Sciencemadness Discussion Board

Successful experiments

Zyklon-A - 27-1-2014 at 16:06


I think there should be a thread on the successful experiments that are done here.
I'll start.
Today (27-1-2014) I extracted lithium from a lithium battery, I've tried at least twice before, and this is the only time it worked.

PICT0051 - Copy.JPG - 128kB

[Edited on 28-1-2014 by Zyklonb]

[Edited on 28-1-2014 by Zyklonb]

confused - 27-1-2014 at 16:12

i always end up with the lithium oxidizing before i can get the casing off, how did you manage to do it?

Zyklon-A - 27-1-2014 at 16:29

It oxidized a little, but I put it in a CO2 (not really inert, but better than air I'm sure) filled vile before much happened.
With the first battery it failed considerably, I just took way to long taking it out, the second time however, I took the pliers and yanked the roll out of the steel casing, without striping the casing at all, I was really surprised at how well it worked.
It was not a energizer ultimate lithium battery, it was a duracell battery.


[Edited on 28-1-2014 by Zyklonb]

Zephyr - 27-1-2014 at 16:50

I recently sodium via sodium hydroxide and it worked much better than I had expected. This will be the 32nd element in my collection!

Zyklon-A - 27-1-2014 at 17:02

I have yet to even try that, I don't have NaOH at the moment, I've always thought that an complex setup is needed, to keep air out and whatnot.

phlogiston - 27-1-2014 at 18:01

While congratulating you with your success, I think the topic of this thread is too unspecific.

Zephyr - 27-1-2014 at 18:04

Zyklomd, the procedure is actually very simple and the one I used is a variation of this.
Everything except the magnesium can be sourced from your local homedepot.

Zyklon-A - 27-1-2014 at 18:15

Thanks, I intended it to be for success in general, isolating elements, making compounds, ect. Not necessarily for everybody who has a successful experiment of course.
There are topics for bad days in the lab, chemist's nightmare and other bad things, why not something for good things?



[Edited on 28-1-2014 by Zyklonb]

[Edited on 28-1-2014 by Zyklonb]

[Edited on 28-1-2014 by Zyklonb]

Zyklon-A - 27-1-2014 at 18:45

@Pinkhippo11, I assumed that you meant you did electrolysis of sodium hydroxide, I have seen that video before but I though the sodium quality would be very bad (contaminated). I can get NaOH, I just don't have it right now.
I guess I will try it now that you said it worked well.

Zephyr - 27-1-2014 at 20:03

Yes, the quality is not exceptional, but I too do not have the equipment to preform such an electrolysis. However, the purification methods in the video are surprisingly effective and do not waste very much sodium metal. Give it a try if you don't have access to sodium metal, it is very useful.

Zyklon-A - 28-1-2014 at 05:41

Did you try any methods other than those shown in the video to purify you product? (sodium)

alexleyenda - 28-1-2014 at 09:21

Personally, when I tried this methode 1° It was an horrible pain in the :) to make a good quantity of magnesium powder from a magnesium fire starter 2° It produced some sodium mixed with some crap but it did not survive the oil/water purification. The fact that I used a fire starter and NaOH from drain cleaner probably mixed with other things instead of pure NaOH may be the cause of the failure, but in the futur there is no doubt I will buy the sodium instead.

You can also see from the video that the sodium produced is quite a good step less reactive than pure sodium.

I must however say that the reaction was quite nice, surprisingly powerful. I was glad I put a concrete block on top of the lid.


[Edited on 28-1-2014 by alexleyenda]

Zyklon-A - 28-1-2014 at 09:45

Here some people talked about using Al instead of Mg, I will try this as soon as I get some NaOH.
Al will react with NaOH because it's amphoteric, but if I can light it quickly it may work.

alexleyenda - 28-1-2014 at 10:12

Give me some news, It's been a while since I did it, I now have pure NaOH and Al powder so I might give it a try if it works.

Zyklon-A - 28-1-2014 at 12:09

Or: Mix 20g powdered aluminum, 6g NaOH, 3g NaCO3, and 5g NaCl in a steel crucible.
Put the crucible over a heat resistant base that allows heating by flame. Cover the crucible with a steel bowl filled with water.
Heat the crucible vigorously with a blowtorch or a heavy duty bunsen burner until a reaction takes place, marked by yellow flames escaping from the crucible.
When the reaction is over and the crucible is no longer red, remove the bowl carefully pouring the water away. There should be a light grey deposit at the botton. Scrape this deposit with a spatula to a 50ml vial with some xylene in it using a funnel. Repeat this procedure four times.
Tacho wrote this, by the way.

MrHomeScientist - 28-1-2014 at 12:17

Such a thin film of sodium would react very quickly with air and moisture, I would think. Also you'd really have to heat this thing to reach the boiling point of sodium (unless the reaction is exothermic enough, I suppose).
What's the reaction equation for this process?

Zyklon-A - 28-1-2014 at 12:38

The reaction is definitely exothermic enough, it's sometimes classified as a thermite reaction.
You can read all about this (and similar reactions) here.
This is getting rather off topic... Further discussion of such things should be continued here as well.

[Edited on 28-1-2014 by Zyklonb]

Mailinmypocket - 28-1-2014 at 14:49

Did a nice small scale synthesis this week, phthalic anhydride to anthranillic acid to methyl red. Might make a post on it with pictures and what not in the next week or so.

Zyklon-A - 4-2-2014 at 10:09

I made about 8 grams of CuCO3 yesterday, it's very bright, rich blue-green color, I'm very impressed.

DraconicAcid - 4-2-2014 at 10:37

I made cis-bis(glycinato)copper(II) the other day. The reactants combined to give a glorious dark purple-blue solution (much like tetraamminecopper(II)), but as it cooled, light powder blue needles started forming, eventually turning the entire solution into a semi-solid mass. This filtered out to a pale blue powder. Actually disappointing.

Zyklon-A - 4-2-2014 at 11:30

Huh, that's too bad, I've had similar disappointments, where it looked like a great product, but it turned out to be rather bland or boring.

Zyklon-A - 6-2-2014 at 16:42

Today I isolated a lot more lithium from a lithium battery. Yields were even better than last time, I might make a guide on how to do it. The batteries that I used are much easier to extract than energizer ultimate lithium batteries.

Zyklon-A - 6-3-2014 at 12:08

Today I made some I2Cl6.
I also plan on making more from direct reaction of I2 and Cl2, as opposed to the method that I used this time.
[EDIT] Well, of course it didn't last very long, It gave off chlorine as it formed iodine monochloride, which in turn, evaporated, leaving nothing to remember all my work...:(
Oh, well.
Recently I've been trying to make lots of covalent Cl- compounds. I plan on making ICl (iodine monochloride), and a few sulfur chlorides too.

[Edited on 6-3-2014 by Zyklonb]

packetforger - 6-3-2014 at 14:06

Extraction of Lithium from batteries: http://spatulatzar.com/lithium/

My advice would be to do the whole process with the battery submerged in mineral oil, like in a large bowl or bucket, if oxidation is such a major issue.

Zyklon-A - 6-3-2014 at 14:46

Hmmm, good idea, best thing next to a glove box.

Zyklon-A - 14-5-2014 at 20:00

Forgot about this thread... Anyway:
Chloroform synthesis, (I did this today), bromine isolation, potassium chlorate synthesis and I'm working on sodium chlorate right now. I've done quite a few other experiments in the last few months, most of which I've forgotten.

The Volatile Chemist - 26-5-2014 at 14:36

I produced a good bit of Barium Carbonate, rather useful for barium compound making.

Zyklon-A - 26-5-2014 at 17:15

Quote: Originally posted by The Volatile Chemist  
I produced a good bit of Barium Carbonate, rather useful for barium compound making.

How'd you make it? Double displacement of barium nitrate and sodium carbonate is how I generally make mine.
I'm making copper (II) chloride right now.
Cu + HCl(aq) and H2O2 very nice color(s).
My sodium chlorate cell is still running, it's taking much longer than I thought.

The Volatile Chemist - 26-5-2014 at 17:44

Quote: Originally posted by Zyklonb  
Quote: Originally posted by The Volatile Chemist  
I produced a good bit of Barium Carbonate, rather useful for barium compound making.

How'd you make it? Double displacement of barium nitrate and sodium carbonate is how I generally make mine.
I'm making copper (II) chloride right now.
Cu + HCl(aq) and H2O2 very nice color(s).
My sodium chlorate cell is still running, it's taking much longer than I thought.

Yes, that's how I made it.. Actually with bicarb. I made some of it's sulfate thinking I could get carbonate from that (barium nitrate & epsom salt) by adding bicarb to IT, but I didn't realize how unreactive barium nitrate was.
I made some copper chloride a while back, but I had no HCl, so I used CaCl2 instead.
Is this the first time you've done a chlorate cell? What are you using as a power supply?

Zyklon-A - 26-5-2014 at 18:24

It's my first sodium chlorate cell.
I've ran quite a few potassium chlorate batches.
I am bought a power supply exactly like this:http://www.circuitspecialists.com/5-volt-30-amp-power-supply... except it pulls 20 amps, not 30. Got it from the same place though, don't know where the one I bought went.
It has two terminals, one puts out 7 amps, the other 13. I'm just using 7 right now.

The Volatile Chemist - 26-5-2014 at 18:29

Quote: Originally posted by Zyklonb  
It's my first sodium chlorate cell.
I've ran quite a few potassium chlorate batches.
I am bought a power supply exactly like this:http://www.circuitspecialists.com/5-volt-30-amp-power-supply... except it pulls 20 amps, not 30. Got it from the same place though, don't know where the one I bought went.
It has two terminals, one puts out 7 amps, the other 13. I'm just using 7 right now.

Wow, mine is a repurposed computer PSU, with a 7A max (At 10v, inconvinient, so I normally run it at 3A 5v)

Hegi - 29-5-2014 at 22:14

There were many of them.. preparation of benzoic acid from toluene, methyl benzoate synthesis, ethyl acetate synthesis, piperine extraction, many copper complexes preparation and the simple ones I am not going to mention. :)

The Volatile Chemist - 1-6-2014 at 11:00

Quote: Originally posted by Hegi  
There were many of them.. preparation of benzoic acid from toluene, methyl benzoate synthesis, ethyl acetate synthesis, piperine extraction, many copper complexes preparation and the simple ones I am not going to mention. :)

Which complexes did you make?

Hegi - 2-6-2014 at 04:31

Quote: Originally posted by The Volatile Chemist  
Quote: Originally posted by Hegi  
There were many of them.. preparation of benzoic acid from toluene, methyl benzoate synthesis, ethyl acetate synthesis, piperine extraction, many copper complexes preparation and the simple ones I am not going to mention. :)

Which complexes did you make?


basic ones, with ammonia, chlorido ligands, copper aspirinate and then I started to work with compounds such as..


The Volatile Chemist - 2-6-2014 at 05:35

Looks like fun, I love copper complexes. Those last ones look exquisite! I wouldn't have half the chemicals to make them, but... :) What colors are those last ones, copper aspirinate and the pictures?
I made some basic chloro complexes, but found a good salt to use for making Amminechlorido (I prefer Amminechloro) copper complexes, Ammonium Chloride :P. Works awful well, I'm pretty sure I made Amminetrichlorocuprate(II) acid (3NH4Cl + CuSO4 >> H[Cu(NH3)Cl3] + (NH4)2SO4). The substance had a pH of about 4 or 5.

Hegi - 2-6-2014 at 12:33

Quote: Originally posted by The Volatile Chemist  
Looks like fun, I love copper complexes. Those last ones look exquisite! I wouldn't have half the chemicals to make them, but... :) What colors are those last ones, copper aspirinate and the pictures?
I made some basic chloro complexes, but found a good salt to use for making Amminechlorido (I prefer Amminechloro) copper complexes, Ammonium Chloride :P. Works awful well, I'm pretty sure I made Amminetrichlorocuprate(II) acid (3NH4Cl + CuSO4 >> H[Cu(NH3)Cl3] + (NH4)2SO4). The substance had a pH of about 4 or 5.


Why are you pretty sure... Have you isolated and characterized the product you think it may be in some way? What is about nomenclature, in our country we switched last year from chloro, bromo.. to chlorido, bromido.. The complexes I did - [Cu(NH3)4] and copper chloride dihydrate, copper acetate, copper bis(oxalate) maybe could be interesting salts as copper benzoate, copper citrate, .. The structure I posted is prepared by reacting potassium hexacyanidochromate with copper complex of compostion as follows [Cu(L)]SO4 . xH2O

and copper aspirinate picture..


The Volatile Chemist - 2-6-2014 at 13:41

Very pretty. With the 3NH4Cl + CuSO4 >> H[Cu(NH3)Cl3] + (NH4)2SO4 reaction, I'm only partially sure because I don't have a scale, and multiple complexes could have formed
I prefer chloro to chlorido, but I guess the second makes sense. It does add a second syllable, though.

alexleyenda - 3-6-2014 at 21:46

Not exactly an experiment, but I had two 250 mL filtering flask, which is a very small volume and filtering was a pain in the A for me... So I took one and made this, it looks very random but it does work well and I now have a 4 L filtering flask :p The green stuff is an epoxy resin which resists to acids, oxidation and bases and the bottle is in HDPE. It is very solid. The only issue is that the HDPE bottle tends to collapse a bit under the vacuum but as long as I am careful It works fine and hey, it is still better than having two 250 mL filtering flask, one being useless. It really looks like it was made by a child though, it's quite funny :p

pho1.bmp - 914kB pho2.png - 1.1MB

[Edited on 4-6-2014 by alexleyenda]

The Volatile Chemist - 4-6-2014 at 07:35

Smart Idea! I like it! To "how much vacuum" will the bottom hold up, do you think? Enough for filtering?

alexleyenda - 4-6-2014 at 08:34

Enough for filtering, I tested it and it worked :) The top and the bottom are actually very tough, there is only the middle of the bottle that twists a bit.

Zyklon-A - 4-6-2014 at 08:38

I'm confused, did you drill a hole in a glass flask? Or is it plastic?

The Volatile Chemist - 4-6-2014 at 11:49

Cool, you got your flask from Home science tools! I get stuff from there too!

Quote: Originally posted by Zyklonb  
I'm confused, did you drill a hole in a glass flask? Or is it plastic?

That flask is from HST, it's glass. It looks like the glass has been broken at the bottom, and the green stuff is some sort of polyeth. glue.

alexleyenda - 4-6-2014 at 15:52

I drilled an hole in the bottom of the flask with a rotary tool and a diamond dust head. and "The green stuff is an epoxy resin which resists to acids, oxidation and bases".

Zyklon-A - 4-6-2014 at 16:20

Quote: Originally posted by alexleyenda  
I drilled an hole in the bottom of the flask with a rotary tool and a diamond dust head.

Nice, I should get one if those. That or a tungsten carbide bit, either works for glass. Must've been pretty expensive, for one that big.

alexleyenda - 4-6-2014 at 16:27

It was very small in fact, I just cut a circle, it took a bit of time but it did the job.

Bert - 4-6-2014 at 19:08

Guys-

I think the title should be "successfuly replicating procedures"? You're mostly talking about replicating someone else's experimental procedure?

A successful experiment is one that you obtain new information from, and possibly can draw some conclusion from... Even if the outcome is not what you'd predicted. A negative answer is STILL valid information, even if it hurts the ego a bit. No is every bit as meaningful an answer as Yes-

http://en.m.wikipedia.org/wiki/Cognitive_bias

Zyklon-A - 4-6-2014 at 20:51

True, go ahead and change it. Only a Mod can.

The Volatile Chemist - 5-6-2014 at 14:17

Quote: Originally posted by Zyklonb  
Quote: Originally posted by alexleyenda  
I drilled an hole in the bottom of the flask with a rotary tool and a diamond dust head.

Nice, I should get one if those. That or a tungsten carbide bit, either works for glass. Must've been pretty expensive, for one that big.

If you need one, sciplus.com has them cheap. I've never bought one from them, but looks like a good deal to me (Sorry, o link to the actual product, use their search if interested).