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Topic: How to collect and store Cl?  (Read 17004 times)

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Z-Malti

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How to collect and store Cl?
« on: April 10, 2006, 11:33:10 AM »
I am trying to make chlorine gas (HCl + MnO2) for my element collection but i am having problems finding ways how to collect the gas in a safe way and how to store it since it corrodes the caps of storage bottles.  Any ideas?
Thx

Offline woelen

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Re: How to collect and store Cl?
« Reply #1 on: April 10, 2006, 12:24:55 PM »
You should bubble the chlorine through a small gas-wash bottle, filled with H2SO4 for drying. Probably, passing it through a tube of dry CaCl2 also does the job. After that, it has to be passed into a glass tube, which has to be melted, such that the gas is trapped into a self-made ampoule. It simply is not possible to find a bottle, such that the sample remains OK for more than a few weeks. Every cap finally will be eaten away by the chlorine gas. You can't store it in a visible way, except in a completely sealed glass ampoule.
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Offline P-man

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Re: How to collect and store Cl?
« Reply #2 on: April 10, 2006, 04:41:40 PM »
Yes, it is one of the most difficult gases to store, if not the most. What woelen is saying is the best way to do it, according to my teacher. If you could find an airtight glass cap the nyou might be O.K., but then the gas might corrode the whatever that makes the cap airtight.
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Offline constant thinker

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Re: How to collect and store Cl?
« Reply #3 on: April 10, 2006, 08:06:12 PM »
Flourine gas is harder to store. It'll corrode just about anything it comes into contact with. ;)
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Re: How to collect and store Cl?
« Reply #4 on: April 11, 2006, 05:01:53 PM »
Which is why I chose the particular grammar that I used.
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Offline jdurg

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Re: How to collect and store Cl?
« Reply #5 on: April 17, 2006, 10:17:56 AM »
You should bubble the chlorine through a small gas-wash bottle, filled with H2SO4 for drying. Probably, passing it through a tube of dry CaCl2 also does the job. After that, it has to be passed into a glass tube, which has to be melted, such that the gas is trapped into a self-made ampoule. It simply is not possible to find a bottle, such that the sample remains OK for more than a few weeks. Every cap finally will be eaten away by the chlorine gas. You can't store it in a visible way, except in a completely sealed glass ampoule.

I'll just re-iterate what Woelen has already stated so perfectly.  Below is the procedure I used to generate and store the chlorine gas which I have as a part of my collection.  (And this method of storage is how I store ALL of my halogens and there simply is no way to safely keep halogens in an openable container without it eventually eating everything).

1):  Setup three different reaction "vessels" all interconnected by glass tubing.  Vessel one is where the chlorine gas will be generated.  Vessel two will be pure distilled water as this will dissolve any acid vapors left over.  Vessel three will be an anhydrous dessicant which will absorb any water that is present without reacting with the chlorine gas.

2):  Since chlorine gas is denser than air, you want to setup your vessels so that each subsequent one is lower than the previous one.  This will force the chlorine along the setup and into your collection tube.

3):  In the reaction vessel, place your MnO2 or Ca(ClO)2 power/slurry.  (I find it works best if it's a slightly damp "mush").

4):  Slowly drip in your concentrated HCl until you start seeing bubbles of a greenish gas forming.  This will be your chlorine and possibly some ClO2 as well.  Keep in mind that you will want to seal off the opening where the HCl was added, and you want your "vessels" to be fairly small so that it forces the formed gas out the only open hole.

5):  The vessel with the distilled water should dissolve all of the HCl vapors, a good deal of the ClO2, and sadly a good deal of your Cl2.  However, the amount of Cl2 that will dissolve should be tiny compared to the amount you are generating.  The inlet tube should be below the water line and the outlet tube should be placed above the water line so that the Cl2 will bubble up and out into your dessicant tube.

6):  For the dessicant, I used anhydrous NaHCO3 because it absorbs water pretty readily and didn't react with the chlorine gas.  Again, the inlet tube was placed below the pile of NaHCO3 so that the opening wasn't visible and the outlet tube was placed at the top above the powder line.  This ensures that the Cl2 coming out would pass through the dessicant before coming out of the tube.

7):  The final outlet of the tube was placed into an upright test tube which had been thoroughly cleaned and dried.  A piece of white cardboard was placed behind the tube to make the chlorine even more visible.  Once the tube had been filled and the green color was readily apparent, the tube was quickly melted shut through the use of some propane torches.  The chlorine gas was now permanently stored inside the tube and you can see the green color VERY readily when looking down the long end.

Sealing the chlorine in the tube is the only way it could be stored safely.  I also took my bromine and iodine samples and sealed them in glass tubes as well to keep them indefinitely and safely.
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Z-Malti

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Re: How to collect and store Cl?
« Reply #6 on: April 17, 2006, 10:59:07 AM »
Thx jdurg and all the rest for helping me!  :)
It's quite wonderful how you can make your own elements with cheap chemicals and find a way to store them.  I tried the set-up and it worked just fine producing some nice Cl2 gas which I quickly sealed and now I have one more element added to my collection! Hurray

P.S: The Cl2 gas produced has quite a high purity, I think It's about 90%-99% pure.  How can you check the purity of gas produced?


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Re: How to collect and store Cl?
« Reply #7 on: April 17, 2006, 11:07:41 AM »
Thx jdurg and all the rest for helping me!  :)
It's quite wonderful how you can make your own elements with cheap chemicals and find a way to store them.  I tried the set-up and it worked just fine producing some nice Cl2 gas which I quickly sealed and now I have one more element added to my collection! Hurray

P.S: The Cl2 gas produced has quite a high purity, I think It's about 90%-99% pure.  How can you check the purity of gas produced?



Glad to here that it worked out for you.  It's always fun when the elements you've added to your collection were made yourself.  My chlorine and red selenium were made myself so they are two of my more "special" samples.   ;D

For checking the purity, the only real way to do that is to collect a sample of your gas in a vacuum so that the only gas inside the tube is the chlorine you had generated.  Then you slowly react all of the chlorine and see if there is any volume left over.  What's left over is your non-chlorine gas.  This is something that is typically VERY difficult to do and really can't be done easily by the home chemist.  If you've allowed the Cl2 to pass through a sufficent amount of distilled water and have dessicated it quite well, your purity should be close to 98-99%.
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Offline Alberto_Kravina

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Re: How to collect and store Cl?
« Reply #8 on: April 17, 2006, 11:21:35 AM »
Quote
How can you check the purity of gas produced?
Hmmm...maybe something like this: You could make react a known volume of chlorine with conc. NaOH (the Cl2 absorbs and reacts to Sodium hypochlorite (Cl2 + NaOH ----> NaOCl + NaCl)). Afterwards you could determine the amount of hypochlorite with a titration.
...you could calculate the percentago of Cl2 like this, but I doubt that it's an accurate method. ???

Offline Borek

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Re: How to collect and store Cl?
« Reply #9 on: April 17, 2006, 04:09:04 PM »
I would rather use Cl2 to displace I- from some iodide solution, than titration of iodine is quite simple with thiosulfate.

The problem is, other gases can be strong oxidizers as well. Spectroscopy will be probably better.
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Offline Alberto_Kravina

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Re: How to collect and store Cl?
« Reply #10 on: April 18, 2006, 01:02:45 PM »
Quote
I would rather use Cl2 to displace I- from some iodide solution, than titration of iodine is quite simple with thiosulfate.
That's a good idea...do you know what, I think that 'll try to perform this analysis as soon as I have enough time. I'm curious what the result will be...

PS: I think that a syringe full of chlorine is enough....I don't think that I need such a big quantity of Cl2... :P

Offline Borek

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Re: How to collect and store Cl?
« Reply #11 on: April 18, 2006, 01:55:35 PM »
Think first, act second ;)

Calculate moles of Cl2 in syringe to estimate volume of thiosulfate solution needed. It may be OK - but it may be not.
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Offline Alberto_Kravina

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Re: How to collect and store Cl?
« Reply #12 on: April 18, 2006, 02:07:16 PM »
Haha! Yeah - you're right, I'll estimate it... ;)
I should have a result on Friday :)

Quote
It may be OK - but it may be not.
Yeah....I wouldn't surprise me to get a "stupid" result

However, do you think that 100% Cl2 reacts with the iodide solution if I just inject the Cl2 in the KI-solution? ???

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Re: How to collect and store Cl?
« Reply #13 on: April 18, 2006, 02:18:45 PM »
However, do you think that 100% Cl2 reacts with the iodide solution if I just inject the Cl2 in the KI-solution? ???

While it will react very fast IMHO, it may bubble out. Try to use high tube with iodide solution and bubble chlorine slowly from the bottom - this way you will see if bubbles reach the top or not.
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Offline Alberto_Kravina

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Re: How to collect and store Cl?
« Reply #14 on: April 23, 2006, 03:33:07 AM »
Well, here the results of my analysis:

2KI + Cl2 ? 2KCl + I2 ...always start by writing a balanced equation... ;)

v(KI)= 20 mL
c(KI)=0,05mol/L (0,1N)
=>n(KI)= c * V = 0,02L * 0,05 mol/L =  0.001 mol

n(Cl2)= 1/2*n(KI)
=> n(Cl2)= 0.001 * 1/2 = 0.0005 mol

So I need about 0.0005 mol of chlorine

1 mol ? 22,4 L
0.0005mol ? 0.0112 L

0.0112 L = 11.2 mL (I took 10 mL)

Titration with thiosulfate (0,1N):

V(Na2S2O3)=14.85 mL
t(Na2S2O3)= 1.0127

I2 + 2 Na2S2O3 ? 2 Na2S4O6 + 2 I-

n(I2)= 1/2*n(Na2S2O3)
n(Na2S2O3)=c*V*t = 0.1 mol/L * 1.0127 * 0.01485 L =0.00150386 mol

=>n(I2)=0.00075193 mol

n(1/2 I2 ) = n(1/2 Cl2)
0.00075193 mol = m/M(1/2 Cl2)
=>m(Cl2)= 0.02665794 g

m(mixture) = Rho(Cl2) * V(Cl2 = 2.95 g/L * 0.01L = 0.0295 g

=>w= 90.36 %
 

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