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Author: Subject: how to get make a nitrogen atmosphere?
XeonTheMGPony
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[*] posted on 21-3-2017 at 12:15


Well what do you have?

There are hundreds of ways to do it but depends what you got on hand and your jerry rigging skills.

I've made gas tight seals with toilet paper, Teflon tape and some capillary tube or needles.

So what do ya got.

[Edited on 21-3-2017 by XeonTheMGPony]
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Db33
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[*] posted on 23-3-2017 at 07:50


i have a lot of flasks, 3 neck and 1 neck and some 2 neck. Round bottom and flat bottom. I plan on getting a nitrogen tank from Amazon. I also have access to various size syringes and needles if that would help, also balloons, etc...

Xeon if you can give me an example of some ways to jerry rig it id appreciate it
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XeonTheMGPony
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[*] posted on 23-3-2017 at 15:55


Ok get a nice medium bore needle, now tightly roll up some toilet paper around the needle till it is a tight fit into the flask neck, now take some Teflon tape and care fully expand it and wrap it care fully around the tissue paper till it is an even thick coat.

this will hold up plenty well for 1 to 2 runs, I used this to seal a nitric acid distillations! You can make it more permanent by soaking superglue into the tissue paper.

Opt 2 is coating a marshmallow care fully in Teflon tape as well works then driving the needle through, use some copper wire to hold it in tight for both options.

[Edited on 23-3-2017 by XeonTheMGPony]
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[*] posted on 23-3-2017 at 18:55


Quote: Originally posted by Db33  
its not a question of what gas to use, im just wondering how to get it from the tank into the flask and keep it there.

All you need to do is get the gas in and stopper it off. The rubber stopper should keep gasses from getting in pretty good.

Also, this may be a dumb question, but why do you need a nitrogen atmosphere when our atmosphere is already 70% nitrogen? Is the reaction oxygen sensitive?
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clearly_not_atara
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[*] posted on 23-3-2017 at 23:15


I think maybe a solution of copper and ascorbic acid can be used as an oxygen scrubber. Subject to degradation of ascorbate of course. Ascorbate is cheap enough that you could deoxygenate a few dozen liters of air by this method -- you just need some means to use it.
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Melgar
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[*] posted on 24-3-2017 at 01:32


My idea for a cheap and easy inert atmosphere: Get two five-gallon (20-liter) buckets, with at least one airtight lid. Fill one with water, then put your favorite oxygen/CO2 scavengers in the other. I recommend Ca(OH)2 in water for CO2, and those Hot Hands reduced-iron hand warmers, torn open, for oxygen. Now rig the lid of the bucket up so that you can have a tube coming in, that goes nearly to the bottom, and a tube going out of the top, that doesn't dangle inside the bucket at all. Check to make sure that the volume of the water plus your scavengers won't reach the outlet of the bucket. After leaving it overnight with the lid on, you can then just put the bucket of water above the bucket with the scavengers in it, and siphon water to it as you need inert gas. Use a drying tube, since there will obviously be moisture in the air, and an on/off valve to turn the inert gas on and off. The siphon will stop moving water when the pressure inside the second bucket builds up enough to counter it. Seems an easy enough to get a decent amount of inert gas.

As a bonus, you have a bucket of water in the end that you can throw a vessel into if it's releasing cyanide gas or acidic vapors unexpectedly, and have those vapors be readily neutralized.
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Db33
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[*] posted on 25-3-2017 at 17:24


So if i was doing a 24 hour reflux... lets say in a 3 neck round bottom flask. If i stoppered 1 neck, then using a hose just flushed the entire flask with nitrogen for like 60 seconds and then stoppered the 2 side necks and had a reflux condenser on the top with some a drying tube on top of that. would that be able to keep most of the nitrogen in and the air out?
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JJay
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[*] posted on 25-3-2017 at 17:28


I think usually they would use a bubbler instead of a drying tube. It would be filled with mineral oil, sulfuric acid, or some other oil that has desirable properties and preferably won't react violently if it somehow mixes with your reaction mixture.



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XeonTheMGPony
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[*] posted on 25-3-2017 at 19:06


you need a balloon to act as a pressure buffer int hat instance, another method I fancy is to make a saturated solvent atmosphere, so what ever the most volatile part of the reaction is add a bit more Ml then pull a deep vacuum while warming and no cooling, once it starts to off gas at the top of the reflux condenser put a stopper in and turn on cooling.

This causes a deep vacuum and the only thing in it is your solvent, Naturally this depends on good sealing! and it significantly reduces the boiling temp, so if that is integral to the reaction that method won't work.
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[*] posted on 25-3-2017 at 19:49


One of these could serve as a bubbler. You'd put just enough oil in it to prevent air from getting into the apparatus while still allowing gases from the reaction to escape. If you have a nitrogen tank, you could let gas slowly diffuse through the apparatus and exit by bubbling through the oil (I think this is called running a reaction in a "stream of nitrogen").

I don't know what your reaction is, but the balloon idea might be a good one. A little positive pressure in the apparatus would help to keep out unwanted gases and vapors. Of course, you want to make sure that your balloon doesn't get eaten up by corrosive vapors or solvents, and if the reaction produces large amounts of gases, a balloon might not be able to contain them.

s-l1600 (4).jpg - 149kB




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XeonTheMGPony
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[*] posted on 26-3-2017 at 04:36


JJay has an excellent point! exactly what IS the reaction, we're trying to hit the toilet in the dark here and that tends to make a mess of it!

More details the more accurate the solution can be offered.
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Db33
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[*] posted on 26-3-2017 at 07:34


the reason the nitrogen atmosphere is needed is because the reducing agent is sodium triacetoxyborohydride, which is sensitive to water and air.
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[*] posted on 27-3-2017 at 01:38


There is the Schlenk manifold option, a flask with a tap on it to evacuate and fill with N2 is the standard accessory. Jerry rigging the concept is doable for a back yarder I'd guess.



That's what they look like when set up.



IMG_1718Sml.JPG - 252kB

[Edited on 27-3-2017 by Chemetix]
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NEMO-Chemistry
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[*] posted on 30-3-2017 at 18:01


I looked into getting Nitrogen, although in the end for me Hydrogen turned out to better.

Where I live Nitrogen didnt seem that easy or particularly cheap to get hold of, also I didnt need much. But I did find a source in the end that is probally availiable in more places than you think.

I noticed a tyre and MOT place had a sign saying, "Nitrogen tyre filling service". Now I have NO IDEA why Nitrogen is sometimes used in car tyres, but apparently it is.

So in my case I used a old small tractor, front wheel inner tube, I took it along to the tyre place and they filled up the inner tube with nitrogen for me.

Actually the guy was really cool and didnt charge me for it. Anyway in a push it might be a solution for you, I am told tyre specialist often have nitrogen to fill car tyres with.
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XeonTheMGPony
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[*] posted on 30-3-2017 at 18:28


Lol it is essentially a scam unless you're a formula 1 racer, Nitrogen expands less under the influence of temperature so the tires remain at a more constant pressure.

But it sounds exotic to your average sheeple consumer so an easy extra buck for the companies pimping it out. But good score on a way to make some real use out of that scam.
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[*] posted on 30-3-2017 at 18:34


Quote: Originally posted by XeonTheMGPony  
Lol it is essentially a scam unless you're a formula 1 racer, Nitrogen expands less under the influence of temperature so the tires remain at a more constant pressure.

But it sounds exotic to your average sheeple consumer so an easy extra buck for the companies pimping it out. But good score on a way to make some real use out of that scam.


Thanks for that! I was going to get my mum to fill her tyres with it! All the guy told me was "its used for low profile, high performance tyres". Sounded kind of neat......

But yes I still have most of my nitrogen in the inner tube :D. Although now I use hydrogen for my methane stuff.
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[*] posted on 30-3-2017 at 20:38


Air is predominately Nitrogen! even low profile tires there is zero need for it as airs expansion is not that drastic with tires.

It is just a hilarious cash grab! Just make sure the tires have good tread and are at proper pressure and you'll be fine! and all ways fill when cold!
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[*] posted on 31-3-2017 at 02:45


Quote: Originally posted by XeonTheMGPony  
Air is predominately Nitrogen! even low profile tires there is zero need for it as airs expansion is not that drastic with tires.

It is just a hilarious cash grab! Just make sure the tires have good tread and are at proper pressure and you'll be fine! and all ways fill when cold!


Funny how with most things, the more you take out, the more it costs :D. I am on alot of Gluten free stuff, it costs a fortune! Same with Nitrogen, take a few other gases out of air and charge a fortune for it :D.

I must go back and take a picture of the sign, it will make you laugh! The claims are many, everything from more MPG, to shorter braking distance :D.

Then again the charge £2 for normal air to inflate your tyres in the garage from a machine!! If nothing else, it might help someone out with a source for small amounts and a way to transport it.

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[*] posted on 31-3-2017 at 04:44


Oh we have the same garbage here, I nearly soiled my self laughing when the guy said I "should" use nitrogen for my electric car, I said ya but then I'll have to charge with lighter electricity to see any real change!
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[*] posted on 31-3-2017 at 04:47


Quote: Originally posted by NEMO-Chemistry  
Funny how with most things, the more you take out, the more it costs :D. I am on alot of Gluten free stuff, it costs a fortune! Same with Nitrogen, take a few other gases out of air and charge a fortune for it :D.

I must go back and take a picture of the sign, it will make you laugh! The claims are many, everything from more MPG, to shorter braking distance :D.

Then again the charge £2 for normal air to inflate your tyres in the garage from a machine!! If nothing else, it might help someone out with a source for small amounts and a way to transport it.

Technically, what they're saying is accurate. Nitrogen is slightly polar, and won't diffuse through a tire as much as oxygen does. Also, a car tire that got hot enough could theoretically pyrolyze more readily if there was oxygen diffusing through it. I mean, filling your tires with nitrogen WILL lead to an increase in all the things they mentioned; what they don't tell you is that increases will likely be on the order of 0.01%, which is hardly something that most people would notice.

The cost of stuff is usually based on how much processing has to go into it, as well as how much they can sell. Putting stuff into something is easy; taking stuff out is much harder. Any chemist who as accidentally used the wrong stir rod when doing multiple reactions at once has probably learned that the hard way.

[Edited on 3/31/17 by Melgar]
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[*] posted on 1-4-2017 at 02:59


Quote: Originally posted by XeonTheMGPony  
Oh we have the same garbage here, I nearly soiled my self laughing when the guy said I "should" use nitrogen for my electric car, I said ya but then I'll have to charge with lighter electricity to see any real change!


Where do you buy your lighter electric from? I have a heavy battery for the boat, lighter electric would make moving it easier :D.

Is it expensive? Couldnt find any on ebay, so I guess its banned in the UK. Maybe its some kind of precursor? :P
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XeonTheMGPony
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[*] posted on 1-4-2017 at 05:04


I lived off grid so I know all about heavy awkward So lets start selling helium refills for batteries! lol batteries, I just kept telling the supplier they needed to hurry up and make lead lighter too!
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[*] posted on 1-4-2017 at 05:42


Quote: Originally posted by XeonTheMGPony  
Nitrogen expands less under the influence of temperature so the tires remain at a more constant pressure.


Barely, if at all
https://en.wikipedia.org/wiki/Charles%27s_law
(and changes in the elasticity of the rubber would make a lot more difference.)
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[*] posted on 1-4-2017 at 05:47


Quote: Originally posted by Melgar  

Technically, what they're saying is accurate. Nitrogen is slightly polar,

[Edited on 3/31/17 by Melgar]

That's a clever trick for a diatomic molecule.

Hypothetically, the fact that nitrogen has more "minor" isotopes may make it true, but I'd not want to have to measure the dipole moment of the 15N14N molecule
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[*] posted on 1-4-2017 at 06:10


Quote: Originally posted by unionised  
Quote: Originally posted by XeonTheMGPony  
Nitrogen expands less under the influence of temperature so the tires remain at a more constant pressure.


Barely, if at all
https://en.wikipedia.org/wiki/Charles%27s_law
(and changes in the elasticity of the rubber would make a lot more difference.)


Hence why it is a SCAM or did you miss that part? but people who buy into it think that's the reason to use Nitrogen, it is magical after all.

In refrigeration testing it has less pressure drift as it is OFN dry, so the pressure swing Vs temp is easily accounted for, but for a tire it is meaningless.
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