Luminous solution...

[Rusl]

Whether somebody did(made) experiences and knows recipes of preparation of a solution luminous in darkness? Help please! Also it is desirable, that the solution shined during long time. Beforehand I than.

(MORON! What the FUCK does this have to do with High EXPLOSIVES?! NOTHING! Moving topic, deleting user.

PS. Hadn't noticed this at first, but you also posted this in the misc section too. DOUBLE POSTING! http://theforum.virtualave.net/ubb/smilies/mad.gif ASSHOLE! NBK2000)

[This message has been edited by nbk2000 (edited July 18, 2001).]

[Rhadon]

Since luminescent solutions aren't high explosives you're in the wrong section :-)
Though, to answer you question: It's quite hard to make phosphorescent compounds or things like that from chemicals that are easy to get. But you could buy luminol from a chemical supplier. Add H2O2 to it and you'll get a nice chemiluminescence.

[deezs]

Luminescence. Interesting topic.
Needs hardly avaliable chemicals.
I know diferent methods. I'm too lazy to translate them now. I write down the luminous chemicals I know, if you can get them, I will write the recipes.

a.)
luminol (5-aminophthalhydrazide)
A fuckin expensive indicator, in Hungary(Eastern-Europe), 5 grams costs about 25 dollars. (Not mistyped! It's in the prize of gold) Btw. I know, how to syntesise it. You can find it in this book:
Louis F. Fieser: Organic experiments 1956 Raytheon Education Company, Lexington, Massachusetts (chapter 45)
to this synthesis you will need:
1g 3-nitro-ftalic acid
3 cm3 8% hidrazine solution
3 cm3 triethylenglicol
3g NaHSO3.2H2O
the yield will be about .5g This way you can get it far cheeper.
This will really produce light in the dark.

b.)
lucigenin
I don't know much about this one, just this is an other indicator. It produces blue light, by which you can even read for about 10-15 minutes.

c.)
pirogallol (don't know if it is it's correct name)
It produces red light for 5-6 minutes, then the folution will become hot, and sometimes it comes out from the erlenmeyer flask.
I haven't foud the synthesis yet.

d.)
fluorescein (C20H12O5)
red crystals with green iridescence
Made by heating phtalic anhydride with resorcinol. In alkaline solution it shows intense green fluorescence. It is used for determining the route of water supplies, leakages. This will not light in the dark, but if light falls on it, it has a nice color
(I have made only this one. Yet.)

e.)
an inorganic fluorescens compound
s
CaO
Na2SO4
Na2BO7.10H2O (borax)
CaF
Bi(NO3)3

f.)
white phosphorous

g.)
troboluminescens compound:
ZnS
MnSO4
This one produces light, when you rub it with a glass rod.

h.)
The easiest:
ZnS is said to be luminescens too, when it contains some CuS.
To make this, dissolve ZnSO4 in water, add a few drops of CuSO4 solution, and (NH4)2S, or Na2S.

As you see, if you need a luminous solution, for practical use (instead of flaslight), you have better to buy it.



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"Don't belive anything, just because there is a good proverb for it."

[Rusl]

Yes, at me all chemical substances are and luminol, except for lucigenin. Send please, all recipes on luminescence and synthesis luminol. Mine e-mail: rusl@uni.udm.ru. Beforehand I thank!

[deezs]

I post my answer here too, if someone else is interested in the topic. I know the mods and the frequent posters doesn't like topics, which are not about explosives, or it's precursors. But I belive, who loves explosives, that likes interesting chemical experiments too.

LUMINOL SYNTHESIS


In a big test tube (20x150 mm) heat 1g 3-nitro-phtalic acid and 2 cm3 8% hidrazin solution, till the solid material dissolves. Add 3 cm3 triethylen-glycol, and fix the test tube in a vertical position above the flame. Insert a thermomether, and a glass tube, which is connected to a vacumpump. Boil the solution (110-130 deg. C), and distill the water down. Let the temperature rise fast (in 3-4 minutes) to 215 deg. C. Take away the flame under the test tube, check the time, and for 2 minutes hold the temperature between 215 and 220 deg. C with heating occasionally. Take out the suction pipe, and allow the liquid to cool down to 100 deg. C. (sometimes crystals of the product precipitate) Bring 15cm3 dest. water to boil, and add to the solution. Cool it down under the tap, and filter the yellow product.
The dry weight of the product should be about 2,7g, but you needn't dry it.
Put the yellow crystals to the test tube (don't wash it after the first reaction). Add 5 cm3 10% NaOH solution, and 3g NaHSO3.2H2O. Boil the solution for 5 minutes (somethimes the product precipitates). Add 2 cm3 acetic acid, cool under the tap, and filter out the luminol. Let the liquid stand for the night, next morning an other fraction of crystals (.1-.2g)should precipitate.
The dry weight of the first precipitated luminol should be about .2-.3g. Dissolve this in 10 cm3 10% NaOH solution, and add 90 cm3 water. This is A solution.
B solution: mix 20 cm3 3% K3[Fe(CN)6] solution with 20 cm3 3% H2O2 and 160 cm3 water.
To 25cm3 A solution add 175 cm3 water, and in a drak place pour this solution with B solution to a big erlenmeyer flask. Shake the flask, and add some lye to increase the brillance.
fom Louis F. Fieser: Organic Experiments, translated by deezs
now I'm bored with translation.
Are you interested in the other compounds(b,c,d,e,g) too? Perhaps tomorrow I post the other experiments too.


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"Don't belive anything, just because there is a good proverb for it."

[deezs]

here are the other recipes:

Lucigenin
In a big erlenmeyer flask to 50 cm3 dest water add 4-5 cm3 NaOH solution, 2-3 cm3 0.05% lucigenin solution, and 3-4 cm3 H2O2. Shake the flask, and add 40-50 cm3 ethanol. The liquid starts to produce turquoise blue light, for about 10-15 minutes. You can even read by this light.
lucigenin: dimethyl-diacridilium-nitrate
If you can draw the structure of this molecule, please send it.
(I think this is an acridine derivative. Acridin looks like antracene, just in the central ring there is a nitrogen, in stead of a carbon.)

pirogallol
In a 200 cm3 erlenmeyer flask add 10 cm3 boiled, and cooled dest water. In this dissolve 1 g pirogallol. To this add 20 cm3 40% K2CO3 solution and 10 cm3 40% HCHO solution. Shake the flask, and add 30 cm3 30% H2O2. The liquid starts to produce red light, for 1-2 minutes it becomes lighter and lighter. It ends after 4-5 minutes. After the reaction the liquid becomes hot, and starts to foam. Then add some water, to stop the reaction.
pirogallol is 1,2,3-trihidroxy-benzene

fluorescein
In a dry test tube mix 0.3g phtalic anhydride and 0.4g resorcinol (1,3-dihydroxy-benzene). Add 5 drops of concentrated sulphuric acid. Heat it above a small flame, till you get dark brown liquid. After it cools down add to it 1 cm3 NH3 solution, and pour it to 1 liter water. It produces yellowish-green fluorescence.
warning! Don't use more sulphuric acid, because it will corrode the paint, formed in the reaction.
0,1 mg fluorescein in 1 l water is still yellowish. It is used for determining the route of water supplies, leakages.
If you need the structure, I can draw it.

inorganic compound
Mix 5g CaO with 4g S, and heat it in a covered porcelain melting pot for 10-15 minutes. To the cooled compound add 0.5g Na2SO4, 0.54g Na2B4O7.10H2O 0.2g CaF2 and 1.5 cm3 Bi(NO3)3 solution. (preparing of the solution: dissolve 0,25g Bi(NO3)3 in 50 cm3 ethanol, and add concentrated hydrochloric acid, till the solution becomes clear) Mix it well, cover the melting pot and heat over a hot flame for 25-30 minutes. In a dark place light the cooled compound with UV light. If it not produces any light, you need hotter flame, perhaps a blow torch.

triboluminescens compound
Mix 5g ZnS with 1g MnSO4 or MnCO3, and heat in a melting pot for 25-30 minutes over a very hot flame. (or in a melting pot oven) After it cooled down, suspend in some water, and filter out the precipitation. Dry it on 120-150 deg C. In a porcelain mortar rub it with a glass stirring rod. It will produce light. Don't know the clour.


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"Don't belive anything, just because there is a good proverb for it."

[Mr Cool]

I've got a good method, but it's a little messy http://theforum.virtualave.net/ubb/smilies/wink.gif
You will need:

A kilo of fireflies,
A big glass beaker,
A drill,
Some thick wire.

Bend the wire into a T-shape, and fix it into the drill. Put the fireflies into the beaker, put in the wire and turn on the drill! This will make a glowing green paste, which is also a great salad dressing http://theforum.virtualave.net/ubb/smilies/smile.gif
Actually, one (Polynesian?) tribe did/does collect luminescent crustaceans from the sea and crush them to use as blue glowing face-paint for rituals etc. It glowed bright blue for quite a long time.

That triboluminescent compound sounds interesting. Rubies will flash bright red if you hit them with a hammer, quartz also emits greenish light when banged hard.
That luminol experiment also needs to have the correct pH. I have a recipe somewhere... no, I've looked and I've deleted it. I do remember that ammonium carbonate is added to raise the pH.

It's easy to grow a culture of Photobacterium Luminescens (sp of last word?). Get a fresh, salt-water fish and suspend it in a jar of cold, boiled sea water so that half the (dead) fish is submerged. After a week in the fridge, to slow the growth of other bacteria, take it into a dark room. When your eyes have adjusted, you should see lots of little colonies of glowing bateria. You can grow these in a salt-water medium with added nutrients. If you have it in a sealed, narrow glass tube then the glowing will stop after a few hours or so since the bacteria aren't getting any oxygen. Invert the tube, and the air bubble at the top will flow throught the culture, causing a burst of green light. A 250mL flask of an active culture is easily enough to read by.

[-A-]

hey mr cool, but in what places and climates do this bacteria grows??? it sound like a cool bio-chemistry experiment...

[nbk2000]

Want to try something really fun?

Get a sample of rewd tide plankton, culture that, and expose live clams to the water. Process the clam livers to extract the toxin, and voila!

You're now the proud possesor of saxitoxin, a paralytic nuerotoxin that kills it's victims in less than a minute, with blood pouring out of every orfice. Looks like ebola. And it only takes a milligram or two.

Was developed for the CIA microinoculator gun.

There's some other toxic critter in the gulf waters that causes skin sores and permanent memory loss. It's airborne too. http://theforum.virtualave.net/ubb/smilies/smile.gif

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"The knowledge that they fear is a weapon to be used against them"

Go here (http://members.nbci.com/angelo_444/dload.html) to download the NBK2000 website PDF.

Go here (http://briefcase.yahoo.com/nbk2k) to download the NBK2000 videos.

[-A-]

And that "critter" is...Pfiesteria Piscicida.

[This message has been edited by nbk2000 (edited July 29, 2001).]

[Gab]

Apparently, you can have "always on" fireflies if you give them nitric oxide.

More info at <a href="http://news.bbc.co.uk/hi/english/sci/tech/newsid_1412000/1412104.stm">http://news.bbc.co.uk/hi/english/sci/tech/newsid_1412000/1412104.stm</a>

[deezs]

Back to inorganic luminescence!
I have found the following recipe:
Pour saturated NaCl solution into a test tube, untill it is half full. Add ccHCl by the wall of the test tube, till it is almost full. Insert a rubber stopper, and go to a dark place. Shake it. It should produce blue light.
I don't know, why, or how should this work. I have tried it, but no sucess. Any idea?


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"Don't belive anything, just because there is a good proverb for it."

"To avoid injury in a battle, watch them from the nearer hill."

[Tony Montana]

Heres a good link:
http://www.deakin.edu.au/~swlewis/mlg.htm

[deezs]

Good page, with nice pics, but contains no recipes.
Anyway thanx!

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"Don't belive anything, just because there is a good proverb for it."

"To avoid injury in a battle, watch them from the nearer hill."

[Tony Montana]

No recipes???
Did you look:
http://www.deakin.edu.au/~swlewis/prop.htm
http://www.deakin.edu.au/~swlewis/2000_CL_demo.PDF
http://www.shsu.edu/~chm_tgc/chemilumdir/chemiluminescence2.html
All linked from the same page, showing mainly luminol reactions. Guess some people are just hard to please, here, this one is not about luminating chemicals but I promise it will impress the tuffest critics:
http://members.optusnet.com.au/~hand/montana/
More quality links brought to you by Tony The King Of Kewl Montana http://theforum.virtualave.net/ubb/smilies/wink.gif

[Mr Cool]

-A-: the bacteria grows in many places, possibly ALL saltwater. I know it grows in the Atlantic, since I've got some from the West coast of England. No warm, tropical waters there!

[Boob Raider]

I was able to order Vibrio fischeri from carolina but they don't have V. phosphoreum or dinoflagellates etc. Anyways I am going fishing ..... again .... soon :rolleyes: .
Can Xylene be oxidized by K persulfate to Phthalic acid, I know KMnO4 does in an H+ soln, but I can't get that :( . Does anyone have any recipies on nitrating phthalic acid on the 3rd Carbon and what function does the triethylene glycol serve, can it be subsituted by something commonly available.

[Marvin]

One of my favourate subjects is chemiluminescence. Several places in the US sell dinoflagilates, I havnt found anyone here yet though. Produce light only when shaken and only at night, they photosynthesize during the day and they need sterile conditions to last more than a few weeks at home. One of the confusing aspects of the literiture on this is that the light producing molecules of all biologicals is called 'luciferin' regardless of its structure.

Pthalic acid nitrites very easily, and care must be taken so it doesnt get out of control, the 3 product is the majority one usually. I dont have this information to hand becuase my chosen synthesis was from napthalene to a-nitronapthalene, to 3-nitropthallic acid. If its a nitro group on the napthalene its the oppasit ring thats broken by oxidation, if its reduced to amine first, the amine ring is the one that goes. I wasnt able to find a reasonable method for making hydrazine hydrate though, so I never finished the attempt. The synth Id use from there is the huntress et al method, which currently isnt to hand either though digging up just the reference details I can do tomorrow. I was working on this some time ago, so the information will be buiried.

30% peroxide and conc hyperchlorite solution when mixed produces volumes of oxygen in the singlet excited state. This forms an excited dimer (A true eximer, unlike so called eximer lasers) which decays in releasing deep red light. NIR side of visible Red. Ive tried this with 6% hydrogen peroxide and 5% hyperchlorite bleach with about 10min dark adapted eyes and saw nothing at all, but Ive talked to people that have done it with proper reagents and confirm it does work. The reaction might be a tad violent, Ive read a safer method is to bubble chlorine into alkaline peroxide solution.

Luminol should be able to be made pretty cheaply with some effort, the oxalate esters are rather more spectacular and should be synthasisable in an advanced home lab, they also have spectacular street prices. I seem to recall another thread with slightly more information on those.

[irish]

Mr cool wrote
"That triboluminescent compound sounds interesting. Rubies will flash bright red if you hit them with a hammer, quartz also emits greenish light when banged hard"

quartz also flashes orange, red or yellow, some bits don't display it as well as others. I have a small shappire mine on my land and it looks good belting a pick thro hard packed quartz and gravel under ground.
I've never found a use for this property of quartz but it is pretty :D .

[Mr Cool]

Maybe we'll find a use one day, Irish :) .
Marvin, I've seen a photo of chlorine being bubbled through strong hydrogen peroxide solution on the web somewhere, and it looked quite bright. But perhaps special camers were used.

[Rhadon]

Mr. Cool, chlorine being bubbled through a solution of NaOH in H2O2 gives a nice red luminescence when the chlorine comes into contact with the liquid. This is due to the formation of singlet oxygen. I tried it, and it works really well. Perhaps that is what you're referring to?

[Leadazide]

Deezs said
"c.) pirogallol (don't know if it is it's correct name)"

The correct name is pyrogallol.

[rooster]

Rhadon: do you have any ratios/concentrations of your method with H2O2, NaOH and Cl2? Sounds very interesting, especially since the precursors are so easily available.

[Rhadon]

No, I don't have any ratios at hand. Perhaps a search on the web will yield some results, but the reaction shouldn't be that sensitive to the amounts used. IIRC, I did just add an excess of NaOH (it didn't dissolve completely) to 30% H2O2 and bubble chlorine through the solution.

[a_bab]

Just found a link here (http://www.pc.chemie.uni-siegen.de/pci/versuche/english/v27-3.html) with the ratios and pictures.

[Marvin]

Looks good but the last part of the explanation is wrong. The energy for 1 molecule in the singlet excited state produced by this reaction is equivalent to a line in the IR spectrum. Normally singlet to singlet transitions are fast, but this particular transition is highly forbidden for electric dipole interactions, you only get a weak line in the IR due to magnetic dipole interactions. The result is you get a high enough population of excited molecules, that eximers form. When a complex of 2 singlet oxygen molecules loses all the energy in 1 transition, you get the red light.