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DraconicAcid
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I spent a couple of hours typing up a document explaining substituents in organic chemistry, including the isoalkyls, neoalkyls, and various aromatic
substituents. Saved it as a pdf and the computer ignored everything in the structures other than the R labels.
So every substituent is an R surrounded by white space.
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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njl
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Anybody have any thoughts on acesulfame potassium (artificial sweetener) as a source for acetoacetic acid? Looking at the structure, I'm hopeful both
the enol ester and amide can be hydrolyzed in one step by boiling with NaOH.
Reflux condenser?? I barely know her!
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arkoma
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INitroethane. Just a few ml, but I count it as a success.
 
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Mateo_swe
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arkoma, what procedure did you use?
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arkoma
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Method 1 from this
*edit* pretty sure i would have had better yield if i had used a blender to mix the dry ingredients.
the sodium ethyl sulfate was where the learning curve kicked in, trust me. finally waited till my oil bath stabilized at 110C before i EVER set my
flask/condenser/addition funnel in to it. temp in bath and internal flask both monitored (it gets warmer than this ya get diethyl either which is a
side product for this procedure), slow dropwise addition of H2SO4 then reflux fer 'bout an hour. neutralized rxn mix with
Na2CO3 until pH 7, suction filtered to remove the sodium sulfate (which i saved for use as dessicant), then evap'ed off the
filtrate
[Edited on 4-18-2021 by arkoma]
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
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JJay
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I maintained my oxidizer storage (which contains a few items that aren't strictly oxidizers). Most things are holding up pretty well. My bromine looks
unchanged in its bottle, and the cap shows no signs of degradation. Some of my sodium dichromate is a bit clumpy. I put some additional layers of
plastic around it. I also have some in a bottle with a cap that is starting to rust. I will probably look for a new bottle. There was a hole in my
ammonium nitrate bag that made a bit of a mess. My mercuric chloride looked unchanged, but the foil that I used to wrap the jar that holds its bottle
was visibly degraded. I put that foil in a solid waste container and rewrapped the jar then threw away the gloves and washed my hands. My chromic acid
looks fine, as do my potassium permanganate, potassium dichromate, and potassium nitrate. My pool chemicals seem to be fuming a bit, but I'm not going
to worry about that unless the packaging starts to degrade.
I am going to have to repackage my phosphorus oxychloride. The cap shows signs of serious degradation and probably imminent failure. I likely have a
suitable bottle, but I will need to set up some sort of a fume hood.
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S.C. Wack
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Quote: Originally posted by arkoma  | Method 1 from this
*edit* pretty sure i would have had better yield if i had used a blender to mix the dry ingredients.
the sodium ethyl sulfate was where the learning curve kicked in, trust me. finally waited till my oil bath stabilized at 110C before i EVER set my
flask/condenser/addition funnel in to it. temp in bath and internal flask both monitored (it gets warmer than this ya get diethyl either which is a
side product for this procedure) |
Eh a couple of learning curves here...heating above 30C is unnecessary and above 50C is detrimental...more serious would be if the vague Rhodium
directions also produce ethyl nitrite which is not mentioned; if it is expected, but trust is given to wikipedia, that it's much more volatile (by
45C) than this time-wasting project has been (maliciously) saying for the past 8 months. It would not surprise me if CA 49, 836 (1955), didn't say
what Rhodium/the-hive says at all, as what it says seems to be a combination of other references, designed to give directions for none of them. I
won't be the one looking it up, since the public has been completely banned from entering the local university libraries for a long time.
(edit: IIRC I looked it up over 15 years ago; the first half is from the reference CA cites but does not represent well (it's not a dry distillation
there) and the second half of the "method 1" is from an earlier reference)
...on topic(?), my last project made brown oil, which can be further qualified as impure and soluble in NaOH, yet it smells exactly like safrole
(after acidification). I also created smoke, coming from inside the control unit of my Buchi R110 (even though the rotation was set slow) and
discovered why few of them still survive, AND confirmed that there is a good reason why Bayer's DE189843 doesn't mention yield in any way.
[Edited on 16-8-2021 by S.C. Wack]
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JJay
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I opened my sodium borohydride, and I was pleased to discover that it was packaged inside multiple layers of thick foil. I had added a couple of
ziplock freezer bags to that, and then abused it horribly. There was some minor clumping, but most of it is still a free-floating crystalline powder,
which I put into a large glass bottle.
I am planning on getting into my sodium next, and then I'll tackle the oxidizers. I don't have a fume hood set up (I don't even have electricity yet),
so I will have to use a gas mask for some of the transfers. I'm using a regular N95 mask for the powders, but I'll use an acid gas mask and probably
swimming goggles for the fuming liquids.
The cleanup from sodium borohydride smells like epoxy glue, and I'm not sure why.
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Texium
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What were you using to clean up the borohydride?
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JJay
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Baby wipes. Ingredients: water, glycerin, pg-dimonium chloride phosphate, natural fragrances, tocopheryl acetate, sodium benzoate, citric acid. I
don't have a baby here, but they were readily at hand.
I didn't have a large enough container on hand for the sodium, but I got my sodium dichromate bottled up. It was encased in five layers of plastic,
and it was a bit clumpy but is free-floating after some shaking in a bottle. It might be a little damper than it should be, but I figure that's pretty
normal, and I can work with that.
My bromine bottle cap is actually not looking so great now, after the bottle sat on a heated floor for a few hours. Very little bromine is missing,
but it looks like there is an orange-stained crack in the cap. Fortunately, I have another cap I can use to replace it. The cap that is on it now has
been there for several years.
[Edited on 20-8-2021 by JJay]
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JJay
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I got my sodium under oil. I had to remove some of it from an aluminum can. The aluminum was actually pretty easy to cut, but removing the last of the
sodium reminded me of scraping used chewing gum off of a cold surface wearing two pairs of gloves. I wiped down the surface, which was actually pretty
exciting since there were tiny pieces of sodium scattered on it, and they burst into flame when touched by a wet cloth. Then I poured water on the
fragments of the can, resulting in a fireball that burned for a minute or so while spitting fireball fragments. It went out eventually and then
reignited when I poured on more water. I made sure it was not burning and completely soaked before I walked away (I'll pick up the trash later).
My bromine is chilling over ice. I am planning on just changing the cap, but I have another bottle close by with a funnel inserted if the replacement
cap won't fit or something.
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JJay
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The cap change for the bromine went without a hitch. I didn't even smell any bromine until I took off my gas mask. I also found a PTFE-lined cap that
happened to fit on my phosphorus oxychloride bottle, so I just changed the cap. The bottle appeared to fume pretty strongly when it was open, and I
didn't leave it open for long.
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arkoma
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Be glad to see you doing chemistry again JJay. I've been so busy traveling this year haven't done much. In Mexico for the SECOND time since May, and
spent all of June in California.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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DraconicAcid
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I've been cleaning up my lab in preparation for September- working syntheses that worked to various degrees.
Making a hopefully-chelating amide from methyl salicylate and en seems to have worked quite well.
Making simple amides from methyl o-toluate and methyl anthranilate did not work very well at all.
Making salicylamide worked very well, but it didn't form a simple complex with copper(II).
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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JJay
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| Quote: Originally posted by arkoma | | Be glad to see you doing chemistry again JJay. I've been so busy traveling this year haven't done much. In Mexico for the SECOND time since May, and
spent all of June in California. |
I went through all of my chemicals and found a couple of leaking plastic jugs, both of which contained half-finished but fortunately non-toxic
experiments that are probably ruined now. I transferred the contents to glass bottles. I reorganized all of my chemicals and most of the glassware.
I am also going to be traveling quite a bit for the next several months, but I have started preparing the site that will eventually be home to my lab.
I am super tempted to take several months off and just do chemistry, but I probably shouldn't do that just yet.
I am going to do a few experiments on the road, though.
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charley1957
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Yesterday I made a couple of batches of ethyl acetate for my bug killing jar. Lately I took apart some large wet cell Nicad batteries to try and
extract cadmium. Not much luck there. Suggestions welcome. Besides that just cleaned up several kilos of very dirty Mercury, 5cc’s at a time. Glad
that’s done. It took days. Right now doing some mods to the lab. Adding a on/off switch at the bench for my water supply pump, and replumbing the
water supply to the bench and fume hood. I decided the off switch was too far away when I developed a big water leak during a distillation the other
day.
You can’t claim you drank all day if you didn’t start early in the morning.
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arkoma
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Hopeful platinum group metal extraction with boiling Aqua Regia and ground up roasted cat converter honeycomb.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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Texium
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Nice! I like your fume hood 
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arkoma
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Works well! House next to me is empty and falling down, other side of house is empty lot, so the only thing it bothers is the metal frame of my
window.............
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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arkoma
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Phenol from salicylic acid. No short path condenser but this adapter seems to be working well.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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j_sum1
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Just mucking around with some antimony chemistry today.
i have made some potassium antimony tartrate crystals. Yield is low but they look really pretty. Equilateral triangular planar as reported elsewhere.
I am keen to see if I can get larger crystals. Mine are in the 0.5mm range.
I am making some Ti(III) iodide because, why not. Currenytly stirring titanium powder in excess iodine in a xylene solvent.
I performed my first ever Marsh test using beaker washings from the antimony.
Yesterday I dittilled a litre of azeotropic HCl. My hardware store product is dirty and needs purification.
Right now I am making some hydrobromic acid.
Nice to be in the lab.
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DraconicAcid
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Made some copper and iron acac complexes.
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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B(a)P
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| Quote: Originally posted by j_sum1 |
Yesterday I dittilled a litre of azeotropic HCl. My hardware store product is dirty and needs purification.
Right now I am making some hydrobromic acid.
Nice to be in the lab. |
Is that Diggers?
Today I unpacked and set up my lab after 9 months in storage. Now I need to replenish my stocks of reagents that were not suitable for long term
storage. Totally agree j_sum1, although I didn't do any reactions it was nice to be setting things up. Looking forward to getting back into chemistry!
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S.C. Wack
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Some aspects of a process for hydrazine sulfate (which has never been described here) needed a precise nailing down, so that I can mess with the last
variables in future optimization attempts with slight confidence. This is the result of the final run to that end; 37.7 g (without cooling, which
would probably give 2-4 g more, after recrystallizing) after drying this morning, from 30 g urea and 496 g 7.5% bleach last night.
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j_sum1
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No. Bondall. But I have had exactly the same issue with Diggers: contaminated with Ti of all things.
[Edit]
I suspect they both come from the same source.[\edit]
(Purple hue after reacting with a metal, and then becoming increasingly cloudy over time. Deep amber complex formed on addition of hydrogen peroxide.)
My solution is to distill azeotropic acid, which is non-fuming and fine for most applications. If I need stronger pure acid then I can react NaCl with
sulfuric and pass the gas through.
[Edited on 1-1-2022 by j_sum1]
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