Recrystallization of Sulfur

[@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

[@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.

[@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.

[@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.

[@AvianYuen]

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

[@andreatgrowwithme6901]

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

[@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!

[@JDeffenb]

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

[@sandhyaprabhu6996]

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

[@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.

[@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.

[@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!

[@kimandreolsen6298]

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

[@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

[@gaming_chutta_malli]

Very nice

[@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??

[@alexanderx33]

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

[@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.

[@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.

[@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

[@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

[@ianboard544]

Isn't Goofoff xylene?

[@kullanicikullanici3206]

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

[@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.

[@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

[@GTLmaster]

you can tell me about paper reference this procedure

[@drysori]

Instead of a refrigerator why not use an ice bath?

[@jeanpierredaviau7478]

Would acetone dilute sulfur?

[@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

[@realedna]

Please drop the 30 s intro!! Who wants to see that every time? :-/ (make a channel intro instead)

[@DougsLab]

+realedna Thanks for the feedback. :) Intro dropped for future vids!

[@ZomBeeNature]

What do you need with super pure sulfur?

[@ZivTheWyrd]

anything where impurities are undesirable :P

[@BackYardScience2000]

It wouldn't be a lab disaster if it caught fire. Lol! It would just be a flamming beaker that can easily be extinguished with a watch glass. I've had that exact thing happen before with 2 liters of xylene and with the same amount of toluene and a watch glass safely put out the flames in both cases. That's not to say that it isn't scary as shit though!

[@craigcain6553]

can you use gasoline or camp fuel

[@antejl7925]

No! Never heat gasoline extreme fire explosion risk.

[@extracrazyguy]

*TING* ASMR for fire bugs.

[@petemcbennett6039]

8:54 I agree.

[@FLODDI100]

"fumehood"

[@jayjanuary4357]

Chemistry scary.

[@carterkapanjie3904]

Nope

[@Gh0sb0ss]

isn't that stuff stinky af

[@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

[@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.

[@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.

[@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.

[@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 :)

[@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.

[@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)

[@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!

[@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?

[@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. :)

[@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.

[@peterholm339]

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

[@Kongfufrank]

what degree of purity after recrystallization?

[@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!

[@ammelr]

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

[@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.

[@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).

[@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.

[@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!

[@hlpayne]

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

[@plazmatter]

so can you make a giant gem?

[@JadAzido]

Man, that intro though...

[@KowboyUSA]

The shot of blue crystals dropping into the Erlenmeyer flask taken to appear the camera was inside the flask: outstanding

[@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 .

[@lrmackmcbride7498]

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

[@rndriver5550]

How can we dissolve sulfur in oil

[@christopherleubner6633]

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

[@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?

[@glasslinesmadhes]

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

[@kristianblerche8443]

2:45 Pling !

[@StevenSchoolAlchemy]

Hello Doug

[@quarantene3072]

I hope hes still free and not exploded ....

[@StevenSchoolAlchemy]

interesting

[@monto39]

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

[@kullanicikullanici3206]

İ. M.have .to.make likid sülfür

[@ElGatoLoco698]

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

[@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 ?

[@sezaicandan3134]

Xylene what iş tihis continus

[@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

[@bonbonpony]

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

[@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!

[@StevenSchoolAlchemy]

I shared this video to a playlist on my channel.

[@AuBjorn]

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

[@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.

[@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?

[@masterdraw10]

how about crystallizing potassium nitrate again?..

[@danstone_0001]

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

[@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.

[@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?

[@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!

[@craigcain6553]

wow got carded for lye today,why,never used lye in an experiment yet,not everyone makes drugs

[@ProjektOchExperiment]

Awesome video Doug! And congratulations to 1K subscribers!

[@shahabjaved1118]

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

[@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.

[@pietrotettamanti7239]

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

[@StevenSchoolAlchemy]

I want some of that!!!!!!

[@FlashBlowout]

Excellent tutorial thanks for sharing it

[@thecrudelab3204]

why not just use gasoline

[@juvanyalbraka9407]

Toluene Not available Is there an alternative substance

[@ogreth9438]

Can you make larger crystals?

[@jayjanuary4357]

Purification keyword.