| Pages:
1
2 |
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
Made Bromine Tonight
Today I performed the most terrifying reaction I have ever done. The synthesis of elemental Bromine. Of course it was done outside with full
protective gear and a respirator. After amoupling the small sample I made, I realized the ampoule didn't fully seal, and some bromine vapor was
detectable, even got a very small whiff of it! Scary! So I went outside and resealed it properly. The Bromine ate up the rubber stopper used pretty
quickly, but the whole apparatus was submerged in Sodium Thiosulfate solution to neutralize all bromine immediately after collecting enough Br for the
element collection.
|
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Cool!
Wait a minute, where's fluorine...?
|
|
|
elementcollector1
International Hazard
Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline
Mood: Molten
|
|
I think he got CaF2 instead, judging from the photo...
Nice wooden Periodic Table!
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
|
|
|
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
That's certainly an element that I'm "cheatingly" displaying for good! The little ampoule you see there is just full of compressed PTFE tape; about a
half roll of it in that little ampoule! Bromine was plenty scary enough!
|
|
|
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
Pretty embarrassing, I just realized in my bromine induced adrenaline rush, I put the Br where Cl belongs.... 
Its now resting in its correct place on the periodic table.
[Edited on 15-9-2013 by BobD1001]
|
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Thought something looked out of place. Wasn't sure if you already had chlorine (cheating aside, fluorine isn't an easy one!). 
Speaking of chlorine, you could ampoule it with the help of dry ice and acetone; think a few here have done it before.
Tim
|
|
|
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
Tim, Thank you for the suggestion! I will certainly look into that! Do you happen to know what kind of pressure is generated from ampouling the
chlorine when it returns to room temperature? I would be concerned about ampoule rupture as mine aren't very thick (just flame sealed pasteur
pipettes).
|
|
|
elementcollector1
International Hazard
Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline
Mood: Molten
|
|
Quote: Originally posted by BobD1001  | | Tim, Thank you for the suggestion! I will certainly look into that! Do you happen to know what kind of pressure is generated from ampouling the
chlorine when it returns to room temperature? I would be concerned about ampoule rupture as mine aren't very thick (just flame sealed pasteur
pipettes). |
The full explanation is, you would generate a few drops of liquid chlorine, allow these to boil (the expanding chlorine gas is heavier than air and
purges the ampoule), and seal it. Liquid chlorine would take much heavier ampoules.
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
|
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
BobD1001, you made a really beautiful display box for the elements. I love to see this kind of work. I myself ampouled bromine and chlorine as well
and I found ampouling of both elements to be quite easy. The most important thing is that you have to make the elements in a REALLY dry state. I used
H2SO4 for drying the Br2 and used a mix of CaCl2 and P4O10 for drying the chlorine:
This is the chlorine ampoule I made (gas only): http://en.wikipedia.org/wiki/File:Chlorine_ampoule.jpg
This is the bromine ampoule I made:
|
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
Indeed, it does not wet glass when dry. The following page contains two movies which demonstrate this effect.
http://woelen.homescience.net/science/chem/compounds/bromine...
|
|
|
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
Now I'm concerned about my small sample of Bromine... It looks to be relatively pure, however I did not dry it as I wanted to minimize the amount I
was working with in addition to minimizing exposure. Is my ampoule in danger of being ruptured? The amount of Bromine I have in it is probably less
than .1 mL
|
|
|
elementcollector1
International Hazard
Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline
Mood: Molten
|
|
| Quote: Originally posted by BobD1001 | | Now I'm concerned about my small sample of Bromine... It looks to be relatively pure, however I did not dry it as I wanted to minimize the amount I
was working with in addition to minimizing exposure. Is my ampoule in danger of being ruptured? The amount of Bromine I have in it is probably less
than .1 mL |
No, not really. 'Wetting' just means leaving some sort of residue on the surface.
(woelen - accidentally deleted post to edit it)
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
|
|
|
kristofvagyok
National Hazard
Posts: 659
Registered: 6-4-2012
Location: Europe
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by BobD1001 | | I realized the ampoule didn't fully seal, and some bromine vapor was detectable, even got a very small whiff of it! Scary! |
If you are so afraid of this compound, than why do you tickle the dragon's tail?
However it is pretty easy to work with bromine, it's not so dangerous, just do not pour it on yourself. If you do not need to store it for a long
time, than it could be easily placed in a glass with teflon or ground joints:
I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:
"You can’t become a chemist and expect to live forever." |
|
|
Pyro
International Hazard
Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline
Mood: No Mood
|
|
yes that's true. I made ampoules of wet Br2 once and it stuck to the glass. over time the water collected to a tiny drop at the bottom, then it
stopped clinging to the glass. I gave those away and now have almost 0,5l of dry bromine  (used 2kg NaBr)
@Woelen: are those ampules prescored? where did you get them? ebay?
It looks like you twisted the end off to seal it, may I suggest that you heat it and gently pull the end off without twisting, that way the glass
isn't stressed as much
[Edited on 15-9-2013 by Pyro]
[Edited on 15-9-2013 by Pyro]
all above information is intellectual property of Pyro.  |
|
|
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by kristofvagyok | | Quote: Originally posted by BobD1001 | | I realized the ampoule didn't fully seal, and some bromine vapor was detectable, even got a very small whiff of it! Scary! |
If you are so afraid of this compound, than why do you tickle the dragon's tail?
However it is pretty easy to work with bromine, it's not so dangerous, just do not pour it on yourself. If you do not need to store it for a long
time, than it could be easily placed in a glass with teflon or ground joints:
|
I wouldn't consider it a fear so much as a very high level of respect, which I believe we all have towards these types of elements. I was comfortable
tackling the reaction, and did so without issue. Yes I do have such Teflon stoppered and also pfte sealed cap bottles, however this was simply to
display on my element collection as I did not need it for any future reactions. If I need it in the future I will simply isolate more, dry, and store
in such a bottle.
|
|
|
softbeard
Hazard to Self
Posts: 69
Registered: 23-7-2013
Member Is Offline
Mood: moody
|
|
Maybe I'm nuts and had narrowly escaped pulmonary edema, but I've never found bromine vapour that bad. No mask, poor ventilation, just some ammonia
water to snort as an antidote if I got too much of a whiff.
Far, far less irritating than chlorine, at least for me. Of course I don't know what it was really doing to my lungs...
Anyhow, nice pics.
|
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
@pyro: I purchased these ampoules on eBay, quite a few years ago. The seller is "sir_flacon". He still sells these ampoules occasionally, he has 20
ml, 10 ml, 5 ml, 2 ml and 1 ml ampoules and he has them with brown glass and colorless glass. If you order something from him, try tyo combine things,
shipping is EUR 12 for 1 box of ampoules, but also EUR 12 for e.g. 5 boxes of ampoules or whatever you put in the package.
Btw, I am curious about what you intend to do with 500 ml of Br2. That is an awful lot of bromine. Please be careful with that. Imagine what can
happen if that bottle breaks!
When I made that ampoule I had some trouble sealing it, because my torch was not sufficiently hot. I just managed to melt the glass with it. Now I
have a better torch, which easily melts the glass of such ampoules. But the samples held up quite well. I made them yearts ago and they still are
good. No loss of vapors!
|
|
|
MrHomeScientist
International Hazard
Posts: 1806
Registered: 24-10-2010
Location: Flerovium
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by BobD1001 | | Now I'm concerned about my small sample of Bromine... It looks to be relatively pure, however I did not dry it as I wanted to minimize the amount I
was working with in addition to minimizing exposure. Is my ampoule in danger of being ruptured? The amount of Bromine I have in it is probably less
than .1 mL |
There is no risk at all of the vial breaking. Bromine doesn't develop nearly enough vapor pressure. I have two ampoules half full of Br liquid (about
20mL total) and I'm not concerned at all. Ampouling is about the only safe, permanent way to store bromine after all! Elementcollector1's method of
ampouling chlorine is the procedure I was going to try, to ensure there's enough pressure to make the gas easily visible.
How did you prepare yours? Mine was made from electrolysis of sodium bromide spa chemical, procedure courtesy of woelen.
|
|
|
Pyro
International Hazard
Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline
Mood: No Mood
|
|
Woelen: It is more like 450ml, It is stored in a 500ml DURAN bottle with a GL45 cap lined with teflon.
I just like to have it available for when its needed. I also keep about 5 ampules of it for small quantities.
I also like to freak out people who ask about my lab.
my chem teacher asked me:''so what kinds of things do you do in your lab?" "oh, I do many things, I have half a litre of Br2 that I made myself, look
here *shows picture*"
just watch the expression and enjoy
all above information is intellectual property of Pyro. |
|
|
BobD1001
Hazard to Others
Posts: 182
Registered: 29-3-2013
Member Is Offline
Mood: No Mood
|
|
Thank you Element Collector, I was somewhat concerned that the bromine may have been able to attack the glass if residual water was contaminating it.
@ Woelen, I truly appreciate the kind comments regarding the display!
@Pyro, what method did you utilize to make that sort of quantity of Bromine? I'm assuming the distillation method?
|
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
The presence of water in the ampoules is not an issue of safety, but it is an issue of pleasing display. The first ampoule of chlorine I made had some
humidity left. On cooling down below 15 C I saw condensed water inside the ampoule and this ruins the nice display of it. It simply looks ugly.
An ampoule with wet bromine is equally ugly. You get all kinds of smears and little blobs on the glass and the bromine wets the glass. The nice
effect, which is shown in the videos of my website and the nice clean looking surface are not present when even tiny amounts of water are present.
Then you have all kinds of 'dross' floating on the bromine, and that looks ugly.
@Pyro: If you store it in a GL 45 capped bottle with a red teflon lines cap, then it is quite safe. I can imagine that the teacher at school is quite
surprised if you show him your 450 ml of home brew bromine. Others brew beer, you brew bromine
[Edited on 17-9-13 by woelen]
|
|
|
Pyro
International Hazard
Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline
Mood: No Mood
|
|
@Bob:it's almost 1kg. I used an adapted version of UC's. KMnO4, NaBr and H2O in a flask with H2SO4 added through a pressure equalized addition funnel.
My way is to have a 1l flask of KMnO4, NaBr and H2O in an ice bath, on top of that a 500ml pressure equalized addition funnel with H2SO4. Next I add
the H2SO4 to the flask with vigorous stirring so that the temperature didn't rise too much. when all the H2SO4 is added, close the stopcock and add
another 50ml of 98% H2SO4. then I put on a 50cm allihn condenser and heated the water bath. The Br2 boils in the flask, moves up the sidearm of the
addition funnel (this acts as a reflux) and then travels up into the condenser where is condenses and drips down under the H2SO4. The dripping into
H2SO4 dries it, there is almost no heat evolved.
when there is no Br2 left in the flask, stop the reaction and let everything cool down. then remove the condenser and drain the Br2 into a storage
bottle.
@Woelen: It is a Blue GL45 cap to which I added a teflon liner from a different bottle. this is an old pic of it from the good old days when I could
find my camera , the brown residue on the teflon is unknown to me, I tried
H2SO4, various solvents,... but it doesn't do any harm.
wet Br2 in an ampule fixes itself. the water forms a blob at the bottom and the Br2 becomes dry.
[Edited on 17-9-2013 by Pyro]
all above information is intellectual property of Pyro. |
|
|
Metacelsus
International Hazard
Posts: 2539
Registered: 26-12-2012
Location: Boston, MA
Member Is Offline
Mood: Double, double, toil and trouble
|
|
Why use expensive KMnO4 when you can just electrolyze the solution to form NaBrO3 and use that as the oxidizer? This last weekend, I myself made
bromine by this process:
103 g of 99% NaBr (spa pool treatment) and 0.5 g K2CR2O7 were dissolved in distilled water such that the solution volume was 175 mL. Next, the
solution was placed in an electrolytic cell and electrolyzed at 3 A for 10 hours using a MMO anode and titanium cathode. The contents of the cell,
which were now around 125 mL due to loss of water, and cloudy, probably due to precipitated KBrO3, were placed in a 500 mL 24/40 two-necked flask. On
one of the necks was placed a Liebig condenser arm with ice water pumped through it; on the other neck was placed an addition funnel with 30 mL of 96%
H2SO4 (Rooto drain cleaner). The flask was warmed on a water bath to approximately 60 C, at which point the acid was slowly added. Over the next few
minutes, bromine collected in the condenser; I collected the first 25 milliliters of bromine, as that was all my ampule could comfortably hold (I was
expecting lower yields). The bromine was dried with more H2SO4 and sealed in an ampule. Enragingly, as I was sealing it, water vapor produced by the
torch flame condensed on the inside of the ampule, thus making the bromine stick to the sides. (Pictures coming soon.) The rest remained dissolved in
the acid solution, and was neutralized with NaHCO3.
| Quote: | | wet Br2 in an ampule fixes itself. the water forms a blob at the bottom and the Br2 becomes dry. |
This is not the case. Bromine is denser than water; holding my ampule feels like holding a roll of quarters. The dissolved water in bromine causes it
to wet glass, which is a good way to tell if bromine is dry or not.
|
|
|
Pyro
International Hazard
Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline
Mood: No Mood
|
|
trust me cheddite, this is the case. here is a picture that shows that on the bottom
I believe it stays at the bottom because of surface tension, I am aware that Br2 is 3,1X heavier than water. The bromine in this ampule doesn't stick
to the glass. note:see that whiteish line? that's where the level of the Br2 is, it seems to be very slowly eating the glass (it has been there about
8 months)
and KMnO4 costs 30EUR/kg. with a bit under 1kg I made all my bromine. I am too lazy to wait for electrolysis and I HATE it, I HATE it, I HATE it! My
way I can make about 100ml of Br2 in +-2hrs
all above information is intellectual property of Pyro. |
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
I agree with Cheddite Cheese. I like the electrolysis very much and this is also how I made my bromine. As acid I used cheap and easy to obtain NaHSO4
(pH minus for swimming pools). The waiting time for the electrolysis is not an issue to me, just switch it on and let it brew for a day or so.
@Cheddite Cheese: Didn't you have any pitting corrosion of the titanium parts of your anode? I also tried to use my MMO anode for making KBrO3, but
this resulted in formation of flocculent stuff from the uncovered titanium mesh of my MMO anode, so I quit the electrolysis. I did not want to
destroy/erode the anode.
@pyro: The white line inside your ampoule is not from eating of the glass. Bromine does not eat glass, wet bromine also does not eat glass. Most
likely you have some impurity in your bromine, which sticks to the glass. I have an ampoule and it already is many years old and still there is not a
single line of residue sticking to the glass. This ampoule has been lying in the same position for many many months. It is most noticeable that the
line is exactly at the border of the liquid bromine and the vapor and I think that hence the impurity must be floating on the bromine.
I think that for experimental purposes your bromine is perfectly fine, but for an element sample I am very critical (maybe a little bit too critical)
and I put a lot of effort in getting the samples very pure and I do not want to see any crap like dirt, condensed water or solid particles floating on
the bromine.
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
