How to Best Dry Solvents

Sdílet
Vložit
  • čas přidán 30. 07. 2024
  • In this video, I discuss the best way to dry THF, toluene, DCM, MeCN, methanol, ethanol, HMPA, DMF, DMSO, acetone, benzene, and 1,4-dioxane.
    / thatchemist
    Community Discord - / discord
    ----------------------------------------------------------------------------------------------------------------------------------
    Links to articles discussed in this episode:
    newest paper - www.doi.org/10.1021/jo101589h
    www.doi.org/10.1021/jo00414a038
    www.doi.org/10.1021/jo00438a024
    ----------------------------------------------------------------------------------------------------------------------------------

Komentáře • 201

  • @JohnWL
    @JohnWL Před 2 lety +64

    An easy way to test if your 3A sieves are activated is by placing a few in your hand and running a few mL of cool water over them. If the sieves get real hot they're sucking up water and good to go. I don't think I've ever gotten a new batch that needed to be activated. Tested solvents after with KF titrator to check in the past too.

    • @That_Chemist
      @That_Chemist  Před 2 lety +15

      interesting to know that they come activated

    • @JohnWL
      @JohnWL Před 2 lety +6

      @@That_Chemist could just be certain brands or batches? We only had to buy a few over my PhD since we regenerated most of them so they lasted a really long time.

    • @robertlapointe4093
      @robertlapointe4093 Před 2 lety +1

      The same test with well dried silica produces a sort of rice crispies effect, as the spheres decrepitate forcefully.

    • @uiucchemistry2664
      @uiucchemistry2664 Před 2 lety +1

      Super helpful & practical tip. Thanks for this advice! I never thought of that haha

    • @FerociousPancake888
      @FerociousPancake888 Před rokem +1

      Used them for the first time the other day and went to put the container away some time later and it was surprisingly hot!

  • @moosehead4497
    @moosehead4497 Před 2 lety +63

    Molecular sieves are really amazing, I've had some very sensitive chemistry become frustrating when inhibited by the smallest traces of water. It doesn't matter if you use bone dry solvents or practice good technique, if its not working, its probably your reagents. Eventually, I dried EACH reagent specifically, dissolving them in reaction solvent to sit over sieves for a few days...and then combining them via cannula, and that went from 0% conversion to 100% conversion!

    • @That_Chemist
      @That_Chemist  Před 2 lety +7

      awesome!

    • @Spoooky738
      @Spoooky738 Před 2 lety

      That's very interesting, may I ask what type of reaction were you doing?

    • @moosehead4497
      @moosehead4497 Před 2 lety +6

      @@Spoooky738 it was a copper catalyzed trifluoromethylthiolation, the active species being a copper(I) SCF3 with a bipyridine or phenanthroline ligand

    • @loganosmolinski4446
      @loganosmolinski4446 Před rokem

      ​@@moosehead4497I must be getting better at reading chemistry because I actually got some of that. Happy day!

  • @venomzmadz
    @venomzmadz Před 2 lety +26

    Someone writing his habilitation had a funny story last week:
    The paper stated, that he has to do a reaction with THF and water added separately
    Didn't work
    Turns out the problem was, he thought the autors used dry THF, whereas the reaction needed (in addition to the added water) more water, which was already present in their poorly dried THF
    Didn't see too dry THF before, I think this is funny

  • @ChromaticDontarius
    @ChromaticDontarius Před 2 lety +38

    Hey I just wanted to say thank you for this channel. I ended up mastering out of my PhD program two years in because I just couldn't do it and never had any success with any project. I'm probably not cut out for research and am still looking for a different avenue in chemistry, but your videos are a nice reminder of the good aspects I remember from being in lab.

  • @MaquiladoraIII
    @MaquiladoraIII Před 2 lety +7

    This video puts me in mind of my PhD days back in the mid 2000s; when one of us used a mechanical press to divide sodium chunks into wire, the other one would HOLD a 5 litre flask by hand underneath to collect said wire. After that, we simply threw in a load of lovely THF and indicator into the flask. God, how I miss those highly dangerous, potentially fire-inducing times!

    • @christopherleubner6633
      @christopherleubner6633 Před rokem +1

      5 liter flask full of air, sodium metal and nice wet THF what could possibly go wrong 😲 Glad you made it keeping all 10 fingers eyes and ears. 🤓❤

  • @alexabbey1
    @alexabbey1 Před 2 lety +16

    This is the kind of content most CZcams chemist's omit. It's really helpful in improving practice.

  • @gamingmarcus
    @gamingmarcus Před 2 lety +8

    The way we used to activate mol sieves (sensitive organometallic chem) was as follows: hang them on your schlenk line, pull max vacuum and blast with a heatgun. As you drive off the water you'll see a very small increase in pressure. Our pressure meters went down to 1x10^-3 mbar and would usually rise to 5-8x10^-3 mbar while drying the sieves. Keep blasting until the pressure stays at a constant minimum.
    Doing it this way you avoid using arbitrary time limits and can judge the progress with a measurement.
    Negative: it's slow as hell because you're heating something inside a vacuum.

    • @sealpiercing8476
      @sealpiercing8476 Před 2 lety +1

      It would be easy and might make that process faster to use a heat lamp to heat the sieves.

    • @Sanutep
      @Sanutep Před 6 měsíci

      a sand bath?

  • @user-kt3lc6rr8u
    @user-kt3lc6rr8u Před 2 lety +12

    I feel so much more confident in my undergrad labs with your videos. These insights are so helpful!!

  • @RobsMiscellania
    @RobsMiscellania Před 2 lety +16

    I've effectively used anhydrous potassium carbonate to lower the water content of alcohols. Ethanol in particular was a great success, obtaining 98-98.5% ethanol after treatment. After decanting, I simply heated the residue in an oven to restore the potassium carbonate to an anhydrous state, regenerating the starting drying agent. I then used the magnesium method to lower the water content some more. But the molecular sieves have so much drying power, they're easy to manage, and reactivation after use is just one more little lab chore, no big deal.
    Speaking of, I also would have made it my own business to ensure everyone was up to speed on the whole "shorting out the heating element" thing. Six errors is no longer a mistake.
    I have an e-copy of the Purifications text you recommended, for sure useful to have around. Good presentation, thanks for sharing.

    • @moosehead4497
      @moosehead4497 Před 2 lety +2

      Potassium carbonate is an excellent desiccant, it's far better than magnesium sulfate, at least for quick drying solvent after an aqueous workup. It also has the benefit of presenting as dense granules, rather then the magnesium sulfate powder, which means you could even get away with just decanting instead of filtering.. I always use it when I am extracting a freebase amine, as well as other compounds that is not sensitive to alkali.

    • @RobsMiscellania
      @RobsMiscellania Před 2 lety

      @@moosehead4497 I agree. The actual physical presentation of the drying agent after its use is very helpful for removing it. It tends to clump together and is very, very easy to decant. I've never had an issue with needing to separate any layers; simply decant the dried alcohol into its own container. Repeat the treatment if necessary (like I said, it usually got to 98% first try).

  • @treelineresearch3387
    @treelineresearch3387 Před 2 lety +3

    Glad this topic got picked! I don't ever need "analytically dry", but "pretty dry" solvents can be useful for predictable paint and finish. The residues in wal-mart grade 91% iso also seem to be mostly aqueous and I think getting some of the water out makes it a bit cleaner although I haven't actually studied it other than "oh that looks a little bit cleaner with the dryer stuff".

  • @Tuxedosam.
    @Tuxedosam. Před 2 lety +8

    Awesome video. Tried to ask my Orgo 2 Prof about this once and got a vague answer. Not his fault, it's not like he could talk for 11 mins on it. But I'm glad to get the full answer here.

    • @That_Chemist
      @That_Chemist  Před 2 lety +3

      it takes humility to admit the limits of your own knowledge

    • @davidfetter
      @davidfetter Před 2 lety +4

      What sounds to you like a vague answer can often involve an internal conversation like this:
      - This person is curious, and I love that, so I want to help
      - But this is a really complicated subject
      - And I don't want to steer this person wrong
      - Oh, and there's that one common thing that would otherwise make this suggestion go really badly wrong, so I can't just say that
      - That meeting I have to attend is in six minutes, and I'd love not to arrive sweating from running to it, and even that wouldn't be enough time

    • @Tuxedosam.
      @Tuxedosam. Před 2 lety +4

      @@davidfetter That mostly sums up why I put that sentence about 'not his fault' in there (I added that just before posting). You can explain a lot more in detail with a video/presentation than an off the cuff response to a question.

  • @Jimbreh
    @Jimbreh Před 2 lety +5

    Our lab usually dries solvent by stirring with CaH for 30 mins over CaCl2 tube, then distill and proceed to add them into activated 3A molecular sieves. But for reactions that need to be very very dry, we have THF dispenser that is dried through a special column which was cool.

    • @christopherleubner6633
      @christopherleubner6633 Před 7 měsíci

      Yup that is the best way to get your THF bone dry. THF soaks up lots of water and it sorta sticks to it like flypaper.

  • @HiwasseeRiver
    @HiwasseeRiver Před 2 lety

    Great topic, I learned some things. On the industrial scale I designed and built a large THF mol sieve column. Regeneration was a beast due to the ceramic nature of mol sieves. - those things heat up and cool down sloooowly. That was not one of my favorite processes - flaring hot THF/N2 gas - yikes. An additional property of hyper dry solvents is the electrical conductivity. On the large scale this becomes an issue. "Wet" solvents quickly dissipate electrical charges acquired by pumping and flowing through pipes. Dry solvent stay charged up and can create discharges. Discharges are not good in large scale solvent systems. Inert atmospheres help managed the hazard but you'd rather not have a solvent tank behaving as a giant capacitor. People have reported looking into large tanks and seeing glowing sort of like the aurora borealis. The known incidents tend to occur when solvent is transferred and hoses are connected/disconnected. One solvent supplier had a recommendation to hang grounding elements inside the tank to collect this type of charge and dissipate it safely. Final story: When a mundane solvent like hexane or heptane is shipped from Houston TX to anywhere north the solvent will cool off, because anywhere north of Yewston is cooler. When the solvent cools water drops out of solution. It's not uncommon to receive a tanker load of solvent and collect a receipt sample and see people (at a Lithium plant) freak TF out because the sample is 99% water. Pro-tip: be prepared to collect, handle and discard some water in these situation.

  • @MaquiladoraIII
    @MaquiladoraIII Před 2 lety +4

    The hardest working CZcamsr since Justin Hawkins Rides Again. Top banana!

  • @hugmynutus
    @hugmynutus Před 2 lety +4

    Not even a chemist, but i really enjoy these videos.

  • @Snizzfart
    @Snizzfart Před 2 lety +2

    Generally what we do for sieves is just heat them at 300 C for 12 hours under dynamic vacuum for 12 hours. Sieves get bone dry and then we store our already dried solvents over them in the glovebox. But I guess that is just what we do since we do very air sensitive chemistry

  • @MaquiladoraIII
    @MaquiladoraIII Před 2 lety +3

    Not sure as to whether this is the go-to in the States, but in Blighty, we used to find the Perrin textbook a terrific resource for drying organic and inorganic chemicals.

  • @GeoStreber
    @GeoStreber Před 2 lety

    Usually heating mol sieves in the glass oven overnight isn't enough for me. What I do is to just put them in a Schlenk or Straus flask, put that in the microwave until I see the water vapour coming off, and then I let them dry in the vacuum until they're cold. Run this three or four times, and that usually does the deal.

  • @chen309
    @chen309 Před 2 lety +1

    Its helpful !! Love your video, which type of video is quite rare in our country.

  • @martinowton7210
    @martinowton7210 Před 2 lety +2

    When I needed ultra pure and dry MeCN for electrosynthesis in my PhD I double distilled it from permanganate first then P2O5.

  • @K1R8Y92
    @K1R8Y92 Před 2 lety +2

    For THF distilleries, I guess one important thing apart from the drying itself is also the removal of the BHT stabilizer before use, which is present in most commercial THF.

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      that is true, but I find that it is pretty rare that the inhibitor is ever an issue

    • @newuser871
      @newuser871 Před 5 měsíci

      the boiling point of bht is 265 C. So it is not an issue if u are distelling

  • @klaus29a
    @klaus29a Před rokem

    In the literature there is a method for purifying acetone via cristallizing the complex with NaI, filtering the solid complex and distilling the acetone from it. Should produce quite pure and dry acetone. Maybe hard to scale, but for small amounts should work well. Didn't use it myself though.

  • @ilovemalaysia
    @ilovemalaysia Před 2 lety +1

    Thank you CZcams recommendations

  • @sebastiand152
    @sebastiand152 Před 2 lety +3

    Often combinations of methods are useful: "Dry with method X and the just store over mol sieves until use."

  • @gabbyh900
    @gabbyh900 Před měsícem

    Hello, sorry to ask. But what would you recommend for cleaning molecular sieves that have been exposed to THF. Thank you

  • @user-uf6hr4jm5i
    @user-uf6hr4jm5i Před rokem

    hello.
    I proceeded with solvent drying using molecular sieves.
    However, after a few minutes the solvent color changed to brown.
    In this case, isn't it possible to use molecular sieves?
    The solvents I used are propylene carbonate and NMP.

  • @liverpoolirish208
    @liverpoolirish208 Před 2 lety +2

    Rigorously dry THF is best obtained by distilling the THF from molten potassium. The norm is to pre-dry over sieves, and then rigorously dry from K or Na/Bz. When using diethyl ether it is dried from NaK.
    With Na/benzophenone, the benzophenone ketyl stays blue (i.e. rate of production of the ketyl at the surface of Na = rate of destruction of the ketyl) at several hundred ppm residual water once all oxygen is consumed (depending on the surface area of the Na). Blue only indicates O2 free, and not dry. The colour will deepen to purple as the rate of destruction of the ketyl goes down. In the Williams and Lawton paper, then tell us the THF was blue, and so it had not reached ultimate dryness.
    A problem for all the "active hydrogen" desiccants (alkali metals, metal hydrides etc.) is that they release H2 gas, which K-F registers as lots of water. K-F readings of superdry solvents dried by these desiccants is much, much lower after degassing.

  • @everythingis2495
    @everythingis2495 Před 5 měsíci

    hey THAT Chemist. not him. YOU.
    question for you. Say, hypothetically, after neutralizing freebase with conc. hcl solution , you have an amine hcl salt dissolved in Toluene azeotrope. you want to crystalize product and would resort to drying solvent using dean stark trap.
    Can one evoke crystallization in your NPS with sieves? just aas one might do using azeotropic distillation? assuming the chemical in question is larger than 3 angstrom in width. would it not get left behind i have never heard of them being used for crystallization . there has to be a reason as to why it does, or it doesn’t work. enlightenment?? thanks for your time.

  • @Chemiolis
    @Chemiolis Před 2 lety +3

    My brain short-circuited when u used methylene chloride instead of DCM

  • @ChoumadaGaming
    @ChoumadaGaming Před 2 lety +3

    Trying to tell another students supervisor who grew up using classical drying techniques such as Na/benzophenone that 3A sieves is better was quite an experience, can be hard to teach an old dog new tricks.

    • @That_Chemist
      @That_Chemist  Před 2 lety +2

      yep!!

    • @That_Chemist
      @That_Chemist  Před 2 lety +3

      I had the same experience when I showed my PI that paper

    • @aspel4x
      @aspel4x Před rokem

      THF after sieves reacts with first portion LAH. THF after Na - not… Mb sieves make really anhydrous THF but sometimes we need something else)

  • @iryanmadayana1904
    @iryanmadayana1904 Před 2 lety +1

    ...huh. Never thought about drying mol sieves with a microwave. I need to look into that!

  • @jaredlowe3927
    @jaredlowe3927 Před 2 lety +4

    When I finally found the paper you get your data from a couple years ago, I was really excited. So how hot do you keep your glassware oven? Mine is usually around 110-120 C

    • @jaredlowe3927
      @jaredlowe3927 Před 2 lety +4

      I've flame dried my sieves under vacuum (what I was told in grad school by older labmates)

    • @That_Chemist
      @That_Chemist  Před 2 lety +3

      I think its like ~130ish but I'm not 100% sure

  • @eggplantlover6662
    @eggplantlover6662 Před 2 lety +1

    In the (inorganic) lab I worked at, we stirred pre-dried (from a solvent purification machine) solvents over NaK Alloy and then distilled them. Also everyone told me that Acetonitrile destroys Molecular Sieves, which speaks for the chemistst beliefs in things that "somebody told them once or something" I guess.

    • @davidfetter
      @davidfetter Před 2 lety +3

      *Way* more of the praxis of science that you would like to imagine works this way.

    • @mytech6779
      @mytech6779 Před 2 lety

      ​@@davidfetter re "somebody told them once or something"
      NaOH seems to be a good example of that, at least outside of professional labs.
      "Errmgrd don't open that bottle of lye without a full hazwopper suit, It's caustic and 'll melt yer arm!".
      Likely stories passed down from old industry where they would do stupid stuff like dump [not pour] a 55galllon drum of lye into an open top water tank at chest level, (I've seen films documenting processes where they do this very thing.) and it was actually the heat of violently boiling water that was the real burn hazard, not the incidental lye solution.
      Side note: I've used my bare fingers to handle small amounts of lye and even for stirring it into solution, it is not a big deal. Circumstance matters.

  • @adrianpip2000
    @adrianpip2000 Před 2 lety +2

    I hate solvent stills, but that's probably because during my undergrad I was doing some reactions using tBuLi in the same hood as a big ether still. It really truly frightens me to think about how bad that could've gone. The benzophenone ketyl colors are really cool though

    • @BradSchmor
      @BradSchmor Před 2 lety

      Even more fun when someone would throw a lump of potassium in and there would be this shiny melted blob of NaK bobbing around.

  • @glibrazumkov5408
    @glibrazumkov5408 Před 2 lety +1

    Thank you, very informative! How often do you re-activate the molecular sieves? And would they be a viable strategy for water removal in moisture-sensitive condensations (like if formation of imine as as an intermediate is expected)?

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      usually if I finish off a bottle of solvent, then I will reactivate the sieves - sometimes I would regen after a couple refills

    • @liverpoolirish208
      @liverpoolirish208 Před 2 lety

      By warned; you can't stir solutions with sieves in them. They turn into mud with no drying power. You can put them in a Soxhlet thimble, and that works.

  • @Orchids.and.Endlers
    @Orchids.and.Endlers Před 2 lety +7

    I LOVE molecular sieves, but MgSO4 is alright as well for basic applications.

    • @Jimbreh
      @Jimbreh Před 2 lety +1

      yoo after almost all my reactions, I extract the organic layer, pump up and dry with MgSO4. then the dreadful column chromatography.

    • @Orchids.and.Endlers
      @Orchids.and.Endlers Před 2 lety

      @@Jimbreh Exactly 🤣 it works well but it’s such a pain to completely remove and isolate from the product

    • @zewski3218
      @zewski3218 Před 2 lety

      @@Jimbreh sure, but there is a difference between getting rid of water for the column and drying solvents for organometallic chemistry

    • @jaredlowe3927
      @jaredlowe3927 Před 2 lety +1

      As long as you don't need to distill

    • @jaredlowe3927
      @jaredlowe3927 Před 2 lety +1

      @@Orchids.and.Endlers How do you filter? I usually use a medium glass frit with vacuum. Buchner funnel or gravity filtration is awful for removing MgSO4 (from experience)

  • @Lukesab3r
    @Lukesab3r Před 3 měsíci

    What about magnesium sulfate?
    I've read a lot of chemists use it for acetone

  • @uiucchemistry2664
    @uiucchemistry2664 Před 2 lety

    Would you ever recommend also passing the solvent through some sort of drying agent before dispensing/storing away that solvent in a flask filled with molecular sieves?

    • @That_Chemist
      @That_Chemist  Před 2 lety

      it depends on how wet the solvent is, and in what context

  • @jonsimpson6690
    @jonsimpson6690 Před 2 lety +2

    I know that there is information on esters when their characterized on the infrared spectrometer, but is it even useful? The peaks are within the fingerprint region, so is it even worth bothering to verfiy the esters using the IR data in a lab setting?

    • @That_Chemist
      @That_Chemist  Před 2 lety

      if it is for library recognition then yes, but typically the only time I would use IR for organic stuff is when my stuff is insoluble, I have literally no idea what it is, or if a reviewer asked for it lol

  • @batkid317
    @batkid317 Před 2 lety +1

    This video reminded me that I need to tell my company's Karl Fischer group to remember to activate their molecular sieves

  • @diablominero
    @diablominero Před 2 lety +1

    My favorite solvent is distilled water. How do I dry that?

  • @briang.valentine4311
    @briang.valentine4311 Před 2 lety +1

    You left out diethyl ether dehydration for Grignard???

  • @Chem-iu5jx
    @Chem-iu5jx Před 2 lety +1

    I still like to use potassium/sodium mirror whenever I can :D

  • @lalosalamancat4550
    @lalosalamancat4550 Před 2 lety +1

    The lab supplier where I work at sells molecular sieves 13X (Aldrich 208647). Do you think it works well to remove water from solvents?

    • @That_Chemist
      @That_Chemist  Před 2 lety

      from aldrich's page "The product (Molecular sieves, 13X) have been used for the abstraction of water from the 100% ethanol. Also, they are widely employed as an adsorbent in adsorption studies"

  • @user255
    @user255 Před 2 lety +3

    What is the explanation for the sodium vs sieves results? Is it just because the amount of sodium (or its surface area) was lower? I don't see why sodium would stop reacting with water when concentration goes below certain limit..?

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      the reaction with sodium is a chemical one, the interaction with molecular sieves is a physical one as far as I know

    • @user255
      @user255 Před 2 lety +2

      @@That_Chemist But does that really matter if given enough time?

  • @dangerdackel
    @dangerdackel Před 2 lety

    For industrial use set a water spec for your reaction based on lab experiments. Do a K-F, if it does not fairy Chuck the solvent away. But I have set water specs for a manufacturer and then everything was ok.

  • @longnguyenhuu0305
    @longnguyenhuu0305 Před rokem

    Sir, may I use Molecular sieve to dry some amine bases like TEA or TMEDA? these amines usually contain water.

  • @dangerdackel
    @dangerdackel Před 2 lety +1

    Try azeotropes especially with toluene

  • @arthurcruikshank1415
    @arthurcruikshank1415 Před 2 lety +1

    I live in south I'm Bama an humidity is oppressive an it's really hard to keep chems an drying agents dry I found maxi pads an puppy pee pads work well to keep things dry

  • @_Galexo
    @_Galexo Před 2 lety +2

    When I tested my analytically dry Dimethoxyethane it still decoloured the sodium benzophenone mixture even though it was stored over 3Å molsive and is supposed to have 2 ppm residual water so now I have been refluxing it over sodium for a further week in hope of drying it further

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      It might just have oxygen in it

    • @_Galexo
      @_Galexo Před 2 lety

      @@That_Chemist I freeze pumped it before bringing it into the box where I added the sodium and benzophenone

  • @arthurcruikshank1415
    @arthurcruikshank1415 Před 2 lety

    I'm no chemist but can you use a air fryer to dry molecular sieves well to gently push out all the water...

  • @martinklucka5036
    @martinklucka5036 Před 8 měsíci

    Hi, Why should I not regenerate the sievs used for drying DMSO ?

    • @newuser871
      @newuser871 Před 5 měsíci

      Dmso and Dmf have high boiling points and When u heat the sieves for activating DMSO doesnt evaporate from the surface of the sieves and if u heat more, DMSO (or Dmf) make a film which covers the pores of the sieves and disables to catch the water.

  • @longnguyenhuu0305
    @longnguyenhuu0305 Před 2 lety

    I have a question. I used the molecular sieve 3A and the solvent looks unclear maybe because of the dust. Is it possible to use that solvent for my reaction without further purification?

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      yes, but I usually allow the dust to settle first

    • @longnguyenhuu0305
      @longnguyenhuu0305 Před 2 lety

      @@That_Chemist thank you very much. Your channel is really helpful.

  • @ohays63yahoocom
    @ohays63yahoocom Před 2 lety +3

    What percent w/v of molecular sieves would you recommend to dry the solvent water?

    • @That_Chemist
      @That_Chemist  Před 2 lety +2

      It depends on how much water there is, and what the application is, but if it’s pretty dry already, 10-20% m/v

    • @ohays63yahoocom
      @ohays63yahoocom Před 2 lety +1

      @@That_Chemist what if my solvent was say... 100% water?

    • @That_Chemist
      @That_Chemist  Před 2 lety +2

      funny guy

    • @ohays63yahoocom
      @ohays63yahoocom Před 2 lety +1

      @@That_Chemist they didnt give me my masters for nothing 😊

  • @arya6085
    @arya6085 Před 2 lety +4

    Love your videos but your nomenclature is so different than what I am taught. I would call CH2CL2 dichloro methane for example. Is this because I'm from the uk?

    • @jaredlowe3927
      @jaredlowe3927 Před 2 lety +3

      In US we use all of the above, DCM, CH2Cl2, dichloromethane, methylene chloride, it's too common to be standardized

    • @arya6085
      @arya6085 Před 2 lety +3

      @@jaredlowe3927 it's probably the same in the UK, I'm just in school right now

  • @conan9853
    @conan9853 Před 2 lety +1

    I was taught to activate molecular sieves by heating at 200 deg C under vacuum, is that overkill?

  • @dangerdackel
    @dangerdackel Před 2 lety

    Want to use mol sieve on 10m3 solvent. Set a spec for the water in your reaction then use the solvent as is

  • @stonedbud
    @stonedbud Před 2 lety +1

    What about pyridine? Pyridine is a solvent, right?

  • @sebastiand152
    @sebastiand152 Před 2 lety +2

    That confuses me: why should sodium be so bad for drying THF and so good for dioxane? I have dryed THF over Na/benzophenone to use it in anionic polymerizations (started with tert. BuLi) and did not encounter issues. Perhaps my initial THF was already quite dry.

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      Most chemistry tolerates a fair bit of water - even the sodium benzophenone method still gets it to a very low percentage of water

    • @sebastiand152
      @sebastiand152 Před 2 lety +1

      @@That_Chemist How about the difference between THF and dioxane in Na? Does anyone have an idea?

    • @d-nied1841
      @d-nied1841 Před rokem

      @@sebastiand152 I also find that inconsistent. I believe it is due to the different references. The third reference also shows that indicators (such as benzophenone) give a false sense of dryness to the user, but prolonged exposure to sodium does significantly increase the dryness. So the results from the first reference are somewhat biased, as they rely on this indicator method. I guess the bottom line is that molecular sieves are a great way to passively dry solvents. Distillation, however, has operational parameters, which differ across users/labs, but remains, in my opinion, one of the best methods to obtain dry and pure compounds.

  • @lalosalamancat4550
    @lalosalamancat4550 Před 2 lety

    For hexane or heptane, is it better to use 4A or 3A sieves?

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      you usually don't need to dry either of those - if its really sensitive, either one is fine

  • @tomflanagan878
    @tomflanagan878 Před 2 lety +1

    Interesting that with dioxane that sodium got the solvent drier than sodium-potassium alloy, which I thought was a whole lot more reactive to water.
    Also, I think when talking about ppm it's useful to think about percentages to get a bigger picture view. Eg 50 ppm on this list isn't that dry but that is still 0.05% water, making your solvent 99.95%. In 100 g of solvent, you only have 0.005 ml of water.

  • @Odin1465
    @Odin1465 Před 2 lety +1

    wow, i didnt expect wet toluene to have double the water content compared to wet THF.

  • @belgarat101
    @belgarat101 Před 2 lety +1

    If you remove other solvents from water, do you make the water wet or dry?

  • @alvinkwok587
    @alvinkwok587 Před 2 lety +3

    I dry my acetone with molecular sieves, after usage I will microwave them so I get to reuse them. P2O5 or Anhydrous MgCl is just too expensive for us amateur and NaCl results aren't great

    • @That_Chemist
      @That_Chemist  Před 2 lety +2

      its pretty rare that you would need anhydrous acetone for amateur chemistry tho

    • @alvinkwok587
      @alvinkwok587 Před 2 lety +1

      @@That_Chemist That's true. I don't do too much water sensitive stuff

  • @eucompsa
    @eucompsa Před rokem

    Tetraglyme is an absolute nightmare to dry, though some of the crown ethers would would likely be worse...

  • @sebastiand152
    @sebastiand152 Před 2 lety

    I did not try this one, but how about drying methanol by dissolving sodium methanolate in it?
    Water should quickly be converted to NaOH and the by-product would be methanol. Distillation would be needed, but I would expect fast and good results.
    And yes, I considered writing about Na metal in this context, but I would not recommend it.

    • @That_Chemist
      @That_Chemist  Před 2 lety

      its still an equilibrium - mol sieves should do a much better job

    • @sebastiand152
      @sebastiand152 Před 2 lety

      @@That_Chemist It being an equilibrium is not a relevant argument. It always depends on the ratio of equilibrium.
      And: Mol sieves also works in an equilibrium between adsorption and desorption of water.

  • @Valdagast
    @Valdagast Před 2 lety +5

    _However,_ mesityl oxide apparently smells good. So that's nice.

  • @chemically_literate
    @chemically_literate Před 2 lety +3

    Yeah, acetone is a tricky one. It forms an addition compound with CaCl2 and MgSO4 doesn't work. Also due to aldol condensation the water content can increase so molecular sieves are no good either. I used freshly oven dried CaSO4, which seems to be the best option and distilled it directly from the desiccant. The literature claims 300 ppm or 0.002 M water with that procedure and that was good enough for my application.

  • @user-rv9nz8en7n
    @user-rv9nz8en7n Před 2 lety

    I am wondering why alcohol such as methanol had to be dry? Methanol contains an acidic proton like water. So, reactions carried out in methanol will not be water sensitive? If it is the case, why do we have to dry methanol in the first place? ( Sorry for the poor English)

    • @That_Chemist
      @That_Chemist  Před 2 lety

      sometimes water may react as a competing nucleophile, reducing overall yield, or producing product that is impure

    • @That_Chemist
      @That_Chemist  Před 2 lety

      often times people are way too concerned about water as a competing nucleophile

  • @johnathancorgan3994
    @johnathancorgan3994 Před 2 lety +2

    I'm curious about diethyl ether, wasn't covered in the reference.

    • @That_Chemist
      @That_Chemist  Před 2 lety

      I typically use 4A mol sieves for diethyl ether

    • @That_Chemist
      @That_Chemist  Před 2 lety +2

      But only when the ether needs to be dry - usually I just use the ether straight from the supplier bottle

    • @johnathancorgan3994
      @johnathancorgan3994 Před 2 lety +1

      @@That_Chemist Thanks. Was thinking in reference to Grignard reactions.

    • @jaredlowe3927
      @jaredlowe3927 Před 2 lety

      @@johnathancorgan3994 In my lab we have an alumina column set up

    • @martinowton7210
      @martinowton7210 Před 2 lety

      @@That_Chemist This is my experience too. The Sureseal bottles of supplier dry solvents are fine for organometallics such as Grignards and alkyllithiums. Most of the lab fires I've heard of are related to solvents stills which is why they were removed from our labs.

  • @_general_error
    @_general_error Před 10 měsíci

    How does one blowtorch something in vacuum?

    • @That_Chemist
      @That_Chemist  Před 10 měsíci

      the outside is blowtorched and the glassware is connected to a vacuum line (e.g. rubber stopper + tube + vacuum tubing -> vacuum pump)

  • @TheZelluloid
    @TheZelluloid Před 2 lety

    Mesityloxide is quite misleading, since I always thing of mesityl being the trimethylbenzene substitutent xD.

  • @simedinson984
    @simedinson984 Před 2 lety

    we have tested the benzophenon sodium thf still in our lab with a reading of 4 ppm so not sure how accurate that document is

    • @simedinson984
      @simedinson984 Před 2 lety

      also the still is usualy longer than 24 hours its more like 1000 hours

    • @That_Chemist
      @That_Chemist  Před 2 lety

      that is a significant factor then

    • @simedinson984
      @simedinson984 Před 2 lety

      @@That_Chemist but its good to think about sieves just think stills that are long term will most likely become better as longer exposure to drying agent bur great video

  • @lukegaming86
    @lukegaming86 Před rokem

    You kids with ur gotdamn mol sieves. Back in my day all we had was anhydrous MgSO4

  • @Conex145
    @Conex145 Před 2 lety

    Couldn't someone use a soxhlet extractor filled with mol sieves, where e.g. THF can pass through after previous drying? Probably over complicated but may lead to satisfying results.

  • @ElSuperNova23
    @ElSuperNova23 Před 2 lety +1

    Aha, this is where that slide that was on chempros came from

  • @crabcrab2024
    @crabcrab2024 Před 2 lety +1

    Some of those charts hardly make sense. How can NaK be 4 times worse than just Na? I would really take that information with a grain of salt. Some facts here definitely contradict the rest of the literature (and my experience too). But in the end 3A MS is a really great thing to dry stuff and generally quite an underestimated one.

  • @WobblycogsUk
    @WobblycogsUk Před rokem

    I'm surprised to hear you say you can microwave sieves. I suppose you can but you've got to be very careful. A guy in one lab I worked in tried drying them in a microwave and they melted straight through the glass dish he was using and most of the way though the glass table in the microwave. We never tried again but I assumed some water remained trapped in the sieve and just got hotter and hotter.

  • @DegradationDomain_stuff

    10:25 why Al2O3 gets 0.6 after 6h, 0.006 after a day, but then rises to 0.2 after 7days?
    Looks sketchy to me.

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      Unclear - maybe it catalyses some obscure reaction - it’s harder for me to say in the case of benzene, where as for something like acetone it is more conceivable

  • @janvisagie231
    @janvisagie231 Před 2 lety

    Purification of lab chemicals is an awesome book. Pretty old-school but that just ads to the charm.
    Edit: Please don't reuse mol sieves 🤢🤮
    Oh and 9:19 here is a pretty neat publication on B2O3: A heterogeneous metal-free lewis acid for CO2 fixation into cyclic carbonates.

    • @That_Chemist
      @That_Chemist  Před 2 lety

      You can totally reuse mol sieves, you just don’t wanna reuse them for bad solvents like DMSO or DMF

  • @viorp5267
    @viorp5267 Před 2 lety +1

    *yeets in some MgSO4

  • @user-sw1lj9qh5y
    @user-sw1lj9qh5y Před 2 lety +1

    Best way to dry hydrocarbon solvent is reflux and partial distillation with sodium metal and place in inert air bottle with some suitable molecule sieve.
    But this way is very tedious and boring works to do. And it doesn't work on protic solvent, above hydrocarbon substituted some halide (e.g. chloroform) because sodium reacts with the hydrogen of solvent and ruins them all.
    So better way I feel is buy the solvent with air-seal, which can be bought from sigma-aldrich, or place the solvent in glove-box as soon as you get.
    And use it all ASAP whenever you get. Don't buy big drum of solvent even if it's cheaper than small one, and you use it within 3 months at least.

    • @That_Chemist
      @That_Chemist  Před 2 lety

      but the question is *how does Aldrich dry their solvent*?

    • @user-sw1lj9qh5y
      @user-sw1lj9qh5y Před 2 lety

      @@That_Chemist I'm in lab so I don't know the whole treatment the aldrich does.
      But in the experiment scale, most of moisture problem was came from old stored solvent, or the someone who doesn't know his reaction and believe the undesired situation in the reaction originated from moisture of solvents.

  • @theSILKROAD210
    @theSILKROAD210 Před 2 lety

    it would have been nice if you had warned the audience, that HMPA is to be avoided at all costs because its highly cancerous. like with the hepafluoroisopropanol for females. it would help young chemists and other scientist to be aware of the dangers of certain substances.
    thank you for your work in highly infomativ videos !

  • @pmathewizard
    @pmathewizard Před 2 lety

    Mission Failed: There are no dramatic and erratic egg breaking

  • @sealpiercing8476
    @sealpiercing8476 Před 2 lety +2

    Uh, that's way more water, and much harder to remove to any significant extent, than I had realized. Hmm.

    • @That_Chemist
      @That_Chemist  Před 2 lety

      For which solvent?

    • @sealpiercing8476
      @sealpiercing8476 Před 2 lety +1

      @@That_Chemist All of them except benzene, but especially methanol and toluene. I didn't realize that toluene could have so much water in it to begin with, and I didn't realize that reducing the water content of methanol was so involved. Benzene acts more like I incorrectly assumed not-very-polar solvents in general acted.
      I'm also mystified as to how to model those ppms of water that stay behind. I would guess sequential drying would achieve better results than longer exposures to the same pile of sieves, but that's not a confident guess since I'm not sure what the limiting factor is here.

    • @davidfetter
      @davidfetter Před 2 lety

      @@sealpiercing8476 re: unexpected things mixing, there are more processes for that out there than solvation. Think about the most recent nasty emulsion you had to break, for example. Or mayonnaise, if you want to look at emulsions in a more positive light.

    • @sealpiercing8476
      @sealpiercing8476 Před 2 lety

      @@davidfetter That makes sense. I'm pretty new to using chemistry for anything but also I want to use a high energy (at least 2.7 eV) triplet sensitizer to drive another reaction in toluene. Something's quenching it within a few hundred ns. I have the dawning sense that I stand atop a deep well of potential troubleshooting.

  • @leeroy144
    @leeroy144 Před 2 lety

    I just microwave my solvents. or put some sodium in it.
    sometimes I microwave them with sodium in them.

    • @leeroy144
      @leeroy144 Před 2 lety +1

      in all seriousness, this did remind me I needed to put some sodium in my dioxane.

    • @That_Chemist
      @That_Chemist  Před 2 lety +1

      smh

  • @juliogallardo3082
    @juliogallardo3082 Před rokem

    And what about chloroform? 🤔

  • @PlexusTen
    @PlexusTen Před 2 lety +3

    this video was quite dry

  • @Rose_Haw
    @Rose_Haw Před rokem +2

    how did I get here I just want my paint to dry🥲