Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2
Author: Subject: Spin off from Phosgene thread
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 15-10-2015 at 03:49


Ok to set a bench mark. what is the LC of phosgene? Seeing as this started with that chemical. I read somewhere the threshold was 3-4ppm, So lets say we aim for something around 1ppm?

I like the suggestions so far, I tried distilling Nitric acid and had it been a large volume I would have had to get out the room. As it happens it was a tiny amount and I only started with 25ml.

I greased the joints etc so not sure what I didnt get right, I see this as a really good way to sharpen skills. I like the smelly non lethal ideas that have been suggested and will start with those.
I think honing skills like this is useful not only to people who actually want to mess with the dangerous stuff but for those with more limited equipment or who live near people.

So I am adding scrubbers etc to what I do, so in complete theory if I did everything correctly I shouldnt smell anything at all! That wont happen but its what I am aiming for




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
aga
Forum Drunkard
*****




Posts: 7030
Registered: 25-3-2014
Member Is Offline


[*] posted on 15-10-2015 at 04:00


For practice, try gently distilling some ammonia.

If the entire glass rig is gas-tight, you should not smell anything at all.

If it does leak, you'll know and it will not cause much panic.

For seriously dangerous chemicals, i guess the next thing is how to safely clean up the glassware ?




View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 15-10-2015 at 04:18


Quote: Originally posted by aga  
For practice, try gently distilling some ammonia.

If the entire glass rig is gas-tight, you should not smell anything at all.

If it does leak, you'll know and it will not cause much panic.

For seriously dangerous chemicals, i guess the next thing is how to safely clean up the glassware ?


Yep that is the next step up, start with something likely to make you vomit but not ill. Then find ways to clean it without said puking. I thought at first this might be met as a bit of a stupid idea, I am pleased others are interested.




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
woelen
Super Administrator
*********




Posts: 7764
Registered: 20-8-2005
Location: Netherlands
Member Is Offline

Mood: interested

[*] posted on 15-10-2015 at 04:40


A very nice experiment with chlorine, which also yields a useful reagent, which can be used for further experiments, is this.

http://woelen.homescience.net/science/chem/exps/KIO4_synth/i...

Instead of KIO3 you can also use KI, or I2. Just adjust the amount of chlorine, passing through the liquid. For conversion of KI instead of KIO3 you need 4 times as much of chlorine. It works equally well.

This experiment can be used as a test for toxic gas containment. You need one more tube, from the beaker in which KIO4 is formed to a scrubber.

The sodium equivalent is described as well:

http://woelen.homescience.net/science/chem/exps/Na2H3IO6/ind...

I did the experiments without a scrubber. I passed chlorine through the liquid until no more was absorbed and then quickly stopped making Cl2. I certainly did smell chlorine at the end stage of the process, but it never became dangerous or too strong.

[Edited on 15-10-15 by woelen]




The art of wondering makes life worth living...
Want to wonder? Look at https://woelen.homescience.net
View user's profile Visit user's homepage View All Posts By User
careysub
International Hazard
*****




Posts: 1339
Registered: 4-8-2014
Location: Coastal Sage Scrub Biome
Member Is Offline

Mood: Lowest quantum state

[*] posted on 15-10-2015 at 05:45


Quote: Originally posted by Little_Ghost_again  
Quote: Originally posted by aga  
For practice, try gently distilling some ammonia.

If the entire glass rig is gas-tight, you should not smell anything at all.

If it does leak, you'll know and it will not cause much panic.

For seriously dangerous chemicals, i guess the next thing is how to safely clean up the glassware ?


Yep that is the next step up, start with something likely to make you vomit but not ill. Then find ways to clean it without said puking. I thought at first this might be met as a bit of a stupid idea, I am pleased others are interested.


Not stupid at all. This is known as simulant testing, and it is widely used in engineering and manufacturing.

The LC_01s (1% fatality rate) are:
Phosgene (1 min) 384
Phosgene (10 min) 38.4
Phosgene (100 min) 3.84
Phosgene (1000 min) 0.384
Phosgene (5000 min) 0.0768 [This is 80 hours, a double shift week.]

The fact that you can accumulate a lethal dose of phosgene due to very low level concentrations over the course of days is the reason that facility workers where phosgene is handled wear cumulative dose badges.

Before the advent of nerve gas phosgene was the number one lethal chemical weapon. 80% of the men killed by gas in WWI were killed by phosgene and diphosgene.

On the other hand John Davy (brother to Humphry), who discovered and named phosgene, survived the experience.

[Edited on 15-10-2015 by careysub]
View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 15-10-2015 at 16:24


Thanks Woelen I might try that. Ammonia was a fail! I got as far as starting to clean up, its way harder to figure out how to take things apart for cleaning without getting exposure than doing the experiment!

I also found out that petroleum gel is not as good as high vacuum grease at keep seals tight. I also found clamps seemed to make better joints than keck clips?? That seems odd to me I would have thought it the other way around.

I will get a fume hood but this is a kind of technique improver so while using things that are safe(ish) its been really good practice, I also found not using a fume hood made me work slower and more deliberate. I often wondered what would happen if half way through something the power went and hood failed?

This way when I do get a hood then i will still try and stop escapes rather than rely on a fume hood to keep me safe.

On a side note I have a 3 year old 20 ltr container of IPA, I got it for cleaning PCB boards and electronics stuff originally. Its has probably 3-4 ltr left in it, I have used 1 ltr bottles for the last year or so as they are easier to handle.
I wanted some today and didnt have any left in the 1 ltr bottle so decided to try and decant off some from the old stuff.
There are some small almost clear like crystals around the thread to the cap??? I have never smelled IPA leak from the container and they look like very fine sugar (sort of) any idea what they are? I didnt think IPA turned into crystals I just assumed it evaporated away.




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
gdflp
Super Moderator
*******




Posts: 1320
Registered: 14-2-2014
Location: NY, USA
Member Is Offline

Mood: Staring at code

[*] posted on 15-10-2015 at 19:00


Quote: Originally posted by Little_Ghost_again  

On a side note I have a 3 year old 20 ltr container of IPA, I got it for cleaning PCB boards and electronics stuff originally. Its has probably 3-4 ltr left in it, I have used 1 ltr bottles for the last year or so as they are easier to handle.
I wanted some today and didnt have any left in the 1 ltr bottle so decided to try and decant off some from the old stuff.
There are some small almost clear like crystals around the thread to the cap??? I have never smelled IPA leak from the container and they look like very fine sugar (sort of) any idea what they are? I didnt think IPA turned into crystals I just assumed it evaporated away.

Anhydrous isopropyl alcohol forms peroxides on extended storage. Typically, peroxides aren't crystalline, but I would test it anyway seeing as how dangerous they are.

It's also possible that it is an antioxidant added to the alcohol to prevent formation of the peroxides which was left behind when alcohol left on the threads evaporated. I can't think of an easy way to test that at the moment though.




View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 16-10-2015 at 00:34


A long time ago when I got it, it was 99.9% so I assume anhydrous. crystals is slightly wrong but its not like a smooth powder, more like a slight gritty feel hence why I thought crystalline.

How do I test for anything nasty? or could I just wash off the deposit? You have made me slightly nervous now lol. I might stick a hole in the bottom of the container to drain it into another container and get rid of the old container.




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
MeshPL
National Hazard
****




Posts: 329
Registered: 20-4-2015
Location: Universe
Member Is Offline

Mood: No Mood

[*] posted on 17-10-2015 at 03:43


I have a MAD, but probably bad idea how to make phosgene. Since chlorine condenses at -35C and calcium chloride/ice cooling bath may get you down to -40C you may attempt to liquify chlorine in some way. Dry ice could also be used. Than you could bubble CO through liquid chlorine to make phosgene. Would that react and have at least 1% of not killing anybody?
View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 17-10-2015 at 04:00


Quote: Originally posted by MeshPL  
I have a MAD, but probably bad idea how to make phosgene. Since chlorine condenses at -35C and calcium chloride/ice cooling bath may get you down to -40C you may attempt to liquify chlorine in some way. Dry ice could also be used. Than you could bubble CO through liquid chlorine to make phosgene. Would that react and have at least 1% of not killing anybody?


Go back to post 1

I AM NOT, NOR HAVE I EVER WANTED TO MAKE PHOSGENE! IS THIS CLEAR?

The point of this thread was a spin off from someone else wanting to make it, the idea of this thread is too sharpen and hone skills not to make war gas

[Edited on 17-10-2015 by Little_Ghost_again]




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
MeshPL
National Hazard
****




Posts: 329
Registered: 20-4-2015
Location: Universe
Member Is Offline

Mood: No Mood

[*] posted on 17-10-2015 at 07:17


Oh... sorry, wrong thread. :(

My apologies.

But your vague term "war gas" also describes chlorine most amateur chemists eventually make.

[Edited on 17-10-2015 by MeshPL]
View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 17-10-2015 at 07:31


Quote: Originally posted by MeshPL  
Oh... sorry, wrong thread. :(

My apologies.

But your vague term "war gas" also describes chlorine most amateur chemists eventually make.

[Edited on 17-10-2015 by MeshPL]


LOL its ok, its just earlier someone else mentioned it :D. Chlorine is something I am and will be making so I can make stronger hypo for some experiments making chloroform.

But the amounts are small and compared to phosgene the risk is pretty small. A couple of wiffs isnt going to kill me or anyone within a few miles!

The point of the thread is actually to hone skills etc, it would be handy for things like distilling Nitric acid. Somehow even when I had a fume hood I got wiffs of that on cleaning up.




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
gdflp
Super Moderator
*******




Posts: 1320
Registered: 14-2-2014
Location: NY, USA
Member Is Offline

Mood: Staring at code

[*] posted on 17-10-2015 at 07:34


Quote: Originally posted by Little_Ghost_again  
A long time ago when I got it, it was 99.9% so I assume anhydrous. crystals is slightly wrong but its not like a smooth powder, more like a slight gritty feel hence why I thought crystalline.

How do I test for anything nasty? or could I just wash off the deposit? You have made me slightly nervous now lol. I might stick a hole in the bottom of the container to drain it into another container and get rid of the old container.

I doubt it has peroxides in it, but it can't hurt to check. To do so, add 1ml of the alcohol to 1ml of acetic acid, then add several drops of 5%KI. A yellow to brown color indicates the presence of peroxides, and the solution should be shaken with slightly acidified ferrous sulfate solution to remove them.




View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 17-10-2015 at 08:25


Quote: Originally posted by gdflp  
Quote: Originally posted by Little_Ghost_again  
A long time ago when I got it, it was 99.9% so I assume anhydrous. crystals is slightly wrong but its not like a smooth powder, more like a slight gritty feel hence why I thought crystalline.

How do I test for anything nasty? or could I just wash off the deposit? You have made me slightly nervous now lol. I might stick a hole in the bottom of the container to drain it into another container and get rid of the old container.

I doubt it has peroxides in it, but it can't hurt to check. To do so, add 1ml of the alcohol to 1ml of acetic acid, then add several drops of 5%KI. A yellow to brown color indicates the presence of peroxides, and the solution should be shaken with slightly acidified ferrous sulfate solution to remove them.


I have checked and its clear, so no idea what was on the threads! but it now also has some water in it which I would expect after all this time. Its 3 and a bit ltrs so will be used mainly for pcb cleaning etc and maybe chloroform.




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
Agari
Banned





Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline

Mood: Lowest Oxidation State

[*] posted on 18-10-2015 at 20:28


Oh my,look at what I found. I just got on to say that the chlorine test, mentioned in Organics, has yielded no noticeable smell. How does cleaning up the "chlorinated" glassware by having the open end be right up against the bottom of a container filled with 1 Molar sodium Hydroxide solution when opening sound like?
View user's profile View All Posts By User
j_sum1
Administrator
********




Posts: 5775
Registered: 4-10-2014
Location: Unmoved
Member Is Offline

Mood: Possessor of a tidy and organised lab. Now to mess it up again.

[*] posted on 18-10-2015 at 21:30


What chlorine test would you be referring to?

The advantages of Cl2 over other more dangerous chemicals in this context are (1) It is not a cumulative poison. Acute, yes. Chronic, no. (2) Its odour threshold is far lower than the level at which it will cause harm. Therefore, if you smell it, you have a chance to escape.

As for cleaning up glassware, there are numerous possibilities.
Flushing with air and sending it all through a scrubber of sodium hydroxide solution would be my first option. Ideally a multi-stage scrub with indicator in the solutions to monitor progress. It sounds like blowing bubbles.
View user's profile View All Posts By User
woelen
Super Administrator
*********




Posts: 7764
Registered: 20-8-2005
Location: Netherlands
Member Is Offline

Mood: interested

[*] posted on 19-10-2015 at 03:23


My method of getting rid of excess chlorine is to lead the gas away outside, through an open window, which is put ajar. Even if you make a few liters of chlorine over a period of a few tens of minutes, then the gas is diluted so much that it cannot do any harm in the neighbourhood.



The art of wondering makes life worth living...
Want to wonder? Look at https://woelen.homescience.net
View user's profile Visit user's homepage View All Posts By User
Agari
Banned





Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline

Mood: Lowest Oxidation State

[*] posted on 19-10-2015 at 11:37


Quote: Originally posted by j_sum1  
What chlorine test would you be referring to?

The advantages of Cl2 over other more dangerous chemicals in this context are (1) It is not a cumulative poison. Acute, yes. Chronic, no. (2) Its odour threshold is far lower than the level at which it will cause harm. Therefore, if you smell it, you have a chance to escape.

As for cleaning up glassware, there are numerous possibilities.
Flushing with air and sending it all through a scrubber of sodium hydroxide solution would be my first option. Ideally a multi-stage scrub with indicator in the solutions to monitor progress. It sounds like blowing bubbles.

I only have a few minutes before I am going to move out for the phosgene synthesis. The chlorine test I was referring to was to set up a chlorine generator linked to the apparatus for phosgene synthesis to determine whether or not it will leak during the synthesis of the REAL toxic chemicals. If enough leaks to smell it, then that would mean that if phosgene was being produced,it would leak enough for a lethal dose to be inhaled.
I will give a status update if I am alive within 72 hours on the Organics thread.
View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 19-10-2015 at 12:29


My troll detector is pegged.



The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
Pasrules
Hazard to Self
**




Posts: 77
Registered: 4-1-2015
Location: Yellow Cake Deposit
Member Is Offline

Mood: Lacking an S orbital

[*] posted on 19-10-2015 at 14:11


To the phosgene chemists go boil a cabbage down and if you smell it at all forget about nerve agents. There are a lot of more enjoyable things to do "less" risk like seperating HF & Nitric from pickling paste.

Edit: No hate intended to OP, I just think cabbage before chlorine is a good start.

[Edited on 19-10-2015 by Pasrules]




Atropine, Bicarb, Calcium.
View user's profile View All Posts By User
Little_Ghost_again
International Hazard
*****




Posts: 985
Registered: 16-9-2014
Member Is Offline

Mood: Baffled

[*] posted on 19-10-2015 at 14:43


Quote: Originally posted by Pasrules  
To the phosgene chemists go boil a cabbage down and if you smell it at all forget about nerve agents. There are a lot of more enjoyable things to do "less" risk like seperating HF & Nitric from pickling paste.

Edit: No hate intended to OP, I just think cabbage before chlorine is a good start.

[Edited on 19-10-2015 by Pasrules]


Another top tip! that one I will definitely try, really really cheap and I can smell it miles off. Great idea and nice and safe, dont get wrong this may seem total over kill as chlorine is about as far as I would go, but I would like my technique to be good and hopefully professional.

I honestly dont think trying to develop a high level of skill is a waste of time even if your not making something nasty.
For example I am lucky and no one near by to annoy with smells, but some people want to make things not particularly harmful but may be a PITA smell wise to others, so developing good technique also stops the neighbors having a problem with your hobby.

As to you know who... Look go do what you want but do it out the way from others, go be kewl and happy, dont put others at risk but do what you want with your own health.




Dont ask me, I only know enough to be dangerous
View user's profile View All Posts By User
 Pages:  1  2

  Go To Top