Author Topic: NaBH4 which has hardened in the bottle  (Read 188 times)

Methyl Man

  • Subordinate Wasp
  • ***
  • Posts: 143
NaBH4 which has hardened in the bottle
« on: September 22, 2010, 08:53:44 PM »
Is it still good? A civet cat I know has some that has been stored for about 8 years in the original amber botle. It is still bright white in color, but most of it is hard and stuck together.

Is it still good as a reducing agent? The cat hopes to break it up with an ice pick or something into powder.

Thanks in advance for any help,
MM
There's a methyl to my madness...
==+==+==+==+==+==+==+==+==+==

java

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 783
Re: NaBH4 which has hardened in the bottle
« Reply #1 on: September 23, 2010, 12:19:23 AM »
"Sodium borohydride, NaBH4, is classified as a flammable solid, is available either as a white powder or as a
12% solution in caustic soda. It is stable to 300°C in dry air and in vacuum to 400°C with only partial
decomposition. In order to prolong the shelf life of sodium borohydride solutions, NaOH is added. Under
normal storage conditions, the loss of NaBH4 in 12% solution by decomposition is less than 0.1% NaBH4
per year [2]."

........there is more, read here,

http://docs.google.com/viewer?a=v&q=cache:DiDHDvKGOqAJ:www.cder.dz/A2H2/Medias/Download/Proc%2520PDF/posters/%255BGV%255D%2520Hydrides/741.pdf+sodium+borohydride+after+long+storage&hl=en&pid=bl&srcid=ADGEESgS8uBpUIzaNgO63950fQivYT5ePSIbyLq7ebGgGyqagAI1b8yt7gHULT-dtbJg-FgbCK8Z3uJxLhH3RlXCGF9ksbddXOvq-OACw_teVbitrkeT7pOBAZIxieusmh202fifhJ-U&sig=AHIEtbRQkKHiFRCz54NntdhMK6YX_DcAVA

¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: NaBH4 which has hardened in the bottle
« Reply #2 on: September 23, 2010, 01:34:27 AM »
I think as Java already stated its a flammable solid so take a small sample and attempt to ignite it, if it fails to combust write it off and dispose of it properly.


Not to nit pick but we also have a short question thread for these sort of topics just as a heads up.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Buzzoff

  • Larvae
  • *
  • Posts: 15
Re: NaBH4 which has hardened in the bottle
« Reply #3 on: September 24, 2010, 09:10:17 PM »
Titrate it.  Take a small weighed amount, react it with acid, and capture the generated H2 in an upside-down graduated cylinder or test tube.

This should tell you if the material has deteriorated, and to what extent.


Wizard X

  • Lord of the Realms
  • Foundress Queen
  • *****
  • Posts: 1,224
Re: NaBH4 which has hardened in the bottle
« Reply #4 on: September 25, 2010, 01:25:56 AM »
Sodium borohydride: Spontaneous ignition can result from solution of sodium borohydride in dimethylformamide. NaBH4 can be recrystallized by dissolving in warm (50 °C) diglyme followed by cooling the solution.

Ref: http://en.wikipedia.org/wiki/Sodium_borohydride

Dissolve in dimethylformamide and expose some on a watch glass. If spontaneous ignition occurs, then ok.
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

Methyl Man

  • Subordinate Wasp
  • ***
  • Posts: 143
Re: NaBH4 which has hardened in the bottle
« Reply #5 on: October 04, 2010, 01:11:37 AM »
Thanks for all those suggestions.

The cat did try igniting some, and it did ignite. He put a little on a small piece of newspaper outside on concrete and lit the newspaper. When the flame got to the BH4, it sputtered to life (probably the water vapor leaving) and then burned with a tiny but ferocious spurt of whitish-yellow chemical flame. He's taking this as a good sign.
« Last Edit: October 04, 2010, 01:14:17 AM by Methyl Man »
There's a methyl to my madness...
==+==+==+==+==+==+==+==+==+==

letters

  • Subordinate Wasp
  • ***
  • Posts: 138
Re: NaBH4 which has hardened in the bottle
« Reply #6 on: November 14, 2010, 05:55:55 PM »
this hardening is usually due to presence of moisture and degradation to sodium borate. yet even if it has hardened to a solid mass, it usually only degrades a bit, which is enough for it to change appearance. however, usually, this is still good enough for reductions.
a good way to test for activity is to dissolve in some alcohol, and look for hydrogen bubbles. also you can drip in acid to see if it gives an even more vigorous hydrogen release. an even better way to test for activity is to try out a reduction reaction which is known to work with proper nabh4. if it works well, you are good.
you can easily do a micro-mol reaction and follow progress with TLC

Methyl Man

  • Subordinate Wasp
  • ***
  • Posts: 143
Re: NaBH4 which has hardened in the bottle
« Reply #7 on: April 10, 2011, 07:47:55 PM »
Thank you, letters.

Sorry for the five-month gap here.  ;D

Will try those easy tests; sounds like they should be clarifying. Still haven't gotten the chance to use it, but it edges ever closer and closer...

MM
There's a methyl to my madness...
==+==+==+==+==+==+==+==+==+==