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Schleimsäure
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Registered: 31-8-2014
Location: good ole Germany
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1l Thionyl chloride
250g 2-Naphtole
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The Volatile Chemist
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Location: 'Stil' in the lab...
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Glassware, used:
500mL Teflon Sep Funnel
250mL Actinic Flask (have little idea *what* to do with it...)
10, 25, 100, 200 mL Volumetric flasks
10 mL beaker 
All from my AP chemistry teacher.
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woelen
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Posts: 8012
Registered: 20-8-2005
Location: Netherlands
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Mood: interested
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5 kg of NaNO2 (99+% food additive containing 0.5% very fine SiO2 added as anticaking agent) and 500 g of glycine.
I want to try making the mysterious blue volatile liquid as described here: http://www.sciencemadness.org/talk/viewthread.php?tid=65553
I ordered a lot of NaNO2, because I also want to try how easy it is to make HNO3 from dilute H2SO4 and NaNO2 and oxygen from air. This is because
nitric acid is not available anymore at all and KNO3, NaNO3 and NH4NO3 are nearly impossible to get where I live. The NaNO2 was cheap, the price is
appr. EUR 25 per 5 kg.
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The Volatile Chemist
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Wow, that is a good price. though I suspect it's slightly industrial-grade.
I just bought 420g NH4NO3 in the form of four cold packs. Cost slightly under $10. Probably confused the dame at the cash
register at the CVS I got it from. She was pretty chill though.
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Texium
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Posts: 4580
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Location: Salt Lake City
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From Duda Diesel:
1L formic acid, 95%
1L acetic acid, 98.9%
2lb potassium hydroxide
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Trevor9424
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Magnesium ribbon (60cm)
Lead(II) Nitrate (30 grams)
Sodium Bisulfate (30 grams)
Ammonium Chloride (30 grams)
Hydrochloric acid 30% (60 ml)
Concentrated sulfuric acid (60ml)
I needed conc. Sulfuric acid for my first Fischer esterification
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Texium
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I see you like to work small scale 
Good luck with the esterification though, they're fun. Which ester are you planning to make?
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Trevor9424
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Quote: Originally posted by zts16  | I see you like to work small scale
Good luck with the esterification though, they're fun. Which ester are you planning to make? |
I just recently did the esterification . I tried making isopropyl salicylate. I
added some salicylic acid powder I made at home and the sulfuric acid(about 1-2 ml) to a 50 ml. Flask with about 10 ml of isopropyl alcohol(it wasn't
anhydrous, it was 70% which likely deteriorated the yield). I heated the solution at reflux through a hot water bath at around 80 degrees Celsius.
Soon, a layer formed so I added the mixture to a separatory funnel and drained off the larger lower layer and added the water layer to another
container. Repeat.
Afterwards: had less than 1/4 a milliliter of the ester...  
Things that could've been done to improve the yield likely:
-Boil off the alcohol, isopropyl alcohol has a lower boiling point than isopropyl salicylate according to a couple sources after a few minutes of
research (I think the ester's boiling point was 100-200 degrees Celsius according to various sources while isopropyl alcohol's is about 82). I've read
that boiling off the alcohol during Fischer esterification can increase yield due to equilibrium of the ester and its reactants.
-Add the product mixture directly to a sodium bicarbonate/carbonate solution to neutralize the sulfuric acid and prevent loss of the ester due to the
reverse reaction.
Overall, there was lots of room for improvement and I'll definitely add the two actions above to improve the yield.
Sources for the ester's boiling point:
http://www.chemspider.com/Chemical-Structure.11345.html
http://chemicalland21.com/specialtychem/NH/ISOPROPYL%20SALIC...
I feel that chemspider's information (120 degrees C) is more reliable than Chemicalland21's info (over 200 degrees C)
[Edited on 7-4-2016 by Trevor9424]
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Texium
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What did it smell like? I tried making isopropyl salicylate once and thought it just smelled gross and vegetal. I didn't attempt it again.
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NeonPulse
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Sodium thiosulfate. 50g
Cerium metal.5g
Sodium benzoate.250g
Dicyandiamide.100g
Boric acid.100g
I have a few experiments lined up in the near future.
Also bought a simax 2l Erlenmeyer flask for reasonably cheap.
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coalminecanary
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It's my time to post something!
These 2 moving boxes just came in the door, I can tell one of them is very heavy...
So I unboxed the stuff, and here is the result.
https://www.youtube.com/watch?v=SnzF837vzcY
Sorry about my weird English!
Was it worth it?
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j_sum1
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You scored well. I can't believe all those bottles fitted into those two boxes.
Pretty cool.
Now for the ground glass and the hotplate/stirrer and the heating mantle and the vacuum pump and the teflon tubing and the DC power supply and the
electrodes and the chemicals and some more chemicals and the storage cabinet and the fume hood and the thermometers and thermocouples and the inert
gases and the glove box and...
Hey you are in the deep end now. There is no escape.
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coalminecanary
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| Quote: Originally posted by j_sum1 | You scored well. I can't believe all those bottles fitted into those two boxes.
Pretty cool.
Now for the ground glass and the hotplate/stirrer and the heating mantle and the vacuum pump and the teflon tubing and the DC power supply and the
electrodes and the chemicals and some more chemicals and the storage cabinet and the fume hood and the thermometers and thermocouples and the inert
gases and the glove box and...
Hey you are in the deep end now. There is no escape. |
Don't worry. Got the teflon tubing on the way, along with a hotplate stirrer, and I have a vacuum pump already.
I need a good mercury thermometer and some more storage space. I'd eventually like to dedicate a room to my lab instead of the messy shed. Not a
pretty sight.
BUt yeah! Pretty stoked about being surronded by media bottles as I'm typing this.
Edit: Also have a motor rig coming for setting up a Lead Dioxide plater for some electrolysis where you should use platinum. Maybe I should do a video
on that?
I was considering doing some chemistry videos to fill the gap of ChemPlayer for entertainment. Although I'm nowhere near as good, I figured it'd be a
good way to get some input along the way. Just gotta fix my shitty accent/English first. Maybe I'll use text-to-speech like ChemPlayer, that works out
great!
[Edited on 5-7-2016 by coalminecanary]
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j_sum1
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Your English is fine.
There is always room for another good chem channel along the lines of nudrage, Doug;s Lab, NileRed and chemplayer, I'll add the now-retired myst32YT
and hkparker to that list too.
All the best with your endeavours. I will watch this space.
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Trevor9424
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| Quote: Originally posted by zts16 | | What did it smell like? I tried making isopropyl salicylate once and thought it just smelled gross and vegetal. I didn't attempt it again.
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My sample (despite smelling slightly of isopropyl alcohol and being small) does smell a bit like an old, warm vegetable. I wish sources would use more
words than "green" to describe an ester's scent.
"Green? Like freshly mowed grass green or cooked spinach green?"
Apparently, isopropyl salicylate is the latter. 
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Texium
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Posts: 4580
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Location: Salt Lake City
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Yeah, that sounds like what I smelled. The only good salicylate ester in my opinion is methyl. I've smelled ethyl, n-propyl, isopropyl, butyl, and
benzyl also and they're all bad.
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coalminecanary
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Got a hotplate stirrer aswell today! Lab is looking pretty promising equipment-wise. I'm considering exchanging it for a 19x19 one though, 12x12 (cm)
seems a little small.
    
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woelen
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Posts: 8012
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Location: Netherlands
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I purchased some KOCN and NaOCN, both general lab reagent grade. Very cheap at the moment at Onyxmet, for just a little more than EUR 5 per 100 grams.
Grab it while it still is there
I've no experience with the cyanate ion and want to explore its chemistry. I already found out that it forms no interesting complex with iron(III), as
opposed to the thiocyanate ion, but it does form an interesting intensely blue colored complex with cobalt(II). Interesting to see that there
analogies between thiocyanate and cyanate, but the analogy does not extend very far.
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coalminecanary
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40$ worth of stuff. Overall happy with the pickup.
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The Volatile Chemist
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Quite the collection coalminecanary...was this an Ebay sale? I don't think you said where you got it in the video.
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coalminecanary
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It was from a sale on the danish version of craigslist. She had some media bottles for sale, I don't think she knew what she had, because they were
listed as "decorative bottles". So I asked if she had more than just bottles, and she said she had a whole box of beakers and stuff she didn't think
she could sell, so she didn't list it. That's where I got it all from.
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Texium
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Posts: 4580
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Location: Salt Lake City
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250g benzophenone
Don't really know what to use it for, other than making the really intense blue benzophenone sodium ketyl if I ever get my hands on some sodium metal,
but it was insanely cheap so I snapped it up.
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AvBaeyer
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Location: CA
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ZTS16,
You can do a photoreduction of benzophenone to benzhydryl alcohol in isopropanol, a reaction which is quite efficient and run in sunlight. The
benzhydryl alcohol can be used to form the the diphenylmethane cation which in turn can be reacted with a variety of nucleophiles producing rather
interesting organic molecules - the Ritter reaction comes to mind as an example. The chemistry can be a bit sophisticated but is easily done by a
knowledgeable hobbyist.
AvB
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Herr Haber
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Definitely a good deal. I know the blue caps and have plenty of the PTFE lined red ones. Great deal indeed if yours are PTFE lined too. Seing all the
red they probably worth 200 $ alone!
Over here I got a new digital magnetic stirrer with a temperature probe under the heating element and an external probe. It wasnt cheap but in 5
minutes I was certain I would love it. It's a lot more responsive that the old one I was given.
Also got a PTFE membrane vacuum pump. Price tag: 666 Euros after discount. I should find something diabolical to do with it but I think for the moment
it will be mostly used to reclaim solvents.
Got 2 meters of Viton tubing and a nice big funnel aswell.
Got a new job aswell... so much to do... so little time
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violet sin
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500g choline chloride, intended for DES experiments with urea. 50# sack of the latter couple weeks ago( few pounds to play with, rest for yard and
garden). Should prove to be fun. Need to find time to recrystalize urea first though.
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