[dolphinsea14]

Hi everyone,
I am synthesizing ferrocene, for that purpose I need cyclopentadiene. I have a question and would be very thankful if you could help me.
Can cracking and distillation of dicyclopentadiene to cyclopentadiene be done without nitrogen atmosphere?
Thanks in advance

[pgk]

Yes, you can but it is not recommended for safety reasons.
1). Both dicyclopentadiene and cyclopentadiene are highly flammable.
2). Besides, the high distillation temperature favors their oxidation in air and will decrease the distillation yield.

[dolphinsea14]

Yeah, I know that it can be dangerous, but I had no idea how much. We don't have nitrogen at university, that's why I asked if it could be done without it.
Thank you very much

[dolphinsea14]

Can you suggest good way to synthesize nitrogen for inert atmosphere, and dry it?
I was thinking about using gas bubbler containing concentrated sulfuric acid, will it be enough to get clean and dry nitrogen? Or can it be done using silica gel?  Is there another way it could be done? (I have no much experience I'm doing a synthesis on my own for the first time, I had to design it myself, please help...)

[pgk]

No, don’t do that. You are going to combine a dangerous technique with another and more dangerous one.
Alternatively, you can distill small amounts of dicyclopentadiene, in the lab fume with a closed safety screen and under adequate ventilation.
But take care and pay attention for any ignition source, nearby.

[dolphinsea14]

So there is no way I can synthetize nitrogen and conduct it in the destillation apparatus? This is how it should look like...

[Arkcon]

Try to get a small tank of clean, dry nitrogen.  It is literally cheaper than air.  That's not a joke, they will actually sell you a tank of nitrogen for less than a tank of air; economy of scale, demand and supply, etc.

[dolphinsea14]

Yeah, that would be great, but I can't buy it, I am a student at college, in country like ours finding and buying chemicals as student, is not that simple. It's a bit complicated...
However, I need a way to synthesize nitrogen and conduct it. Buying is not an option.

[Borek]

If you are doing it as a part of your course it is not up to you to buy the chemicals, it is up to the school to provide you with the necessary reagents and hardware. Have you talked with your supervisor?

[Arkcon]

You could also get another school to lend you a nitrogen generator, basically a system that pulls air over an oxygen consuming reagent and gives you clean dry nitrogen.

When a chemist needs nitrogen, they get it from a tank or the atmosphere.  Finding the most energetic nitrogenous compound, and decomposing it, carefully, to get nitrogen gas is beating a wasp's nest with a stick because you need a sheet of paper.

[dolphinsea14]

Yes, of course I talked to my supervisor and to the lab assistant. I asked for nitrogen. They said I will have to synthesize it, because we don't have nitrogen.

[dolphinsea14]

I know Arkcon, that's true, I totally agree, but unfortunately things in Macedonia don't work that way. It's a bit  silly, they ask us to make something, don't have all the necessary stuff, so we have to make our own solutions, find alternatives. Sad, but true.

[clarkstill]

Finding the most energetic nitrogenous compound, and decomposing it, carefully, to get nitrogen gas is beating a wasp's nest with a stick because you need a sheet of paper.

that is an outstanding metaphor

[Enthalpy]

Could clean argon be easier to find in your university? It serves for welding.

[wildfyr]

Purposefully generating nitrogen from a solid is reasonably similar to setting off an explosive on purpose. Have you heard of ammonium nitrate or azide explosions? Those are examples of generating nitrogen from a solid.

We aren't trying to pile on, we are just telling you, with the weight of decades of experience among the respondents, that it is very very dangerous to try to make nitrogen in situ like that, and finding nitrogen already in gas form is so much easier and better in every single way. Argon would work too.

Do you have a biology department? They often use liquid nitrogen. If you can get that you can get some you can add it in small amounts to an attached container and it should supply N₂ to a reaction. It sure is more cumbersome than just a tank. OR you may be able to charge a gas tank off the liquid nitrogen container.

Heres an odd angle that I can't find a counterargument to aside from price. What about helium? They have it in party stores. You could buy a whole bunch of balloons...please shoot me down if I'm missing something obvious.

Another note about the sulfuric acid bubbler: that removes water, not O₂ which is what you are trying to exclude.