Distilling pure anhydrous ammonia----make money online

when you hear the word ammonia you might

think of this blue glass cleaner but

actually this is mostly water with

ammonia gas dissolved in it but for some

future experiments I have planned I need

the pure ammonia out of this damn

hydrous ammonia meaning ammonia without

water so in this video I'm going to talk

about how to transform this into an

hydrous ammonia and also how to store

the product the material safety data

sheet is a little sketchy but it's

likely that this contains about five

percent by mass pure ammonia and we

could use that and that would work just

fine however there's other chemicals in

here too that might get in the way so

you can also buy this on eBay and this

is actually thirty percent by mass pure

ammonia so think about that if you took

a third of this entire jug you could

actually extract that liquid and have

pure anhydrous liquid ammonia of about a

third of this entire jug so there's

quite a lot dissolved in there the trick

is that water loses its ability to hold

ammonia as we raise the temperature so

at room temperature thirty percent by

mass is about as high as we can get but

if we start to boil this or if we raise

the temperature on the way to 100

degrees C all of the gas will start

being emitted and by the time we reach

100 degrees C it'll just be pure water

and all the ammonia will have been

driven off the first part of the process

is to put the ammonia solution into a

vessel where we can easily raise the

temperature I originally thought about

using a sand bath or an oil bath to put

this flask in or you know what would be

even better as a heating mantle but I

don't have any of that and since the

temperatures aren't very high this flat

bottom flask on a standard hot plate

worked out just fine and then I stuck a

temperature probe on the outside just to

keep an eye on that and since we're

going to be raising the temperature up

to about a hundred C we're also going to

be getting a lot of water vapor off of

this and the problem is that we don't

want that water vapor in our ammonia gas

as this thing bubbles will be getting

both off and we want to separate out the

ammonia from the water vapor

so the next stage is to put a condenser

on top of the flask and here I just have

very cold water at about five degrees C

running through the coil so as the water

vapor drifts upward through the

condenser it condenses on the coils and

drips back down at refluxes back into

the flask whereas the ammonia gas that's

been liberated from the solution

continues upward through the apparatus

I've used these Keck clamps to hold

together the apparatus but there's a

plug at the top here that purposefully

doesn't have a clamp this is so that if

the pressure increases high enough it'll

just push this cork upward and vent the

ammonia out instead of exploding the

glassware and spraying ammonia

everywhere

which reminds me you'd have to be

totally nuts not to do this in a fume

hood

I used silicone grease on all the ground

glass seals to make sure that everything

was gas tight so at this point in the

system we have fairly dry ammonia gas

but there's still a fair bit of water

vapor mixed in and we'd like to remove

that so that when we compress or chill

our ammonia gas into a liquid we don't

have lots of water contamination so what

we want to do is pass this through a

column of substance that will absorb the

water basically it's a desiccant or a

dehydrator and if you go to a hardware

store you'll find a product called damp

rid which you can't use for this

application because damper it is

actually calcium chloride and that would

react with the ammonia gas

I think silica gel also would actually

react although I couldn't come up with a

definitive answer for that from my

research however there is a desiccant

that works great and that is sodium

hydroxide or lye 100% lye potassium

hydroxide would be even better but

that's harder to find the stuff you can

get at the hardware store so I have this

glass column and at the tip here I've

put some glass wool just to keep the

granules of sodium hydroxide from

slipping through and then I dumped in

you know about a handful just the amount

is not too critical of sodium hydroxide

and as the gas sort of diffuses through

these NaOH pellets the water will be

absorbed and the ammonia will pass right

through so at this stage in the system

we have fairly dry ammonia

gasps at just over one atmosphere of

pressure in order to store that gas we

either have to compress it using a you

know a mechanical compressor or we could

chill it to the point where it condenses

into a liquid and then we could pour the

liquid into a vessel and that's that's

the route that I chose to use this piece

of equipment is a cryogenic freezer it

has a well that's filled with alcohol in

here and when it's running it can get

all the way down to negative 100 degrees

C so my plan originally was to get a

small round bottom flask and get this

hose adapter and then connect this hose

up to the ammonia stream coming out of

the glassware that we just saw and then

put this down into the cold trap

so as the ammonia gas went into the

flask it would condense in here and I'd

end up with a full flask of liquid

ammonia this ended up not working

probably because the thermal transfer

through the glass wasn't very good and

also when the system starts up there's a

lot of air that has to be purged out of

all that glassware and so you have to

sit there for a long time with with this

system open so that to get the air out

and meanwhile there's you know tons of

ammonia vapor coming coming out as well

so ideally we'd have a condenser setup

just like above the boiling flask where

there's like a cold liquid flowing

through and then as the ammonia drifts

through it condenses on those coils so

for a while I thought well maybe I could

do like a submersible pumping here that

would pump the cryogen up into a coil

then the thing would drip down is that

pump is a problem in priming it and the

rubber is freeze and all that kind of

stuff so eventually I came up with this

system this is a stainless steel piece

of apparatus in fact it was originally a

nitrogen purification cartridge this is

what the top of it looked like nitrogen

purification now this wasn't a nitrogen

separation membrane this thing requires

that your gas already be 99% pure and

then this will take you up to 99.999 or

whatever and it was already spent so I

cut it up and wanted it just for the

fittings and the fact that it was made

of stainless steel all the fittings are

stainless including the sealing ferrule

that's inside there and I bent the tube

around so that when this thing sits down

into the cold

the cold alcohol in there the ammonia

will have more than enough chance to

condense and it will flow up in here as

a liquid and then this thing will you

know hold all the liquid until I'm ready

to put it in the storage container and

this ended up working quite well the

storage tank for the anhydrous ammonia

must have all steel or stainless steel

construction because the ammonia will

corrode brass and other copper

containing alloys the tank must also be

about you know this big to hold the

quantity that I needed and also have a

small enough diameter to fit down into

the cryogenic freezer and must also have

a working pressure of a few hundred psi

so this tank is pretty much perfect this

is a liquid propane tank that you can

get at the store for just a few dollars

really and I set about converting it for

use with ammonia I used a really coarse

screw to yank out this plastic collar

that's on the inside of the neck and

then used a Schrader valve tool to

remove both the main valve that's in the

the neck of the cylinder and also the

safety relief valve

I found a 1/8 to 3/8 pipe fitting that

had an outer diameter almost exactly the

same as the propane cylinder neck and I

TIG welded this on after the weld was

cool I hooked up the cylinder to a

pressure manifold and then used an old

refrigeration compressor to just pump

air into the cylinder as a pressure test

and one thing that I found interesting

is that the safety valve doesn't have a

hard stop it's not like you screw in the

safety valve and it has a preset

pressure it actually the set pressure

goes up as you screw the valve in

further and further and there's no

definitive stop in there which I found

kind of weird so I used my AC this high

pressure gage on the AC manifold to

check the pressure while I screwed the

valve in further and set it to a relief

pressure of just over 300 psi so here's

the whole system running we've got the

ammonia solution bubbling away we've got

the cold water circulating and

condensing the water vapor which we

don't want and then the gas the ammonia

being dried and passing down into the

cryogenic freezer where it's being

liquefied and then every half hour or so

my little stainless condenser would be

filled up

and I would manually tip it out and pour

the ammonia into the storage container

and I had to remove the emergency

expansion valve off of the container to

provide a vent path the neck is still

very small diameter inside there and so

even using a funnel the boiling vapor

would just cause the ammonia to splatter

everywhere and if you're wondering yes

the smell was terrible in fact the the

vapor that this thing puts off is you

know ridiculously strong actually and I

did in fact use this when I was doing

the ammonia transfers

I really couldn't endorse it since this

is kind of more of a you know a novelty

almost at this point it's it is actually

a real gas mask but this cartridge is

old however despite all that using this

made it such that I could almost not

even smell the ammonia inside the mask

so I was very happy to have this today

another problem I had is that the

cryogenic freezer has only an on/off

switch it's meant as a cold trap device

and as soon as you switch it on it tries

to get down to negative 100 C as quickly

as it can however the melting point of

ammonia is negative 78 C so if the cold

trap got all the way down to negative

100 instead of condensing it actually

freeze the ammonia solid and I actually

found this out the hard way too so in

that narrow passageway at the bottom of

the condenser this this will become

solid ammonia and then nothing passes

through and the system pressure builds

up until that glass cork pops off and

sprays ammonia out so I don't have a

temperature controller for this so I was

just switching the freezer on and off

manually

anyway after getting all these kinks

worked out after about half a day today

I built up quite a bit of liquid ammonia

and I took the storage container out of

the freezer and screwed in this steel

valve so that now the thing you can hear

the liquid sloshing around in there but

now I can control it very easily through

this steel needle valve here's an

interesting demonstration we can do with

some of the anhydrous ammonia that I

just created so I have a beaker filled

with some of the chilled alcohol and

then inside the test tube is the

anhydrous M

and I have a little stir bar sitting at

the bottom there and this whole thing is

on a stir plate and the idea with using

this beaker of cold ammonia or cold

alcohol is just to give this more

thermal mass so that the ammonia doesn't

boil away so I'll start the stir bar

spinning a little bit and to it I'm

going to add lithium metal

I just put in a flake about the side

let's do another one and you can hear a

slight amount of boiling right as the

lithium goes in and hits the cold

ammonia this is called the birch

reduction and the color actually comes

from free solvated electrons so what

you're looking at is an extremely good

electrical conductor because it has free

electrons

as you can see after I add more lithium

metal these solution changes from a dark

blue color to this very metallic bronze

color it's really a beautiful color

ammonia gas is technically flammable but

not really I hooked it up to my manifold

and made a primitive torch and then

sprayed pure ammonia over an alcohol

flame as you can see it actually puts

the flame out it's it doesn't catch at

all in that sort of circumstance so I

decided to up the ante and I mixed the

ammonia with pure oxygen and then shot

that out of the makeshift torch and as

you can see it still doesn't even

sustain a flame I tried different

mixtures I probably could have dialed it

a little bit more carefully but needless

to say it's not really much of a fire

hazard since it's just so difficult to

get started I believe the ignition

temperature is even higher than the

flame temperature which you know it

means it doesn't self-sustained okay

stay tuned to see what I have plans next

for this see you next time bye invest online and earn money, best online money making, online money income, view ads and earn money without investment, earn money online by clicking, online money income site, money earning sites, online earning sites, best website to earn money, free money earning sites, money earning websites, get money online, online earning tips, online earning without investment, earn money online without investment for students, earn money by clicking ads, earn money online without investment, online earn money website, online jobs to earn money, best online income site, top 10 online money earning sites, easy income online, easy online earning, earn money online from home, make money online legit, earn money online free fast and easy, online earning websites list, genuine online money earning sites, online work to earn money, online surveys to earn money, earn money through internet, best online income, earn money online data entry, easy ways to make money online, best online earning websites, top websites to earn money, online typing jobs for students to earn money, earn skrill money online, earn skrill money,