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Rainwater
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Registered: 22-12-2021
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Friends insisted that we make some fire for new years so before the celebration began i showed them what a 10 monutes of nitration will do to a 3
grams of cotton. Shot @ 800fps.
Attachment: 20211231_183012_1_1.mp4 (3.8MB)
This file has been downloaded 131 times
"You can't do that" - challenge accepted
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j_sum1
Administrator
Posts: 5641
Registered: 4-10-2014
Location: Oz
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Mood: d jolly / dt > 0
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In my attempts to be conscientious, I have numerous solutions of waste waiting to be recycled. Today was the day for at least some of them.
I am discovering that many of them are quite dilute and need litres of boiling down before recovery can be done. I am slowly becoming convinced that
it is not worth it for just a few grams of iodine or barium hydroxide.
Nevertheless, it has been a pleasnt day in the lab and I have been working my way through chemplayer videos again.
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j_sum1
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Location: Oz
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Mood: d jolly / dt > 0
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Damn I like it when things work out nice.
The other day my new set of scales arrived and so it was time to properly titrate the HBr that I synthesised last week.
I made a rough initial estimate which was basically pulling a figure out of thin air based on my guess of how much of my distillate came over at
azeotropic temperature.
Then I measured density. But not having a density table for HBr I used the one data point available for azeotropic and assumed the curve would be the
same as HCl.
I then pulled out the volumetric flasks, pipettes and burette and got going.
Nice correlation between all three figures -- certainly within measurement error.
Estimate 30%
Density 30.45%
Titration 30.65%
I don't have a fancy label for the bottle. But even my hand-written sticker felt like an achievement badge.
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AvBaeyer
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Registered: 25-2-2014
Location: CA
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j-sum,
There are density tables for most common acids and bases and related solutions in the back of Vogel "Practical Organic Chemistry". I believe that
various editions of this book are easily available.
AvB
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Tsjerk
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Posts: 2719
Registered: 20-4-2005
Location: Netherlands
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Mood: Mood
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I just ran a distillation of chloral from chloral hydrate and sulfuric acid.
Now running the reaction of chloral and fluorobenzene with sulfuric acid. The 1947 procedure I'm following calls for oleum, so I added some P2O5 to my
sulfuric acid.
I was supprised by the exotherm between the P2O5 and 96% sulfuric acid.
Attachment: bradlow1947.pdf (431kB)
This file has been downloaded 70 times
Edit: I love my IKA mag stir, my reaction is running in a five degree shed, the 100 ml round bottom is in a couple 100 ml water in a beaker rapped in
alu foil. I just put my mag stir set to what I supposed to be about between 20 and 30 degrees. Has been between 20 and 25 for hours now.
[Edited on 23-1-2022 by Tsjerk]
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Sulaiman
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Registered: 8-2-2015
Location: UK ... on extended Holiday in Malaysia
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I need a coolant system to get below 25oC 
.................................
Unrelated, current mini-project:
For reasons still unclear to myself,
I recently recrystalised commercial potassium nitrate multiple times to 'purify' it.
(a few mini-fireworks made with used 120mm filter papers)
Problem is, I don't know the initial or final purities.
Everything I observed makes me 'think' that the original kno3 was/is quite pure.
(no sediments, colors, change in crystal shapes etc)
Some research reqd.
CAUTION : Hobby Chemist, not Professional or even Amateur
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mayko
International Hazard
Posts: 1120
Registered: 17-1-2013
Location: Carrboro, NC
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Mood: anomalous (Euclid class)
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Took my recently acquired heating mantle/variac for a spin, steam distilling citrus peels ... all went smoothly
al-khemie is not a terrorist organization
"Chemicals, chemicals... I need chemicals!" - George Hayduke
"Wubbalubba dub-dub!" - Rick Sanchez
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Rainwater
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Registered: 22-12-2021
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Tried to extract, purify, and dry anthocyanin. Sourced from red cabbage, beats, and then finally amazon. This molecule is very, very easy to
destroy/decompose. I wanted to test it as a catalyst for the "alcohol catalyzed perduction of sodium metal" reaction.
Extraction was easy. Drying was not.
After 20 drying experiments, which decomposed the anthocyanin, I used store bought freeze dried.
Exposure to mineral oil from the same bottle of oil and anthocyanin from the same bag perduced verying results each time. Solved by bubbling h2
through the oil with 200c heat under vacuum (-15inhg) for 1 hour to clean/dry the oil
Test tube:
Exposure to sodium jump start at 105c produced a passiveation layer (brown oil) on the sodium and bottom on the flask. Sometimes, the sodium could be
brought to the top of this layer and reacted more, but soon was covered again.
25ml round bottom flask:
Heavy stirring was added, and the results were a thick brown layer. Additions of magnesium metal produced a hard, solid black tar after a few minutes.
I added NaOH even with the listed problems. The tar that resulted was difficult to remove and contain unreacted sodium metal. 10%
H2SO4(aq) was able to remove it with violent effectiveness
I think instead of working to find an easier to obtain catalyst, I will search for a more available reducing agent. Magnesium is not as cheap or as
available as other metals. Aluminum should not work, so I'll start their. My thoughts on this are: Magnesium shouldn't work because it's lower on the
reactivity series. NaOH + Mg = Na + MgOH works.
I know aluminum and sodium will produce an almogum, but maybe an excess of sodium hydroxide will be able to separate the mixture and force the
reaction to completion. Baby steps.
"You can't do that" - challenge accepted
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Tsjerk
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Posts: 2719
Registered: 20-4-2005
Location: Netherlands
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Mood: Mood
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Recrystallizing some vanillyl oxime now to reduce with U-Ni-NH3 made in situ with zinc. I didn't look at what method to use for the oxime reduction,
only to realize I could probably also directly aminate vanillin with this method. So I will just try both.
Is there an amateur capsaicinoid synth with actual characterization around? I could only find the one below, but it is without characterization of the
product or intermediates. Also on YouTube nothing found, only preps for the precursors.
https://www.sciencemadness.org/whisper/viewthread.php?tid=23...
Waiting for octanoic acid and triphenylphosphine to arrive to make octanoyl chloride with TCCA.
[Edited on 14-3-2022 by Tsjerk]
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DraconicAcid
International Hazard
Posts: 3926
Registered: 1-2-2013
Location: The tiniest college campus ever....
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Mood: Semi-victorious.
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So I tried nitrating p-anisic acid. Dissolved 1.22 g of it in 20 mL acetic acid, added a mL each of nitric and sulphuric acids. No change. Heated
to dissolve everything, let it stir for an hour or two, gave a white precipitate when it cooled down. Several cycles of adding more nitric, adding
more sulphuric, stirring it overnight, heating to 70 C or so, etc, and finally cooled it down, added 100 mL water, and filtered. The precipitate was
white (I expected yellow, like nitrobenzoic or nitrovanillin), and gave a mp of 188 C when dried. Really close to the lit mp of p-anisic acid, so I
figured it was a failure.
Then I did a mixed mp of it with the original p-anisic acid. It's not p-anisic acid, and the lit mp of the nitro compound is 195 C. So it's the
product I wanted (I think)- it just needs recrystallization.
This is the first time I've gotten useful information out of a mixed-melting point since first year organic chem.
[Edited on 16-5-2022 by DraconicAcid]
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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