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snateraar
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[*] posted on 15-7-2013 at 03:03
Where do I start?


Edit: If this is in the wrong board, please move it. As I have some chemical experience I thought it didn't fit in the Beginnings board, but that could just be me :P

Hello guys! I just made an account on here after a user of the Chemistry reddit page linked me here.

I've set up a small home lab a week ago; glassware(lots of it!), heater plate, stirbar thing(DIY version), some chemicals including sulfur and copper sulfate and various other things.

I wanted to set up this home lab in preparation for the chemistry college that I'll attend in a few months. A bit of practice never is bad, isn't it?

Either way, I obviously want to do it as organized as possible, with some precision and taking note of everything.


My question is: Where do I start?
I've always wanted to try to make sulfuric acid by electrolysis of copper sulfate, but other than that I have no idea what else to do.

Could you guys provide help/tips?

Thanks in advance.


If I won't reply: I am currently on vacation in a country with really shitty internet.

[Edited on 15-7-2013 by snateraar]
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Vargouille
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[*] posted on 15-7-2013 at 04:57


Well, it really depends on what you have, but I'm quite fond of copper salts and complexes. There's tetraamminecopper (II) sulfate, both blue and green versions of "cupric chloride" (If only I could run X-ray crystallography), various cyanurate salts (cyanuric acid as a pool stabilizer), the mystery salt formed form mixing with sodium dichloroisocyanurate (a pool shock), and what ever else catches your fancy. If you have chemical experience, then you should be able to get preparations for all of these, or make them yourself, without too much trouble. Don't forget your different solvents!
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snateraar
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[*] posted on 15-7-2013 at 06:07


It seems my definition of ' some experience in chemistry ' is a bit off: I know the basics like ionic bonds, simple stoichiometry and separations/extractions and electrolysis, but not much more.
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[*] posted on 15-7-2013 at 06:13


Before undertaking anything that involves chemicals. Read as much as you can before you start mixing chemicals willy nilly. There can be some severe consequences from mixing the wrong things together. If a reaction is going to give off something that can gas you then you need to know this and take precautions, like doing them in a fume hood or outside and upwind of them.
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[*] posted on 15-7-2013 at 06:40


Try to obtain a feeling of what is dangerous and what is not. Most of the chemicals are not dangerous at all and these allow you quite some freedom in trying things out. Do not simply mix random chemicals. Try to think about what could happen when you mix certain chemicals and then try it. It becomes more fun when you have a basic understanding and are capable of predicting some reactions.

This webpage about starting a home lab may also be interesting for you:

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




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snateraar
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[*] posted on 15-7-2013 at 09:16


Quote: Originally posted by hyfalcon  
Before undertaking anything that involves chemicals. Read as much as you can before you start mixing chemicals willy nilly. There can be some severe consequences from mixing the wrong things together. If a reaction is going to give off something that can gas you then you need to know this and take precautions, like doing them in a fume hood or outside and upwind of them.


I have this advanced college-level chem book (this one) which I've read + I have previous home chem experience, albeit without proper measurements nor precision.

I think you could consider me mid-level; knows how to handle simple-ish things but doesn't know where to start :P

Quote: Originally posted by woelen  
Try to obtain a feeling of what is dangerous and what is not. Most of the chemicals are not dangerous at all and these allow you quite some freedom in trying things out. Do not simply mix random chemicals. Try to think about what could happen when you mix certain chemicals and then try it. It becomes more fun when you have a basic understanding and are capable of predicting some reactions.

This webpage about starting a home lab may also be interesting for you:

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


Ohey, a fellow Dutchie. Thanks for the page refer, that will come in handy.

I was also planning on executing various of experiments in this book, although it holds some 'dangerous' projects (fabrication of chloroform, for example. Useful as solvent but not really nice to do inside..) which is why it was banned for use back then.




In regards to the first reply to my thread(by Vargouille), I too like copper salts and already have made various crystals, but do you guys perhaps know other chemicals with which to make crystals? Is such a thing possible with sulfur(melting > solidifying)?


[Edited on 15-7-2013 by snateraar]
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[*] posted on 15-7-2013 at 09:44


A good start would be to give us an itemized list of what you have, and in what quantity, then we can give you some ideas for experiments.
It all depends on which reagents you have, but one of my favorite 'beginner' organic chem experiments is making Methyl Salicylate. You only need MeOH, salicylic acid, and a small amount of catalytic acid, you can rig up a reflux system easily.

If the above is below your skills than another simple (but dangerous*) experiment relating to smells is making Ethyl Mercaptan, bubbling H2S into EtOH over a bed of catalyst alumina. The smell is absolutely putrid so do it outside or in a strong fume hood. For the first time I would only work in mL amounts. The purpose of such a nasty experiment is to have a source of ethyl sulfonic acid which can be tricky to obtain, or, you can just collect different thiols/mercaptans and sulfur compunds like I do. Sulfur is one of my three favorite elements, hydrogen and oxygen being the others. Mercury would be a runner-up

*I enjoy working with H2S and performing many experiments with it. Please be aware that it can kill you very quickly, it smells of rotten eggs but soon it will dull your senses and you will become unaware of its presence. It has been compared to hydrogen cyanide in its killing power.

[Edited on 7-15-2013 by chemcam]




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snateraar
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[*] posted on 15-7-2013 at 11:44



The salycylic bit sounds fun to do and possible with my (limited) resources, as doing things outside is hardly an option for me. (I'd probably get weird looks from neighbors and smell complaints, as the ethyl mercaptan compound is the one that's used in flammable gases to indicate it's there, isn't it?)

Chemicals I have access to:

- 500g CuSO4
- 500g S

As much NaOH as I can get(not very pure, though).

That's about it because the lab site I order from only sells in amounts this big, and because this particular country has 21% taxes on everything which is pretty damn expensive.

Other chemicals can probably be made from household things(such as the salycylic acid you mentioned).

I'm also interested in the creation of reagents such as nitric/hydrochloric acid for use in further experiments.

Glassware includes two Erlenmeyers, a few beakers and everything on this picture(a generous donation from the high school I graduated at about two weeks ago):
http://i.imgur.com/Ro99l3S.jpg
Image not in BBCode as it's rather large.

Not on the picture: Two destillation apparatuses with built-in condensor.
In the background you can see a bottle labeled FFT: That's the phenolphtalein indicator in a not very clean bottle :C
I hope this helps.

[Edited on 15-7-2013 by snateraar]
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[*] posted on 15-7-2013 at 12:42


You can make many different metal sulfides which should cost you almost nothing. But I'm not sure of uses for CuSO4.
Read about SO2 method for making H2SO4, then NaCl to make HCl. For nitric acid you'll need a nitrate salt.

Basically the most important acid in home chemistry is sulfuric acid so you should focus on finding that. I believe battery acid is ~30% H2SO4 which can be concentrated/purified.

Edited for spelling.

[Edited on 7-15-2013 by chemcam]




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Vargouille
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[*] posted on 15-7-2013 at 12:55


CuSO4 is a good starting point for making various copper salts. It's what I use, personally, for many of them. You can try making Cu(OH)2 and then dehydrate to CuO. Ammonia is something you can get that'll make some impressive complexes, from tetraamminecopper (II) to Schweizer's reagent. You can make crystals with sulfur, but it's usually done with solvents like toluene or carbon disulfide. Right now, I would work on gathering up more chemicals, though I don't know how easy that will be. Sulfites, other transition metal salts, nitrates, chlorides, acids, etc. This page has a good list of some beginner chemicals, and while generally it's best to look for chemicals to do specific experiments, in your case it might be better to gather the chemicals and cobble together procedures to work with them.
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[*] posted on 15-7-2013 at 14:37


Well, let's start with what you can get for useful chemicals, there are many pages devoted to this topic, but let's name the easy ones:

HCl = hardware store muriatic acid
H2SO4 = drain cleaner
NaOH = drain cleaner or lye
Sodium hypochlorite = bleach
MgSO4 = Epsom salts at the pharmacy
H2O2 = also at the pharmacy
Isopropyl alcohol = also at the pharmacy
EtOH = grain alcohol, need to be 21 for this one in the US
NaHCO3 = Baking soda

When I started in this hobby, all I had was copper sulfate and baking soda and a few acids. In the post above mine, Vargouille tells you that you can make Cu(OH)2 and then use that to make and of the corresponding salts with acids. This is a fun way to get into chemistry since it will be colorful and it is all well worked out. Plus, you can practice your stoichiometry. (My personal preference is to make Copper carbonate and make the salts that way).

Grab some other reagents and we can help you find some fun stuff to do with it :D we are what you call "experts".




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[*] posted on 15-7-2013 at 20:41


Snateraar,

I second previous posters in saying that the best place to start a lab is not in the lab per se, but in the library. Personally I don't think you need to start stocking your lab up with chemicals yet. I'd advice you to find a lab textbook (preferably the one you're going to be using during your studies) and start at the beginning. This means only getting the necessary reagents and equipment to complete the first couple of experiments, and once you're done with those, purchase reagents and equipment for the following ones. In my opinion this method, while less appealing to your inner kid-in-a-candy-store nerd self, is the most cost effective. Get a lab notebook and have a specific experiment you wish to perform in mind. That way you can focus both your research and your resources. Organic chemistry lab textbooks generally start off by teaching you basic techniques, while general chemistry lab textbooks go with the general course sequence (first scientific method experiments, then stoichiometry experiments, then gas law experiments, etc). If you're just starting out, get a gen chem lab textbook. They generally do a good job teaching you the basics. One book I'd recommend, from having skimmed it a bit, is The Illustrated Guide to Home Chemistry Experiments: All Lab, No Lecture, although any college level lab text will do. As far as the dangerous experiments issue goes, it is recommended you do your chemistry outside or in a place that's VERY well ventilated. That said, you can cut down on a lot of the waste and fumes and such by going microscale. This is sort of a pet concern of mine :D There are a lot of forums discussing the benefits and drawbacks of small scale chemistry, please take a look at those. Here are some books I recommend perusing:

Microscale General Chemistry Laboratory: with Selected Macroscale Experiments
A nice microscale gen chem manual

Chemical Technicians' Ready Reference Handbook, 5th Edition
Almost everything you need to know on a practical level (from how to pour your chemicals to how to do basic service on vacuum pumps)

Experiments in General Chemistry
My old gen chem manual

Microscale and Miniscale Organic Chemistry Laboratory Experiments
My old ochem lab manual.




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[*] posted on 17-7-2013 at 09:47


I guess I'm more of a buy first, find experiments later kind of amateur chemist. In my real lab, and most professional labs, you buy reagents long after you have studied what you would like to make and create.

At home, I am much more haphazzard :P




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[*] posted on 18-7-2013 at 15:43



In the past, I find that (as Vargouille has suggested), copper sulfate can be transformed into slimy Cu(OH)2 upon treatment with NaOH. When this is heated, black CuO forms. I really liked synthesizing copper acetate from this material. I used acetic anhydride and water (a waste of Ac2O, I know, but I only had a little), but glacial acetic acid works just fine. Copper acetate is a quite beautiful deep blue solid.

I also highly suggest Vogel's Textbook of Practical Organic Chemistry if you want to try out organic chemistry. It can be a bit complicated for people who have not taken an organic chemistry class yet (like myself), but I am so thankful that I found that book.

Perhaps synthesis of diazonium salts would be interesting?

Anyways, you should try to keep some solvents around. Ethanol, acetone, and toluene sound like good starter solvents. Mineral acids are quite useful as well (HCl can be purchased from many hardware stores as well as H2SO4). Also invest in nice strong glassware. I have often fallen for the trap of purchasing glassware that only lasted me a week before shattering.
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[*] posted on 18-7-2013 at 16:46


Quote: Originally posted by snateraar  



Chemicals I have access to:

- 500g CuSO4
- 500g S

As much NaOH as I can get(not very pure, though).



Get some ascorbic acid and you can reduce the copper sulfate to copper metal. It is a nice experiment.
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[*] posted on 20-7-2013 at 12:52


Get some basic OTC stuff, like acetic acid and other stuff mentioned before. Also, visit pharmacy for even more fun:
- Get syringes for gas experiments (Microscale gas chemistry) and as primitive chromatography columns. Not to mention usage for measuring liquids and gases for stoichiometric addition.
- Get several elementary non-recipe medicines like vitamin C, aspirin (or similar acetylsalycilic acid tablets) and such stuff, and practice separations and purifications - You would not believe how handy it will be some day during your college education and beyond.

Plan your experiments, measure everything you can, and practice scientific approach as much as you can.

And read, read, read, and then do some more reading!




...and then I disappeared in the mist...
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