> chemistry > organiques-simples > hydrazine > synthesis-of-hydrazine-sulfate-part-1-uc235

Synthesis of Hydrazine Sulfate: Part 1

UC235 - 2011-02-28

Hydrazine sulfate is prepared from readily available chemicals using the Hofmann rearrangement. Workup of the product is designed to prevent exposure to toxic hydrazine fumes, an important consideration for the amateur experimenter lacking a fume hood. The mechanism of the Hofmann rearrangement is also discussed. The intro music clip is from "Stealing Fat" by The Dust Brothers. I believe this falls under fair use.

UC235 - 2012-01-23

@RatkoUSA I usually use the convect setting at ~130C to dry the glass in a short amount of time.

UC235 - 2011-03-21

@TakronRust I take good care of my equipment. It wasn't free. Also, especially with organic chem, sometimes small traces of contaminants can mess up a reaction so you get used to cleaning everything very thoroughly.

Sterlingjob - 2013-08-21

Its like watching Jamie Oliver!!

UC235 - 2011-03-21

@ConorC96 MEK is easy to find in the hardware stores where I live. I'd go with dye additive urea for the most pure material, though it certainly isn't reagent grade.

NurdRage - 2011-02-28

Nicely done!

Joe Anderson - Wales, UK - 2012-02-09

@ChemCrazy81 Try it and tell us!

UC235 - 2011-04-13

@g3ov4n12 I only heated after mixing the two solutions and the foam subsided. The color change indicates the reaction progress and it will not go colorless without heating nearly to boiling.

Elyjah Vasquez - 2016-08-18

+UC235 Where've you been, man?

AzureFeldspar - 2013-01-14

Ok thanks

hkparker - 2011-03-02

Great job!

UC235 - 2011-03-21

@NADHHH 1) Biuret may lower yield; I don't know. Biuret has much lower water solubility than urea, though they may act differently when mixed. Prepare the solution with excess urea and more water and filter any solid. 2) Don't use oxalate. Sodium oxalate is poorly soluble and may precipitate causing problems. If you have EDTA or a salt of it, use that. If not, stick to gelatin. 3)Stirring when mixing the solutions is critical. After, heating almost to boiling to finish the reaction is necessary.

coxox iowery - 2013-10-10

one taing i like to no how do it work if it evaporated

Kowboy USA - 2012-01-23

@UC235 Do you cook your glassware in the oven after cleaning? I've found that doing so for approximately 30 minutes at 450-475 degrees removes most traces of contaminants and water left behind from the washing process.

acidum984 - 2011-02-28

Eagerly waiting for part 2 and aftermath of entire process! So far nice work. (as usually)

UC235 - 2013-01-14

Aliens.

TheMaDMAli - 2011-03-02

hahaha you reffed, sciencemadness, biggup

Jacky Ly - 2011-03-27

@UC235 Any useful tips on how to clean the glassware thoroughly? :D

UC235 - 2011-03-05

@ConorC96 Fertilizer, certain instant cold packs (others are ammonium nitrate), and it is sold as an additive for applying certain types of dyes to fabrics. The latter two sources will likely give you a more pure starting material. I use urea sold as a dye additive. When melted, it became somewhat brown indicating that it wasn't totally pure. I recrystallized it from mixed denatured alcohol and water (with significant loss, but it is cheap) and it no longer discolors when melted.

hongkongsmartboy - 2012-07-21

Superacids

mark wellman - 2014-07-29

@UC235, If you used Calcium Hydroxide in place of Sodium hydroxide; would reaction yield increase?

Blackline - 2015-12-06

+mark wellman I don't think so, this is not solluble in water.

ziane bouzekri - 2019-07-26

N2 H5 oh or no

ConorC96 - 2011-03-06

Also, how do you get the ethyl methyl ketone?

ConorC96 - 2011-03-06

@UC235 Which gives you the most pure urea?

ChemCrazy81 - 2011-05-10

Can you mix the MEK directly with the urea and then add the hypochlorite like in the ketazine process?

ConorC96 - 2011-03-05

Where can you come by the urea

UC235 - 2013-01-14

It is possible to make concentrated NaOCl solutions from calcium hypochlorite and sodium hydroxide solutions. The calcium hydroxide is filtered off. Calcium hypochlorite typically is only sold as ~60% blended with calcium hydroxide and byproduct calcium chloride. It doesn't form a solution, so much as a gloppy suspension, and I think that with the gas evolution in the reaction, you'd have a huge mess on your hands.

Maanuve - 2016-03-24

Why is it so toxic? Can you explain some chemistry in the body?

spiffinz - 2018-02-10

Maanuve https://youtu.be/N2e_-KAJHqE

AzureFeldspar - 2013-01-14

Can one use an equivalent amount of calcium hypochlorite instead of the 12.5% sodium hypochlorite? (12.5% sodium hypochlorite is hard to find in my area and I lack the apparatus to make my own but I have calcium hypochlorite)

Scott S. - 2019-10-08

I wonder if he passed away.

UC235 - 2019-10-19

Nope. Life situation changes and I get more than enough lab time at work.

g3ov4n12 - 2011-04-11

I dont got it, why you heated when you were pouring the hypochlorite/hydroxide?

TakronRust - 2011-03-03

Your glassware looks immaculate. It doesn't look like it's ever been used. lol

gunthreadadapters.com - 2013-01-21

Am I the only one who thinks he sounds like Kermit The Frog got 10 years older and does Science now?

robson melo - 2018-08-14

Cool. Please. How can I produce a hydrazine solution from hydrazine sulfate?

VMan - 2013-05-31

I'm sorry but could you write the names of reagents and in what order they should confuse the issue with the translation (I'll understand more on video) Sorry my English)))))))))))))))