Recrystallization of Sulfur

[@nunyabisnass1141]

For those that may be curious, a cooler with ice can be a safe alternative to chilling a mixture that has flammable solvents. You may not want to use that cooler for anything else afterwards though.

[@xXCatalystic37Xx]

Very good video. As a fellow chemist I enjoy all the nuances and subtle comments you mention off hand. Also as a fellow educator, I appreciate all the safety you discuss.

[@TheChemistryShack]

Really beautiful! I've never seen crystalline sulfur like that!

[@shonaoneill5151]

TheChemistryShack agreed, I would love to make some, but don't have a fume hood......so, it's really nice to see.

[@BackYardScience2000]

@@shonaoneill5151 , you don't necessarily need a fume hood. You could so it outdoors on a day with some decent wind. That's what I've been doing anyways while I collect the supplies to build a new fume hood.

[@jhyland87]

@@shonaoneill5151 I don't have a fume hood either, but you can still just do it outside, which is how I do it.

[@magnuswootton6181]

nice little seeds! notice how they didnt stick to the plastic, they only stick to themselves, this is also a really cool elemental crystal too, how come it isnt metallic?

[@TheBackyardScientist]

Very nice!

[@BackYardScience2000]

@Bill Howitzer I'll help you with that. 🤘👊

[@uxleumas]

@Bill Howitzer hello

[@LFTRnow]

This works, and very well, but I found several issues. 1) after you are done retrieving your sulfur, it out-gasses xylene(s) for some time after, days if you spread it out. Heating it helps, but you have to be gentle or you will easily melt the sulfur. It seems the xylene(s) act like a flux (think of soldering) which makes the sulfur melt easily and evenly. Without it, it will just harden into an orange mass. 2) It uses a LOT of Xylene(s), even recycling it you go through a lot and quickly. Plus recycling it only will absorb about half as much new sulfur, which gives you an idea how much sulfur is locked into your xylene(s). 3) it is a crazy amount of work and cost in the end. BTW, I found using an ice bath for doing the crystallization helpful, an IR thermometer was a handy tool, and finally, having an ice/ice-water filled round flask placed over the near-boiling xylene beaker was helpful to keep fumes down and reduce waste, though that was fairly small. All of these tests were outside, away from the house. (my tips to follow)

[@LFTRnow]

The short answer so far is buying pure sulfur if that is what you want. However, experimenting did improve on the 3 issues mentioned above. What I found helpful, was to take the pure or fairly pure sulfur from a few small runs of the method shown by Doug, but then to heat the mixture up on a hot plate slowly raising the temperature to 110-120C while keeping some xylenes in the beaker. A 400 ml beaker was used and keeping ~20+ ml of xylene(s) was a reasonable amount. The layers stratified while molten into the lower layer (~2g/cm3) orange molten sulfur, followed by a black filmy/syrupy layer of contaminants, and then an upper layer of clean (but saturated with sulfur) xylene(s). When done stratifying, you can pour in more bad/original source sulfur to separate it, or at any time, stop and let it cool down. The upper layer of fairly clean xylenes can be saved with gentle pouring, and the rest is a pasty layer of dirty xylene and contamination. The sulfur forms a hard mass and the gunk mostly stays on top and can be washed off. Wash off all the gunk and remelt with more xylenes to clean again. Repeat as desired. Again, it is helpful to cover the beaker while doing this with at least a watch glass (10 cm worked well with 400 ml beaker). Use caution when heating up and lots of xylenes initially as it helps prevent "burning" the sulfur. Don't boil the xylene. I found that when it started bubbling, it was too hot, but a perfect time to add more impure material as that cools it down and moves along your process. 130C is too hot - both for the xylenes and for the sulfur, stay away from temps much over 130C or you will both boil the xylenes and turn your sulfur into hard to remove goo. It was also found that if the xylene gets too dirty, simply adding more will cause it to separate back into a dark contaminated layer and a clean one and greatly improve the product quality. Also interesting is trying a borosilicate (pyrex) pipette to remove the lower layer. It works, but you must heat it up first and be ready for the inside of it to cake up. Easier is to keep cleaning the sulfur, then either let it cool into a hard mass, or pour it in water to get easy to remove (though hard) beads.

[@glassmyth]

@@LFTRnow thank you; I am attempting to make TEOS from scratch and I will be referencing your notes.

[@Chollanger148-pv8jp]

You can sublime sulphur by heating and then pour it to condense it on a cold surface

[@FreezeDriedGirolles]

You should totally do a Q&A! I'm sure everyone would be interested in knowing more about you, and the particulars of running a home lab.

[@DougsLab]

+Freeze Dried Girolles I think that'll be the 1000 sub special! Stay tuned. :)

[@Qn0Bi6]

In my opinion you could use a roundbottom with refluxcondenser attached, so that the fire hazard is less. To cool it, you could use an ice bath if you don´t have a fridge, that is suitable for flamable solvents. Great video btw :)

[@AuBjorn]

Always enjoy watching your videos Doug's Lab. 👍 awesome techniques and explanations.

[@lightvsdark21]

Yay!!! Soooo glad you're back! I hope you keep making these great vids. I've so enjoyed all your vids! Thanks for making them.

[@GMCLabs]

Nice work, could have placed a round bottom flask of cold water during the heating stage, to condense the fumes though. Also would sublimation of the sulfer, and bubbling though cold water purify it as well as xylene recrystallization?

[@peterholm339]

Would it not have been safer doing the recrystalisation in af reflux set-up to prevent the formation of flammable vapours?

[@budove58]

I subscribed. I really like the way you do your videos. You explain things thoroughly and especially point out potential mistakes to watch out for. I appreciate that. I love your "underground" lab setup too!

[@TheDuckofDoom.]

While blends vary by refinery and season, toluene is a significant component of high grade gasoline as it has desirable octane boosting properties. esp if you can find alcohol free 92octane fuel, or unleaded or "low lead" 110+ racing gas or aviation gas(note it uses a different octane scale than highway fuel) may be able to use fractional distillation to get the toluene. Around here a gallon of toluene is the same price as xylenes. 50/50 toluene and MEK is a very strong solvent blend btw at least for greases, varnish, eats up nitrile gloves.

[@redoxalchemist9754]

Awesome yield! I've never seen crystallized Sulfur before, very beautiful! Maybe you could melt it down to show the polymer like allotrope of S. Glad your back!

[@zinckensteel]

easy way to upgrade to reflux: use a loose sheet of plastic wrap on top, pushed in a bit to form a shallow cone, and then fill it with salted ice cubes. This works great with other solvents, not 100% sure it would work with xylene considering what you stated about the vapor pressure being similar to water. It also has a safety feature: if the condensation can't keep up, the pressure builds a little bit and pushes some ice-cold water over the side, providing vapor-change cooling to the hot plate :-) ..then again, if you're refluxing, you could use a more expensive solvent.

[@electrotoxins]

"boiling xylene is no joke" *constantly waves unprotected hand around boiling xylene*

[@electrotoxins]

great video though, sulfur is one of my favorite elements despite its difficulty to clean up.

[@Petemate69]

Can vouch for this, i had a reaction go out of control after dropwisre addition and hit me in the eye through safety glasses and fumehood sash. Good times!

[@nind3282]

What was your %yeild for this recrystallization?

[@BackYardScience2000]

You probably won't get an answer as Doug has went awol again. But it looks like it was a pretty good yield. If you were to distill the xylene you could get a nearly 100% yield. Minus any impurities of course.

[@andreatgrowwithme6901]

Nice video. Have you any idea on what the pH (range) of disolved sulphur might be.

[@Alex-ee5pl]

This is like my fifth time watching this video and I lolirl'd when I noticed you sharpie'd an 's' onto your can of xylene(s). Nice going Doug!

[@derrickfoster644]

my first re-crystallization was of sulfur from powdered insecticide using dimethyldisulfide from paint stripper. the yield was horrible (think i got about a gram or two) but the crystals are so pretty. i keep them in a vile and just like to look at them. this process seams so much easier than what i used congratulations on your videos they are very well produced

[@craigcain6553]

thanks for the info,gonna try dmso see what that does,99% percent pure at farm stores for horse probs,really cheap

[@craigcain6553]

just tried got immediate super saturation at room temp, if anything can purify the sulfer to the 99.99% range

[@nunyabisnass1141]

Craig Cain I used garden acidifyier sulphur pellets. But it contains some clay based additives that can be separated by dissolving in water. The sulphur will remain.

[@anyideasa.i.8090]

I have to say the best chemistry channel to exist. Now this is completely off topic, but could you in the future explore the making of epoxy using the glycerin method.

[@wb5rue]

I suppose if you wanted to get very large crystals of sulfur you could wrap the flask in some sort of insulation and let it cool over several hours

[@poecilia1329]

Very helpful.I will do so.

[@JavDSilva]

awesome! i had never seen sulphur being so crystaline and shiny

[@bonbonpony]

It would be cool to see recrystalizing it as some actual geometrical crystals, and I mean some big ones :J

[@Kongfufrank]

what degree of purity after recrystallization?

[@glasslinesmadhes]

Flat bottom flask multineck parallel may be useful for such reaction with thermometer pocket and power dropping funnel. Useful video.

[@gazzarrr666]

Just a thought re keeping the xylene vapours in and minimising loss of xylene. You could put up a crude ice-bath on top of the beaker to set up a simple reflux system. Obviously, need to make sure the bowl you put on top isn't to heavy / doesn't fit too well to avoid breaking the beaker (that Would be a disaster). Some water might then condense out of the air, but that would be easily to remove from the solution (before cooling) with dried silica gel / molecular sieve.

[@sandhyaprabhu6996]

waaaaw!! super impressive. tq for the video. i was actually looking for recrystalization information when i came across this on YT.

[@hlpayne]

Seems like a Soxhlet Extractor would be perfect for that. Have you considered a Soxhlet with another solvent?

[@ProjektOchExperiment]

Awesome video Doug! And congratulations to 1K subscribers!

[@KevFlaAVCHD]

Good lab practice is to raise the thermometer off the bottom of the beaker and keep it vertical, as contact with the glass/hotplate will give a higher indicated temperature than the surrounding liquid due to conduction.

[@pietrotettamanti7239]

I've seen only 2 videos of you. Both about sulphur. Both awesome. I love sulphur. Subbed.

[@kimandreolsen6298]

Nice video! Mind if I ask what the yield was? :)

[@kalolord]

If you can't put it in the fridge, putting it on an ice bath is a good alternative (after letting it reach room temperature on its own).

[@LFTRnow]

What was the mass of recovered sulfur? And, if you have done this since then, how much does that vary? It looks like the differential in solubility is enough to use the cold saturated solvent over and oven by simply heating, dissolving and cooling/recrystallizing over and over. Nice work.

[@magnuswootton6181]

he lost some when he poured out the solution, it was sulfur contaminated, cause it was still yellow not clear.

[@JDeffenb]

glad you're back! can't wait for more videos!!!

[@xelionizer]

Reminds me of my early piperine extractions. Oh boy if it was only hat easy to recrystallize piperine...! Thanks for posting all your nice videos;) Play safe!

[@ammelr]

Cool process! But maybe you should get a boiling flask and reflux condenser?

[@AuBjorn]

I do realize this video was made 9 years ago so perfectly understandable If you do not know. I was wondering what final yield might have been with the initial 50 sulfer

[@bpark10001]

If you save the solvent, won't contaminates accumulate in the solvent to eventually contaminate the subsequent batches? This would be true especially for oil-type substances.

[@AvianYuen]

8:59 *exhales as he destroys the crystals* ......."For chemistry" 😭

[@alexanderx33]

What is being removed here? Also wouldn't whats being removed accumulate in the solvent if you reuse it?

[@rndriver5550]

How can we dissolve sulfur in oil

[@StevenSchoolAlchemy]

I shared this video to a playlist on my channel.

[@grandpabear5493]

Please forgive my ignorance! Filter the solution into another large beaker. This will remove all remaining contamination? So NONE of the impurities will dissolve in the Xylenes??

[@monto39]

What was the yield %? (did I miss it somewhere?)

[@InfiniteExia184]

The pure sulfur looked so shiny and I wanted to eat it

[@ArmoredSoul1]

This urge is why I could never be a chemist. I can resist the urge to put things like mercury in my mouth in my day to day life, but if I said, worked with it on a daily basis I'd die.

[@spiderdude2099]

InfiniteExia184 I don't recommend it.

[@jbrev7951]

There is people eating this yellow sulphur for health. I have done it a couple of times , do feel better but cant say if its good for the long run. dip it in sugarcube or on bread , just one cube side or breadbite size

[@uxleumas]

@@jbrev7951 it could be the placebo effect if you're serious, don't eat sulfur please (you probably wouldn't die very soon but just don't)

[@bonbonpony]

Could this crystalline sulphur be now used to produce sulphuric acid?

[@ogreth9438]

Can you make larger crystals?

[@plazmatter]

so can you make a giant gem?

[@squirlboy250]

Couldn't you get much larger crystals if you cooled it down real slow?

[@bpark10001]

If you don't filter the hot solution, are you NOT purifying?

[@christopherleubner6633]

This is very useful if you have to get sulfur from agricultural sulfur or other less than pure sources. ❤🤓

[@shahabjaved1118]

doug's lab does it become water-soluble after this recrystallization?

[@S.ASmith]

If you don't have, or can't afford a, fume hood then a respirator is always good as well. Don't forget to make sure you've got the correct filters too. If you do get a fume-hood make sure the Flue outlet points to the sky outside, not towards your neighbour's house.

[@ianboard544]

Isn't Goofoff xylene?

[@phonotical]

are these sped up

[@---xb3tv]

does it has smell?

[@conevin2479]

Umm I'm not rly good at chems lol this might be a dumb question but could u use isopropyl alcohol to dissolve the sulfer?

[@masterdraw10]

how about crystallizing potassium nitrate again?..

[@jeanpierredaviau7478]

Would acetone dilute sulfur?

[@napoleon_bonaparte2462]

One thing you should note about heating xylene, is it's flash point, 30 deg. C. This means that if any of it's vapors come in contact with your hotplate (which may reach to 100+ deg C on setting one), they are likely to spontaneously ignite. If you left it sitting open near a hotplate like that, there's a risk of the vapors flash igniting and trailing back to your beaker resulting in explosion.

[@EpicXXProductions]

+Bloodmoon Flash point is the temperature at which a vapor/air mixture can react with oxygen, that doesn't mean it will ignite at it's flash point, or even close to it.

[@jpdemer5]

NATO: True enough. There is the danger of xylene vapors boiling out of the flask and, being denser than air, flowing down to the hotplate, where the on/off switches - certainly well above 30ºC - present a potential source of sparks. Lots of lab fires are started this way, although more often with more volatile solvents like ether and acetone. The take-home lesson is, don't boil flammable solvents in beakers on hot plates. Doug was careful to keep the xylenes well below the boiling point (ca. 140ºC), but that means attending to the setup constantly - you don't go to lunch and leave the hot plate on.

[@daveb5041]

In America you can get toluene for 14$ at sherman Williams paints in gallon cans . I used to use it to make 110 octane gasoline

[@juvanyalbraka9407]

Toluene Not available Is there an alternative substance

[@zodd0001]

I make you congratulations as ever but do you know how much has been dangerous this experiments ? You know about dehydration with sulfur with production of poisonous sulfhydric acid in gas form ?

[@shanejohns7901]

It seems to me that you should add more sulfur to the xylenes to just the point where it no longer goes into the solution. And once you realize that you have a tiny bit of sulfur that won't go into solution, add a sufficient amount more of xylenes to allow that bit of sulfur to go into solution. Then, and only then, should you cool it down to cause the sulfur to crystalize out.

[@chemistryofquestionablequa6252]

That's how I'd do it

[@andynon6226]

Hey there Doug's Lab, would this work for sulfide minerals such as Cinnabar for growing pure large crystals or is the chemistry very different for sulfide minerals. Great vids by the way, very informative.

[@alllove1754]

Thanks, just learned something today because of this. I did NOT know sulfur was dissolvable by anything I could get my hands on. It's funny how a simple reaction like this lets you know that someone knows their shiz

[@isaackalashnikov3681]

You will never be a w o m a n

[@alllove1754]

@@isaackalashnikov3681 ask yourself something: why is that even on your mind? Everyone can see this, btw.

[@GTLmaster]

you can tell me about paper reference this procedure

[@krap101]

What happened to Doug?

[@kullanicikullanici3206]

Hello. .bana türkce dilinde çeviri yapıp gonderebilirmisin. .o.kutudaki nedir hangi kimyasal

[@danstone_0001]

I have DEGASSED Sulfur in pellet form, how can I make sulfuric acid for the purposes of making lead acid battery electrolyte?

[@RaExpIn]

Have you seen my video about sulfur or is it coincidence? :) It's really fun to recrystalize sulfur, but I thought there is no use to it or is it? I mean you can wash out sulfuric acid that forms, when i'ts stored for a longer period of time, but all in all. Is it needed for a Grignard reaction to make thiols with sulfur?

[@DougsLab]

+Random Experiments International Totally coincidence! Nice video though. I subscribed! You can see what I did with the sulfur in this video: kzbin.info/www/bejne/pYraaWyfmsuZl5Y

[@RaExpIn]

I have seen that video ;) Nice synthesis!

[@FlashBlowout]

Excellent tutorial thanks for sharing it

[@Austingame]

+Doug's Lab Hey, i know this is kinda random, but i wanted to say thank you for inspiring me a lot lately. I have just started my own chemistry channel and i hope to become a chemist when i get older. I wanted to sincerely say thanks a bunch, and i hope you keep making awesome videos for a long time!

[@jeffreyyoung4104]

Beautiful recrystallization Sir! It reminds me of the old name for sulfur crystals, Flowers of Sulfur. I understand filtering the sulfur for mechanical impurities, but what about chemical impurities?

[@petermorgan679]

Left in solution for the most part

[@MadScientist267]

In the process of crystal formation, one of the things that tends to take place is the lattice pushing impurities out as the crystal forms. Anything with an incompatible structure can't easily become part of the growing mass, resulting in purification.

[@jhyland87]

Anyone have any suggestions in regards to how to clean the glassware and equipment after recrystallizing some sulfur? Obviously it's soluble in toluene and xylene(s), but is there another solvent/method/trick that can do it at room temperature and doesn't require more highly flammable and stinky vapors?

[@LucS0042]

How do you know the impurities didn't also get dissolved into the xylenes and subsequently recrystallized with the sulfur?

[@DougsLab]

+Luc Serre That can happen! I am relying on this method to select only compounds which exhibit solubility in xylenes very similar to sulfur. I don't think there is much out there that fits those requirements and is also found in my raw sulfur, but it is a definite possibility. Another way to achieve very high purity is to sublime the sulfur in a vacuum. Unfortunately, I don't have the apparatus for that, so I have to take the best I can get. :)

[@ib9rt]

+Doug's Lab Some dissolved impurities may remain in the liquid xylenes wetting the crystals before drying. Better purity could be obtained by washing the crystals with clean cold xylenes before the drying step.

[@rich1051414]

+ib9rt Or washing with a different solvent which sulfur is not soluble in. Heptane maybe? It would at the very least remove the smell of zylenes from the sulfur.

[@craigcain6553]

do you get better crystals using toluene or benzene ,just doing this for slow large crystal growth

[@bhartley1024]

I haven't tried xylenes but toluene once accidently gave me a large pea sized crystal. I had the sulfur toluene solution in storage and forgot about it, the container allowed the toluene to escape very slowly and I was left with a nice crystal when I found it a year or so later.

[@DeanBiddler]

Why don't you remove the stirbar when waiting for the sulfur to recrystallize? If you did it won't serve as a site for nucleation and you wont have to recovery the solid off the stirbar.

[@erwinrommel9509]

Robert Hoppe some of the product will stick to the stir bar resulting in product loss. It's better to remove it at the end when the product has dried and none of it sticks

[@drysori]

Instead of a refrigerator why not use an ice bath?

[@codymatthew9206]

Yay your back!

[@Spycyzygy]

How is toluene precious? I got a jug just like that xylenes one at ace hardeare

[@K0ester]

Canada, different restrictions

[@businessideasandknowledge9199]

Can u make a video on pesticide

[@gaming_chutta_malli]

Very nice

[@erwinrommel9509]

It can be misleading to say that xylenes are similar to gasoline. It's only similar to gasoline in the sense that it's flammable

[@ZomBeeNature]

What do you need with super pure sulfur?

[@ZivTheWyrd]

anything where impurities are undesirable :P

[@joeestes8114]

Great video! i didn't know that sulfer was a crystal, because its always powder and clumps.

[@erwinrommel9509]

Joe Estes anytime something is a powder is because it's had its crystal structure destroyed by mechanical stress like crushing,etc.

[@PauloConstantino167]

Doug, are you a chemist or do you do this for fun ?

[@bonbonpony]

I think the answer is "yes" :J

[@cannagorilla]

your awesome Doug!😉

[@lrmackmcbride7498]

Good news is with modern refrigerators using flammable refrigerants, they are explosion proof.

[@craigcain6553]

can you use gasoline or camp fuel

[@antejl7925]

No! Never heat gasoline extreme fire explosion risk.

[@ElGatoLoco698]

Can anyone tell me how to make liver of sulfur? Can I just mix sulfur with sodium hydroxide in some water?

[@michaelcorbidge7914]

.....oh, so you have to heat the xylene to dissolve the sulphur. With carbon disulphide it dissolves easily , but of course if you want crystals then the temperature factor is an advantage to employ, to make crystals using CS² would require evaporation of all the CS² .

[@jordancypihot496]

Ice bath?

[@jamesmatheson5813]

You should let.me ask if current can make sulphuric acid in a lead battery boil It will allow a current to make things boil instead of heat which will make.a huge improvement to millions of industries

[@TheDuckofDoom.]

rather surprised you weren't refluxing to avoid solvent loss.

[@uxleumas]

eh it's pretty cheap i guess

[@TheDuckofDoom.]

@@uxleumas Xylol is not particularly cheap at the retail level.($20 per gallon around here) But I was thinking more of generally reducing the fume load more for health, fire, and environmental reasons. Just a simple condenser with cool water, maybe just a round bottom flask with ice water set on top of the flask.

[@zanpekosak2383]

Toluene is in a lacquer thinner.

[@bhartley1024]

I like to cool it slowly to get bigger crystals.

[@bas12345654321]

I love recrystallization, altough the procedure is a bit boring and can take up mutch time, the end result is always beautiful

[@bigrockets]

xylenes are Not the same thing as gasoline. Gasolines have various ingredients that produce a distillation curve this is done to allow for good vaporization in a wide range of temperature such as winter and summer driving. This makes starting easier and xylenes have poor anti- knock charateristics.