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Texium (zts16)
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[*] posted on 22-12-2015 at 08:36
Everyday Chemistry


Recently there's been discussion about how lately there has been much more talking than doing. One of the reasons for this, I think, is that the more experienced members find that some of the routine chemistry they do does not merit posting on here. For instance, while distilling nitric acid is an exciting milestone for a beginner, by the 3rd or 4th time it becomes rather mundane. So, this thread is simply to report the stuff that you do in the lab every day that isn't particularly novel. That way you can prove that you are doing and not just talking. :)

Example:
On Sunday, I replenished my stocks of nitric acid and chloroform. Yesterday I cleaned and reorganized my lab (I think a post to Tour my Lab is in order). Today, I'm going to dry and distill the crude chloroform, and I might make a batch of hydrazine sulfate later.




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[*] posted on 22-12-2015 at 09:13


There's been a flurry of interesting new syntheses and experiments on Youtube lately, a number of which are from members here, yet they have clearly chosen not to report on them here. I suspect that's because reporting on something you've done here has become a lose-lose proposition. Report something that isn't completely new, and you'll get "UTFSE". Report something new, it will be attacked mercilessly. That's why there isn't anything new and exciting being done: it is, it's just not being reported here.

I made purified calcium nitrate from cold-pack "calcium ammonium nitrate" (double salt), using two other OTC reagents and a process that, though exceedingly simple, doesn't seem to have been reported here yet. Not sure if this is "novel" enough to post about. At the same time, I'm attempting to produce calcium nitrate through a more-or-less novel (and much more time consuming) process, which is why I wanted some relatively pure stuff (for testing/comparison). This I will be reporting on in an existing thread.

[Edited on 22-12-2015 by MolecularWorld]




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[*] posted on 22-12-2015 at 09:21


I started making a heating mantle from sodium silicate, play sand, perlite, and a used toaster. First I removed the nichrome wire from the toaster and measured its resistance, determining that one piece was the correct size for making a 300 watt mantle. Then I dipped a 500 mL flask in wax and let it cool. Then I mixed sodium silicate with play sand to make a thick cement and spread a 0.25 inch layer on the flask. I then attempted to wrap the nichrome wire around it but found that the wire didn't want to hold in place, so I wrapped it around a pencil and held it there with a rubber band.
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Little_Ghost_again
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[*] posted on 22-12-2015 at 10:08


I spent an hour in a cow shed behind a cow with a glass jar and small can lighter gas. I was waiting for the cow to take a shit, after around 50 mins it did! However only after it had seen me put the jar down to rub my cold hands together!!

So I am still without fresh cow shit! Hopefully over the next few days I will capture some and place under a butane atmosphere until I can get it into my reactor.

Tried to purify my iodine by heating under sulphuric acid, was a good reminder to get a move on and make a new fume hood!

Trying to learn analytical chemistry and how to prepare standards, I will at this point be happy to get 3 out of 5 readings the same on titration!

Making a list of the reagents I need/want and how then going to work out how I can afford to get/make them.

Finally took my prized copper sulphate huge crystal out of the growing jar!! it has taken 16 months to grow and looked fantastic, I have taken care to razor blade any blemish as it grew and was very proud of it. I placed in a plastic display case thing you get from craft shops and went to go down stairs to show it off to the family, it was a great day for learning about gravity when I dropped the box down the stairs!

I thought copper sulphate crystals were a bit more sturdy than that! so now back to grinding it into a powder and starting again!

My copper nitrate crystal refuses point blank to grow past 1 1/34 inches so I guess its finished, its staying in the desiccator until I figure out how to preserve it!

Made some cardboard boiler pellets (biomass boiler) from cardboard mush and sawdust with a little sodium Chlorate added as the liquid, dried them down to around 15% moisture. I was going to try them out but on checking wikipedia it mentions chlorates and anything combustible not being a good idea, so now I dont know what I should do with them, part of me thinks just drop in a bucket of water and use as weed killer on the drive.

Part of me is curious how well they will burn if added to the boiler, I only used 2 grams of chlorate to a 2 gallon bucket of very wet mush so there cant be much chlorate in each pellet. Then I think of how much the boiler cost and therefore I am in a quandary.

Bleach experiments for making IPA chloroform have had mixed results, my lab is unheated and now drops below freezing at night! and gets to about 5c during the day.

My pristine clear 98% sulphuric acid is turning black/grey in the bottle......... peed off with that




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[*] posted on 22-12-2015 at 10:12


Quote: Originally posted by MolecularWorld  
There's been a flurry of interesting new syntheses and experiments on Youtube lately, a number of which are from members here, yet they have clearly chosen not to report on them here. I suspect that's because reporting on something you've done here has become a lose-lose proposition. Report something that isn't completely new, and you'll get "UTFSE". Report something new, it will be attacked mercilessly. That's why there isn't anything new and exciting being done: it is, it's just not being reported here.
Nah. It's hard to find the time, honestly. I'm a full-time mechanical engineer on top of getting a degree in chemistry on top of filming videos on top of being a homeowner. I'll get around to it eventually. I think if we get the chemfig LaTeX plugin I'll be motivated enough. :)

Lately in the lab I prepared pyridine from niacin including the prep of the chromite catalyst a la UC235, tested a new catalyst for the preparation of phenol from salicylic acid, made CrO3, hydrazine sulfate, CuCO3 and filmed/published the videos, and I'm working on a New Year's Eve ultra-fast thermite special because the fireworks will cover up the bang. I'll also be preparing pyridinium chlorochromate soon and I might use that to do a vid on benzaldehyde, but I need to make the benzyl alcohol video first. Busy busy.

The hydrazine prep used a new method and I'm working on a publication for that.

Quote: Originally posted by zts16  
I cleaned and reorganized my lab (I think a post to Tour my Lab is in order)..
Looking forward to it.



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[*] posted on 22-12-2015 at 10:23


I recently ampouled some of my more nasty chemicals (PBr3, TeBr4 in HBr) in perfectly sealed ampoules, so that they can be stored without issues. I usually do not write about such things ;)

I made some chemicals, to be used as display samples:
- Cs2TeBr6 (from HBr, Cs2CO3, and TeO2)
- HgCrO4 (from Hg, HNO3, CrO3 and NaOH)
- HgCr2O7 (from Hg, HNO3, CrO3)
- Ni(en)3SO4 (from (en) and NiSO4.7H2O)
- VO(acac)2 (from V2O4, H2SO4, (acac)H, and NaOH)
- shiny arsenic (from oxidized arsenic, dilute H2SO4, K2Cr2O7, Na2SO3)
- Cs-Cr-alum (from Cs2CO3, H2SO4, Cr2(SO4)3)
- Cu4I4(py)4 (from CuSO4, Na2SO3, KI, (py))

Some of these were smooth and easy synths, the Cs-Cr-alum and HgCr2O7 were a real pain in the ass. They do not separate easily and can only be prepared with huge losses. With the Cs-Cr-alum I finally gave up accepting loss of nearly half of the added Cs. I recovered most of that as CsClO4, which is easy to isolate and get in the pure state.

These were different small projects, took me a few Saturday mornings.

Besides that, I have been working on a library for polynomial root finding in Java, some routines being at standard IEEE 754 double precision, one routine at so-called double double precision (also in Java) and a multiprecision version, written in C and Java (using JNI as bridge between the two language domains). I use these libraries for all kinds of mathematical experiments. A web page will follow on those experiments soon and I will also make the software with source code available for download (suitable for Windows on x86-32 and x86-64 architectures and Linux on x86-32 and x86-64 architectures and ARM32 architecture).

Now you have an idea of what keeps me busy besides moderating sciencemadness and doing my job and taking care of my family ;)


[Edited on 22-12-15 by woelen]




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[*] posted on 22-12-2015 at 11:10


Quote: Originally posted by Little_Ghost_again  
My pristine clear 98% sulphuric acid is turning black/grey in the bottle......... peed off with that


Is it from dudadiesel in a HDPE bottle? Find a good glass bottle to transfer it into. I too, had a fit of rage when after a few months I saw the liquid appeared to have turned gray.

It seems to mostly be discoloration of the plastic. The acid itself is still pretty clear.
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Little_Ghost_again
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[*] posted on 22-12-2015 at 13:26


Quote: Originally posted by UC235  
Quote: Originally posted by Little_Ghost_again  
My pristine clear 98% sulphuric acid is turning black/grey in the bottle......... peed off with that


Is it from dudadiesel in a HDPE bottle? Find a good glass bottle to transfer it into. I too, had a fit of rage when after a few months I saw the liquid appeared to have turned gray.

It seems to mostly be discoloration of the plastic. The acid itself is still pretty clear.


Not sure who it was from, I got it from Amazon as it was cheap, a week later I went to get more and the listing had gone! but yes I think its a HDPE bottle, I did almost transfer to glass but I have a habit of dropping bottles.

Still I cant be having my clear sulphuric turning colour can I!

Reading up on making lead dioxide, I am interested in a perchlorate cell, I would rather not use the MMO for that.




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[*] posted on 22-12-2015 at 13:39


I have recently prepared a batch of KOCN, well, it´s not something I do everyday but one of my latest syntheses.
From urea and K2CO3.
Work-up is easy, but I don´t like it.
Another thing I have done was the epoxidation of styrene, and preparation of the diisopropylamide of indoleglyoxylchloride.

Also, washing beakers and flask for like two hours... don´t skip to tomorrow what you can do today, easily said but not so easily done :D
So, I´ve also prepared piranha solution exactly for that task...
Man, I wish I wasn´t so lazy... I wish I would clean them like I do with my dishes... But even more, I wish I had a laboratory dishwashing machine at home :D
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[*] posted on 22-12-2015 at 17:00


Quote: Originally posted by Little_Ghost_again  
I spent an hour in a cow shed behind a cow with a glass jar and small can lighter gas. I was waiting for the cow to take a shit, after around 50 mins it did! However only after it had seen me put the jar down to rub my cold hands together!!


Your dedication to science is astounding!




The single most important condition for a successful synthesis is good mixing - Nicodem
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[*] posted on 22-12-2015 at 17:59


I am visiting extended family for a few days but looking forward to getting back in the lab.
Before leaving I had some attempts at Si and Ti thermites. They went ok, but I am looking at getting a better quality product for the element collection.
When I get back I hope to have another go at the thermites. Also due for some work is the next round of aga's nitric acid challenge. My soy beans have been lying around for too long. There is also some iodine to make -- I will try a persulfate method, nitric acid to distill, sulfuric acid to boil down and a new method of making sulfuric acid to attempt. I will have some new glassware adapters arriving which will greatly improve my chlorine generation. I intend to make some more bromine at some stage. Rising up my list of things to do is to make some hydrazine sulfate. This is a new one for me and not something I had considered before. But I would love to make a copper mirror. As well as that I have come across a source of OTC lithium hypochlorite. I will use it as a hypochlorite source for a few things and then collect the lithium salt byproducts. Later I will have a go at lithium electrolysis.

On top of these projects is quite a lot of work making labels and taking photos of my element display. And also some cyanotype pictures to have a try at. At some stage I also intend to take pix of my lab for the tour my lab thread. I have been meaning to do that for months. Right now it is reasonably tidy and somewhat organised so it might be a good moment.

J.




A little shameless self-promotion: New stuff on the YT channel. Some premature celebration. Or you can tour my lab.
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[*] posted on 22-12-2015 at 18:13


The only chemistry I've done lately is revamp one of the labs involving nickel. We have some fancy new spectrometers that use fricken lasers and work better than the old spec 20s....except they only work at certain wavelengths, and nickel(II) just don't absorb worth spit in any of those wavelengths. The tris(glycinato) complex absorbs a lot better in at least one of those wavelengths.

Yeah, work-related, so off-topic for SciMadness.




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[*] posted on 22-12-2015 at 18:45


I've been intrigued with Magnolia trees. M. Grandiflora. I did a acetone extraction of 20 gms bark and yielded 1.1 gms yellow sorta crystally extract. THINK it is a mixture of honokiol and magnolol.



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[*] posted on 22-12-2015 at 19:26


Quote: Originally posted by arkoma  
I've been intrigued with Magnolia trees. M. Grandiflora. I did a acetone extraction of 20 gms bark and yielded 1.1 gms yellow sorta crystally extract. THINK it is a mixture of honokiol and magnolol.


Nice, does it smell like anything?

As for myself, I've just prepared prepared anthranilic acid from phthalic anhydride and got a nice yield of methyl anthranilate from it. I've also just prepared more nitric acid and used it for lead and silver nitrates(boring), and tomorrow I plan to investigate some coordination complexes of nickel(II).




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[*] posted on 22-12-2015 at 20:13


I've spent the bulk of the last week writing a disclosure to the USPTO. All the while, two 60 MHz NMR's were begging for my attention.

Bah,

O3




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[*] posted on 22-12-2015 at 20:14


the m. grandiflora has just finished flowering here. you will have to see whet you can get from the flowers!




Celebrating completion of element collection. Planning a display of some sort.
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[*] posted on 23-12-2015 at 02:32


Quote: Originally posted by Magpie  
Quote: Originally posted by Little_Ghost_again  
I spent an hour in a cow shed behind a cow with a glass jar and small can lighter gas. I was waiting for the cow to take a shit, after around 50 mins it did! However only after it had seen me put the jar down to rub my cold hands together!!


Your dedication to science is astounding!

LOL
In theory the center of a cow pat should be air free, but it dosnt work like that. I am after an organism that if I were rich I could buy! But being not so rich decided to go direct to the supplier :D.

I did eventually get the prize this morning, I should have known to go in the shed just after they are brought in.

Now my main reactor is complete, fingers crossed the pH drops by tonight




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[*] posted on 23-12-2015 at 07:20


My living room floor is covered with a layer of Magnolia leaves so they can dry. Can y'all tell my wife doesn't live with me LOL?

I steam distilled some bark the other day and all I got was a very weak hydrosol, no discernible oil but it did smell good.

Another note:

powdered cinnamon is EVIL. I'm bound and determined to pull off steam disty one of these days. Last night 1 liter RBF, a scant 200ml H2O, and 15gm cinnamon. AS USUAL, that crap turned into the crawling blob monster from a 50's horror film and crawled right up into my condenser again. :mad: Guess I'm going to have to buy some sticks instead of using whats laying around :P

BTW, this is a great thread, thanks ZTS




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[*] posted on 23-12-2015 at 07:58


Yeah, my one attempt at processing anything from cinnamon (actually cassia, same as you, I imagine) turned into a hideously slimy mess. The stuff is only 1-3% essential oil so good luck getting any reasonable product yield.

Easy to do steam distillations would probably be sweet orange rind and nutmeg. Nutmeg is also interesting in that the fat in it is almost entirely trimyristin. You can solvent extract the ground spice to give mass of great-smelling "nutmeg butter," which is steam distilled to obtain the essential oil. What's left over can be recrystallized from alcohol for trimyristin.

http://www.orgsyn.org/demo.aspx?prep=CV1P0538

Ether is quite unnecessary. I think I used hexanes.
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[*] posted on 23-12-2015 at 09:11


I did a steam distillation of ground cinnamon once before (and I made sure that it was real cinnamon). I got similar results. I had to cut it off early because it started foaming up like crazy, and it was before the advent of magnetic stirring in my lab, so most of the cinnamon formed a very hard lump at the bottom of the boiling flask that was bumping like crazy.

I did see a few drops of a yellow, oily liquid floating on the surface of the water in the receiving flask, but it wasn't enough to retrieve using a separatory funnel. So I solvent extracted it with chloroform, and got a lovely smelling chloroform solution of cinnamon oil which I still have.




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[*] posted on 23-12-2015 at 10:00


I have steam distilled cloves, sage fronds, and juniper fronds. All yielded nice smelling oils. Mass spectrometry of the juniper (arborvitae) oil showed many components which included thujone, camphor, and wintergreen.



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[*] posted on 23-12-2015 at 11:35


The compounds I mentioned in this thread are available at Onyxmet's webshop. Just visit his homepage: http://onyxmet.com/

and look at the latest additions. The last 7 or so are made by me :)

In this way, I obtain interesting chemicals. I do not ask money, we exchange materials.




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[*] posted on 23-12-2015 at 12:31


I've had good results on some steam disty's, just not daggum cinnamon.



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[*] posted on 23-12-2015 at 22:36


I spent a few hours today putting together a series of traps to protect my vacuum pump. I built this wooden rack to hold everything together in a neat assembly. I used a plank and a dowel that I had laying around, and gave it a couple coats of stain. The jars from left to right are empty, 50% NaOH, empty, conc. H2SO4, empty. It seems to be sufficient for removing acid fumes and water from a vacuum filtration apparatus. Condensation is observed in the inlet tube when in use, while the outlet tube appears to be completely dry.

IMGP0017.JPG - 546kB




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[*] posted on 24-12-2015 at 15:39


the only chemistry I have done today is internal-----------allowing my liver to dis-combobulate the ethanol in a lovely bottle of cabernet



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