Home Made Glow Stick

[Alexein]

ok... not exactly a "stick" its more of a vial... but it demonstrates chemiluminescence.

 

Recipie is quite straightforward: Start with Diethyl Phthalate, add bis(2,4,6-trichlorophenyl) oxalate "TCPO", stir in some hydrogen peroxide, a bit of sodium acetate to improve the effect of the peroxide and a dash of bis(phenyethynyl)anthracene for color.

 

First picture is the vial with the flash on, the second picture is the vial with the flash off. Its hard to see, but those "rocks" in the bottom are actually pure crystals of TCPO. if you look closely, you can tell its not the crystals that are growing, but the surface as the crystals dissolve and react with the peroxide. It doesn't look like much, but there is enough in there to give a week of useful light, and a month of detectable light.

 

third and fourth pictures use 9,10-diphenylanthracene for blue color. I like the last picture the most since you can clearly see the crystals and the "glow layer" as they dissolve.

 

making TCPO was the hard part and not something i reccomend for those without proper fumehooded labs.

[Gilded]

Awesome! I've always wanted to do something like that but as noted stuff like TCPO or luminol isn't exactly easy to make at home.

[Alexein]

Awesome! I've always wanted to do something like that but as noted stuff like TCPO or luminol isn't exactly easy to make at home.

 

Yeah, that always seems to be the bottleneck for most amateurs. I'm thinking of making a sizeable batch of TCPO and selling it online. the other chemicals for the reaction are relatively easy to come by. heck you could just crack open a used glow-stick and revive it by adding the TCPO.

[Alexein]

Here is a video of the actual TCPO crystals and their use.

 

http://www.youtube.com/watch?v=cVQ9jjdU0l8

[science_nerd]

I too was searching to make my own glow sticks. Here is what I found from this glow sticks site under their FAQ section.

 

4 g Sodium Carbonate

0.2 g Luminol

0.5 g Ammonium Carbonate

0.4 g Copper Sulfate Pentahydrate

approx. 1 litre of Distilled Water

50 ml of 3% Hydrogen Peroxide

 

Has anyone tried using the above stuff?

[Alexein]

yeah, gives a nice blue glow for about 30 seconds. In my opinion it doesn't last long enough to be a worthwhile light source.

 

luminol is more useful for forensics.

 

Personally, i think you're better off using Peroxylate chemiluminescence. The website is outdated, glowsticks exclusively use peroxylates.

Edited December 4, 2008 by Alexein

[Victoria]

I don't think my husband would appreciate me giving this one a go...

 

 

How long would that glow before needing more TCPO?

[Sayonara]

The website is outdated, glowsticks exclusively use peroxylates.

That's a shame, because it looks like Science_nerd joined us exclusively to stealth-spam links to that site

[Alexein]

I don't think my husband would appreciate me giving this one a go...

 

 

How long would that glow before needing more TCPO?

 

The vials at the beginning of the post give a week of useful light and another two to three weeks of detectable light (depends on the initial quality of the reagents). The dish in the video gives only about 10 minutes of light.

 

The huge difference arises from the solvents. The TCPO is not very stable in ethyl acetate. But has excellent stability in diethyl phthalate which is what the vials used.

 

 

 

That's a shame, because it looks like Science_nerd joined us exclusively to stealth-spam links to that site

 

Yeah, if you're going to stealth-spam at least spam with useful info.

[hermanntrude]

do you have details for the synthesis of TCPO? I can make TCP or buy it and i have oxalic acid... would those be good starting materials?

[UC]

Oxalic acid simply doesn't work here, or a lot more people would have made this stuff by now.

 

Quoting Alexein from his post on sciencemadness.org:

 

"Start with 2,4,6-trichlorophenol and dissolve it in dry toluene or dry dichloromethane. "wet" solvents are ok but the yield will be reduced. Add one molar equivalent of a suitable organic base. I used triethylamine. stir until everything is dissolved.

 

chill the solution with ice and add in SLOWLY 0.5 mol equivalents of oxalyl chloride. Its going to heat up.... ALOT... so keep it stirring and chilled.

 

Once its all added remove the ice and let it warm to room temperature with continous stirring. I find purity increases if you let it stir overnight.

 

The TCPO is a fine white powder mixed with triethylamine hydrohloride at this point. Suction filter the mixture and keep the suction on to dry out the powder. Discard the filtrate.

 

pour water directly onto the white powder and wash out the triethylamine hydrochloride. Dry the powder again.

 

The powder is TCPO, its still pretty impure but usable. If you want nice big pure crystals (like the ones in the picture) you can dissolve TCPO in tetrahydrofuran, filter, and recrystalize. "

[Alexein]

What he said

[hermanntrude]

is diethyl phthalate your solvent for the vials above?

[Alexein]

Yes it is. And i highly reccomend getting it if you want a nice long-lasting glow.

[nitric]

are there any other usable solvents since diethyl phthalate is not a everyday common solvent or easily made

[UC]

bis-(2-ethylhexyl) phthalate (common PVC plasticizer) should work as well. Alkyl benzoates as well, I assume.

Edited February 13, 2009 by UC

[hermanntrude]

these are all cheap materials. I might try this one day. After the end of the financial year :0)

[Alexein]

are there any other usable solvents since diethyl phthalate is not a everyday common solvent or easily made

 

most dialkyl phthalates (of which diethyl phthalate is a member) will work.

 

ethyl acetate also works. but that glow lasts for about 2-10 minutes.

 

If you can't get your hands on a dialkyl phthalate i don't reccomend expending the effort on getting the other materials. TCPO is expensive, even if you make it yourself, and not using a good solvent is like buying a sports car and never driving it.

[Alexein]

I made some of my glow stick experimenst into videos:

 

<--- Simple reaction in a vial

 

<--- Scaled up to two LITERS

 

<--- Complete assembly of a glow stick

[yahz]

im a bit out of my league. are there more common ingredients that can be used safely?

[myztic_man]

Very impressive. With some fine tuning, and some sealed plastic casing you could begin competing with the likes of GlowSticks LTD!