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coppercone
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Storage of liquid chlorine
I am curious about this.
A cheap way would be to store it in a seamless stainless steel tube of 310 stainless steel.
The pipe could be closed off using swagelock fittings. A ball valve could be used on one end and a end cap could be fitted on one end.
I thought this would be highly reliable. A 3/4 inch wide pipe at a foot long would store a useful amount of chlorine for laboratory synthesis.
There is no risk of problems stemming from water residue in weld porosity.. I would not be confident in gas tight tig welding. The ball valve could be
closed with a thread when not in use.
The only issue i see is water ingress at the valve interface when the gas is used. I thought that closing the valve and putting the fitting under high
vacuum and gentle heat after use would evaporate any residual chlorine after use, then it could be capped hot to further protect the valve.
Thoughts? I was personally very impressed eith swagelock. Gyrolok might be a bit better however.
Small nonpenetrating welds can be made after assembly but prior to filling to prevent something stupid like someone trying to undscrew a container at
roughly 100 psi.
Also, is there some kind of method of preventing liquid chlorine from shooting out of the cylinder?
Something analgous to tbe stem found in butane lighter that only lets gas through. I feel such a stem would greatly increase the saftey. The gas could
simply be recondensed when desired in liquid form. I rarely see liquid chlorine being used in synthesis, and if it is you are cooling it antway so
adewar condenser should be available.
A needle valve might be abetter choice since the flow of chlorine would be severely restricted as compared to a ball valve so even a catastrophic
acident gives you more time to react.
[Edited on 24-5-2018 by coppercone]
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Ubya
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i wanted to store chlorine for a long time, but i fear a metal tube under pressure corroding and exploding turning my lab in a gas chamber.
a needle valve i think is a must, i once pressurized an empty fire extinguisher after modifying the default valve with a ball valve, i had the
brilliant idea of opening all the way the valve while there were maybe 3 bars of pressure inside the extinguisher, ears ringing and a strong
knockback. forgetting if the tube is pressurized with chlotine and opening the ball valve would spry lots of chlorine gas, a needle valve or regulator
should be used, but will an off the shelf part survive corrosion?
[Edited on 24-5-2018 by Ubya]
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feel free to correct my grammar, or any mistakes i make
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coppercone
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I am investigating this issue in corporate literature currently.
I know certain gases are stored in a laboratory setting. I have seen ammonia and other more toxic gasses stored in cylinder form. I am not sure what
measures are taken exactly, other then anhydrousness.
I also think that a special storage unit is required, I.e. a vented armored column that will contain the gas in the event of a leak and distribute it
to a roof. The amount of gas stored should be such that if a leak occurs lethal concentrations are not approached. Active measures can be taken such
as a detector which turns on an evacuation fan, but risk should be minimized. I was suprized how I saw toxic gasses being stored in a laboratory
setting actually, I thought it was reckless.
I do not believe this to be wise to do unless you have a significant property and a chain link fence around your laboratory.
It should probably be stored like ammunition inside of a modern battle tank.
I don't particularly like generation of gasses specifically for a reaction, unless the toxicity is extremely high, but this reactions I will not do
(i.e. phosgene, ketene) due to the inherent danger.
The problem with the needle valve is of course its rather wimpy. I believe that a ball valve should be used in conjunction with a needle valve, they
are mechanically rather robust.
[Edited on 24-5-2018 by coppercone]
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VSEPR_VOID
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I had a some what similar idea a long time ago, well I had means I saw a similar video on the storage of CO2 by Cody.
https://www.youtube.com/watch?v=rPxPyD5jSR4
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coppercone
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Yea but I think the difference is swagelok will have a few orders of magnitude more reliability then some galvnized NPT threads.
And I recognized a fatal flaw in most of these, which is the lack of burst disks... with swagelok parts you can get an aftermarket burst disk that
will go at like some custom PSI level.
Otherwise if there is a fire that thing will go off at its maximum pressure....
You would need to add a T-junction and a burst disk
And we still need to devise some kind of anti-liquid chlorine siphon thingy
[Edited on 24-5-2018 by coppercone]
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Sulaiman
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300ml liquid chlorine in an amateur lab ?
Obvious but I'll mention it anyway;
300ml liquid chlorine = 468g = 13.4 moles = c300 litres gaseous chlorine 
Given that 1000ppm is a lethal concentration,
300ml of liquid chlorine would fill a space of 300,000 litres (300 cubic metres) to a level where a few breaths are lethal
... a space larger than most amateur or even professional labs.
and, given that chlorine is denser than air, an even larger area would be lethal.
[Edited on 24-5-2018 by Sulaiman]
CAUTION : Hobby Chemist, not Professional or even Amateur
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coppercone
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Quote: Originally posted by Sulaiman  | Obvious but I'll mention it anyway;
300ml liquid chlorine = 468g = 13.4 moles = c300 litres gaseous chlorine
Given that 1000ppm is a lethal concentration,
300ml of liquid chlorine would fill a space of 300,000 litres (300 cubic metres) to a level where a few breaths are lethal
... a space larger than most amateur or even professional labs.
and, given that chlorine is denser than air, an even larger area would be lethal.
[Edited on 24-5-2018 by Sulaiman] |
no I meant 30mL sorry. Extra 0. The volume of the tube itself would be close to 300mL, 0.75 inches * 12 inches cylinder = 21.21 inches cubed =
347.56963 cubic mL,
You would not want to fill it more then 10% or so because it may boil upon opening and you want to ensure that gas comes out not liquid chlorine
sputtering, so 10% of 350 ~ 30mL
If liquid chlorine aresol came out of it while it was connected to any kind of glassware you might have serious problems and or an explosion I think.
That guy just raged my typing. I am sure you can understand being accused of terrorism is an irritant.
The chemical is much less convenient then bromine.
Pretty sure that generating 300 liters of chlorine is insane in itself, that requires serious land to do safely.
This is meant for things like stannic, aluminum, iron, etc chloride generation etc
[Edited on 25-5-2018 by coppercone]
[Edited on 25-5-2018 by coppercone]
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Bert
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Thread Split
24-5-2018 at 17:25 |
XeonTheMGPony
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Do not use ball or needle, the proper valve for this application is a pack less globe valve, some have integral rupture disks.
for dry chlorine steel is acceptable, 316L stainless will last dam well forever, make sure it is a design that allows for easy seal replacement as
most wreck valves by over tightening them <_<
https://www.evergreenmidwest.com/6674-series-316l-ss-diaphra...
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coppercone
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Interesting. Any idea on the siphon? So its absolutely impossible for liquid chlorine to go and squirt out, like in a butane lighter?
The little white stem bit that you take out if you want to make a dangerous/prank lighter.
And I guess 316 is a better choice then 310? Still mean to read the literature though.
Swagelok sells globe valves too.
Can you tell us more about the design of the valve you chose and why its superior (is there something other then the burst disk? does the geometry of
it give it enhanced corrosion resistance?)
Having to get tanks that feature the NGT thread is probably difficult in 316, and so is machining/tapping a NGT thread possibly, I assume you would
need a carbide tap to do stainless 316, I assume its very tough.
Then again grainger sells threaded pipe for like 40$
I guess you just need to find a female to male adapter... 100 psi is not much. So long you gave it a small weld after you put it together to prevent
unscrewing it might be pretty decent, but you still get more failure modes then a real tank because you will have much more mating surfaces.
https://www.eng.ufl.edu/labsafety/wp-content/uploads/sites/2... good literature
Also what is wrong with a needle valve? I thought they are 'globe type'?
[Edited on 25-5-2018 by coppercone]
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LearnedAmateur
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They use inert fibres (asbestos, glass, agamassan, etc.) in acetylene tanks to stop it from exploding when pressurised, the gas is adsorbed by the
porous material. Does that seem like a plausible method for keeping it from spraying out at high pressure? I don’t have much experience with
pressurised gases but it sounds like it could help out and be far better than a bare tank.
In chemistry, sometimes the solution is the problem.
It’s been a while, but I’m not dead! Updated 7/1/2020. Shout out to Aga, we got along well.
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coppercone
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I thought acetylene has it dissolved in acetone soaked into porous material
Does not matter too much since youare just burning it for heat.
[Edited on 25-5-2018 by coppercone]
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LearnedAmateur
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Oh yeah, it is dissolved in acetone or other suitable solvent and comes out of solution with reduced pressure, but still presents an explosion hazard
unless the porous material is present; I thought the same idea could be applied here to help it be released as a gas as opposed to a spray/aerosol -
one of the functions of the ‘wick’ in a disposable butane lighter is to help with that especially when held upside down, where it will spray
flammable droplets if released through a simple valve alone. I was thinking that liquid chlorine may behave in a similar matter, but like I said I
don’t have much experience so take it with a grain of salt.
In chemistry, sometimes the solution is the problem.
It’s been a while, but I’m not dead! Updated 7/1/2020. Shout out to Aga, we got along well.
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unionised
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The stuff about odd storage acetylene is due to the fact that acetylene under pressure is explosive
on its own;
without air.
Not sure whether I'd prefer to be near a failing C2H2 cylinder or a Cl2 cylinder.
Choice between trying to run far enough away fast enough that you had a sporting change of not getting hit by shrapnel or trying to run while holding
your breath (for extra points, run up hill.)
My choice would be... neither.
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VSEPR_VOID
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https://www.sigmaaldrich.com/catalog/product/aldrich/295132?...
They use a steel container with a steel valve. As long as there was not too much pressure you could build a tank from pipes or something like a
propane tank.
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coppercone
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Well, Looking at chemical compatibility charts:
https://www.industrialspec.com/images/files/316l-stainless-s...
Anhydrous Chlorine, Liquid : C = Fair -- Moderate Effect, not recommended
304 stainless steel
https://media.distributordatasolutions.com/ThomasAndBetts/v2...
-same as 316
What are we left with? What has a A- rating for liquid anhydrous chlorine?
All I can find is NICKEL ALLOY C276
[Edited on 25-5-2018 by coppercone]
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LearnedAmateur
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Could use Teflon spray and treat the canister appropriately so that the coating is ready to use - I think you’re supposed to ‘bake’ them
Chlorine gas shouldn’t react with it if well polymerised, but I’m not sure about other safety considerations regarding pressure and such, doubt
they’d impact much since PFTE is one of the most chemically resistant polymers known to man.
I feel like this will be handy, for PFTE coatings in general:
http://www.ptfecoatings.com/what-we-do/faq.php
In chemistry, sometimes the solution is the problem.
It’s been a while, but I’m not dead! Updated 7/1/2020. Shout out to Aga, we got along well.
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coppercone
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I don't think it would be wise to rely on a coating for long term storage of chlorine. That's asking for trouble.
Coatings are a bitch to do properly.
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aga
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I don't think it would be wise to store chlorine at all.
I think it was either IrC or unionised that first made me aware of this simple, yet very powerful fact :-
"if you know how to make it, you never need to store it"
Once i learned that lesson, there was much less worry, or struggle with containing benzene, phenol, rabid monkeys, lizard aliens etc.
There is no longer any need nor desire to store dangerous stuff at all.
[Edited on 25-5-2018 by aga]
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coppercone
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how is it worse then the big bottle of bromine most people have laying around? Usually in glass lol, good to keep frozen I guess
the process of generating it anhydrous combined with what you need to use it for typically is just too much setup.
SO you are gonna setup a anhydrous chlorine generator, figure out all the flow rate control shit through your dryers and whatnot, into a damn tube
furnace? its almost a fucking rupe goldberg machine.
then you gotta worry about a gas generator AND a clogged tube furnace AND a washer for your fume hood all at the same time.
I would feel LESS stress having it on hand then running such a complicated process.
You can super dry it, cryogenically distill it, do all kinds of complicated pain in the ass things to get super purity, store it, and have a better
reaction.
[Edited on 25-5-2018 by coppercone]
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weilawei
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I have an FEP bottle for bromine storage, which I keep at ~-13°C. If the power were to fail, it would still be safe until I could again actively cool
it, because there's only a few mL in a 1000 mL bottle. I have decided that this is an acceptable set of storage conditions for my environment. Room
temperature is no big deal. But chlorine, now that's got a boiling point 93 °C lower than bromine. They have similar heats of vaporization, but in
chlorine's case, you're fighting a low boiling point and the potential for exposure to room temperature.
TL;DR: Storing liquid bromine is a heck of a lot easier than liquid chlorine. For me, liquid Cl is not feasible to store. I'd rather manage a gas
generator than a need for storage below -34°C and a pressure hazard.
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aga
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| Quote: Originally posted by coppercone | | ... SO you are gonna setup a anhydrous chlorine generator, figure out all the flow rate control shit through your dryers and whatnot,
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Yep.
Worked every time so far.
But then again, maybe i just imagined doing those experiments, taking photos, posting them on SM.
Wish i'd gotten with the program and just talked random shit instead.
The chlorine rusted up my shed and everything in it !
Edit:
Tools and stuff were no bother, as they were cheap anyway.
There was a bit of structural damage, but not enough to eat through the paper-thin steel shed. Hammerite now covers it.
My biggest regret (about not having an adequate extractor fan) is the stereo microscope.
It's steel bits are Rusty, which is really Bad for German engineered parts.
[Edited on 25-5-2018 by aga]
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phlogiston
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| Quote: Originally posted by coppercone |
the process of generating it anhydrous combined with what you need to use it for typically is just too much setup.[Edited on 25-5-2018 by coppercone]
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The effort that goes into storing it safely in a homemade pressure vessel is 'not insignificant' either (understatement of the week), . There is the
added worry that you might have overlooked something critical while trying to improvise on tried-and-true methods.
You clearly are aware of the hazards of chlorine, and some of your comments suggest that you realise risking killing your neighbours with poison gas
is somewhat undesirable. (no less of an understatement)
So, I'd suggest you either shelve out the money to buy a commercial, reliable and small cylinder of chlorine gas if you are able to (most suppliers
won't sell to individuals (for good reason IMO as evidenced by this thread)), and that level of convenience is worth it to you, or stick with
generating and drying small amounts in a controllable manner as necessary even if not particularly convenient.
[Edited on 25-5-2018 by phlogiston]
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coppercone
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Well its certainly a luxury given the price of hastalloy valves, you might as well put the money into buying a new property and storing the shit in a
wooden barrel 
There does not appear to be a good solution to this problem due to the exotic metals required. SW still wants a quote AFTER registration for the
necessary hardware. this means your wallet is gonna get FUCKED UP
Now you can store it in cheap 316 stainless, in gaseous form, but its undesirably large container... though pv=nrt, you might get pressure fluctuate
during synthesis due to cooling so it might be actually advantageous to store it in gas form, but then you need to put safety margins on temperature,
you don't want it condensing if heating goes out in your lab..
I don't know how sigma sells for so cheap. Unfortunately they wont do buisness with us 
Any idea where you can get the containers they use? If they are selling it filled with chlorine for 350$ the container must be pretty cheap.
[Edited on 25-5-2018 by coppercone]
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coppercone
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What exactly are they selling? their website is in chinglish
"1000 mL of steel cylinder equipped with stainless steel valve. "
claims to be 1lb of gas, kind of dangerous really. the volume I mean.
Based on someones calculations in this thread, this is a full 300mL of chlorine, in a 1000mL bottle, meaning its in liquid form right?
Bromine is better because it won't all rapidly fill a space if spilled, not like something that boils at -34c
Also, out of curiosity:
"Steel is the most common material used in dry chlorine service. At temperatures above 300°F (149°C) a chlorine/steel fire can result. It is
important to make sure steel in chlorine service does not go above this temperature either through internal/external heating or mechanical abrasion."
that's rather low. Are the exotic alloys also flammable?
And I found this gem:
http://www2.lbl.gov/ehs/Lessons/pdf/AHFcylinderLL.pdf
I would recommend making your own out of the right alloy rather then buying their shit LOL 
told you coatings are trash, and they also use a weld! its not seamless. buncha yahoos are running that operation at sigma, nice use of burst disk
too, that thing flattened out like a fucking bomb
IMO this shit should be stored like this:
there should be a inline burst disk, connected to a vent pipe, that leads off to some high up place, in case something over pressurizes, so it leads
to a far away location devoid of people, but it might be useful if there is a fire, so the stuff does not add to the toxic environment of the flames
themselves.
Kinda wish my welding gas regulators had that feature I don't want the god damn acetylene tank venting in my shop. I did get the long hoses though, so
I can be away from it if there is a fire burning, 20 feet hopefully enough to jump away from a fireball like bruce willis
interesting youtube channel about industrial chemistry accidents and safety recommendations (bit large for us)
https://www.youtube.com/user/USCSB/videos
[Edited on 26-5-2018 by coppercone]
[Edited on 26-5-2018 by coppercone]
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j_sum1
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Seems to me there are a lot of dumb and hazardous ideas being thrown around in this thread. Why not throw a couple of litres of liquid chlorine in an
aluminium dive cylinder and be done with it. If you are into hazardous storage then why make it over-complicated.
I think there are only three feasible solutions to the question of Cl2 storage.
1. Store 0.2mL of liquid chlorine in a glass ampoule and bury the whole thing in acrylic for an element display.
2. Get a proper lecture cylinder of Cl2 gas. Be prepared to pay the bucks and go through proper channels.
3. Make Cl2 gas as needed, employing good lab practice.
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