we recently acquired an interesting chemical sodium hypophosphate it's the .
sodium salt of hypophosphorus acid which can apparently be used together with iodine instead .
of red phosphorus to reduce alcohols to the corresponding alkane first we wanted to see .
if we could prepare the acid from the salt so we started by measuring out 100 grams of .
sodium hypophosphate crystals these are the dihydrate salt the theory was to see if we .
could perform the displacement reaction using a strong mineral acid .
so we measured out 30 mils of concentrated hydrochloric acid initially this is half the .
molar equivalent we placed the salt on a hot plate and then added the acid to the crystal .
these seem to dissolve and a much lighter colored solid appeared in the suspension this is a good .
sign that sodium chloride is being created and precipitated .
due to the concentration we gave the mixture the good stir and heated it on a hot plate we .
then prepared a further 30 mils of concentrated hydrochloric acid which should make up to one .
mole of HCl per mole of sodium hypophosphate we added this to the hot mixture and stirred again .
you can see that the white crystalline deposit is quite thick .
and different to the original salt we stirred the mixture for a few minutes .
and heated up to around 80 degrees C then allowed it to cool right down to .
nearly zero degrees in order to precipitate as much of the sodium .
chloride salt as possible on chilling for a few hours the salt fell to the .
bottom of the beaker leaving the clear solution so we set up for vacuum .
filtration and removed the white salt from the liquid .
we allowed all the liquid to filter through and for the salt to become reasonably dry .
we ended up with covering 40 grams of sodium chloride as you can see here it's slightly damp .
but even so according to the stoichiometry of the reaction we would expect 47 grams to be produced .
in total so this is not bad at all .
so this is not bad at all .
so this is not bad at all .
so this is not bad at all .
so this is not bad at all .
our filtrate is slightly yellow due to our filter not being totally clean .
however it tells us that we've got a lot of hypophosphorus acid as .
hypophosphite and hydrogen ions in this solution so we transferred this into a .
250 ml flask to see if we could distill of some of the water we added a small .
magnetic stirred bar so that we could stir to prevent the mixture from bumping .
and then used a hot plate to heat the mixture with a .
simple distillation app with a setup .
and then used a hot plate to heat the mixture with a simple distillation app with a setup .
we also used a vacuum pump to help drive off the water at a lower temperature .
we know that hypophosphorus acid decomposes temperatures higher than about 100 degrees .
c to form explosive and toxic phosphine gas so we wanted to be very careful about this .
soon we saw some condensation appearing .
and we insulated the flask using some aluminium foil to make the distillation more efficient .
and we insulated the flask using some aluminium foil to make the distillation more efficient .
Despite all these measures the distillation of water was incredibly .
slow and after an hour we had only managed to obtain around 10 mils of .
water distilled.
At this point we noticed a white precipitate, presumably more sodium .
chloride forming in the boiling flask, so we allowed the mixture to cool at this .
point and chilled it down again to zero degrees.
Once again we filtered this on a vacuum and we noticed that the liquid was now actually .
quite viscous and syrupy.
We got a further four grams of sodium chloride from this filtration, so we .
figured that we must have a relatively strong hypophosphorus acid solution by .
now. And here's the filtrate. Exactly 100 grams .
in weight.
And the filtrate is now 100 grams in weight.
We started measuring 74 mils giving a density of 1.35. The pure acid has a .
literature density of 1.49, so this is looking good.
So let's first put it to the test by reducing some iodine. We placed a small .
amount in a beaker and added a spatula of solid iodine at room temperature.
I'd say that worked pretty well. Maybe a bit too well.
Let's now see if the acid can be decomposed by heat. This will also tell .
us how safe it is to boil a reflux. We heated a small amount in a beaker on a .
hot plate. First we got some condensation.
Then very slight boiling. Then tiny explosion.
So we've definitely got some good stuff here, and we'll have a go in a future .
video at using it to reduce an alcohol.
In the meantime we'll leave you with our final experiment, evaporating the liquid .
to dryness on a glass petri dish. Enjoy.
The hot plate is only at about 150 degrees C, so this is a good warning about .
the reactivity of this compound. Huge clouds of white phosphorus pentoxide are .
generated as the phosphine gas produced spontaneously combusts in air.
Stay tuned.
Closed Captioning by Kris Brandhagen. brandhagen.com .