Preparation of Hydrazine Sulfate by the Hypochlorite Ketazine Method

[sciencenurd2]

So thanks to the description. You are planning to make luminol with it. Yes?

[hkparker]

@sciencenurd2 I was planning on it, but I ran out of time before I had to go to college. Perhaps over the summer or in a few years.

[andreh4eva]

what is that thing you use as vacuum pump?

[hkparker]

@andreh4eva Its a hand pump that came with my vacuum filter kit.

[ConorC96]

Where did you get your lab apparatus?

[hkparker]

@ConorC96 see my video on that

[ConorC96]

I think to get a higher yield, you should increase the amount of Bleach, Ammonia, and MEK. Also, the amount of Sulfuric Acid and water.

[98JMA]

@ConorC96

That is obvious - more reactants = more average product.

[macbeth41science]

Only 2 grams? what happened? Good luck with the project!

[hkparker]

@macbeth41science I wasn't disappointed with my yield. I probably could have gotten more if I refiltered my filtrate after heating again, as a bit more HS did precipitate days later, but eh, like I said the chemicals were cheap. I only need mg of HS anyway. Thanks about the project, but I've ran into a large complication and will not be able to complete in the foreseeable future :(. A video soon will explain it.

[HackSilent]

Great video!

[hkparker]

@HackSilent Thank you!

[TakronRust]

One thing I found when separating the layers. Adding NaCl to it will speed up the process of separation as my first batch didnt really separate much until I changed the density. Then it separated very quickly.

[hkparker]

@TakronRust good to know, thank you

[AlChemicalLife]

when i make phthalic anhydride i boiled it for 1hr 55m and it didnt work to well. d ou know y

[hkparker]

@AlChemicalLife ...what?

[AlChemicalLife]

@hkparker when im makeing phthalic anhydride i get a crapy amount to no amount of it and i dont know y. i refluxed it for 1hr 55m but it wont give me a good yeild

[hkparker]

@AlChemicalLife reflux? You mean you were trying to decompose phthalic acid to the anhydride and collect it like NurdRage did? Your heat source probably doesnt get hot enough.

[Aranwu]

lol your hint "I just cut up a ton of vinyl gloves..." made me smile :)

I've tried it and found out that acetone ain't a good choice in performing the extraction of phthalates from the gloves, hot acetone , or even at room temp. will dissolve the PVC in the gloves making it really hard to hydrolysing it to sodium phthalate as when i poored in the solution of NaOH tons of crap precipate out and as the solution cooled a lot of pvc precipate out as well

[hkparker]

@Aranwu Good to know. The common way is to use isopropanol. Ive extracted from 400 grams of gloves that way with a ton of success. Some pvc did dissolve but it was removed with filtering.

[Aranwu]

@hkparker

yes i know that the common way is to use isopropanol, :) i was out of that alcohol so i wanted to try with acetone. looks like your going far , 400 grams :) I've only done about 100 grams, but haven't converted the acid into the anhydried yet as i haven't much lucky with the nurdrage method, it pretty tricky hope you show a nice method

[hkparker]

@Aranwu How well did your acid precipitate? I have had the hardest time getting it to precipitate with the NurdRage method.

[Aranwu]

@hkparker

haven't weight it and i don't think i will be doing it , im coverting it into anhydride as we speak , i've retried his method , the key is patience ,. but when they acid was dried i think i would have got about 10 grams (approximatly) and i only used up about 5 gloves about 6 grams for each gloves. i will let you know how much anhydride i will get tonight

[911Rstar]

Oh i think

3-aminopthalhydrazide

[AlChemicalLife]

luminol it is

[XAtom1c]

For extraction of DEHP I refluxed for three hours.

[aaronjhard]

Great video ,,

[lexichronicle2]

Great work and thanks for the video!

[chemicalbombgang]

ur makin luminol right ??????????

[hkparker]

@chemicalbombgang yea...

[MrTechGuy1995]

@chemicalbombgang Thanks eagle eyes!

[g3ov4n12]

when you have to measure something always check in the height of the eyes, to check the meniscus.

[coolliger]

"if you wanna go pro" haha, great quote

nice video

[hkparker]

@coolliger haha, yea, thanks

[Aranwu]

Good work :)

[hkparker]

@Aranwu Thank you :)

[Kendrana]

Good to see it finally works! :P

So finally starting on luminol eh? :D

[hkparker]

@Kendrana yep! Today I got to the production of phthallic acid, but cant get it to crystallize :(! Well, time to boil down and add more HCl...

[spotlightman1234]

@hkparker me too i'm having the exact same problem :(

[hkparker]

@spotlightman1234 really? Good to know! I'm thinking either I didn't boil it with NaOH long enough or I'm just too diluted. Tomorrow I will find out. Tell me about your procedure, how long did you boil with NaOH with?

[spotlightman1234]

@hkparker ya I probablly didn't get enough diethylhexyl phthalate out of the gloves when I refluxed them. I relfuxed the diethylhexyl phthalate with NaOH for and hour and a half. I didn't get much of an upper alcohol layer so maybe I didn't boil it long enough or who knows. I'm going to try again but use more alcohol and boil the gloves in alcohol for longer.

[hkparker]

@spotlightman1234 huh, my gloves were nice and brittle, and I got a decent amount of alcohol. I would check every couple of minutes and the layer stopped getting visibly bigger. I will let you know the results of tomorrow.

[spotlightman1234]

@hkparker good luck, my best decision would be to boil it a bit more to concentrate it and boil it with NaOH for longer.

[hkparker]

@spotlightman1234 Ok, I boiled it down and added HCl. Recrystallized again and got more product but... not much. I will soon be doing this again but get the reactions last very long. Extract for an hour and a half or 2. Boil with NaOH for over an hour.

[spotlightman1234]

@hkparker hmm longer boiling seems like the way to go. good luck, hope you get it to work.

[hkparker]

@spotlightman1234 best of luck to you as well.