Sciencemadness Discussion Board

Spin off from Phosgene thread

Little_Ghost_again - 14-10-2015 at 11:00

Hi,
I am sure most are aware of the phosgene thread currently in Organics.

It did however give me an idea, in the thread someone mentioned (sorry I forget now who it was) That first the person should try and make say Chlorine and do a clean up without getting a single wiff of it.

I think this could actually be really useful for noobs like me to try!
Although I am making a Chlorine generator for bleach lets put that aside for a minuet.

What I was thinking was collecting some ideas of synths that all produce a stench or some kind of nasty but non lethal effect if they are smelt.

Now I dont have a clue which would qualify for this but how about starting with some that are pretty harmless but the idea is you try and do it with ANY exposure, those with the knowledge can explain how best to do the clear up etc.
These could then progress upto say Chlorine, that way some of us would get a really good practice at techniques and there would be a thread for those with over ambitious ideas to start lower and work up without much risk.

Does any of that makes sense?

aga - 14-10-2015 at 11:15

Sounds very sensible indeed.

Chlorine would be OK so long as the calculated volume were very low.

You;d be able to smell it, and (if the calculation is correct) there would never be enough to kill you.

Edit:

Having one tiny whiff of it is a Good idea - you know what it smells like after that.

[Edited on 14-10-2015 by aga]

OneEyedPyro - 14-10-2015 at 11:20

A little whiff of chlorine isn't going to kill you and it can be smelled at very low concentrations, just the fact that you considered making phosgene but are having second thoughts about making Cl is kind of ridiculous sounding :D

Realistically making Cl is not that dangerous generally speaking, now if you can synthesize chloroacetone and cleanup without smelling Cl or feeling the effects of the chloroacetone you're doing pretty well.

Little_Ghost_again - 14-10-2015 at 11:29

Quote: Originally posted by aga  
Sounds very sensible indeed.

Chlorine would be OK so long as the calculated volume were very low.

You;d be able to smell it, and (if the calculation is correct) there would never be enough to kill you.

Edit:

Having one tiny whiff of it is a Good idea - you know what it smells like after that.

[Edited on 14-10-2015 by aga]


My reasoning for starting with something other than Chlorine is this.
If a real noob like me gets it wrong in a bad way I will get more than a wiff, that is apparently not good.

So I thought there must be other chemicals that humans can detect in tiny amounts by the nose that are fairly harmless if the very worse happens.
I am thinking maybe putricine?? I dont actually know which one to start at hence the thread, but getting a list of procedures together that got up in risk might be good training.

I know some do little more than stream the eyes and hurt like hell, but that is a good way to learn, I think it might sharpen us noobs up. Slowly increasing the risk also means you take it seriously (or should), look at the phosgene thread!! No matter what gets said nothing is going to convince the guy a single wiff is bye bye, but if people start at something harmless but hurts alot, and know each synth increases in risk then hopefully skills will be truly honed.

I am especially keen to learn how the hell you clean some of this equipment up afterwards! I distilled Nitric acid and cleaning the condenser etc was a real mare, I am sure people here who have had training and proper education know a few tricks on how to do this in a safe way.

I wouldnt suggest starting at chlorine as getting it badly wrong isnt going to end well. Think of it as a complete beginners guide to handling synths with risk

aga - 14-10-2015 at 11:30

What does Cl smell like ?

I've only ever smelt Cl2.

LG2.397 was not the one trying to make phosgene.

OneEyedPyro - 14-10-2015 at 11:37

I believe Cl is immediately oxidized to ClO₂ upon but that's a good question, what does Cl smell like? I know Br smells very similar to ClO₂ so I'd guess the same goes for Cl.

[Edited on 14-10-2015 by OneEyedPyro]

aga - 14-10-2015 at 11:45

Cl immediately forms Cl2 on hitting Cl.

Cl is never seen, ever.

Closest is Cl<sup>-</sup> as the ion.

Cl2 experiment :-

Test tube with a few grains of TCCA (trichlorocyanuric acid) Pool Shock stuff.

1 drop of HCl.

At 20% HCl concentration that should eventually release a total of 0.004114 mol of Cl2 which equates to around 100ml of the gas.

Edit:

Enough to Whiff, not enough to Stiff.

[Edited on 14-10-2015 by aga]

Detonationology - 14-10-2015 at 11:50

Chlorine gas is said to have slight smell of almonds. My chlorates always always have a nutty smell.

OneEyedPyro - 14-10-2015 at 11:58

Well, yes of course. Just like oxygen, nitrogen, hydrogen etc they exist diatomically.
When I saw Cl I automatically thought of Cl₂ and failed to make the distinction.

softbeard - 14-10-2015 at 12:24

Quote: Originally posted by Little_Ghost_again  


What I was thinking was collecting some ideas of synths that all produce a stench or some kind of nasty but non lethal effect if they are smelt.


Why don't you try to synthesize concentrated ammonia water "ammonium hydroxide" with an ammonia gas generator and water.

Don't forget, it is possible to induce pulmonary edema with NH3 but the NH3 concentration necessary is intolerable.
Ammonia gas is usually considered safe enough vs. lethal poisoning so long as a person isn't forced to breath it by circumstances.

See if your containment system allows you to do the preparation without smelling ammonia.

Magpie - 14-10-2015 at 12:28

I have made Cl2 many times. Never without smelling it. My powerful fume hood allows me to have small mishaps without consequence. After much practice I now have an equipment train for creating dry chlorine without equipment failure.

There is an experiment in Brewster for making malachite dye. The author says that if you can make this dye without getting green all over your person and clothes you are a good chemist. :D I was doing fine until I did one manipulation poorly. I ended up with green all over the place!

Why does this test chemical have to be dangerous or toxic. Why not try making benzaldehyde or amyl acetate without smelling them?

edit: tip for LGA and others wanting to rid their vessels of poisonous gases at the end of a synthesis: top those vessels off with water before removing them from the hood.

[Edited on 14-10-2015 by Magpie]

battoussai114 - 14-10-2015 at 12:35

Ammonia, Thioacetone or Thiols in general are what I can think of...

[Edited on 14-10-2015 by battoussai114]

j_sum1 - 14-10-2015 at 12:46

Quote: Originally posted by Magpie  
edit: tip for LGA and others wanting to rid their vessels of poisonous gases at the end of a synthesis: top those vessels off with water before removing them from the hood.

First get a hood!


Actually I really like this as a challenge. Make something smelly without smelling it. What excellent practice and opportunity to develop skills and test equipment and technique.
I am pretty sure I could do ammonia even without a fume hood. But I'd be relying on the fact that it is absorbed by water so well. Chlorine? Not so much. But it doesn't scare me like it used to. I am not sure if that is a good thing or not.

Little_Ghost_again - 14-10-2015 at 13:27

I had a fume hood, I will get another at some point. And just for the record NO it wasnt me trying to make phosgene!!

Malachite green I like the sound of, and the water tip is noted.

They dont have to be dangerous, especially at the start. But once you kind of master the less toxic stuff it would be good to add a little fear and see if you can still perform. I am just thinking that mentally there might be a difference to how you approach something you know wont hurt and something you know would hurt.

The smells one is great! So what smells at very very low concentrations and isnt toxic? This would make a great aga challenge if we had a scratch and sniff forum!

deltaH - 14-10-2015 at 13:42

Organic isocyanides (from wiki):

Quote:

Their disagreeable odour is legendary. To quote from Lieke, "Es besitzt einen penetranten, höchst unangenehmen Geruch; das Oeffnen eines Gefässes mit Cyanallyl reicht hin, die Luft eines Zimmers mehrere Tage lang zu verpesten, ..." (It has a penetrating, extremely unpleasant odour; the opening of a flask of allyl [iso]cyanide is enough to foul up the air in a room for several days). Note that in Lieke's day, the difference between isocyanide and nitrile was not fully appreciated.
Ivar Karl Ugi states that "The development of the chemistry of isocyanides has probably suffered ... through the characteristic odor of volatile isonitriles, which has been described by Hofmann and Gautier as 'highly specific, almost overpowering', 'horrible', and 'extremely distressing'. It is true that many potential workers in this field have been turned away by the odour."[5] Isocyanides have been investigated as potential non-lethal weapons.[6]
Some isocyanides convey less offensive odours such as malt, natural rubber, creosote, mild cherry or old wood.[7] Non-volatile derivatives such as tosylmethyl isocyanide do not have objectionable odors.[8]


They can be prepared from primary amines easily with reagents you have:

Quote:
In the carbylamine reaction (also known as the Hofmann isocyanide synthesis) potassium hydroxide reacts with chloroform to produce dichlorocarbene. This then converts primary amines to isocyanides. As it is only effective for primary amines it is used as a chemical test for their presence.

aga - 14-10-2015 at 13:57

Quote: Originally posted by OneEyedPyro  
When I saw Cl I automatically thought of Cl₂ and failed to make the distinction.

First place Cl was mentioned was in your own post.

[Edited on 14-10-2015 by aga]

gdflp - 14-10-2015 at 14:07

Quote: Originally posted by aga  
Cl immediately forms Cl2 on hitting Cl.

Cl is never seen, ever.

Closest is Cl<sup>-</sup> as the ion.

Not true. Look up chlorine radicals, they're important intermediates in many organic reactions, and they do exist. Has blogfast not covered that yet in your class?;)

phlogiston - 14-10-2015 at 14:31

Nice idea. Two candidates:

<b>Tetrahydrothiophene</b> has an odour threshold of just 1 ppb. In many countries, this compound is added to natural gas to allow a leak to be detected by smell. If you fuck up with this compound, expect a massive response from whoever is responsible for handling a gas leak.

The odour threshold of <b>trimethylamine</b> is about 0.21 ppb. Its smell resembles spoiled fish. However, about 7% of people are anosmic to its odour.

aga - 14-10-2015 at 15:02

Quote: Originally posted by gdflp  
Look up chlorine radicals, they're important intermediates in many organic reactions, and they do exist. Has blogfast not covered that yet in your class?;)

I wish at this this point to Thank Everyone in this forum from whom i have managed to gain the small amount of knowledge of Chemistry that i currently possess.

The New (to me) knowledge that has been freely given is very much appreciated, so a huge THANK YOU to all contributors.

blogfast25 stands out (for me) as an excellent educator.

You have tought me as well gdflp, like it or not.

careysub - 14-10-2015 at 15:45

The standard of not having *any* exposure is impossible to reach without (or maybe even with) a completely sealed perfectly engineered system.

It is standard procedure for example for spies looking for uranium enrichment or chemical weapon production sites to detect them by environmental sampling outside the plant. No plant is so good that traces are not detectable.

You need to discuss what levels are acceptable/unacceptable.

Chlorine is detectable at 0.5 ppm, can cause slight temporary respiratory impairment at 1 ppm if inhaled for a few hours, is intolerably irritating at 10 ppm, but at that level is not a lethal hazard even after hours of exposure. Immediately hazardous concentrations are in the hundreds of ppm.

Thus this is a reasonable experiment to test how good you are at keeping the gas contained at the 1 ppm level. If you exceed this by much you will know it right away, and be motivated to clear the area immediately.

Really potent odiferous compounds (ethanethiol and other thiols) can be detected at 0.0002 ppm. With these compounds making them in any but micro quantities becomes a problem not because they are dangerous, but because of the nuisance odor problem.

j_sum1 - 14-10-2015 at 16:32

Interesting careysub.

My problem with these kinds of descriptions is having some sort of reasonable guestimate as to how potent the thing is that I am smelling. I find that I need some kind of frame of reference. A couple of examples:

I open the door to the shed containing the pool filter and also where the pool chemicals are stored. There is an obvious smell of chlorine in the air. Not exactly unpleasant, but not somewhere i want to sit down and have a picnic. On the scale above, what kinds of concentrations am I experiencing here.

I lived in an area with quite a bit of geothermal activity. H2S would literally come out of the ground. Mostly it would disperse in the wind but there were still days with low lying cloud where the smell would be a lot more noticeable. To the point that you could fart and no one would notice.
I regularly read here how toxic H2S is, how vile it smells and what ought to be done to avoid exposure. Low levels don't bother me a bit and I associate the smell with hot mineral springs -- quite pleasant memories. My question: what level of H2S exposure am I likely to have been experiencing and how does this compare with levels at which one should take precautions?

gdflp - 14-10-2015 at 16:44

Quote: Originally posted by aga  
Quote: Originally posted by gdflp  
Look up chlorine radicals, they're important intermediates in many organic reactions, and they do exist. Has blogfast not covered that yet in your class?;)

I wish at this this point to Thank Everyone in this forum from whom i have managed to gain the small amount of knowledge of Chemistry that i currently possess.

The New (to me) knowledge that has been freely given is very much appreciated, so a huge THANK YOU to all contributors.

blogfast25 stands out (for me) as an excellent educator.

You have tought me as well gdflp, like it or not.

Indeed, that is the reason all of us are here, both to learn new information and teach others what we know. That's why this forum is so successful, because the members are willing to share their knowledge with others, while still keeping open ears and recognizing that some have more knowledge and experience in different areas, be they chemistry, physics, or any other topic.

careysub - 14-10-2015 at 16:52

Quote: Originally posted by j_sum1  
Interesting careysub.

My problem with these kinds of descriptions is having some sort of reasonable guestimate as to how potent the thing is that I am smelling. I find that I need some kind of frame of reference. A couple of examples:

I open the door to the shed containing the pool filter and also where the pool chemicals are stored. There is an obvious smell of chlorine in the air. Not exactly unpleasant, but not somewhere i want to sit down and have a picnic. On the scale above, what kinds of concentrations am I experiencing here.


A few ppm.


Quote:
I lived in an area with quite a bit of geothermal activity. H2S would literally come out of the ground. Mostly it would disperse in the wind but there were still days with low lying cloud where the smell would be a lot more noticeable. To the point that you could fart and no one would notice.
I regularly read here how toxic H2S is, how vile it smells and what ought to be done to avoid exposure. Low levels don't bother me a bit and I associate the smell with hot mineral springs -- quite pleasant memories. My question: what level of H2S exposure am I likely to have been experiencing and how does this compare with levels at which one should take precautions?


H2S is faintly detectable at 1 ppm, easily detectable at 5 ppm, strongly unpleasant at 25 ppm, causes eye irritation and coughing from 50-100 ppm, the LC01 concentration for 30 minute exposure is 200 ppm.

A special problem with H2S is that 10 minute exposure at 50-100 ppm destroys the sense of smell and thus results in the loss of ability to sense its presence through smell.

j_sum1 - 14-10-2015 at 21:07

Ok. By that reckoning, the day I caught a strong whiff of Cl2, held my breath and evacuated the shed, it was probably tens of ppm and climbing. Strongly irritating was the word I would use, but I also knew the concentration was climbing and it wasn't going to get any better in the short term.


I am aware of that particular issue with H2S. I guess the rule of thumb is that if you smell it, it is not going to necessarily cause harm. If it smells really unpleasant, you should be out of the situation and breathing some fresh air. And if you know it is around but can't smell anything, then you are in deep serious yoghurt.

I understand that the same olfactory numbing occurs with thioacetone. Is this a general thing with sulfur compounds?

edit: spelling

[Edited on 15-10-2015 by j_sum1]

careysub - 14-10-2015 at 21:36

Right.

If you ever encounter a strongly unpleasant smell of hydrogen sulfide, your nose is telling you to get the *bleep* out of there!

Little_Ghost_again - 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

aga - 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 ?

Little_Ghost_again - 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.

woelen - 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]

careysub - 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]

Little_Ghost_again - 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.

gdflp - 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.

Little_Ghost_again - 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.

MeshPL - 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?

Little_Ghost_again - 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]

MeshPL - 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]

Little_Ghost_again - 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.

gdflp - 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.

Little_Ghost_again - 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.

Agari - 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?

j_sum1 - 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.

woelen - 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.

Agari - 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.

Magpie - 19-10-2015 at 12:29

My troll detector is pegged.

Pasrules - 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]

Little_Ghost_again - 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.