12
$\begingroup$

I was wondering, how can I clean my RBF after doing a distillation? Cleaning it with a simple pipe-cleaner or similar cleaner is a headache, due to the roundness of the flask.

Is there a more effective method?

$\endgroup$
17
$\begingroup$

@Permeakra suggests some good cleaning solutions. I have rearranged them (adding a few) in a suggested order from mildest to most evil. The specific thing you want to use will vary based on what you want to clean. If an initial rinse isn't good enough, you may want to let it soak for a few hours. Always take safety precautions (don't add acid washes to basic compounds, for example) and where the appropriate personal protection equipment (PPE).

  • Detergent + water + "elbow grease" - there is a lab grade soap out there called "microwash" that is pretty good, and I also tell my students that things are more soluble in elbow grease than water.
  • Acetone - Acetone will dissolve most organics, and it is less harmful to you and the environment than other organics.
  • Dilute acid (HCl or H2SO4) - good for some "baked"-on stuff or for inorganic compounds. Watch out for vigorous acid-base reactions.
  • Dilute nitric acid (HNO3) - since most nitrate salts are soluble, nitric acid does a better job with resistant inorganics. It is also an oxidant and will convert resistance organics to more soluble compounds. Also watch for acid-base reactions.
  • Other organic solvents - Use whatever will dissolve your crud, but use proper personal protective equipment (PPE), fume hoods, and waste disposal.
  • "Base bath" (saturated KOH in isopropanol) - This solution eats a fine layer off the glass, which also removes the crud stuck to it. Rinse first with water or neutralize any acid present to avoid vigorous reaction with the bath. Immerse the flask into the bath for a few hours to overnight and it should come out clean. Base bath will dissolve silicone grease. Leave it in too long and it will come out etched. Use heavy butyl gloves.
  • Concentrated HCl - more powerful than dilute acids, but more dangerous. Neutralize any bases present to avoid vigorous reaction. Use proper PPE.
  • KOH + KMnO4 + H2O - this solution is basic (eats a fine layer of glass) and oxidative (converts many things, like organics, to a more soluble form). Neutralize any acids present and wear appropriate PPE.
  • Concentrated H2SO4 - has the added bonus of reacting with some insoluble organics, like polyaromatics, to form soluble sulfonates. H2SO4 is more dangerous than HCl. Follow the same precautions, and be more careful. I would use use butyl gloves instead of nitrile or latex. It will cause serious chemical burns.
  • "No-Chromix" - a non-chromium alternative to chromerge (below), no-chromix is a proprietary cleaner that is added to sufluric acid. The main ingredient is ammonium persulfate (NH4)2S2O8. You can make a reasonable knock-off by dissolving 2 g of (NH4)2S2O8 in 100 mL of water and adding to 2.5 L of sulfuric acid. Feel free to scale down, as this stuff has no shelf-life to speak of.

The following five items have dangerous reputations, and for good reasons. Use them as last resorts.

  • Concentrated HNO3 - strongly acidic and powerfully oxidizing. Dissolves many resistant things, including burned-on crud, but may ignite low molecular weight organics (like solvents). Rinse the flask first with water to remove bases, then with acetone to remove organics, and then with water to remove acetone before adding HNO3. Use butyl gloves.
  • Dilute HF (no more than 5%) - HF eats glass also, and it does so more quickly than base baths. However, the the hazards associated with HF are severe. HF burns are not like other acid burns. The HF continues to bore into you and the damage might not be evident until later. DO NOT USE UNLESS YOU HAVE THE BURN ANTIDOTE HANDY. The burn antidote is calcium gluconate, which neutralizes the acid and more important sequesters the fluoride ions. It is available as a gel or cream. You should still go overboard on PPE.
  • Aqua Regia: 1 part Concentrated HNO3 to 3 parts concentrated HCl. This is more powerful than just concentrated HNO3, since HCl is a stronger acid. It also decomposes to form NO2 and Cl2, both more powerful oxidants than Concentrated HNO3 alone. Aqua regia is famous as the only substance that can dissolve gold. It will also dissolve all manner of inorganics and organics, including silicone and hydrocarbon grease. Treat aqua regia with the respect deserved of its two components and keep it in the fume hood. Do not seal the vessels since it gives off gas. Aqua regia has no shelf life, but it remains a strong acid and will need neutralized before disposal. Note that aqua regia will not dissolve metallic rhodium, iridium, osmium, and ruthenium (all less active than gold).
  • Piranha solution: H2SO4 + H2O2 - this strongly acidic strongly oxidizing solution will eat off a lot of metal, organic, and inorganic residues by oxidizing then to more soluble forms. As a strong acid oxidant, it shares the same incompatibility warnings that concentrated nitric acid has. Piranha solution is good for glassware that needs to remain calibrated (volumetrics) or uniform (NMR tubes) since it does not eat glass. Piranha solution does not have a long shelf life.
  • Chromerge H2SO4 + K2Cr2O7 - forms chromic acid, a powerful oxidant. This stuff is considered toxic waste in most jurisdictions, meaning it will be expensive to get rid of. You can store it, however, if you store it in teflon. Do not use on NMR tubes, since chromium is paramagnetic. Treat chromerge with a respect due to the sum of everything above it on this list.
$\endgroup$
  • $\begingroup$ Note for Piranha solution: it gives fumes with clear oxidative smell, beware. Note for $KOH + KMnO_4 + H_2O$ do not keep for long or have some $H_2C_2O_4$ to clean $MnO_2$ afterwards. General note: despite $KMnO_4$ being effective oxidizer in acidic solutions never, never make $KMnO_4 + H_2SO_4(cons)$ mixture. The resulting green $Mn_2O_7$ is really dangerous staff. $\endgroup$ – permeakra Oct 11 '12 at 16:46
  • $\begingroup$ note for $H_2O_2$ based staff: it degrades quickly in presence of some d-element ions, like $Fe$ or $Mn$. $\endgroup$ – permeakra Oct 11 '12 at 17:17
  • $\begingroup$ Another one for the "dangerous" list: Bromium + methanol. Don't ask me about specifics, i've prefered to never use it. $\endgroup$ – Karl Dec 12 '15 at 13:45
1
$\begingroup$

Make up a basebath out of conc KOH in isopropyl alcohol (Or whatever recipe you prefer). Leave it in there for an hour or two, then rinse with distilled water. Most of the time it will come out sparkling clean.

Be careful: Saturated base baths should be handled with care, rubber gloves (dish gloves) over lab gloves are a very, very good idea.

$\endgroup$
1
$\begingroup$

The simplest way is using some cleaning solution. The nature of solution depends on nature of remnants. In my practice, I used

  • $H_2SO_4(conc) + K_2Cr_2O_7$
  • $H_2SO_4(conc) + H_2O_2$ (porous glass filters mostly)
  • $KOH + iPrOH$
  • $KOH + KMnO_4 + H_2O$
  • $H_2C_2O_4 + H_2O$ (cleaning $MnO_2$ and $FeOOH$)
  • $HCl$(2%).
  • $HCl$ (conc.)
  • Organic solvents (toluene, alcohol, hexane, dichloromethane)

Again, the nature of cleaning solution depends on what you are cleaning after.

$\endgroup$

Your Answer

By clicking “Post Your Answer”, you agree to our terms of service, privacy policy and cookie policy

Not the answer you're looking for? Browse other questions tagged or ask your own question.