Sciencemadness Discussion Board

Keeping things safe while learning, but still being exciting

binbin - 3-6-2015 at 04:35

I study organic chemistry at home as a hobby. It's been an on-again, off-again thing for me. I have all the basic stuff, beakers, flasks, acids, bases, advanced laboy distillery kit. I have created KCl03 by electrolysis (I have Ti and MMO eletrodes) and will be trying to make KCl04 soon, lots of cool things by nurdrage, and lately, created Nitric Acid because I can't buy the friggin stuff and it is used in so many other cool experiments. My first batch of nitric I used to create some copper nitrate which is drying now. My second batch yielded about 50ml which I keep in a glass RBF with a glass stopper. Can someone recommend a reagent bottle that I can buy to keep this stuff? It's red fuming nitric acid and will set a nitrile glove on fire with 1ml, so rubber is out.

I use a lab coat, full face shield, 3M 6006 respirator, and gloves when the chemicals aren't trying to set them on fire (nitric acid vs nitrile.)

Nitric Acid isn't the nicest stuff. However I want to keep experimenting and learning but I want to keep it safe until I gain more and more experience with reactions and methods.

Anyone have any good and more safe ideas of reactions/experiments I can do that will compliment at home studies? I am currently reading through "Organic Chemistry" by T. W. Graham Solomons. I now have 50ml of nitric acid, but would rather not have to distil any more any time soon!

Thanks!


[Edited on 3-6-2015 by binbin]

Loptr - 3-6-2015 at 04:46

I don't have any, so I can't recommend, but you need an amber glass jar with a ground glass stopper. This ground glass stopper can be greased on the top to help keep it from escaping, and the amber will keep the decomposition down.

There is a picture of one around here in a post by Magpie when he distilled azeotropic nitric acid, among others.

byko3y - 3-6-2015 at 04:50

In fact, I'm ranting a lot about the fact that safe and suitable for home experiments are little known, while you are often told about use of ethylene, ethylene oxide, phosgen, cyanides, LAH and NaH, chlorine, palladium (I want to emphasize this one, it's not easy to work with because of catalyst poisoning).
There's really a lot of things you can do with much risk for your life, including organic nitriles and bromine.

greenlight - 3-6-2015 at 06:14

These Schott Duran storage bottles are great for storing Nitric acid. I used to use glass slip in stopper bottles with PTFE tape around the stopper for Nitric and Sulphuric but have since changed to these. They are great and pour really well if you don't mind spending the money.
I also have a 100ml one for 99% Nitric acid.
Yous should have no problems storing red fuming Nitric acid in them.

http://www.ebay.com/itm/Schott-Duran-21801365-250mL-Laborato...




[Edited on 3-6-2015 by greenlight]

Loptr - 3-6-2015 at 08:28

Quote: Originally posted by greenlight  
These Schott Duran storage bottles are great for storing Nitric acid. I used to use glass slip in stopper bottles with PTFE tape around the stopper for Nitric and Sulphuric but have since changed to these. They are great and pour really well if you don't mind spending the money.
I also have a 100ml one for 99% Nitric acid.
Yous should have no problems storing red fuming Nitric acid in them.

http://www.ebay.com/itm/Schott-Duran-21801365-250mL-Laborato...
[Edited on 3-6-2015 by greenlight]


I have several of these from Dr.Bob. They are very nice reagent bottles. I hadn't thought about storing fuming nitric acid in them, though. I had a PTFE thermoset cap that was pretty mangled up on the inside and threads by anhydrous nitric acid, which has me thinking twice before attempting to store the stuff. I diluted it down to a 70% solution, which is much more manageable.

greenlight - 3-6-2015 at 08:45

I have 70% Nitric acid stored in mine all the time in a fridge and the acid does not attack the plastic cap or pouring ring at all.
I have the 100ml one for anhydrous acid but only distill it and store it at this concentration for about a week or two max as I distill it when I am going to need it. My 100ml reagent bottle has no damage to the cap or ring either.

Schott Duran states that they have high chemical resistance which seems to be true because these bottles seem to hold up extremely well to concentrated acids.

binbin - 3-6-2015 at 08:59

Where can I find these bottle in Canada? Any ideas? The ebay listing wants $26 to ship to Ontario, Canada.

Thanks!

greenlight - 3-6-2015 at 09:21

Keep trying ebay, one may come up in your country.. The shipping for mine on ebay was about the same.
Either that or you could try a scientific supply store if you have one around your area. I don't think there would be any laws about buying reagent bottles.

Sulaiman - 3-6-2015 at 10:22

binbin, you may have been operating with a false sense of safety from HNO3, NO2, NO etc.
the 3M 6006 is approved for
Ammonia‎ , Chlorine‎ , Chlorine dioxide‎ , Formaldehyde‎ , Hydrogen chloride‎ , Hydrogen Fluoride‎ , Hydrogen sulfide‎ , Methylamine‎ , Organic Vapors‎ , Sulfur dioxide‎
http://solutions.3m.com/wps/portal/3M/en_US/GovernmentSoluti...

trapping / filtering NOx is not easy, as many threads here have shown.

'safety' I have found to be a very relative thing,
it takes a surprisingly small quantity of some substances to cause a significant safety risk.
If you follow well tried and prescribed experiments the risks will already have been mitigated.
If, like me, you only have a very superficial knowledge of chemistry,
but like experimenting, then the risks may be significant.
e.g. I have this last year started chemistry
(I'm 60+ so I know that I shall not have time to 'master' chemistry, just to learn and 'play')
and I unknowingly made Mn2O7, a green oily liquid, which I later found out is somewhat unstable!
I was blindly following a YouTube video 'lightning in a bottle' or something similar.
the given chemical formula was KMnO4 + H2SO4 = K2SO4 + MnSO4 +H2O+[O] or similar.
No mention of Mn2O7.
Even so I have demonstrated this experiment a few times to friends and family as it is fun and (I'm told) not too dangerous in SMALL amounts.
and
just yesterday I was separating Iodine and Bromine from their salts,
somewhere from the mists of my memory ... iodine forms a complex with ammonia solution.....
just after mixing I remembered what the complex is ... I detonated it today !
(I could have just neutralised it, but where's the fun in that ? ;)

I have been reading Vogel (free from the SM 'library'), 90% of it I can't retain, but there is so much interesting stuff between syntheses,
some of the intermediate or side products have toxic or explosive properties,
so to mitigate future accidents due to unexpected production of explosive chemicals
I have decided to synthesise and evaluate the danger of as many 'side reactions' as I have time for :)


[Edited on 3-6-2015 by Sulaiman]

[Edited on 3-6-2015 by Sulaiman]

[Edited on 3-6-2015 by Sulaiman]

binbin - 3-6-2015 at 12:09

Quote: Originally posted by Sulaiman  
binbin, you may have been operating with a false sense of safety from HNO3, NO2, NO etc.
the 3M 6006 is approved for
Ammonia‎ , Chlorine‎ , Chlorine dioxide‎ , Formaldehyde‎ , Hydrogen chloride‎ , Hydrogen Fluoride‎ , Hydrogen sulfide‎ , Methylamine‎ , Organic Vapors‎ , Sulfur dioxide‎
http://solutions.3m.com/wps/portal/3M/en_US/GovernmentSoluti...

trapping / filtering NOx is not easy, as many threads here have shown.


Thanks! I found out pretty quickly that acid fumes could be sensed through the filter. I went to a local safety store up here and the gentlemen provided a booklet listing all organic materials and what 3M recommends for each. Both for nitric acid fumes and nitrogen dioxide, they recommend forced air units only. Therefore I still use a fan and stay far away when I know acid fumes are going to be present and when nitrogen dioxide begins to be generated. Once in a while I get a wiff of each, but since I'm outside and I take a small sniff first, it's never been much of an issue other than the smell. If I smell something I immediately exit the area until I'm sure it's died down or the wind changes and/or get behind my fan.

Ohh here's my setup: http://imgur.com/a/7U9Iy

Since my distillery kit is a complete closed system (besides the vacuum port which is left open for pressure purposes,) I don't really have much problem with fumes. It's only when I'm adding new chemicals to the reaction RBF, tearing down the kit, or the very first instance of the reaction when generous amounts of NOx are generated. I am aware of these times so I either get far back and behind the fan, or just exit the area.

How else do you deal with acid/nitrogen dioxide safely? Just a fume hood? What is the home chemist to do besides what I'm doing? Is there such things as teflon coated gloves? :P



[Edited on 3-6-2015 by binbin]

Sulaiman - 3-6-2015 at 13:29

like many others here, I perform such experiments outdoors, subject to weather conditions.
Some members have a fume hood/cabinet,
some just vent fumes out of the lab from the receiver adapter etc.
presently I can do neither as I have nowhere safe to vent to.
If you have a sink or toilet you can push a plastic vent pipe past the u-bend,
just be sure your pump is on 'blow', not 'suck' :P

A workmate of mine (not yet a member here) does NOx type experiments in his bath and vents down the waste pipe.


[Edited on 3-6-2015 by Sulaiman]

[Edited on 3-6-2015 by Sulaiman]