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Holiday Experiments

hodges - 2-1-2004 at 18:50

Not much activity here lately - so I thought I would post some of the chemistry stuff I did over the holiday.

I made KNO3 from NH4NO3 and KCl. I am quite familiar with KNO3 from my high school pyro days, but had not used any since graduating from college. Ended up with the familiar white crystals. When dry, I tested by mixing about 1/2 gram with an equal amount of powdered sugar. Lit with a butane torch and confirmed it burned fairly well (not as good as black powder, but it did confirm I had KNO3).

I also made KClO3/4(?) using electrolysis. I used a small plastic container with about 150ml of saturated NaCl solution. For the anode, I used two carbon rods connected in parallel from a "heavy duty" lantern battery. For the cathode I used a piece of steel plate from a gas grill igniter. I ran around 2 amps through the solution for about 48 hours. About half the rods got eaten away in that time. I filtered out the graphite and then mixed with KCl and chilled. Got around 11g of precipitate (theoretical is 30g or more, but the temperature of the solution was too cold for efficiency - it was sitting outside on my 3rd floor patio). I mixed about 0.5 grams with an equal amount of powdered sugar and it burned almost in a flash when lit with a butane torch. I then made another small batch of the KClO3/sugar and dropped concentrated H2SO4 (drain cleaner) on it. This made a splattering/frying sound for about a second, then ignited and burned rapidly.

I tried making sodium acetate using baking soda and vinegar, but did not have any luck making the supersaturated solution that crystalizes all at once when you drop in a crystal of sodium acetate. I neutralized about 1 pint of distilled white vinegar with baking soda. I wanted excess carbonate so that when I boiled the solution away there would be no vinegar smell. But I found I still had NaHCO3 left and this started to precipitate when about 20% of the water was left. So I added more vinegar, this time checking pH until I had a slightly acidic solution. I was able to get down to less than 10% of the water before crystals started forming. But when I let it cool, I had a somewhat thick yellow solution that would not crystalize anything no matter how many crystals I dropped in. I tried heating it some more and crystals immediately formed. It was almost as if crystals were forming more at higher temperatures than at lower temperatures.

I obtained Mg ribbon. Although at one time I had powdered magnesium, I have never had Mg ribbon before. I was surprised that this burned rather poorly. It took 5 to 10 seconds to ignite with a butane torch. I had the ribbon sticking out with the end sitting on a scrap steel plate. The Mg kept going out even before it reached the steel, and even heating it with a torch would not get it to burn in contact with the steel. The result looked like I ended up with mostly oxide. I had read that Mg produces mainly the nitride when burning in air. I added a couple drops of water to the ash and did not smell any NH3.

I also obtained some calcium metal in 0.2g chunks. I had read conflicting reports about its reactivity. The WebElements (www.webelements.com) says that calcium will react slowly with water, beginning to liberate hydrogen after "an hour or so". Other places have described the reaction as vigerous enough to set the H2 on fire. When I dropped the calcium into water, I immediately got hydrogen bubbles at a fairly brisk rate. The Ca initially sank but eventually floated due to all the bubbles once it got small enough. It took only a minute or two for all the Ca to be used up. The MSDS with the Ca said it is extremely flamable. I tried burning a 0.2g piece with butane torch, expecting a bright red flame, but was disapointed. I heated it to a dull red glow, and still it did not burn. I heated some more until an orange glow. I took the torch away and the orange glow got brighter, so I assume it was burning. It looked about the color of burning coals. But I never saw any red, and the reaction soon stopped. After it cooled, I added water. Again, I had read that Ca forms mostly the nitride when burning in air. I expected to smell NH3 but did not. It did bubble a bit, but I think this was probably H from remaining unreacted Ca.

Any ideas for interesting things (not necessary pyro) to do with the Mg and Ca? I was thinking the Ca would probably react directly with S to produce CaS. Would this reaction likely be violent (Ca is a chunk, not a powder).

Hodges

Mumbles - 2-1-2004 at 19:35

Can't really think of anything off the top of my head you could do with either of those things. I did think I would share what I accomplished over the break though.

I made Nitrocellulose. I used a nitrate/acid method and got pretty good results. something like 75% yield. I don't know whats normal, but it seems good enough. It burns very fast with a nice poof. I actually made two batches. One with cotton pads, and another with paper towel. I used equal amounts of both and let them nitrate for the same amount of time.

The paper towel product is pure crap. Its burns slower, with residue and smoke, and for some reason it turned brown. Its a very odd product. It dissolves in acetone, but when I add water I don't get a precipitate, or a very little one. I'll probably just keep burning it for fun until it runs out.

I also made some octanitrosucrose. It's sticky. Well some is. I have floating blobs that are very sticky at temps above about 10, and this fine gritty powder thats not sticky(higher nitrated probably). Its still drying so I don't know yields, but it looks not too bad.

I also disposed of some Iron Picrate that had formed. It wasn't much, just a couple crystals. I also disposed of my entire batch of iron oxide just for safety.

Other than that I did a bit of partying. I also went through and cleaned up my lab. It was begining to be a bit of a mess. I cleaned all my glassware too. I found out about this homeschool store a few towns over. I'm checking that out tommorow. I have broken a few "beakers" lately, and my supply is running low. I've always wanted real beakers I can heat to a decent temperature. Well, I hope everyone had a nice safe holiday.

The_Davster - 2-1-2004 at 22:34

I, unfortunatly, was not around untill 2am this morning but while i was away have planned on making SnCl4, sodium(by electrolysis and thermit reactions), CHCl3 and a few other things. All I have actually done since I got back is KMno4 + glycerin because I found a little jar of KMnO4 in a drugstore during holidaying.

blip - 3-1-2004 at 13:48

If I were you, I'd save both metals in a noble gas atmosphere if possible and under lock and key, for making Grignard reagents in the future. I wouldn't be too thrilled if someone decided to burn it.

Probably the most exciting thing I did during these holidays was to burn some steel wool. I started out using Brillo, but used up most of my MEK dissolving away the soap. I dumped the saturated solutions on concrete, leaving a stubborn bright white stain from impurities (it was nothing more than nail polish remover). When I actually fluffed it up and burned it, I made sure I wasn't going to get hit by the sparks so I gloved and goggled up. When I looked closely, it was like red to yellow worms were crawling through the wire rather than points. I didn't set off any fireworks, but instead got some boric acid, steel wool without soap in it, and a bit of titanium.

The other chemistry related thing I did was to make chlorine to gas some algae and bugs. I had a lot of MnO2 left over from gutting out lantern batteries and HCl, so I mixed a lot of both together making sure I didn't get even a whiff. Too bad I did after about 30 minutes when I wasn't paying attention for a bit. It burned my nose some and that's when I quit. I considered trying steel wool and chlorine together, but it was much to windy to capture the latter in sufficient quantities and I wasn't about to try it indoors even in my shed. Not too exciting, eh?

hodges - 3-1-2004 at 14:48

Quote:

Originally posted by blip
I considered trying steel wool and chlorine together, but it was much to windy to capture the latter in sufficient quantities and I wasn't about to try it indoors even in my shed.

If you use fine steel wool, it will ignite spontaneously in chlorine, producing an orange cloud of smoke. If it is not fine enough, you can ignite it first and then lower into the chlorine for the same orange smoke. Do this outdoors of course!

Hodges

overseer - 4-1-2004 at 07:00

>Any ideas for interesting things (not necessary pyro) to do with the Mg and Ca?

You could try obtaining some Si through a simple, yet *dangerous* reduction procedure involving Mg:

SiO2 + 2Mg -> Si + 2MgO

You'll need 3 g SiO2 (quartz, sand), 2.4 g Mg-dust and some HCl 1:1. Since You have the ribbon, You'd have to do some shredding. In addition, You'd need: a larger test tube made of high-temp glass or a flask similar to the one in the Figure, a 250 ml beaker, a porcelain grinding bowl, some standard lab stuff and very good *dark* goggles.

Procedure:

A mixture of 3 g finely powdered SiO2 and 2.4 g Mg is put into the flask and mixed thoroughly with a glass rod. The flask is then mounted as shown in the Figure, and heated with a Bunsen burner. Initially, the whole mixture is heated, but later only the bottom of the flask, until the mixture begins to glow (sometimes it takes 2-3 mins). Upon ignition, the flame is removed, since the reaction proceeds vigorously, liberating much heat and with a strong flash of light.

Obtaining amorphous silicon in this manner creates also some Mg2Si, through a reaction between reduced Si and free Mg, at the high reaction temperature. After cooling, the reaction mixture is poured onto a suitable piece of paper (usually the flask has to be broken in the process) and is then added slowly, with mixing, into a beaker with HCl 1:1. After the MgO and Mg2Si have dissolved completely (which is indicated by the cessation of sparking, popping and development of white fumes over the acid surface), the dark residue in the bottom is amorphous Si. The reaction between MgO, Mg2Si and HCl involve the creation of silanes, that immediately ignite on contact with air and burn giving off SiO2 and H2O.

Finally, the liquid is poured off, and the residue washed several times with dilute HCl and finally with water. The amorphous Si dust is dried on 100 deg. Celsius. Do not heat it above the said temp. since it reacts on the surface with air oxygen, creating SiO2 again. It can be dissolved in HF acid with some HNO3 added.

This procedure is from an introductory inorganic preparative chemistry textbook. Again, it is very dangerous, so You're doing it at Your own risk! Don't do it unless You have enough experience. From my experience, many types of glass are prone to cracking when cooled from high temps, and some high-temp type glasses can crack with small pieces flying all around after even cooling in air, back to a room temperature, if it was red hot (goes esp. for thick wall vessels). The procedure should be done under the hood, so You should at least do it outdoors.

Obtaining_Si.jpg - 15kB

Sand and Mg

hodges - 4-1-2004 at 14:16

It is interesting that the Mg reacts with SiO2. I have seen in MSDS for Mg that one way to extinguish a Mg fire is with sand. Apparently if you dump sand over burning Mg, the Mg goes out. Perhaps the silicon reduction only occurs if both the Mg and Si are finely powdered and well mixed.

I also know that Mg fires should not be faught using water, because hydrogen is produced. However, apparently an excess of water will still put out a magnesium fire (though of course possibly producing enough H2 to be dangerous). I took a short piece of Mg ribbon and put one end in water and lit the other end. It went out upon reaching the water. I also tried burning a coiled piece of Mg ribbon that had just a drop of water in the center. It produced a finely divided ash (MgO I'm sure) which got blown into the air (probably by steam) and it took a couple minutes before the last bit of MgO "snow" fell out of the air because the ash was so fine and light. I did get a slight but definite NH3 smell that time(from magnesium nitride produced by burning in air, and the water).

Hodges

Al Koholic - 4-1-2004 at 15:29

Well, since my distillation thermometer broke a couple weeks back I wasn't able to proceed with a vacuum distillation of nitric acid from KNO3/H2SO4, and I decided to wait on making another batch of chloroform because I couldn't monitor the purification properly. I was also going to distill chloropicrin but....

All I managed to get around to doing was to oxidize naphthalene with a 5:1 KMnO4/naph ratio in boiling solution for 4 hours. I was faced with some interesting and forseen problems during the procedure like how to get the damn naphthalene back down into the flask from the condensation on the walls of the reflux condenser. I made a nice steam generator from a flask, stopper, and glass tubing that actually worked better than I thought it would. Could probably use it for a steam bath...

The experiment went ok and all but after the KMnO4 had dissipated (clear rxn mix) I suction filtered all the MnO2 off and kept the liquid which should have been mostly K2CO3, potassium phthalate, and water. I added enough 35% H2SO4 to make the solution fairly acidic and got alot of bubbling so I know the carbonate was decomposed and now I figure "ok, phthalic acid should precip much before the sulfate because of low solubility". So I boil it down and nothing precips...damn back to the drawing board. Unfortunately this next semester will be a bitch and a half so I might be waiting awhile before any MAJOR stuff happens other than passsive things like electrolysis....Overall a good holidays though!

unionised - 4-1-2004 at 15:41

The traditional solution is to stop the cooling water in the condenser until the naphthalene melts and runs back into the mix. (Or poke it with a stick).

Haggis - 4-1-2004 at 16:02

Distill Chloropicrin!?!

Wow. I hope you know what you can get yourself into, which you probably do, more than likely having dealt with the stuff before. Personally, I would rather not get it more volitile as it already is.

I also assume you have a resipirator of some sort. Is it simple charcoal filtration? Good luck though, and post the results in the Chloropicrin thread.

Al Koholic - 5-1-2004 at 08:02

Traditionally that is true. I ran some steam through the coils of the condenser for a brief time and it seemed to melt the naphthalene much quicker. Just turning off the water did let some fall back into the flask but also let more naphthalene get further up in the condenser...

The chloropicrin results will be posted don't worry! I have read a synth for guanidine starting from chloropicrin and ammonia/alcohol. Sure would be a nice OTC way.

[Edited on 5-1-2004 by Al Koholic]

blip - 5-1-2004 at 13:22

I've made Mg burn under water, but it took 6 bits with the last working. It flashed orange as it passed through the surface tension. More weird color flashes: Way back in chem class when we burned some, my group's flashed green upon ignition and I saw one flash purple on a chem video online.

My 100th post!

Silicone Oxide

Acid Test - 6-1-2004 at 12:37

Silicone Oxide is created from the fusion
of a silicone atom with oxygen.A great deal
of energy is required and no ameteur,novice
or general home lab would be able to produce
it.
A very high voltage is required(over 150,000)
and is created by normal sand clouds during
electical storms.
It can be created in a labratory with special
equiptment that is not accesable to any street
chemist.It is like trying to access a particle
accelerator or atom smasher.

Mumbles - 6-1-2004 at 17:55

And this has something to do with the topic how? This message goes to pretty much all your posts. Settle down, and quit posting garbage. Urinate in a jar full of Bleach to generate chlorine gas? All I have to say is, WTF. Chloramine maybe. Maybe even Hydrazine if you're lucky.

Acid Test - 7-1-2004 at 11:22

My posts are far off from being garbage.
Likewise Hydrazine will not be produced
from NaOCl and urea.
Hydrazine is NH2-NH2 and is a three step
synthesis procedure from human urea to remove
the cabon and then remove the oxygen bond
between the two NH2 structures.Then of course
NH2 must bond with NH2.
I don't think this is possable from urea.
I would stick to getting hydrazine from
ammonia

guaguanco - 7-1-2004 at 11:37

Quote:

Originally posted by Acid Test
My posts are far off from being garbage.
Likewise Hydrazine will not be produced
from NaOCl and urea.
Hydrazine is NH2-NH2 and is a three step
synthesis procedure from human urea to remove
the cabon and then remove the oxygen bond
between the two NH2 structures.Then of course
NH2 must bond with NH2.
I don't think this is possable from urea.
I would stick to getting hydrazine from
ammonia

Sorry, you're quite wrong:

hrdrazine synthesis 
hydrazine synthesis

[Edited on 7-1-2004 by guaguanco]

Acid Test - 7-1-2004 at 12:55

As i have pointed out in the HCl and Cl2
subcategory of this forum(read it)

Hydrazine is produced in this manner:

2NH3+NaOCl+heat=NH2-NH2+NaOH+Cl

The addition of chlorine gas is unnessecary
for the synthesis of hydrazine.It is complete
in the procedure.Chlorine will dissolve into
the mixture while it is being heated.
This will crystallize as Hydrazine Chlorate
in the NaOH solution.
The creation of dissolvable Hydrazine Salts
with acids is unnesecary.Chlorine is an
acid and will create a dissolvable salt

blip - 7-1-2004 at 23:11

OMFG, can you research more please and quit speculating all of the time; it's fine sometimes though. Yes, I did the same when I first came here, but then I made an effort to find really what mechanisms were driving things "behind the scenes". Admitting you're wrong is a very positive trait, especially for a scientist. I remember doing all of the above wrong when I thought that Na reacted with H2 in the Sodium! thread in the described conditions. Boy, I was quite embarrassed, and very sorry for pissing off Organikum.

Before NaOH and Cl2 produces chlorates, it first produces hypochlorites. Btw, chloramines will likely be produced (this is how I understand it currently, please correct me if I'm wrong somewhere):
NaOCl + H2O <s><</s> <s>  ></s>  HOCl + NaOH
NaCl + H2O <s><</s> <s>  ></s>  HCl + NaOH
HOCl + HCl <s><</s> <s>  ></s>  H2O + Cl2
Cl2 <s><</s> <s>  ></s>  2Cl*
NH3 + Cl* <s>  ></s> NH2* + HCl
NH2* + Cl* <s>  ></s> NH2Cl
NaOH + HCl <s>  ></s> NaCl + H2O
I think NH2Cl is less basic than ammonia because the electronegative chlorine atom pulls the lone pair closer to itself than that found in ammonia. This would make it less accessible to a proton. Because OH- is still left over from some NaOH, and amines are in equilibrium with water (NH2X + H2O <s><</s> <s>  ></s>  NH3X+ + OH- <tt>where X = Cl or H</tt>

, the residual OH- forces the equilibrium more to the left which favors products that can more easily go into the gas phase from aqueous. Hydrazine is also produced, but is very easily oxidized to less hydrogenated products eventually having nitrogen gas leave the system.

Acid Test - 8-1-2004 at 06:12

You are quite correct.
In fact NaCl+H2O requires a stronger
reaction procedure than normal heat.I think
that a current will do it.
You then draw off the HCl from the NaOH with
a glass baster

Acid Test - 8-1-2004 at 08:21

Thanks.. I was up all last night figuring out
certain hydrazine procedures and disproven
two.

I was referring to the equation NaCl+H2O as
a way of getting NaOH and HCl when there
is a need for it in the lab.

It requires the equiptment.I don't see a need
to add HCl to NaOH to make salt water.
It is pointless
To me it sounds like a job for God

Acid Test - 8-1-2004 at 08:54

Thanks but i was up all night working out
theory on synthesis of hydrazine,determining
authenticity.I went through 4 seperate
procedures plus my own which was:

NH2-CO-NH2 + NaClO = NH2-NH2 + CO + NaO + Cl

I don't see where chloramine is being produced
The brownish in the reacted solution is the CO
It has to be expelled.The NaO has to be removed
This requires precise reactions to extract
the NH2-NH2 before you crystalize it with an acid

It is a trick equation.It is obvious that
chloramine is not produced.If this were boiled
it would create HCON + NH3 + NaO which would
react with the Formamide.This is why the
CO has to be removed.THAT IS CRAP

Acid Test - 8-1-2004 at 09:54

CO is a colourless gas but when it is
dissolved in a liquid it is a brownish
tinge,especially in the presence of other
substances.
It is a known pollutant and it causes
asphykiation.
I would think my theory is correct
Chemistsss want you to think NaO doesn't
exist.

chemoleo - 8-1-2004 at 10:03

Acid Test, are you taking the piss out of everyone??

Do you test acid by placing a drop of it on the back of your tongue, just like you test acetaldehyde? The simplest and easiest test for sure

BromicAcid - 8-1-2004 at 10:15

From Hydrazine and it's derivatives Copyright 1985:

Quote:

Two different reactions have been proposed fro the conversion of urea into hydrazine with the aid of sodium hypochlorite. The older publications assume that N,N'-dichlorourea and para-urazine are formed as intermediate products.... "Most steps are currently believed to have semicarbazide as the intermediate product".... An N-chlorourea anion H2N-CO-N-Cl is believe to be an active intermediate in the reacation.

CO(NH2)2 + 2NaOCl ----> CO(NHCl)2 + 2NaOH

CO(NHCl)2 + 2NH3 ----> RING(-NH-NH-CO-NNH2-CO-) +H2SO4 ----> N2H4*H2SO4 + 2CO2

The urea processes can be used with the Bayer process using ketazines for seperation.

Acid Test - 8-1-2004 at 10:41

Chemleo-I test an acid by putting it on a piece
of cigarette foil.
I test for a base by diluting in 1ml of
water and dropping it on my tongue.It is
a surefire test.
KOH will tingle with a solid on contact.
I am not stupid.
Anything below KOH is probably strong.I wouldn't
Even attempt to test a solid OH below KOH without
diluting it.

Bromic Acid:
I did the Bayer-Whiff procedure last night
with a batch of my new procedure for
treating urine.I treat it with NaOH.Stand 24h.
Baste out liquid-NO PRECIPITATE-It contains
precursers for barbituric acid.The real
percipitate which forms 8 hrs later will smother
this just don't collect any precipitate.
(Optional-Treat with an alcohol of choice,besides pentyl alcohol)
Wash with Pentyl Alcohol or approriate solvent.
(Don'T use Naptha.Reserve this for clean
washing,not for removing waste out of urea.
Naptha can be reused for a period of time when
working with iso-lysergic acids from seeds)
Remove layers of waste with baster.
Add 2 oz of water and 1 oz of lemen juice
and shake
Liquid should be aqua clear
Put liquid in new flask.Add equal part NH3
Heat on med-low heat until mixture stops
giving ammonia smell.You should have 1/2
of what you started with.
Next cool down-and collect your thoughts and
perceptions because you'll need them.
Take 1 oz of this newly created urine and
simmer on med-low heat with a metal catalyst.
I used Al
When it is about to boil away stick your nose
over the pot.
A FAINT WHIFF OF AMMONIA
This is not excess from above procedures.
If you think this is so do another ounce.\
Smell at the begining of boiling...No NH3
I think this patent is a bogus
It is a patent for the manufacture of ammonia
for making hydrazine.

Acid Test - 8-1-2004 at 10:58

I have better things to do than impress
you.I have genuine scientific progress and
is not clandistine.
I have reported my procedures to proper
authorities,except for my isolates
Barbituric Acid is not illegal when sitting
in a jar.Sodium Pentanthol is not illegal.
So what
What are you going to do about it

BromicAcid - 8-1-2004 at 11:21

WTG are you talking about Acid Test. I don't care how respectable your work is and the progress you have made

, I have cited my source, Hydrazine and it's Derivatives, it is THE definitive reference for hydrazine and you claim that this reference work used by chemists in the hydrazine trade the world over is wrong on some fundamental level?

And why did you drag drug precursors into this?

Your ramblings amuse me highly but I am curious about the methodology here!

Do you even know about the Bayer procedure?

[Edited on 1/8/2004 by BromicAcid]

Acid Test - 8-1-2004 at 11:31

Sorry-I should of told you..I don't synthesize
urea.I am using my own bodily urine.
I am trying to slowly isolate NH2-CO-NH2
AFTER my work is complete.
Sweden is Scandanavia's major pharmaceutical
industry,and i am sure we have had enough
of peoples benzodiazepine trips,barbiturite
trips,and sedative/hypnotic trips.
I have reported my progress to Sweden with
logical and sensable science rhetorical about
theroetical use of my isolate from my urine.

chemoleo - 8-1-2004 at 11:45

OMG, take a break Acidtest, I think we are all losing any appreciation for your 'jokes'. :mad:

PS sigh... so many threads now with random stuff/crap in it.... how can anyone keep track?

[Edited on 8-1-2004 by chemoleo]

Mumbles - 8-1-2004 at 15:43

What might this nomenclature be for this ellusive NaO? The only way you are going to get away with it is if you are writing the reduced(empirical I think) formula of Na2O2.

HCON is Fulminic Acid/Cyanic Acid/Isocyanic acid. Well, the combonation can me at least. I can't find anything with that specific geometry though.