Sciencemadness Discussion Board

Storage of liquid chlorine

coppercone - 24-5-2018 at 08:48

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]

Ubya - 24-5-2018 at 10:05

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]

coppercone - 24-5-2018 at 11:08

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]

VSEPR_VOID - 24-5-2018 at 13:07

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


coppercone - 24-5-2018 at 14:22

Quote: Originally posted by VSEPR_VOID  
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



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]

300ml liquid chlorine in an amateur lab ?

Sulaiman - 24-5-2018 at 15:17

Obvious but I'll mention it anyway;
300ml liquid chlorine = 468g = 13.4 moles = c300 litres gaseous chlorine :o

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]

coppercone - 24-5-2018 at 16:23

Quote: Originally posted by Sulaiman  
Obvious but I'll mention it anyway;
300ml liquid chlorine = 468g = 13.4 moles = c300 litres gaseous chlorine :o

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 :o

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]

XeonTheMGPony - 25-5-2018 at 03:39

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...

coppercone - 25-5-2018 at 06:40

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]

LearnedAmateur - 25-5-2018 at 07:37

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.

coppercone - 25-5-2018 at 08:19

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]

LearnedAmateur - 25-5-2018 at 09:17

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.

unionised - 25-5-2018 at 09:28

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.

VSEPR_VOID - 25-5-2018 at 10:00

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.

coppercone - 25-5-2018 at 10:20

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]

LearnedAmateur - 25-5-2018 at 11:01

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

coppercone - 25-5-2018 at 11:04

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.

aga - 25-5-2018 at 11:11

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]

coppercone - 25-5-2018 at 11:30

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]

weilawei - 25-5-2018 at 12:54

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.

aga - 25-5-2018 at 13:05

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,

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]

phlogiston - 25-5-2018 at 13:58

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]


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]

coppercone - 25-5-2018 at 15:34

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 :P

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]

coppercone - 25-5-2018 at 15:44

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 :D

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]

j_sum1 - 25-5-2018 at 18:04

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.

XeonTheMGPony - 25-5-2018 at 18:16

Quote: Originally posted by j_sum1  
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.


My favorite has all ways been the chloro Alkylie cell

two electrodes, some mercury, systolic pump, adjustable power supply, and I get free sodium hydroxide and hydrogen while at it!

Very easy to adjust the flow too

coppercone - 26-5-2018 at 08:09

I don't see how buying rated parts and putting them together to make something is dumb and hazardous

unionised - 26-5-2018 at 08:35

Rated for use with (possibly wet) chlorine?

coppercone - 26-5-2018 at 10:01

it should not be wet, but again the only material I can find, listed as compatible without any coating wizardry is hastalloy, which is expensive, meaning this is a serious luxury.

I have a feeling that Sigma aldrich actually sells chlorine in regular stainless steel containers which have some kind of fancy coating.. they claim stainless, and their corrosive gas regulator stations are made of Monel (which is actually incompatible with anhydrous chlorine liquid), so you are reliant on not having any splashing.

Theoretically if you make something out of seamless hastalloy C tubing and valves for use with liquid anhydrous chlorine, it will outperform the reliability of what Sigma is selling.

Also, if you use things like swagelok or gyrolok, you can actually do a full disassembly to completely clean out the container and do a full visual inspection without worrying about things like weld fatigue, since there are no welds, or coating flaking, as the materials are intrinsically compatible.

Since you are using simple pipe, you can also cut the swaged area off after a single use, and buy replacement compression fittings to reuse with the same threads and stuff... they are also generally much more reliable with repeated use then NPT anyway, so you can be confident doing something like a yearly visual inspection on storage cylinder integrity using a boroscope


for storage of things like Hydrogen-halogens, you also don't want welds because they offer a good area for hydrogen to diffuse into and cause metal fatigue, because they will be inherently more porous then the seamless tubing.

If you have a hydrogen stressed weld, it can actually fail at a lower pressure then your burst disk, so the discharge of hazardous material will occur in a different area then anticipated, I think (I would like for someone to confirm this, I am not a welding engineer but this is my understanding of it).


I caution anyone attempting to do this to investigate the compatibility of hastalloy with anhydrous chlorine though, I am not entirely convinced it is at this point in time, I would need to actually talk to a manufacturer.

If it requires any kind of coatings I would say no one should do this at home, just because its a complete pain, especially like coating a valve surface, it would probably need to be reengineered to ensure the coating is not stressed.

[Edited on 26-5-2018 by coppercone]

Panache - 29-5-2018 at 06:54

i stored liquid chlorine in an ordinary reagent bottle in my ultralow freezer for years, its a very pretty colour.
So fuck the hastaloy, the inconel (how is that spelt), the making it whilst trying to use it. btw copper cone i am completely on side as per not be running two reactions simultaneously. Everytime i have used chlorine for something it was....challenging. So you just need to befriend someone in a biosciences lab that cycles their ultralow freezers into scrap every three years, i got mine for $500, or maybe it was $1500.

coppercone - 29-5-2018 at 07:02

How many watts is that to run? I can probobly engineer a multistage freezer, actually for a fixed load a peltier cascade might work if the insulation is good but i dont want a jurassic park situation on my hands.. I had like 14 days no power this year.. The last shit i need is some fucking generator fucking up

Like a well engineered one, how long does it stay cold before you have the return of the living dead on your hands?

I also suspect that a compressor cooled one would stay cold longer then peltiers because the refrigerant can be pumped to the heat exchanger through a thin poor conductor of heat that is well insulated..

[Edited on 29-5-2018 by coppercone]

markx - 29-5-2018 at 11:35

I worked with coupious amounts of chlorine during my days in the supercapacitor/carbide derived carbon related field at the beginning of the 2000s. We had a rather sizeable stockpile of pressurized high purity chlorine in standard 50L sized cylinders that held about 60kg of the liquified gas in a fully charged state if I remember correctly (guess there was some headspace left in the cylinder). Sometimes we had five of those cylinders in house and two flowing concurrently. The cylinders were made of common (or perhaps less common) carbon steel, but no fancy stainless alloys. The valves on the cylinders were made from a brass alloy. They were chrome plated on the outside, but inside was bare brass.
Well long story short.....absolutely everything corroded in contact with chlorine and moisture from the air. As long as the chlorine is anhydrous, there is little chance of major corrosion taking place and even common alloys can withstand the effects, but wet chlorine is a totally different animal. None of the components that came after the actual chlorine cylinder and became exposed to moisture at some point, held for long and were subject to constant failures due to corrosion. The alloy composition was quite irrelevant....high grade stainless steel and special alloys corroded at a visually observable rate and none of the fancy "chlorine rated" components from "Swagelok" justified their astronomic cost. In fact we used regular copper tubing and standard brass pipe fittings and ball valves for years in the low pressure chlorine supply systems for feeding the reactors. To be honest these held up better than the specialty grade components and cost basically nothing in comparison. Also the high end chlorine pressure regulators at the cylinders were subject to failure as the membranes corroded and started leaking quite often. There is no escape from corrosion damage when dealing with chlorine gas that is not completely anhydrous and the only way to get some service life out of the operation is to engineer the system from massive and robust components. For membrane regulators and thinwalled parts the only thing that worked was pure PTFE or fully PTFE lined components.
It was a nightmare to maintain the systems....everything, invariant of alloys used, became coated in hygroscopic deposits of chlorides and was constantly wet, slimy and rusting away under your very eyes. A situation I would not want to encounter on my personal work premises....
As for the lethality of chlorine....well it is not a very effective poison...I survived the nice "atmosphere" for years :D Not to say that suddenly stepping into a room full of the good stuff will not knock you on your ass (don't ask how I know), but for sure you will not keel over dead at the very first breath.
All in all a nasty subctance to work with, especially if you are not prepared to sacrifice all of your tools and equipment as subjects for feeding the abhorrent corrosion that surrounds this element inherently.

WGTR - 29-5-2018 at 11:40

Rather than storing chlorine in liquid or gas form, perhaps storing it on silica gel would work for you as a practical and safer compromise. Adsorb it at low temperatures, desorb it by passing a heated gas through the silica bed.

Note the short section about chlorine storage. It pertains to stripping chlorine of low partial pressure from air.

Attachment: US3063218.pdf (456kB)
This file has been downloaded 262 times

Partial pressures closer to 1atm will get you much better results:

https://pubs.acs.org/doi/pdf/10.1021/j150415a004

(sorry, link only)

coppercone - 29-5-2018 at 15:42

Interesting storage method, like storing hydrogen in palladium or whatever.

Markx, are you sure there was not some kind of process defect from swagelok? I honestly expect nothing but the best from them.

Did you bake the fittings prior to use age? I believe they come lightly greased sometimes. Maybe they were using old grease or something?

And did you have any kind of problems with moisture getting back into the regulators/valves after they were used? (my idea was to basically heat the fittings after use, pull a vacuum on them, then quickly cap them off.

On another note, is there some kind of nonreactive moisture scavanger that can be used inside of the tanks? Like if you put molecular sieves in em. (2A ? need to look at molecule size)

And by low pressure I assume you mean the vaporization pressure of chlorine (~100psi)?

[Edited on 29-5-2018 by coppercone]

markx - 29-5-2018 at 23:47

Quote: Originally posted by coppercone  
Interesting storage method, like storing hydrogen in palladium or whatever.

Markx, are you sure there was not some kind of process defect from swagelok? I honestly expect nothing but the best from them.

Did you bake the fittings prior to use age? I believe they come lightly greased sometimes. Maybe they were using old grease or something?

And did you have any kind of problems with moisture getting back into the regulators/valves after they were used? (my idea was to basically heat the fittings after use, pull a vacuum on them, then quickly cap them off.

On another note, is there some kind of nonreactive moisture scavanger that can be used inside of the tanks? Like if you put molecular sieves in em. (2A ? need to look at molecule size)

And by low pressure I assume you mean the vaporization pressure of chlorine (~100psi)?

[Edited on 29-5-2018 by coppercone]


Don't misunderstand my intentions...I have no plans to claim that Swagelok fittings suffer from any kind of quality defect regarding workmanship or material choice. They make high end components that are really excellent. My point was just that in such an agressive production environment that we had, absolutely everything corrodes and fails irrelevant of material and quality. Throwing expensive fittings to the slaughter at the mercy of the corrosion made no sense.
The scrubbing systems can be applied on the lines, but moisture gets in anyway (unless you work in a space suit under inert and totally dry atmosphere). Changing the cylinders and performing maintenance work will allow moisture to creep in momentarily and that is enough. Unless you dissassemble the whole system, clean it out with water and bake it dry afterwards...then assemble anew. Would make sense in small scale lab setup, but on an industrial setting it is unthinkable practice. And oh yes...the scrubber systems will also corrode and fail (I know from practice :) )

coppercone - 30-5-2018 at 05:50

ok but what do you expect from this procedure.

After use a vacuum is hooked up to the closed valve. Vacuum and heat are applied. The swagelok cap is heated in the oven to 150c.

The vacuum is broken and the hot cap is quickly tightened over the valve. The cap has a silica gel packet glued in it.

Do you think this will protect the valve?


Or are you saying air diffuses into the blasted thing as its operating? I figured it would be connected to any glassware through some kind of trap.

Perhaps after being connected to the glassware aetup a vacuum can be pulled and heat applied to the closed valve to discourage backflow of any humidity.

Then turn on argon purge and add the reactants to the reactors , seal the system against moisture with cacl2 trap, disable purge gas, then start chlorine flow.

Its a bit of procedure to go through but it should work? Or still some kind of problem exists?

The next level of complication that i can phatom would be to add a copper tube on a t junction by the valve exit, cap the thing, and pull a vacuum on the tube then heat it and seal the thing with silver solder each time after use.

I think it will work unless you get water going backwords through the fucking chlorine gas as backflow even with the baking and calcium chloride.

I say to cap it after every use because i figure the valve might leak a tiny tiny bit, enough for corrosion to start.

[Edited on 30-5-2018 by coppercone]

aga - 30-5-2018 at 10:56

Do i recall correctly that len1 came up with some storage method for chlorine involving salt water ?

Suppose i'd better read his paper again (it's in the library).

Edit:

Perhaps i'm missing the point and there's some reaction an Amateur would really want to do at about -40C with large volumes of liquid chlorine ?

[Edited on 30-5-2018 by aga]

Panache - 30-5-2018 at 21:10

Sharp makes an ultralow with vacuum plates as insulation, once at temp they sit idle for most of the time. There isn a power failure backup that is essentially a upside-down log cylinder that vents the atmosphere that i think is right for quite a long time, it uses the normal evaporator not he ultralow.
the second stage on ultra lows always use ethane as the refrigerant.