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mayko
International Hazard
Posts: 1218
Registered: 17-1-2013
Location: Carrboro, NC
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Mood: anomalous (Euclid class)
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Everyday Chemistry
restarting this thread; hopefully it will be merged when the One, True Thread reappears.
I tried my first vacuum distillation the other day, to clean up some phenol from destructive decomposition of salicylic acid. It was a dark pink,
looking like a manganese salt, but definitely smelling like phenol. (I can't tell if the cherry undertones are real, or if it's just an associative
memory linked to chloraseptic throat spray).
The distillation was a mixed success. The glassware didn't implode, but I couldn't keep the stillhead warm enough to keep the solid from depositing
there... the vapors didn't make it as far as the warm-water condenser  on the other
hand, what I manually scraped out was much cleaner in appearance.
Edit by Texium: Changed title because the "one true thread" will likely never reappear, unfortunately.
[Edited on 4-11-2023 by Texium]
al-khemie is not a terrorist organization
"Chemicals, chemicals... I need chemicals!" - George Hayduke
"Wubbalubba dub-dub!" - Rick Sanchez
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mayko
International Hazard
Posts: 1218
Registered: 17-1-2013
Location: Carrboro, NC
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Mood: anomalous (Euclid class)
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Got a bunch of scrap iron sitting in a bucket of muriatic acid, on its way to Fe2O3
al-khemie is not a terrorist organization
"Chemicals, chemicals... I need chemicals!" - George Hayduke
"Wubbalubba dub-dub!" - Rick Sanchez
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DraconicAcid
International Hazard
Posts: 4278
Registered: 1-2-2013
Location: The tiniest college campus ever....
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Mood: Semi-victorious.
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I tested some labs for the organic course. You would think a simple acid-base separation of cinnamic acid from benzophenone would be trivial, right?
Sodium cinnamate is pretty insoluble in water, and benzophenone has too low of a melting point to crystallize. Bah.
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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Sigmatropic
Hazard to Others
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Oxidized an alcohol to the carboxylic acid but couldn't fully get rid of the sideproducts. I'm feeling rather down with all these byproducts in the
system.
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arkoma
Redneck Overlord
Posts: 1761
Registered: 3-2-2014
Location: On a Big Blue Marble hurtling through space
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Mood: украї́нська
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Still ain't worked up the Benzyl Acetate I made; waiting on a new see funnel. They have a short life span at my house. First post from my mobile!
"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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CobaltChloride
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Location: Romania
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I made some concentrated aqueous ammonia and KNO3 a few days ago. I also made some 13% NaClO from Ca(ClO)2. I also bought some drain cleaner sulfuric
acid called Cleamen 420 which is a colorless, odorless, transparent, viscous liquid and measured its density as 1.835 g/cm^3.
[Edited on 28-6-2018 by CobaltChloride]
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wg48
National Hazard
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So what happened to the original thread mods, anybody ?
Borosilicate glass:
Good temperature resistance and good thermal shock resistance but finite.
For normal, standard service typically 200-230°C, for short-term (minutes) service max 400°C
Maximum thermal shock resistance is 160°C
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roXefeller
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Registered: 9-9-2013
Location: 13 Colonies
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Mood: 220 221 whatever it takes
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I need to get some of that going. Looking for a handy way to light a tenaciously wet barrel fire, in style. Got the aluminum, but I don't think I
ever bought iron oxide.
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
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I cleaned and organized glassware. I also organized some of the chemicals.
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
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I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The
can still smells like DCM, so I'll try to finish it ths weekend.
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DraconicAcid
International Hazard
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Registered: 1-2-2013
Location: The tiniest college campus ever....
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Tested different versions of the piperine extraction from black pepper lab.
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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symboom
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Mood: Doing science while it is still legal since 2010
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Tested bromine in silica to see if it will absorb
Studied about internal oxidtion on such as light sensitive potassium ferrioxalate and ammonium permanganate
[Edited on 6-7-2018 by symboom]
[Edited on 6-7-2018 by symboom]
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TheMrbunGee
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Quote: Originally posted by JJay  | | I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The
can still smells like DCM, so I'll try to finish it ths weekend. |
I had success distilling DCM just with cold tap water, 30 cm Liebig condenser @ 400ml/h
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JJay
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| Quote: Originally posted by TheMrbunGee | | Quote: Originally posted by JJay | | I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The
can still smells like DCM, so I'll try to finish it ths weekend. |
I had success distilling DCM just with cold tap water, 30 cm Liebig condenser @ 400ml/h |
I did it with that exact setup when I was first starting out, but I don't think it's as efficient as using ice water with a 30 cm Dimroth, and I had
horrible nosebleeds the next day after trying it with a Liebig. Also, I didn't have a convenient tap the other day.
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TheMrbunGee
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| Quote: Originally posted by JJay | | Quote: Originally posted by TheMrbunGee | | Quote: Originally posted by JJay | | I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The
can still smells like DCM, so I'll try to finish it ths weekend. |
I had success distilling DCM just with cold tap water, 30 cm Liebig condenser @ 400ml/h |
I did it with that exact setup when I was first starting out, but I don't think it's as efficient as using ice water with a 30 cm Dimroth, and I had
horrible nosebleeds the next day after trying it with a Liebig. Also, I didn't have a convenient tap the other day. |
It could be faster, but I had a closed system (not counting vacuum nozzle, and no vapor came out of it.
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Plunkett
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Location: The Richest Hill on Earth
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A few weeks ago I went rockhounding at an old zinc mine and picked up some glossy black rocks which I thought were sphalerite, hoping to isolate zinc
from them. Yesterday, I began to crush the rocks up with a hammer and the powder was red which I thought was strange, but I do not know a lot about
minerals so I figured it was nothing and kept going. It was not until I noticed rock fragments sticking to a nearby magnet that I realized the
mineral was hematite, not sphalerite. A little disappointed, I cleaned up the hematite and instead made a small dot of copper metal by the
carbothermal reduction of basic copper carbonate recovered from the inside of some old copper pipes. I have some malachite and azurite fragments from
the same mine and once I get my technique down I want to try and smelt them.
[Edited on 13-7-2018 by Plunkett]
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AlexC
banned
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Registered: 11-7-2018
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Rock is always useful. I mean you are not searching for anything in rock. Whole rock is something. All elements we need. Like H, He, Li, Be, B, C, N,
O, F, N, O, F, Ne...whole periodic table. That's what changed my perception about life. I noticed everything is elements. It would be stupid to just
try to extract one element and throw processed rock away. When doing something, do it completely. Do not steal minerals from Mother Nature, she will
punish you.
Or this whole post in one sentence: TAKE IT OR LEAVE IT.
[Edited on 13-7-2018 by AlexC]
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DraconicAcid
International Hazard
Posts: 4278
Registered: 1-2-2013
Location: The tiniest college campus ever....
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Mood: Semi-victorious.
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I tried to convince my dean to look for funding for a benchtop NMR spectrometer.
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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j_sum1
Administrator
Posts: 6218
Registered: 4-10-2014
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Back in the lab after a bit of absence. Preoccupied with -- well, life stuff.
Huge pile of dirty stuff to clean up from last time all of which had accumulated a decent layer of dust.
I managed to break a beaker and the stem of a take-off adapter. My most common cause of breakages is me cleaning stuff.
I installed a screen in the lab (spare TV) and attached it via HDMI socket to the computer in the office next door. Already it is more useful than I
imagined it would be. So nice to be able to look up stuff while working in the lab.
I am half-way through purifying some dioxane I made last night. I managed to get the tarry mess at the end of the synth to boil over and flood the
condenser. Twice. But now it is fractionally distilling nicely and it looks like I will have a good product.
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
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I put 100 grams of technical barium carbonate into a 5L beaker and added 1000 mL of 5% cleaning vinegar. Phew! It stinks! After it finishes reacting,
I am going to filter, add sodium hydroxide, evaporate off some of the water at low heat, chill, then recrystallize the precipitate and dry it in my
desiccator. I'm going to have to read up on suitable desiccants... removing the last water of hydration is very hard, but I'd like to get the product
as dry as practical.
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Loptr
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Registered: 20-5-2014
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I want to ask you guys how do you have time for such a number of experiments in conjunction with life? I have a wife and two kids. They demand most of
the time I have outside of work.
How do you guys do it? I used to have a lot of time to myself for stuff like this. It's really got me down lately.
"Question everything generally thought to be obvious." - Dieter Rams
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j_sum1
Administrator
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Hang in there, Lotptr. I am in the same position. Basically, I am finding that I need to schedule in some lab time in a chunk and go hard when I get
the chance. And accept the fact that it doesn't happen as regularly as I would like.
I got into the lab the other night for a continuation of dioxane synthesis and found that it had been three weeks since my last visit. Distillation
took longer than I anticipated and I ended up going to bed at 2:00 am
I can see that in a couple of months work things might be a bit more settled and I might be able to do more. But then again, it is probable that
other priorities will sneak in and it will be just as difficult. Ultimately I have to recognise that a bit of me-in-the-lab time is important enough
for me to have to schedule it. And I have to accept that much of the time I will have to get my fix by dropping in here and reading.
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Loptr
International Hazard
Posts: 1347
Registered: 20-5-2014
Location: USA
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| Quote: Originally posted by j_sum1 | Hang in there, Lotptr. I am in the same position. Basically, I am finding that I need to schedule in some lab time in a chunk and go hard when I get
the chance. And accept the fact that it doesn't happen as regularly as I would like.
I got into the lab the other night for a continuation of dioxane synthesis and found that it had been three weeks since my last visit. Distillation
took longer than I anticipated and I ended up going to bed at 2:00 am
I can see that in a couple of months work things might be a bit more settled and I might be able to do more. But then again, it is probable that
other priorities will sneak in and it will be just as difficult. Ultimately I have to recognise that a bit of me-in-the-lab time is important enough
for me to have to schedule it. And I have to accept that much of the time I will have to get my fix by dropping in here and reading.
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See that is me right there! Thanks for that j_sum1. I appreciate the advice.
"Question everything generally thought to be obvious." - Dieter Rams
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
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I usually try to run multiple low-maintenance experiments simultaneously while I do other things. I'm planning on using the barium hydroxide to purify
the product from a couple of experimental glyoxylic acid synths, but I'll also put some in a bottle so that I have some ready to go next time I want
some (it's pretty useful).
Technical grade barium carbonate is almost as cheap as dirt, but it is very impure. I think it's possible to prepare rather pure barium compounds from
it, though, if the right steps are taken.
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happyfooddance
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Posts: 530
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Location: Los Angeles, Ca.
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I just finished purifying some phenolphthalein that I made about a week ago. I used phthalic anhydride that I prepared from phthalic acid from
hydrolysis of phthalate esters extracted from scrap vinyl, and phenol that I prepared from aspirin from the dollar store. A lot of work but rewarding.
Now I have to prepare some standardized solutions (sodium carbonate, HCl, NaOH, ethanolic KOH)... It is hot in the lab though, so keeping everything
20°C is a chore that I am not looking forward to. Does anybody else feel like any time one task is completed, another 10 get added to the to-do list?
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