rid of the solder and it turned a deep lavender\purple colour. I also wondered what h2o2 would do and I got that same colour change to orange. Looks like I was dealing with antomony. You've saved my brain a LOT of trouble trying to figure this one out. Big thumbs up to you!!!!
I found another comment saying it might also be titanium: I will quote what Ian McClellan-Johnson wrote: That color change is possibly due to a peroxo-metal complex. I know titanium likes to do that. It dissolves at an ungodly slow speed in HCl forming a purple solution; and, when you add hydrogen peroxide, it suddenly goes a very intense and bright orange color as it forms peroxo-titanium chloride.
Antimony is used to harden lead alloys because it’s cheaper than tin, It also increases molten lead’s fluidity, and cavity filling properties. Hard lead is used in ammunition and lead-acid batteries. I’ve noticed that Antimony washes off of my hands VERY easily. So much more so than lead, which is by far the hardest thing to wash off my hands
If you want to make a better (and cheap) heater for your condenser re-circ water, I have found that if you use one of these generic plastic ammo boxes (or dry boxes of that style) you can drill some holes in the top and install an immersion heater. I do not mean the expensive ones from a scientific catalog but an element for a small home electric hot water heater (very cheap) through the side. You could use any container that has a top and I think probably a cooler if you wanted, but it's not necessary. You need to have a lid and a hole for a thermocouple wire. Do not let the heating element itself to touch anything but the water. You do not want it to be airtight so vapor can escape. You will need to top off the water periodically but you will worse with your open rigs. You can use a temperature controller if you like (but more expensive) but a rheostat is fine and an on/off (percentage of time) controller works just dandy for this as well. You can easily control the temperature to about 1 degree F once you get there (it takes a bit of time, but then you watch it and you have a much bigger dash pot at that temperature). Find the right place on your percentage on off controller (cheap) and boom. You can use it over and over again too. I prefer to use silicone tubing for this type of heated water though I know it's not needed and is more expensive, it is so much easier to work with and again you can use it over and over again, even for much hotter stuff. I really enjoy your channel! I don't know if that helps, but it works like a champ. Cheers!
One can use a simple Lamp Dimmer of appropriate wattage to control any resistive heating element, either the kind you mentioned or just incandescent lightbulbs. I have boiled water in a glass jar using the heat from a 500-watt (sealed beam) spotlight right below it, and it could go MUCH hotter with other fluids! A slight note of caution is in order if using glassware that may not withstand the temperature and/or rate of heating, and halogen bulbs will not last their rated lifetimes if used on dimmers. For additional safety, the lightbulbs could be put alongside the heated container, though there will be some loss of efficiency as the convective heating fraction will tend to be lost in that configuration. One may be tempted to 'be more efficient' by insulating the entire heater, but be wary of sealing up hot lightbulbs. They do need some cooling, and the normal wires and sockets even more so. Special bulbs, sockets and fiberglass-insulated wiring are available, as used to illuminate baking ovens; those can be run continuously at 560 K (550 ºF, 285 ºC, ) or a bit hotter. Silicon and Teflon insulated wires cannot long be used at such elevated temperatures.
Nice one friend, good suggestion. Also, for higher temps consider not using water at all but instead, place the element you mentioned in a metal box with sand inside. Old spiral stove elements are also good and cheap. I go to the local recycling and get such things for pretty much free. For really high temps, coat the glassware with a 1cn layer of clay that has a lot of sand worked into it so it doesn't crack too much when it dries. The clay supports the glass when it gets above the softening point. Pout a layer of Al foil around the clay to hold it all together. Regarding the element construction and if its up the the task. The outer casing is some form of steel (melts at 1500˚C), Inside is nichrome wire (also good for about 1500), surrounding the nichrome is a white powder which is magnesium oxide (good for 2700˚C). Also. I really like using the REX-C100 PID controller from ebay or aliexpress for about $10. They are great. By default they max at 400˚ but you can tweak the settings and get 1300˚C out of them. In conjunction with a simmerstat scavenged from the same old oven the element came from, and heat proof wire which I recommend you grab while you are at it.
Watching this vid again. Others have said the same, but I would like to confirm: there is Ti contaminant in the acid. I have the same brand and the same problem. It produces the same purple coloration of titanium trichloride. Then gives the orange tetraperoxo complex when the H2O2 is added.
I must've missed/forgotten that being mentioned, because that comes as a surprise to me. Titanium! That's a bit odd, how does it make it's way into there you think?
@@ExtractionsAndIre Yeah. Came as a surprise to me too. Not that I have done full analytics yet but nothing else I know matches. I think Ti4+ in the acid, reduces to 3+ when teacting with Mg or Zn (and other metals). Then hydrolyses to make fine cloudy precipitate. Try adding a little peroxide to the straight acid to see if complex occurs. The orange / beer bottle colour is indicative of peroxide complex. I have taken to distilling my HCl before use at the moment. The plus sude is that I am more accurate since I know the conc of the azeotrope. If I need higher concentration then I can always make some HCl gas to bubble through.
I've heard you say that the HCl you use is often contaminated with iron. Three colors associated with iron oxidation states are orange-red, green, and purple. I don't know how much iron is in the HCl, but this observation is worth considering.
To me, "Antimony" was a girl from a webcomic about a girl going to a boarding school for science next to a magic forest. Imagine my surprise when I learned that it's an element 😆
This color change, purple to orange, is compatible with amounts of TITANIUM as impurities in this material. Because titanium trichloride (TiCl3) is purple, and titanium forms a red-orange complex with peroxide: [TiOH(O2)(H2O)3](+). This antimony was impure.
I did my engineering thesis about synthesising antimony oxides and as people said before, the white stuff is antimony oxychlorides or oxides. Main antimony source for my experiments was an old jar of SbCl3 which was very wet and hydrolysed. I had to manually scrape the white crust of oxychlorides from a few big crystals and then keep the chloride in a dessicator. I used to make solutions of SbCl3 in anhydrous ethanol and only in a beaker covered with some parafilm or the hydrolysis would occur. Maybe instead of distilling SbCl3 in dry HCl or chlorine, recrystallisation from an anhydrous solvent under nitrogen/argon wolud be enough? Also, my saples of antimony oxides/oxychlorides in ethanol would often change colour from white to orange the next day after the synth. Neither me nor my supervisor found out why it happened, but it might explain the orange colour. Probably nobody's going to read that comment after 4 years but hey, better late than never.
@@ExtractionsAndIre If so, keep going mate. Great videos. I miss the ones from the first E&F channel tho. Tbh I thought that if I ever see antimony here it would be the famous *unstable* allotrope but this is a nice surprise too.
The moment you said "trichloride" I first understood "trifluoride" and I remembered reading about Fluorantimonic acid and thought "Oh. This is gonna be interesting".
9:38 hehe, I'm one of those privileged chemists : we got our own glassblowers in my university. They do all sorts of _really cool_ custom glassware for us! (Which often is a necessity when you're doing unusual air-sensitive chemistry.)
@@piranha031091 The French say, its the fate of glass to break. which is a nice metaphor for impermanence (reincarnation). Its also part of the lamp workers clever business model. They get the rent paid when you break their stuff!
More inorganic Chem please! I signed up for inorganic 1 at school. It’s not required for grad school but I just wanted to take the lab. Then I found out it is only lecture and no lab! I made a solution of gallium chloride but I just filtered it and put it in a bottle after I made it becaue I didn’t know what to do next 😂(I’ve only taken 1st and 2nd semester chemistry so far, no distillations or extractions yet). But now I might try something like this. Also…. Make a gallium explosive 😁😁
Awesome, I love your videos mate. Can I just say, when you fondle your glassware over concrete it makes me feel very uneasy. Do it over grass and I'll enjoy your videos even more. 😁 Greetings from the UK.
Ah, yes, SbCl3. I used to sublime it under vacuum at my uni to purify it, to make organoantimony compounds. Freshly sublimed crystals hydrolyze very fast in open air, I'd say in about 10-15 seconds a small piece becomes a small acidic puddle, that fumes HCl. Stained all my gloves I wore, had to change like half a dozen every time I worked with it. Good times.
Try to make some indium chloride. Just put some Indium or metallic indium waste into some hydrochloric acid and hydrogen peroxide. It sublimes at round about 418°C forming an iridescent snow as it resublimes what I think is really cool.
@@ExtractionsAndIre I got indium slag lying around as I melted some indium. Just for interest I decided to do some indium chemistry instead of throwing it away. The indium chloride solution was standing in my shelf for a couple of months until I was bored and looked up the properties of indium(III)-chloride. Eventually I boiled the solution in an ampoul, strongly heated the residue and saw the snow of the iridescent crystals forming as they resublime. Even though the reaction is still not that efficient due to yellowish indium oxide forming after strong heating. instagram.com/p/BnaxNGWnzsj/?igshid=4apurgb27t2v
I do this synthesis a mot and here is how I do it I dry distill antimony oxide with dry copper chloride in a simple wide 90° short neck into a double opening glass flask
Great book on sciencemadness library called chem of fire and explosives first few chapters deals w pyrotechnics, or fireworks production and this element in a salt form finds use in "star" production.
@@benjaminpainter378 i dont really remember. I believe i was curious specifically about catalysts and some organic chemistry methods, perhaps Friedel and Crafts, but also gold chemistry
Have you been able to make the explosive form of antimony yet? :) I've got elemental antimony for my collection, but I've also got antimony I've extracted from old tire weights and bullets. I've also got arsenic from old bullets, but this is about antimony damn it. Anyhow, I don't know if it's the extremely small amount of antimony trichloride I have in solution, but the electrolysis is depositing antimony onto the cathode, but it's not explosive. It burns with that pale green flame seen with antimony, but no boom.
what process do you use to separate the Pb from Sb? I guess I would try dissolving with HN03 then precipitating the Pb with NaCl and if this leaves the Sb in solution maybe an iron rod would drop out the Sb..
@@waynoswaynos I dissolve the lead in concentrated acetic acid with concentrated hydrogen peroxide. The antimony acetate that forms is a white solid precipitate. It is mildly soluble in water, but I know any of the white precip is not lead acetate so I can mechanically separate the two compounds from each other.
@@mwilson14 I found this recently that you might find of use. "Patent US1584151A Shimadzu Genzo, Process of manufacturing lead oxide". Quite a simple set up. Makes such a fine powderded Pb that the conversion to Lead Acetate would be almost instant. Quote "…this invention removes all these drawbacks, and consists in taking pieces of metallic lead into a revolvable drum, and revolving the drum slowly at a rate of about twenty-five revolutions per minute, blowing the air into the drum all the while. Then the heat generated by friction and oxidation (within the drum) of the lead pieces will raise the temperature within the drum and maintain it at not less than 60° C. The friction too will form new metallic surface on the lead pieces, which as soon as formed will be converted into lead suboxide by the heat and the oxygen in the air. The film of lead suboxide thus formed will be reduced to powder by abrasion, but not by lead pieces striking against one another, like in the case of a common tube mill or ball mill. When the lead suboxide film is abraded off, a new metallic surface will be formed, which as soon as formed will be abraded off as before, thus continually producing fine powder of lead suboxide intermingled with metallic lead powder directly and in dry condition. The lead suboxide powder intermingled with metallic lead powder thus, obtained is so fine and chemically active that if a lighted match be applied to part of its pile or a few drops of water be dropped on it, oxidation will instantly commence, igniting it briskly…"
Well thats fascinating. I want to synthesize butter of antimony from antimony trioxide instead of the elemental metal. Sb2O3 + 6HCl => 2SbCl3 + 3H2O. Have to so some stoichiometry to get it close. if I distill off the water what is left? SBCl3 and SBCl5?
I should mention that the impure antimony oxychloride, chloride, and pentachloride eben hydrolysed might work for my applicaiton which is mixing it with an oil and using as a browning agent on steel rifle barrel. Butter of antimony may have been impure to begin with. And its completely removed after the fact.
I thought about Cl2, I don't often pass up an opportunity to use it, I've stated my love for working with it a few times before. But I think antimony is just a bit unreactive, so we'd need to heat the system too, and really dry the chlorine, and I think it looked just a bit messy. Glad I took the aqueous route
I load and make my own bullets and lead wheel weights are great because it has a touch of antimony with the lead making the bullets a little harder. It's great shit!
Hi, did you distillated sbcl3 twice? The first time the excess amount of HCl was temoved? And the second time, sbcl3 itself was boiled? I didnt understand this part... Wat was the temperature? First time it was about 100 C and the second time it reached boiling point of SbCl3, i.e. 230 C? I need to synthesize SbCl3 :(
That's exactly it! You probably don't need to distill the SbCl3 if your antimony and HCl are pure enough. But I wanted very pure SbCl3 so I distilled it. I also just wanted to see if I could, as reaching a boiling point over 200 degrees C was a challenge!
@@ExtractionsAndIre Thanks for your reply. Yeah, I have pure Sb2O3 so I think the first distillation will be enough. And can I just use room temperature water for the first one as circulating water? And I have to add 20:80 HCl:Water ratio to my oxide to reach to the azeotrope? Right? Is the color of the azeotrope as orange as the one you showed in the video? Or your color is because of impiorities? Why should we use distillation? Cant we just let the azeotrope to evaporate freely and gather the remaining material as SbCl3?
Me too. I was thinking air condenser with maybe hot air input. I have a diabolical plan to make a hot-air widget with tunable temp output. The key component is a big mass of temp-controlled copper. Would be just the ticket here I reckon.
@@jamesg1367 You can get really hot by heating with light, including infrared. The Sun, for instance, is about 5800 K, so sunlight can heat to about that temperature. (Actually, hotter than that, if enough UV photons are concentrated.)
Is there any chance, that you still have that antimony trichloride and can attempt making pentachloride by reaction with chlorine gas bubbling through the liquid? It would be awesome. Apart from numerous uses as a catalyst and oxidizer, it appears, that it can be converted to fluoroantimonic acid, if treated with concentrated HF. Always wanted to see it in work... Protonating benzene, dissolving wax... It's highly corrosive, toxic and such, but who cares when it's so cool. I'm just thinking of doing it in my lab. Is that as bad an idea as I think?
Fun fact: One of antimony's historical uses was as an addition to wine at Roman banquets. They'd drink the antimonial wine, which would induce vomiting so they could eat more. en.wikipedia.org/wiki/Antimonial_cup Later, slugs of antimony were swallowed to cause bowel movements, then recovered from said movements for reuse. So that's fun.
I've had to order a few things off eBay for it, and can't really film the video until it's all here unfortunately. Chinese eBay shipping times are often very long so I might not have everything until December.... Which is annoying but lots of other projects to work on in the meantime
+@@ExtractionsAndIre For some reason half of the Chinese stuff I ordered this summer from eBay never arrived. They claimed resending the stuff, but two months have passed again... problems in Chinese post? Last year everything still worked without problems.
@@user255: I get some weird results buying from China. The odd item is omitted, just never arrives. Sometimes a wrong item or not as advertised (pay for 5 pieces, get one etc.). The screwy stuff never has much value. I wonder if they know Americans just shrug when a $3 order item goes missing. But it's bad business. Makes me cautious, and sometimes I just don't buy from China if it's something I can't wait forever to receive, or can't do without. They're the losers in that game.
@@jamesg1367 Yeah, even when it's just few bucks I always use the money back guarantee, whether the item never arrives or it's crap. That's only way to stop the scam and polluting with crappy products.
It's very odd that antimony is somewhat toxic since I recently purchased some lead-free plumbing solder (I'm in the US) and it contains about 3% antimony (97% tin). A rather strange additive for solder used in home plumbing, perhaps it's just that unreactive in treated municipal water?
Australian kettle? That's Scandinavian design by danish company Bodum. Didn't know they were sold outside Denmark and suddenly it's used for super cool chemistry on the other side of the world
A family member once gave it to my grandma as a present I think... And my grandma thought it was awful haha so it ended up with my family and we already had a kettle so that's how I ended up with a fancy Scandinavian kettle to heat water for a chemistry lab. Good spot! I said it was an 'Australian kettle' because most of America uses gas kettles right..? And electric Kettles on our powerful 240V is where it's at 😎😎🤙🤙🤙
@@ExtractionsAndIre Hahahaha I haven't seen many in that color here either, so I don't blame your grandma for not liking this particular piece of Scandinavian design 😂 And I think you're absolutely right with the Americans, these things are much more common in places with glorious 230-240v. Your mad scientist youtuber colleague Photonicinduction even has a few videos overvolting kettles so they draw up to 8kW and boil water super fast 😀
FWIW I know bodum sells products in the states as well. I've not looked to closely to see if they sell electric kettles but I've definitely seen a french press and maybe a coffee grinder?
You forgot about its most important use of yesteryear, specifically as a medicine. Rich people would, when they thought they needed to, pour wine into little cups made of antimony overnight. The acid in the wine would impart a small amount of antimony salts to the wine, which you would then drink in order to give yourself the shitting pukes. People did this on purpose. If you weren't as wealthy, instead of wine in a cup, you would simply swallow a pill made of antimony to give yourself the shitting pukes. When you were done, you'd carefully fish the pill out and save it for next time. Typically, a family would have one or two of these pills and would use them over and over again for years. Also, in case you were wondering, the pill would normally go all the way through you. In order to make recovery easier, one would use a chamberpot instead of the outhouse. It's much easier to dig for (metaphoric) gold in a small bucket, than in a big hole in the ground.
