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the mad chemist
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smile.gif posted on 22-9-2015 at 02:29
main chemicals for home lab setup


hi everyone,
just wondering any possible way to have some main chemicals(specially house hold ones) that help me make a lot of other complex chemicals and if you have any experience with these things please share it here or send me link to it
wish the best
the mad chemist
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[*] posted on 22-9-2015 at 02:53


Reading this page may be helpful if you are starting and want to set up a home lab:

http://woelen.homescience.net/science/chem/misc/homelab.html




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[*] posted on 22-9-2015 at 02:55


No time for a full reply right now.
Your answer: it depends on what you are wanting to do.
I suggest you search. This Q gets asked regularly. It won't take too long before you find a list or a link to a list.
My suggestion: build stock and equipment project by project.

(edit)
I was going to recommend woelen's link.

[Edited on 22-9-2015 by j_sum1]
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the mad chemist
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[*] posted on 22-9-2015 at 02:56


good website but i mean if any one know the main key chemicals for making a lot of other chemicals
cheers
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[*] posted on 22-9-2015 at 02:58


more interested in making chemical for low prices and extraction of organic and inorganic compounds

also wow i got replys fairly fast thanks

[Edited on 22-9-2015 by the mad chemist]
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[*] posted on 22-9-2015 at 03:02
Basic supplies


When is started off I just scavenged the food, drug, and hardware stores. You'll need baking soda, and vinegar for spills and reactions. You will also need lye(drain cleaner) and sulfuric acid (drain cleaner). These two may not be pure, but will still work ok. Please go to
https://en.m.wikipedia.org/wiki/List_of_commonly_available_c...

I started by picking an experiment, and then buying the chemicals at the store, or online. After awhile I had a large selection of them.

For supplies I started out with a funnel, a glass rod, filter paper, some flasks and beakers, a graduated cylinder, and an alcohol burner.

Finally, for saftey get some good goggles, a face shield, a respirator(hardware store, a fire extinguisher, some latex gloves, and some chemical resistant gloves. Search up glove compatability chart.
Most chemicals a hard to find at a store, so buy them from Amazon, eBay, home science tools etc.

https://m.youtube.com/watch?v=xjbwk9f9mcY
https://m.youtube.com/watch?v=0k7-drcTl4M
https://m.youtube.com/watch?v=zhDypc8SCoE
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[*] posted on 22-9-2015 at 03:11


thanks just needed that i wish i could have the setup easy
regards the mad chemist
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[*] posted on 22-9-2015 at 08:19


In case if sulfuric acid drain opener is not available where you live (in my country, conc. sulfuric is a FSKN List IV chemical, which makes it illegal as an OTC consumer product), you should learn to "Boil the Bat". That is, boil down battery acid to concentrate it. This is what will become your new Pater Noster.



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[*] posted on 22-9-2015 at 13:48


FYI you don't need to buy straight-up lye (NaOH), you can make it out of regular table salt via electrolysis.
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[*] posted on 22-9-2015 at 16:05


Quote: Originally posted by Upsilon  
FYI you don't need to buy straight-up lye (NaOH), you can make it out of regular table salt via electrolysis.


Even that is not required. Regular drain openers (as opposed to those with sulfuric acid) are usually NaOH based. Especially convenient are dry and granulated ones, in which NaOH is in granules and everything else is a fine powder. Any old kitchen sieve can be used to separate NaOH from everything else. Sometimes you can find "Pure Lye Bead" openers, with these you do not even need the sieve.

KOH on the other hand... This you have to either buy, electrolyze from potassium fertilizers or sodium-free salt, or leach from old alkaline cells and then concentrate by boiling down.


[Edited on 23-9-2015 by ave369]




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[*] posted on 22-9-2015 at 22:31


Quote: Originally posted by Upsilon  
FYI you don't need to buy straight-up lye (NaOH), you can make it out of regular table salt via electrolysis.
Please, try it and report back on your results!

if you do some practical chemistry then you soon will discover that making (and isolating!!) basic chemicals can be very hard.




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[*] posted on 23-9-2015 at 10:39


Quote: Originally posted by woelen  
Quote: Originally posted by Upsilon  
FYI you don't need to buy straight-up lye (NaOH), you can make it out of regular table salt via electrolysis.
Please, try it and report back on your results!

if you do some practical chemistry then you soon will discover that making (and isolating!!) basic chemicals can be very hard.


If you separate the setup into half cells connected by a salt bridge then it's really not that bad. As long as you can run the cathode cell to completion, there shouldn't be too much NaCl contamination left over. And there are ways to deal with any NaCl contamination if you need even higher purity.
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[*] posted on 23-9-2015 at 12:40


Electrolysis for even a lab scale quantity is not easy.
Various forms of salt bridge are possible but you get contamination.
From my experience you can get a couple of percent out of an agar
bridge. And you have some agar in your solution as well as salt.

Membranes make it easy but they are very expensive. They give
a really high purity product. The cost of up to US$300 per sq ft
is a major drawback. You can purify a lot of drain cleaner for that price.

A mercury cell is not that easy either as the mercury amalgam will
solidify if it gets too high in sodium. And mercury is toxic.

A diaphram cell is much easier than the others and purifying your
sodium hydroxide then becomes the problem.

Having said all of that, purifying drain cleaner is not the worst way
to go if you have more time than money.

The other big chemical is sulfuric acid. If you master electrolysis,
then epsom salt is your friend. A diaphram cell or membrane cell
is necessary here. Epsom salt can also be decomposed to sulfur
trioxide and dioxide gas at extreme temperature (1100+C).
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[*] posted on 23-9-2015 at 13:09


Quote: Originally posted by Upsilon  
Quote: Originally posted by woelen  
Quote: Originally posted by Upsilon  
FYI you don't need to buy straight-up lye (NaOH), you can make it out of regular table salt via electrolysis.
Please, try it and report back on your results!

if you do some practical chemistry then you soon will discover that making (and isolating!!) basic chemicals can be very hard.


If you separate the setup into half cells connected by a salt bridge then it's really not that bad. As long as you can run the cathode cell to completion, there shouldn't be too much NaCl contamination left over. And there are ways to deal with any NaCl contamination if you need even higher purity.

On paper many syntheses look simple and of course, there always are ways to purify things. But in practice this is HARD, very HARD! Try it, then you will see yourself. You can buy pure (99% NaOH) for a few euros (or dollars) per pound, and there is no substitute for that. I am doing home chemistry for 20 years or so by now and from experience I know that making, isolating and purifying new chemicals in many cases is very hard and requires a lot of work, decent equipment and a lot of patience. Many chemicals which are made from naturally occuring simple stuff like NaCl, CaCO3, N2 from air, water, etc. by the multitonne on an industrial scale are amazingly hard to make at home (e.g. NaOH, H2SO4, conc. HCl, HNO3). The basic reactions are very simple, but from an engineering perspective it is extemely hard.

NaOH and H2SO4 really are basic chemicals you need to buy. With these as starting point, you can make many other interesting chemicals relatively easily, using easy to obtain chemicals (e.g. HCl from NaCl, NH3 from NH4Cl or (NH4)2SO4, HNO3 from KNO3 or NaNO3). Many of these chemicals, however, also can be purchased easily in many countries (HNO3 becomes harder to obtain nowadays due to anti-terrorism regulations).




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[*] posted on 23-9-2015 at 16:37


I actually am in the middle of an NaCl electrolysis right now. It's taking an extremely long time (about 2L of highly concentrated NaCl solution, using a 24V 0.5A DC adapter). I've separated the half cells and connected them with a salt bridge, and I'm using graphite electrodes I extracted from regular pencils. It's going to take several days of collective runtime to go all the way, so it'll be a while before I can share any results.

HNO3 is easier to create than NaOH, though. If you're able to work with a slightly contaminated sample, you can react a solution of calcium nitrate with sulfuric acid (both pretty cheap). Then just filter the calcium sulfate precipitate. A small amount of it will dissolve and contaminate the HNO3 (it's not much, it will be about 2.4 grams of calcium sulfate contamination per liter of acid); to prevent this barium nitrate can be used in place of calcium nitrate. Barium nitrate is a little expensive, though.

EDIT: It might be possible to use oxalic acid (still cheap) instead of sulfuric acid, since calcium oxalate is much less soluble than calcium sulfate. I have suspicions though that nitric acid would attack the calcium oxalate. This would be something to experiment with.

[Edited on 24-9-2015 by Upsilon]
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[*] posted on 24-9-2015 at 00:54


Quote: Originally posted by Upsilon  


HNO3 is easier to create than NaOH, though. If you're able to work with a slightly contaminated sample, you can react a solution of calcium nitrate with sulfuric acid (both pretty cheap). Then just filter the calcium sulfate precipitate. A small amount of it will dissolve and contaminate the HNO3 (it's not much, it will be about 2.4 grams of calcium sulfate contamination per liter of acid); to prevent this barium nitrate can be used in place of calcium nitrate. Barium nitrate is a little expensive, though.
[Edited on 24-9-2015 by Upsilon]


Do you have a Buchner set for that? The precipitate of CaSO4 is huge and messy, and it's a pain in the ass to filter it through paper.




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[*] posted on 24-9-2015 at 09:00


Quote: Originally posted by ave369  
Quote: Originally posted by Upsilon  


HNO3 is easier to create than NaOH, though. If you're able to work with a slightly contaminated sample, you can react a solution of calcium nitrate with sulfuric acid (both pretty cheap). Then just filter the calcium sulfate precipitate. A small amount of it will dissolve and contaminate the HNO3 (it's not much, it will be about 2.4 grams of calcium sulfate contamination per liter of acid); to prevent this barium nitrate can be used in place of calcium nitrate. Barium nitrate is a little expensive, though.
[Edited on 24-9-2015 by Upsilon]


Do you have a Buchner set for that? The precipitate of CaSO4 is huge and messy, and it's a pain in the ass to filter it through paper.


It's doable with just a Buchner funnel and some filter paper. You'll just need some object to squeeze the liquid from the calcium sulfate while it's in the funnel. Sure, you'll get more out of it with vacuum distillation, but it gets pretty expensive for a working setup.
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[*] posted on 24-9-2015 at 10:58


Quote: Originally posted by Upsilon  

It's doable with just a Buchner funnel and some filter paper. You'll just need some object to squeeze the liquid from the calcium sulfate while it's in the funnel. Sure, you'll get more out of it with vacuum distillation, but it gets pretty expensive for a working setup.

No it's not possible at all, have you ever actually tried that before? There's no way you'll be able to filter a mixture that acidic with filter paper, it will tear in under a second. You will need at the very minimum a glass frit with the correct pore size so as not to get clogged. And removing calcium sulfate from a frit will be a pain in the ass, not to mention that decently sized frits aren't cheap. There's a reason that distillation is the common way to go when making nitric acid, and a distillation setup is not that expensive. If you buy Chinese glass, you can typically get one for under $40, and it can be used for a lot more than preparing nitric acid.




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[*] posted on 24-9-2015 at 11:44


It's possible if the acid is dilute enough. Say, battery acid diluted with equal amount of water, with calcium nitrate in stoichiometric amount. Did this, didn't eat through any paper, but getting rid of calcium sulfate is hell. I'd better distill some nitric acid from sulfuric & saltpeter in a retort. Did this yesterday, prepared 90+% nitric acid.



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[*] posted on 24-9-2015 at 15:12


Quote: Originally posted by ave369  
It's possible if the acid is dilute enough. Say, battery acid diluted with equal amount of water, with calcium nitrate in stoichiometric amount. Did this, didn't eat through any paper, but getting rid of calcium sulfate is hell. I'd better distill some nitric acid from sulfuric & saltpeter in a retort. Did this yesterday, prepared 90+% nitric acid.
I was talking about making acid of a reasonable concentration, but I could see it being possible to filter a dilute solution. But as you saw for yourself, distillation is the easier method, and the only method if you want acid of a decent conc. in a good yield.



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[*] posted on 24-9-2015 at 15:36


I do have a rough distillation setup (it uses rubber stoppers instead of glass joints, but I have all of the glassware needed). In theory, I could make a 68% solution by adding correct amounts of sulfuric acid, calcium nitrate, and water, which would then boil at exactly 121C? Sounds fairly simple.
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[*] posted on 24-9-2015 at 16:16


Quote: Originally posted by Upsilon  
I do have a rough distillation setup (it uses rubber stoppers instead of glass joints, but I have all of the glassware needed). In theory, I could make a 68% solution by adding correct amounts of sulfuric acid, calcium nitrate, and water, which would then boil at exactly 121C? Sounds fairly simple.
Yes, but you can't distill conc. nitric acid in an apparatus where the vapors will come into contact with rubber. The hot vapors will destroy rubber quite rapidly.



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[*] posted on 24-9-2015 at 16:43


Quote: Originally posted by gdflp  
Quote: Originally posted by Upsilon  
I do have a rough distillation setup (it uses rubber stoppers instead of glass joints, but I have all of the glassware needed). In theory, I could make a 68% solution by adding correct amounts of sulfuric acid, calcium nitrate, and water, which would then boil at exactly 121C? Sounds fairly simple.
Yes, but you can't distill conc. nitric acid in an apparatus where the vapors will come into contact with rubber. The hot vapors will destroy rubber quite rapidly.


Would it be feasible, then, to wrap the rubber stoppers in Teflon tape? The vapors are traveling through glass tubes, so I would only need to worry about covering the exposed surfaces of the rubber. It'll make the stoppers slippery as hell in the flask opening, but it'll save me from buying extra glassware.
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[*] posted on 24-9-2015 at 18:49


I doubt that would work. In my experience, the nitric vapors have gotten through a ground glass joint greased with conc. sulfuric acid and destroyed my Keck clips every time. Attempting this with rubber fittings, even coated in Teflon tape, sounds like a disaster waiting to happen.



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[*] posted on 24-9-2015 at 19:02


It is possible with the rubber stoppers wrapped in teflon tape.
But you need a special heat gun with an inert gas supply (plastic welder)
to make the tape actually fuse to itself and the rubber stoppers.
But don't plan on using the rubber stoppers more than
a couple of times.

You can do this in a crude manner with a hair dryer in an
aquarium filled with carbon dioxide.
You might be able to achieve the same thing in a toaster oven
with baking soda which would act as a carbon dioxide source.
I haven't tried either of these methods. A plastic welder
with inert gas isn't cheap though.

It is really easier to buy a glass vacuum
distillation set and a water aspirator vacuum pump.
You can get one of these for under $200, which isn't
cheap but is a lot better than breathing nitric.
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