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woelen
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[*] posted on 31-7-2007 at 06:09
Home experimenting or using a lab?


If I read the posts of several members, then I see a great variation in what kind of reagents people work with. Most people seem to use inorganics (albeit sometimes quite toxic) materials, some do things with energetic stuff or pyrotechnics, and others do things with electrolysis, etc. This all is stuff, which to quite some extent can be done well at home, certainly if experiments are done on a microscale. I do the latter myself, and then I can handle even quite nasty stuff without unacceptable risks.

But for some people (e.g. Sauron, garage chemist, nicodem)I see that they are doing fantastic things with all kinds of organics, using or making chemicals, which I can only dream of (just to mention a few: PCl5, SOCl2, organic ...yl chlorides (e.g. oxalyl chloride, benzoyl chloride), CCl3COOH, SO3) and using solvents as if they are using distilled water :o. I really wonder, are these experiments at home, or in a true lab (possibly in spare time)?

I myself experiment at home, but for that reason I have to seriously limit what I can do. No organic syntheses, no use of chems like PCl5, HSO3Cl, only limited extractions and isolations of chemicals. I think this is sad, but I simply can't do much more at home. Even if I could get stuff like PCl5 or SOCl2, I doubt if I can ever safely store and handle such materials with the limited equipment I have at home. I have some NbCl5 and that already is a real pain on storage and handling (container with pressurized HCl-gas, deterioriation of material, due to reaction with air, corrosion of nearby metal objects).

I just am curious about other members, who are actively experimenting, and if they do really advanced things at home, how they manage to do so (safely).




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not_important
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[*] posted on 31-7-2007 at 06:54


I've been at both places, changing as I moved. Having an outbuilding makes it practical to build a lab, work with larger amounts of materials and have more complex apparatus because you have the room. The problem of leakage of reagents is less, as they're not in the next room from the kitchen or bedroom. People who work with wood, metal, or clay often have separate work buildings for the same reason; sawdust, metals fumes, and clay dust are poor condiments.

Right now I have an outbuilding that would make a decent lab, if work was put into constructing it. Could have a fume cupboard, water still, recirculating aspirators and mechanical pump, as I own that hardware. But financial constraints prevent that, meaning experimentation is closer to what you do than some of the others here. Much of my equipment is packed away, from lack of space to assemble it in, and no desire to do those experiments in the dwelling.
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garage chemist
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[*] posted on 31-7-2007 at 07:29


I do my experiments and syntheses at home in a garage well away from the house. I have a simple selfbuilt fumehood there and a water pump for washing and aspirator, also an old baking oven for drying substances and glassware with heat.

The organic -yl chlorides you mention can indeed only be handled under the fume hood, and some of them I cannot buy, like oxalyl chloride and PCl5 because those are considered toxic.
My PCl5 is selfmade, from red P and chlorine gas in dried and purified (alcohol-free) chloroform as solvent and diluting agent (the synthesis is documented at versuchschemie.de). Oxalyl chloride I do not have, but could make from PCl5 and oxalic acid. This would only be practical for small amounts since the synthesis uses a huge amount of PCl5 to get a small amount of (COCl)2.
SOCl2 I can buy and I use it to activate various organic acids by forming the acyl chlorides.

Such experiments , and most of the organic syntheses can not be carried out in test-tubes because often distillation, sometimes in vacuum or with a column is necessary to isolate the products. If you want to start doing organic chemistry, get round-bottom flasks and a distillation setup, also a separating funnel and a Dimroth condenser. Oh, and a sintered glass filter for suction filtration is very useful both in inorganic and organic chemistry for rapid filtering and washing without having to use filter paper. I use it all the time!

And solvents can often not be used straight out of the bottle: they may need to be dried or freed from stabilizers. Dry solvents do not stay dry on storage because they are hygroscopic, and unstabilized ones may decompose or form peroxides etc...

Organic chemistry is indeed often less straightforward than inorganic, and often it is much more work to actually isolate a product than to only carry out the reaction.
But I still think that synthetic organic chemistry is the most interesting part of home chemistry due to the nearly endless possibilities.

You could start with e.g. the newest Gattermann (in the SM library), it gives a good introduction to organic chemistry. The experiments are however not all suited to the home experimenter, and some of the reagents may need to be made beforehand due to them being impossible to get, like benzene.

[Edited on 31-7-2007 by garage chemist]




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vulture
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[*] posted on 31-7-2007 at 07:33


Don't get all worked up over "real labs". I've seen stuff happen in pro labs that I would deem unacceptable in my home lab.

The greatest hazard when doing organic synthesis is fire. So four concrete walls and nothing flammable is all you want. It's pretty easy to contain possible fires by creating fire lanes, for example clearing a space or hallway near your lab where there's nothing a possible fire could use to jump to another room.




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[*] posted on 31-7-2007 at 10:59


I`m the same as Woelen, although my Lab is somewhat more of an Annex to the house rather than In it.

micro scale things here also, and mostly always inorganic.




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[*] posted on 31-7-2007 at 13:18


I do a bit of both, some macro and some microscale. Mostly my organic chemistry involves explosives and purification is only recrystallization, if even. I think it would be interesting to load up crude nitrated product onto a chromotography column and see what comes out, but I don't have $600 for a barrel of sand. I do microscale stuff in test tubes (a la woelen) and most of my macro stuff in a detached garage workspace. All of the microscale expirementation is generally inorganic.

This summer I did have the pleasure of working in a university organic chemistry lab for 6 weeks. My desk was seperated from the lab by a line of tape, 4 feet away from me was lithium powder under argon, couple kilos of sodium metal, 5 pound jar of iodine, et cetera. That was some of the most fun I have ever had. I learned that, yes, product purification IS the hardest/longest part (all of my reactions required column chromotography to seperate products). We had a nice stereo system to keep us awake. I started with 60g of starting material and over the course of 8 synthetic steps ended up with 4 grams of an impure, novel compound that was worth several times more than its weight in gold (judging by the time and regent expenses). Quite an experience, especially for someone my age (16).

Never did have time to do any side-reactions, but that was the type of lab group who would not have minded, they encouraged me to act freely. It was fun to actually be able to use what I have learned over 3 years of reading and expirementing. Also, it was nice to see that while I could fit in and work there, there was so much that I did not know and learned.

[Edited on 31-7-2007 by Swany]
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[*] posted on 31-7-2007 at 18:10


I try to only do the inorganic stuff these days, but something interesting always draws me back to try an organic experiment. But I now limit myself to organic reactions which are done in aqueous or acid based medium, as I hate solvent smells.

And yes "organic ...yl chlorides" are not for an only decently ventilated lab without a hood. (mildly amusing story here...)

I used to do things when younger that now I would not do, looking back a couple seem ultra stupid, which I will pay for at some point in my later years...But thats how one learns, and why I am very safe now.

I also do my own thing in the lab I work at, not stuff for my current research, but stuff I find interesting. I did a ponzio reaction, because the chemistry there I thought was really cool, and will soon be making some organic carbonates(actually in a bizare twist became part of my research project)...and we all know that that means....phosgene:D

[Edited on 31-7-2007 by The_Davster]




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[*] posted on 8-6-2008 at 16:14


I recall reading some time ago regarding leakage incidents of reagents from plastic bottles. I could not find the thread so am posting here.

Yesterday, upon arrival at our studio, I noticed liquid on the concrete floor near an exterior wall - and around the bottoms of several gallon cans of solvents (acetone, EtOH, mineral spirits). I at first thought that rain water had somehow leaked in as it had been raining very hard the night before. Upon further inspection (and to my dismay) it became apparent that the liquid was from a now-very-empty gallon jug of 35% H2O2. The puddle had spread over (and under) approx. 12 sq. ft. wetting a stack of exotic woods and a vacuum pump. It had also spread to the inside wooden wall brace.

Thoughts of the material becoming concentrated on/in the wood and resulting in a fire led me to mix up some KMnO4 and sprayed (hand spay bottle) down the area. Interesting how much foaming/bubbling occurred. I sprayed until the purple color just started to persist.

Next, my un-gloved hands (I know, I know...) managed to become stained brown and "burned" white during the fun process of trying to extricate the lumber.

Just wanted to "share" my fun experience with all here in hope that others won't have the same pleasure. The plastic container was the translucent type of HDPE commonly used and was the original. Several hairline cracks were visible in the bottom of the jug. Jug was probably ten years old and not mistreated - but anybody's guess how it was bounced around before. Oxidation and stress probably, and it was hot weather, so pressure build-up also. I will put an outer plastic "boot" around my remaining jug.

I am about to go down again now and inspect the lumber. Should be an interesting combination of bleaching and Mn staining.

Cheers
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[*] posted on 8-6-2008 at 17:57


I'm actually having some problems in placing myself into a category (micro, macro- scale etc.).

Maybe someone of you who have watched my videos may be of help.

I usually refer to myself as an inorganic chemist. My lab is actually a kitchen in my basement, which I find OK because I don't have any chemicals that is in need of special consideration when it comes to storage. Of course, all necessary safety precautions have been taken in the event of an unwanted happening. For instance: I have two smoke detectors, three fire extinguishers and a fire blanket.

argyrium, interesting experience. The handling of the "plastic container" would need to be handled extremely rough for something like that to happen after only 10 years (ca).
Also, how very strange that you managed to get burnt without using gloves...:P




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[*] posted on 8-6-2008 at 21:19


I can say, from first hand experience, that 35% H2O2 burns are horrible. They bleach your skin white and it causes this slow very painful stinging sensation that just persists. It will not go away. It's very unpleasant. Then, the skin just rots away leaving a hole.

It's one of the worst burns I've ever had.

I do all of my experiments at home, by the way.




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[*] posted on 8-6-2008 at 22:34


Quote:
Originally posted by MagicJigPipe
I can say, from first hand experience, that 35% H2O2 burns are horrible. They bleach your skin white and it causes this slow very painful stinging sensation that just persists. It will not go away. It's very unpleasant.
________________________________________

MagicJigPipe, your dwell time must have been much longer than mine. Sounds nasty.

My exposure was very short and had water on-hand to dilute the deposits on my skin. Unless one has experienced it, it is difficult to describe. Rather an electric bite feeling then the skin bleaches; but in my experience (short contact times) the white disappears shortly as does the discomfort/pain.

I checked the HDPE jug this afternoon and closely examine the bottom. While pressing against it the whole underside and part of the wall just cracked into a craze pattern. Very brittle.

Also sprayed more KMnO4 sol. onto the now dried dirty residue - still reacted, but no visible frothing.

Lesson learned for me. No long term storage of oxidisers in this type of plastic and use gloves when "stuff happens".

[Edited on 9-6-2008 by argyrium]
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[*] posted on 9-6-2008 at 11:05


I am not a very active experimentalist and I work mainly at Uni lab. I have to say that I always get the MSDS for the reagents and products (if available) involved in a new experiment. When possible I carry out some modeling for target molecules.
BTW I am devoted to photochemical condensations of amines and diols.
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[*] posted on 10-6-2008 at 08:12


I do my experiments in a spare room at home. I mostly experiment with synthesizing inorganic salts, some electrochemistry, and some low-vacuum plasma experiments.

Whether microscale or macroscale, I'm not sure where the line is drawn. I make Copper(II) Sulfate solution by electrolysis in batches of several liters at a time. (This uses somewhere around 4 kilos of MgS04•7H20)

But I make my first batch of any new salt I'm curious about in plastic 35mm film canisters or 24oz polyethylene "party cups".




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[*] posted on 10-6-2008 at 15:22


Storage,
If you can, use glass.
For many chemicals HDPE is just fine.
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[*] posted on 10-6-2008 at 16:00


Quote:
Originally posted by MagicJigPipe
I can say, from first hand experience, that 35% H2O2 burns are horrible. They bleach your skin white and it causes this slow very painful stinging sensation that just persists. It will not go away. It's very unpleasant. Then, the skin just rots away leaving a hole.

It's one of the worst burns I've ever had.

I do all of my experiments at home, by the way.


My friend got a peroxide burn said it itched like crazy and turend his skin white till it fell off. I have used 35% peroxide quite a bit and have never gotten burnt. Can't say the same for silver nitrate my fingernails and fingertips are brown/black %*@&!!!


I am defiantly a home experimenter I do my experiments in my garage all inorganic.




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[*] posted on 10-6-2008 at 21:10


Depends! If it is something really hazardous or needing special apparatus, I do it in a commercial lab at work. If it's general inorganic chem and small scale, I do it at home outside or in the garage. I'm fortunate to have good neighbours!



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[*] posted on 11-6-2008 at 12:22


My lab is in an attached garage. Since I have an efficient fume hood I can do many experiments that I would otherwise not feel comfortable doing. I also have friendly neighbors who I take care not to offend.

Because I'm not into pyro, explosives, or poisonous gases I'm rarely tempted to exceed my capabilities. I would have no trouble working with acetyl chloride or thionyl chloride in my lab. With H2S or HCN I might do the experiment outside.

I consider laboratory hygiene to be very important and try to keep my equipment clean and orderly. I think that my home lab has better hygiene than any of the labs I used when in school. In school you are not really sure of the state of cleanliness of shared equipment and work areas. Also you don't really have control of what (unsafe acts) others might do in your vicinity.

As vulture says, fire is a big risk. Most homes, including mine, are just crammed with wood, paper, cloth, and other flamables. So this is something I try to be especially careful about. Working alone is the norm for the home chemist. This is a risk not normally present in a school or industrial lab.
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[*] posted on 18-6-2008 at 11:27


I work at home with most of the stuff i do but if i am planning to use some of the more "nasty" stuff then a professional uni lab (with permission) is available :)
but at home, my garden/balcony does the job :)
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[*] posted on 25-6-2008 at 17:09


I do all my personal reactions at home, in the garage. Using schlenk glassware, vacuum and argon, you can handle small amounts of dangerous products no problem. The only time any exposure is possible, is when opening/using the reagent bottle, and in that case I use good ventilation or for the more dangerous stuff a home-made dry box.

I still think I really need a fume hood, and have put a few projects asides since a bad aventure involving H2S. I also would like to build a proper storage closet,w ith adequate ventilation, as most of my precious reagents are inside a regular wood closet, and there is a slight "chemical" smell, nothing distintive.

I do more involved reactions at work, in a very recent lab (the team moved in only a year ago, from the old old lab that are currently been demolished), with excellent equipment (really schlenk lines, beautifull glove box, spacefull fume hoods, etc etc).
The storage room is something I will never forget though. You litteral need to hold your breath when going in, and can stay 5min looking for something... Even if there is strong ventialtion, an dmost of the more reactive/flammable/toxic reagents are in fire-proff isoalted closets (the kind in which you can burn 5L of solvents without smelling anything :) ), the smell is unbearable.

Ina few case, i think i work more cleanly at home that certain colleagues at work.. I have founf dozens of mercury-filled old electrodes in the containers in which the desktop litter is put, even though there is a special room for the used solvents, cans for heavy meatsl, silica gels, etc etc.
In a few teams there are also 20L jerricans half full of solvents (solvent "bin"), on the floor, opened, untilit's full and disposed of. What's the use of having such fume hoods....

I also agree on fire been one of the major hazards at home. I have a few powder extingushers around the lab, 2buckets of sand, 50L of vermiculite (to absorb any dangerous spills), and a water hose close. But I would really feel safe only when i have a proper closet.




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[*] posted on 26-6-2008 at 11:16


I do all my Chemistry in a storage room in my basement and in a tiny room at the back of my house that is well ventilated and one that used to be a Toilet. We had everything, minus the basin removed. I don't do much Chemistry and experimenting there though. I tend to do preparations there, before going downstairs.
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[*] posted on 16-8-2008 at 14:15
Jealousy


I wish I could work at home! I have a home office where I work outsourcing drop-ships and consulting, but I can't do anything because of having a tax-paying business and being unable to do any chemistry (except for household stuff of course) because I'm not zoned for it, and my county's zoning commission is a bunch of evil bribe oriented creeps. Having a zoning waver would end my life! Once they inspected, no satellite dish outside, no potted plants larger than some size, and on, and on.

So, I've been looking for a legally zoned lab to rent, but this is harder than I could have believed. With the US economy crumbling, you'd think someone would want my money! Finding the right (and affordable, not 50, 000 square feet) has been so much harder than I could believe!

*jealous jealous jealous*
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