@vmelkon I don't know. In fact, I recently discovered that the company (Kleanstrip) producing the only MEK I can find in my area has discontinued the product. I went out and searched hardware stores for any remaining cans. I could only find a gallon can that was kind of beaten up. I bought it anyway, and it was fortunately discounted significantly. Also very nice is that the replacement product is pure ethyl acetate.
@g3ov4n12 Because the impurities may be insoluble in absolute ethanol and if they precipitate and get caught on the product, what good does washing it do for me? Hydrazine sulfate is not that soluble in ice water so I'm not losing much. That's how washing works, generally. You trade a little yield for improved purity.
I have made hydrazine also by mixing H2O2 and ammonia in a stainless steel mug. I believe the mug had nickel in it which serves as a catalyst. Now you're probably wonering how i new it was hydrazine right? I knew it was hydrazine because when mixed with Cu(II)SO4 it formed a dark brown ppt instead of a dark blue Cu(II) amine complex. I think the dark brown ppt was copper reduced out of solution. Good vid.
@UC235 Ok ill get on it, I'm going to do another sub4science video soon so it will be in there. Im glad your making videos, most channels on youtube dont go into as much detail as yours.
@UC235 yeah the video is great, and i'm sure everyone would appreciate the detail and time that you put into it. I'm really impressed.
You're going to be making luminol with all of this? when do you think that will be ready? I filmed my luminol approach but editing the video is taking forever.
@NurdRage I have no idea. I'm so readily sidetracked with various syntheses. I have a benzamide reaction mixture that still needs to be worked up and some 6-methylquinoline that I've been avoiding doing anything with for months. It's occupying one of my 500ml RB flasks under water. I think I will do a dehydration of phthalic acid to phthalic anhydride as a video soon and once I've made some nitric acid, I have everything I need to get to luminol in short order.
@UC235 Gotcha, i've been sitting on making sulfuric acid by the electrocatalyst process for almost a year. So i understand how life gets in the way.
what kind of reductant are you planning to use? or have you not decided? I went with a dissolving metal reduction, but the yield is horrible and the wastage high.
@NurdRage Well, I have a little bit of the preferred reductant which is sodium dithionite. It's also the bulk of a commercial product called super iron out and I suspect the reduction can be carried out directly with this product. Alternately, I have thiourea dioxide (thiox), a potent and readily available reducing agent used for small scale indigo dyeing. I suspect that the latter is more than suited for the final reduction.
@UC235 ah interesting. I can't acquire either of those chemicals domestically, one of the downsides of being Canadian. I look forward to your results.
At the beginning ,he said that one could use domestic source of hypochlorite, however, one can not know for how long it has been on the shelves and it may have started degrading.
@acidum984 Yes, bleach can be used. However, a higher concentration is preferred to reduce solution volume. If only 5-6% is available, then you could add NaCl to it to so that it's almost saturated and the solubility of the organic phase later on is minimized. If you can only get even more dilute solutions (I believe this to be the case in parts of europe, you'd be better off making your own. Using the 12.5% that I prepared, the solution is just about saturated already and no excess is needed.
@acidum984 2) Hypochlorite in excess destroys hydrazine and lowers the yield. In fact, hypochlorite destroys a good portion of the hydrazine anyway, which is why the yield is about 50% and not more like 90%. The use of urea slows the formation of hydrazine relative to the Raschig process and improves yield. Here is an example of the Raschig process: bit(dot)ly/dRJvAG Notice only 35-37% yield
3) Urea is used in excess to minimize 2, and yield should be calculated from the limiting reagent.
Great explanation, bravo.
RatkoUSA 1 month ago
Why isn't there any MEK in Canadian hw stores?
vmelkon 7 months ago
@vmelkon I don't know. In fact, I recently discovered that the company (Kleanstrip) producing the only MEK I can find in my area has discontinued the product. I went out and searched hardware stores for any remaining cans. I could only find a gallon can that was kind of beaten up. I bought it anyway, and it was fortunately discounted significantly. Also very nice is that the replacement product is pure ethyl acetate.
UC235 3 months ago
Very Cool!! Thanks!!
myst32YT 10 months ago
Why didnt you used absolute ethanol to rinse? Since hydrazine sulfate is insoluble in it.
g3ov4n12 10 months ago
@g3ov4n12 Because the impurities may be insoluble in absolute ethanol and if they precipitate and get caught on the product, what good does washing it do for me? Hydrazine sulfate is not that soluble in ice water so I'm not losing much. That's how washing works, generally. You trade a little yield for improved purity.
UC235 10 months ago
I have made hydrazine also by mixing H2O2 and ammonia in a stainless steel mug. I believe the mug had nickel in it which serves as a catalyst. Now you're probably wonering how i new it was hydrazine right? I knew it was hydrazine because when mixed with Cu(II)SO4 it formed a dark brown ppt instead of a dark blue Cu(II) amine complex. I think the dark brown ppt was copper reduced out of solution. Good vid.
69iron69 11 months ago
Could you also do a video on the suzuki catalyitic process?
ConorC96 1 year ago
Can I do a promotional video about you on my channel?
hkparker 1 year ago
@hkparker Feel free to. I'd appreciate it a lot! I should have more good stuff coming up soonish, not making any guarantees on time.
UC235 1 year ago
@UC235 Ok ill get on it, I'm going to do another sub4science video soon so it will be in there. Im glad your making videos, most channels on youtube dont go into as much detail as yours.
hkparker 1 year ago
I'm impressed with the level of detail in both these videos. Keep up the good work!
ScienceBroadcast 1 year ago
You rule.
Diazodinitrophenol 1 year ago
nice work, post it on sciencemadness!
NurdRage 1 year ago
@NurdRage I already did, just not in video form. I guess I could add add a link in ye olde hydrazine thread.
UC235 1 year ago
@UC235 yeah the video is great, and i'm sure everyone would appreciate the detail and time that you put into it. I'm really impressed.
You're going to be making luminol with all of this? when do you think that will be ready? I filmed my luminol approach but editing the video is taking forever.
NurdRage 1 year ago
@NurdRage I have no idea. I'm so readily sidetracked with various syntheses. I have a benzamide reaction mixture that still needs to be worked up and some 6-methylquinoline that I've been avoiding doing anything with for months. It's occupying one of my 500ml RB flasks under water. I think I will do a dehydration of phthalic acid to phthalic anhydride as a video soon and once I've made some nitric acid, I have everything I need to get to luminol in short order.
UC235 1 year ago
@UC235 Gotcha, i've been sitting on making sulfuric acid by the electrocatalyst process for almost a year. So i understand how life gets in the way.
what kind of reductant are you planning to use? or have you not decided? I went with a dissolving metal reduction, but the yield is horrible and the wastage high.
NurdRage 1 year ago
@NurdRage Well, I have a little bit of the preferred reductant which is sodium dithionite. It's also the bulk of a commercial product called super iron out and I suspect the reduction can be carried out directly with this product. Alternately, I have thiourea dioxide (thiox), a potent and readily available reducing agent used for small scale indigo dyeing. I suspect that the latter is more than suited for the final reduction.
UC235 1 year ago
@UC235 ah interesting. I can't acquire either of those chemicals domestically, one of the downsides of being Canadian. I look forward to your results.
NurdRage 1 year ago
Excellent!
Now, some questions...
1) Could one use bleach as a domestic source of hipochlorite?
2) Why don't You use excess of hipochlorite, since it can easily degrade?
3) Why do You calculate yield to hipochlorite and not to urea, which is far stabile?
acidum984 1 year ago
@acidum984
Hey,
At the beginning ,he said that one could use domestic source of hypochlorite, however, one can not know for how long it has been on the shelves and it may have started degrading.
Aranwu 1 year ago
@acidum984 Yes, bleach can be used. However, a higher concentration is preferred to reduce solution volume. If only 5-6% is available, then you could add NaCl to it to so that it's almost saturated and the solubility of the organic phase later on is minimized. If you can only get even more dilute solutions (I believe this to be the case in parts of europe, you'd be better off making your own. Using the 12.5% that I prepared, the solution is just about saturated already and no excess is needed.
UC235 1 year ago
@acidum984 2) Hypochlorite in excess destroys hydrazine and lowers the yield. In fact, hypochlorite destroys a good portion of the hydrazine anyway, which is why the yield is about 50% and not more like 90%. The use of urea slows the formation of hydrazine relative to the Raschig process and improves yield. Here is an example of the Raschig process: bit(dot)ly/dRJvAG Notice only 35-37% yield
3) Urea is used in excess to minimize 2, and yield should be calculated from the limiting reagent.
UC235 1 year ago