Sciencemadness Discussion Board

Everyday Chemistry (provisional)

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DraconicAcid - 11-12-2020 at 19:37

I made it once, and I thought it smelled like celery.

TriiodideFrog - 12-12-2020 at 20:20

Made sodium hydroxide and calcium carbonate from sodium carbonate and calcium hydroxide.

MidLifeChemist - 12-12-2020 at 20:26

Quote: Originally posted by TriiodideFrog  
Made sodium hydroxide and calcium carbonate from sodium carbonate and calcium hydroxide.


Interesting. I made sodium carbonate by putting baking soda into the oven.

arkoma - 12-12-2020 at 21:20

Quote: Originally posted by Bedlasky  
Arkoma: How propyl salicylate smells like? I plan to make propyl benzoate or salicylate, I am not sure which one I'll pick.


Similar to the methyl ester, but not as "strong". Smells good.

j_sum1 - 12-12-2020 at 22:34

I have made ethyl salycilate before. It is really similar to methyl salycilate. Maybe not quite as feisty. I eould imagine that the propyl ester follows trend.
Having said that, ester odours do present surprises.

Bedlasky - 16-12-2020 at 14:47

Yesterday I tried to make sodium orthoperiodate by persulfate method from NaI. I started from KI, which I converted to NaI by precipitation of potassium as bitartrate. Than I added 30 g of NaOH and 77,5 g of Na2S2O8 in small portions (after each addition quite exothermic reaction took place). Than I heated it in hot water bath for 15 minutes, added 15g of NaOH and after that I heated it for 30 minutes. Than I added 100 mils of water to dissolve all sulfate and heated it for 10 minutes. I allowed the solution to cool for several hours, decanted as much liquid as possible and added another 50 mils of water, heated for a while and again let it cool. Just now I filtering the solid and wash it with ice cold distilled water.

arkoma - 16-12-2020 at 15:05

Tossed some n-propyl alcohol, citric acid, and few drops h2so4 into a RBF, Refluxing now.

j_sum1 - 16-12-2020 at 20:42

Quote: Originally posted by arkoma  
Tossed some n-propyl alcohol, citric acid, and few drops h2so4 into a RBF, Refluxing now.


Your target is an ester I presume.


I am nearing the end of preparing some silver nitrate. I had two nearly empty containers that had partially decomposed and looked quite grey. I also had some AgCl precipitate that I had collected following some student experiments. (Might be some AgI and AgBr in there too.) As well as that were several filter papers of silver crystals: the result of silver tree experimemts. These had copper contamination and were probably impure for other reasons too. I have combined it all together and have converted it all to elemental silver: I probably have around 20-30 grams of black finely divided silver at the moment. Just need to hit that with some nitric acid.

I think I might do an ester or two just for fun before Christmas. I discovered I have some butanol the other day which might be interesting.

TriiodideFrog - 17-12-2020 at 04:51

Quote: Originally posted by MidLifeChemist  
Quote: Originally posted by TriiodideFrog  
Made sodium hydroxide and calcium carbonate from sodium carbonate and calcium hydroxide.


Interesting. I made sodium carbonate by putting baking soda into the oven.


I see. I made mine by heating it on a saucepan.:)

arkoma - 17-12-2020 at 09:28

Yes, after an ester. p-toluenesulfonic acid is on my list for later Today.

teodor - 24-12-2020 at 04:18

I am 4 days experimenting with making di-n-butyl ether, preparation III,57 by Vogel. Methods of separation given in the book don't work for me for some reason: I've got less than 5ml yield from 62ml of the alcohol with 50% H2SO4 method. Making the synthesis 3 times I found that the problem is that the ether creates a stable mix with n-butyl alcohol and this mix separates during 2nd H2SO4 wash as a middle layer which is much voluminous than the pure ether (top) layer.
I tried to make this alkaline and purify by CaCl2 method (2nd method of separation given in the book) but the result is that the final liquid dissolves a bit of CaCl2 used for final drying creating a paste consistency.
What really works is separating this n-butyl alcohol + di-n-butyl ether middle layer and treating only this twice with 25ml of 50% H2SO4 solution. First time it gives the same 3 layers, few ml of the ether and most volume in the mix, but the second treatment of this middle layer with 50% H2SO4 gives very thin middle layer, so this way I can collect most of the product.

Also I found than the technique of initial mix of n-butyl alcohol and sulfuric acid before synthesis is somehow important - when I poured the acid by pipette it created to much heat in too little volume forming brown spots which was a problem - they accumulated the heat during the synthesis and the whole product became coffee-brown this way. But when I mixed alcohol with the acid pouring the latest from a beaker the liquid stayed clear at the beginning till the end.
Unfortunately this had no impact of the middle layer formation.

Now I am thinking how dry was my n-butyl alcohol. Some water in it can cause more alcohol residue because the Dean-Stark tube collects the amount calculated based on 100% dry alcohol.

I think wikipedia describes di-n-butyl ether smell as "peculiar" and it is not far from truth - the smell is very interesting and not similar to something else. I can find connection with n-butyl alcohol smell but it is changed the way I didn't encounter before. I think it would be interesting to check will I precipitate the same relation between alcohol and ether smell for higher alcohols.

[Edited on 24-12-2020 by teodor]

[Edited on 24-12-2020 by teodor]

teodor - 27-12-2020 at 06:13

I distilled dibutyl ehter. I did it in a claisen flasks with a fractionating arm - not the best glassware for this purpose considering that the boiling point of Bu2O is 142C and the flash point is 175C, so I had no more than 33 degrees in between - but my glassware collection is still not full and I don't have anything more suitable for distilling small volume like 20-25ml.
So I put a second thermometer inside the flask itself to control the temperature over the liquid surface. I used a heatgun between 360 and 370C heating the pear-shaped flask from its very bottom allowing the stream of hot air touch the liquid first and then sides of the flask. After some lower-boiling component with "chloride" smell (it appeared after drying on CaCl2) I've got a perfect fraction 139-141C and at this point the temp. inside the flask touched 156C - the limit of my second thermometer, so I stopped the process preferring low yield to compromised safety.
Probably will try to distil the rest after getting the glassware with more short path before a condenser.

[Edited on 27-12-2020 by teodor]

[Edited on 27-12-2020 by teodor]

j_sum1 - 27-12-2020 at 19:42

Currently chugging away at a synthesis of ammonium oxalate.
I have an ammonia generator feeding into an oxalic acid solution via an inverted funnel. (I never enjoy working with ammonia: it is fickle when it comes to suck-back and accidental dissolving.)

One thing has me intrigued: When I first started pushing the NH3 into the solution, a precipitate started to form after only a minute or so. Then I realised I had forgotten to put the receiving beaker in a cold water bath. A couple of minutes after packing it with ice, the solution completely cleared up. I am unsure whether this is an effect of temperature or whether I had first made some monoammonium salt, or something else. Any ideas?


I intend to use the product to separate out cobalt and lithium salts derived from a growing pile of Li-ion batteries I have.

RustyShackleford - 28-12-2020 at 03:16

Quote: Originally posted by j_sum1  
One thing has me intrigued: When I first started pushing the NH3 into the solution, a precipitate started to form after only a minute or so. Then I realised I had forgotten to put the receiving beaker in a cold water bath. A couple of minutes after packing it with ice, the solution completely cleared up. I am unsure whether this is an effect of temperature or whether I had first made some monoammonium salt, or something else. Any ideas?

Probably just the solution at the surface becoming saturated. Ive seen similar with HCl scrubber

j_sum1 - 28-12-2020 at 03:41

Quote: Originally posted by RustyShackleford  
Quote: Originally posted by j_sum1  
One thing has me intrigued: When I first started pushing the NH3 into the solution, a precipitate started to form after only a minute or so. Then I realised I had forgotten to put the receiving beaker in a cold water bath. A couple of minutes after packing it with ice, the solution completely cleared up. I am unsure whether this is an effect of temperature or whether I had first made some monoammonium salt, or something else. Any ideas?

Probably just the solution at the surface becoming saturated. Ive seen similar with HCl scrubber


I don't think so. When I was preparing the ice bath, I took it off the stirrer and a good crop of crystals rained down: to a depth of nearly 1cm in a 1L beaker. There was enough that it took s bit of work for the stir bar to engage again.

teodor - 1-1-2021 at 07:04

I have distilled methyl salicylate. It's a good start of the new year - the first batch of the crude ester I've got more than 2 years ago, but the distillation at 221-224C was a challenge. Today I used a mercury thermometer calibrated on 1-decanol. It allowed me precise temp. control during the process (and I didn't get any success with other types of thermometers). As a heat source I used a heatgun @ 450-460C

arkoma - 22-1-2021 at 10:01

Brought two ounces of turmeric home from Mexico last year (raided Mom's spice cabinet) and fnally Soxhlet extracted it. Turned a bit of the resultant into Rosacyanine with Boric Acid. Alas, I had my phone and a pair of pliers in the same back pocket yesterday (and sat down), so no pics yet.

Tsjerk - 22-1-2021 at 14:15

Quote: Originally posted by arkoma  
Brought two ounces of turmeric home from Mexico last year (raided Mom's spice cabinet) and fnally Soxhlet extracted it. Turned a bit of the resultant into Rosacyanine with Boric Acid. Alas, I had my phone and a pair of pliers in the same back pocket yesterday (and sat down), so no pics yet.


Cool, I would like to see those photos.

arkoma - 22-1-2021 at 16:35

i'll rig up the webcam. pretty cool results from basically the spice cabinet and roach proof. and i forgot to mention the emerald green of the Boron ion in a flame.

KMnO4 recrystallisation suggestions

Sulaiman - 23-1-2021 at 03:27

I'm recrystalising some potassium permanganate to try to get as little impurities as practical.
( https://www.sciencemadness.org/whisper/viewthread.php?tid=15... )
I made a near saturated solution of commercial grade potassium permanganate in distilled water and left it for the water to slowly evaporate :

KMnO4 crystalising.jpg - 82kB

does anyone know of a way to stop crystals forming on the walls above the liquid level ?
as I assume they will be no more pure than the liquor below so a waste of evaporation time - which is already about a month.
(I'm hoping for at least one 'nice' crystal at the bottom of the jar, and I've distilled some sulphuric acid already).

can anyone give me a guestimate of how many times to recrystalise KMnO4 to obtain potassium permanganate pure enough for the experiment in the thread that I pointed to above ?

AvBaeyer - 23-1-2021 at 18:42

Sulaiman,

Potassium permanganate needs to be recrystallized from water very quickly and with minimal light exposure. The compound will decompose in water on long standing or excessive heating which you can note by a brown film on your recrystallization container. If you do not work fast, your sample will contaminated with manganese dioxide (the brown color.)

According to Perrin and Amarego (Purification of Laboratory Chemicals):

1. Crystallize KMnO4 from hot water at 65 C using 4 ml per gram. filter then dry in a vacuum desiccator over CaSO4. [Though not mentioned, I assume that the solution is cooled to ambient before filtration.]

2. Saturate an aqueous solution at 60 C, cool to room temperature in the dark the filter through a sinter glass funnel. Allow the filtrate to evaporate in air in the dark for 12 hours, decant the supernatent from the crystals which are dried as quickly as possible on filter paper.

One thing seems to be clear - do not overheat and work quickly.

Hope this helps,
AvB

rosocyanine

arkoma - 23-1-2021 at 21:50

Pictures from the other day.

https://en.wikipedia.org/wiki/Rosocyanine


Turmeric extract 91% IPA
2021-01-23-003324.jpg - 35kB

After gentle heating/stirring with Boric acid
2021-01-23-003312.jpg - 48kB


Hard to see the green of the Rosocyanine, but it's there
2021-01-23-005128.jpg - 41kB

ChemTalk - 24-1-2021 at 09:12

We've been trying the reaction between potassium permanganate and hydrogen peroxide in a few slightly different ways.

It's a simple well-known reaction but we think it has a sweet spot in the category of easy yet somewhat dramatic reactions / experiments.

Piroz - 24-1-2021 at 14:05

I started with winemaking (dog rose wine) as source of carbon dioxide. Few months ago I got by this way sodium bicarbonate and ammonium bicarbonate (and got some apple cider by the way). Now it's time to potassium bicarbonate from wood ash extract, it's needed for purification of potassium compounds from ashes- by crystallisation of KHCO3.

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[Edited on 24-1-2021 by Piroz]

arkoma - 30-1-2021 at 01:35

clobbered together a small electric furnace this afternoon. can finally have some CaO; have some lime in it now.

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[Edited on 1-30-2021 by arkoma]

karlos³ - 30-1-2021 at 18:04

My stirrers heating broke down(loose contact) and I tried to fix it...without being good or even skilled with technic stuff but more like my hands growing out of my ass, and the inevitable happened, I failed to put it together and don't want to try it myself in the fear of irreversible damaging it.

But I had a reaction to run, a ring closure/amidation for thalidomide, and simply tried it on the hotplate with four little stirbars as sort of boiling chips and as a help when swirling manually.
Worked as expected, surprisingly, even slightly better than the last time!

Encouraged by this, I spontanously made an experiment under the same conditions, except with oleic acid as substrate, to produce oleamide.
Worked fine too!

That felt a bit archaic, observing everything with hawkeyes throughout the reaction(only 45min each), but I am proud to be able to improvise , with insufficient equipment and all, and that without being affected negatively, or even at all by this drawback :)

But I already look forward to get back to my the pet-project(s) when a stirrer is on hand... those two amidations were just a poor substitute for it, but at least I could still do a little bit of the simple lab work.

arkoma - 1-2-2021 at 13:16

fractional distillation of EtOH. notice the SM patch......



2021-02-01-151249.jpg - 67kB

ChemTalk - 1-2-2021 at 14:24

Quote: Originally posted by arkoma  
fractional distillation of EtOH. notice the SM patch......





I keep noticing the nice periodic table.

arkoma - 4-2-2021 at 15:08

Success!!! CaO. Roasted pickling lime at a red heat for an hour. Put a couple grams in a piece of foil and dripped water on it, and it proceeded to get HOT and sizzle. YAY. 99% EtOH here I come!!!

Broke the EtOH and H2O Azeoterope, yippee!!

arkoma - 5-2-2021 at 20:26

Had a terrible recovery, but don't care, I broke the ^&^%&*$ azeotrope!!!
Been an obsession.....

50 gms CaO and 250ml of 95% EtOH were refluxed for five hours, then allowed to sit for 8. I kept my moisture discipline up (drying tubes, quick stoppering, oven dried glass), and when I distilled the mixture I got 70mls that read about 98-99 on my hydrometer (my house just happened to be 20C inside, no temperature corrections necessary).

Procedure from Vogel's Third.

What happened to my potassium permanganate ?

Sulaiman - 11-2-2021 at 17:48

Some re-crystallised potassium permanganate

kmno4 start.jpg - 833kB

I left the KMnO4 crystals exposed to air for a couple of weeks,
in the cupboard where I keep glassware and solid chemicals in 'sealed' containers - no liquids,
and found this

kmno4 after.jpg - 1.1MB

what happened ? what are the white crystals ?

(the most volatile substances in the cupboard are;
ammonium bicarbonate, TCCA, sodium metabisulphite
... all kept in glass bottles)

Unknown metal oxide

arkoma - 13-2-2021 at 09:59

Wasn't my intent, but when melting some white metal the other night I inadvertently got some (X)O. Opened the front of my furnace and there was what looked like and actual flame coming off the crucible content.


20210213_123606.jpg - 2.9MB

Texium - 23-2-2021 at 19:47

Testing to see if posting to this thread works...

Piroz - 24-2-2021 at 12:50

I used my furnance to preparation calcium oxide from old, carbonated slaked lime. I need CaO for preaparation both ammonia and calcium nitrate.

https://youtu.be/d6vDtND4HSU

Bedlasky - 26-2-2021 at 15:11

Currently waiting for crystals of copper(II) tris complexes - specifically [Cu(H-1tris)2(H2O)] and [Cu(tris)4](ClO4)2. The latter one should be energetic.

j_sum1 - 5-3-2021 at 21:21

Did some titration with my son. Just for the fun of it.
Tried out a few different indicators. And he got to play with some precise measuring equipment.

IMG20210306150758.jpg - 2.8MB

ChemTalk - 6-3-2021 at 08:24

Quote: Originally posted by j_sum1  
Did some titration with my son. Just for the fun of it.
Tried out a few different indicators. And he got to play with some precise measuring equipment.



Oh, that's awesome, sounds like fun. My son might do some chemistry this weekend also.

njl - 6-3-2021 at 09:24

What the heck is the difference between diazomethane and methane diazonium salt? Other than the obvious structural difference. How do their reactivities compare? One review says they're completely different and yet another implies they are interchangeable. Can diazonium compounds eliminate H+ to form a diazo compound?

Texium - 6-3-2021 at 15:12

Diazomethane is a highly unstable and reactive gas, but it is still isolable and finds a lot of use in synthesis. The methyldiazonium ion makes it looks tame by comparison. It is so unstable that it is only observed transiently. Aliphatic diazonium salts are generally far too reactive to be synthetically useful or safe, while aryl diazonium salts are significantly more stable. In the future, please cite these “reviews” that you speak of. I don’t know why anyone would say that the two species are equivalent. Perhaps they exist in equilibrium, under certain conditions, but they are not the same thing.

Piroz - 8-3-2021 at 15:20

Finally I got potassium chloride from wood ashes practically free from sodium compounds. I used crystallisation from saturated hot solution in plastic bottle (>50 deg. C), sodium was removed in crystalline mass, leaved potassium chloride in the solution. However crystallisation from cold solution (several times) wasn't enough to remove some sodium.
Flame analysis suprised me, potassium chloride from chem store reffered as 99% purity have more sodium than my potassium chloride from wood ashes.

Flame_colour1.jpg - 60kB Flame_colour2.jpg - 50kB Flame_colour3.jpg - 53kB Flame_colour4.jpg - 42kB

[Edited on 8-3-2021 by Piroz]

j_sum1 - 8-3-2021 at 15:27

Nice work, Piroz.

njl - 8-3-2021 at 16:05

Is there a conclusion one can draw from that?

arkoma - 8-3-2021 at 21:41

Yes, from the flame colors. Takes barely any Na ions to color a flame yellow. The hot xtallized KCl is a lovely violet.

*edit* Conclusion being that his own work-up had a much better flame color. obviously violet, unlike the commercial. Hence his contained less Na ion.

[Edited on 3-9-2021 by arkoma]

Bezaleel - 11-3-2021 at 15:05

Good job, Piroz!

Elemental Phosphorus - 14-3-2021 at 20:04

I just did a little extraction of capsaicin from dried habaneros, hope to do it on a larger scale this week, but it was just a small scale run.

Wish I had a soxhlet extractor to use, but I just used boiling acetone in a flask and then poured it off and evaporated. Final product was a little bit of orange oil, and of course I had to taste a tiny bit, so I just put a knife tip in it and tasted it and it was definitely spicy (I know it’s not best practice, but I had to try).

Also did woelen’s demonstration with the oxidation states of vanadium, since I had some V2O5 laying around.

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arkoma - 15-3-2021 at 18:42

i've only used my soxhlet a few times, but it is dang sure a cool piece of gear. seems like it was <$30US from nanshinglass

Bezaleel - 16-3-2021 at 12:42

Vacuum setup repairs
The rotary vane pump I use is not really suited for pumping on liquids which give off corrosive fumes. Obviously, if you ignore that, then your setup will degrade over time. I took apart several joints of the type shown in the picture.
IMG_3654.JPG - 416kB
On the majority of the flanges, there was corrosion, revealing itself as white powdery crusts. Typically, the components shown are made of aluminium, which is a really bad choice for components used in a corrosive environment. (But who would dare to complain when you receive all of this for free?)

Anyway, there are two points of interest:
* For one joint I did not have a spacer when I received the vacuum components, and I made one from PTFE on a lathe (shown in the photo). The connection which had this spacer was much less corroded than the joints which have aluminium spacers.
* I polished the flanges with a household grinding pad and some household grinding/polishing powder, washed it and let everything dry over night. I re-assembled it the other day using a very small amount of silicone vacuum grease on the flanges and the O-rings.

When I pulled a vacuum I was disappointed to stay at 10 mBar of pressure, but after the system had dried for another day, it rapidly went down to the limit of my pressure gauge. So apparently, it was due to droplets of water which were evaporating that the pressure initially stayed at 10mBar.

njl - 18-3-2021 at 06:55

How will the basicity of sodium isopropoxide compare to that of sodium methoxide in the claisen condensation, and how might that effect the reaction outcome? I can't find anything detailing NaOiPr properties.

DraconicAcid - 18-3-2021 at 09:02

Quote: Originally posted by njl  
How will the basicity of sodium isopropoxide compare to that of sodium methoxide in the claisen condensation, and how might that effect the reaction outcome? I can't find anything detailing NaOiPr properties.


I would expect it to be slightly more basic, but suitable.

PS- anyone know if magnesium alkoxides would work in that reaction? I've got far more magnesium than sodium.....

[Edited on 18-3-2021 by DraconicAcid]

njl - 18-3-2021 at 09:35

Yes, I believe even MgO can be used to form the basic species.

DraconicAcid - 21-3-2021 at 21:30

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.

njl - 22-3-2021 at 08:15

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.

arkoma - 11-4-2021 at 09:53

INitroethane. Just a few ml, but I count it as a success.

IMG_20210411_124920009.jpg - 1.9MB IMG_20210411_124933384.jpg - 1.9MB

Mateo_swe - 18-4-2021 at 05:38

arkoma, what procedure did you use?

arkoma - 18-4-2021 at 12:56

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]

JJay - 15-8-2021 at 06:40

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.

S.C. Wack - 15-8-2021 at 20:55

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]

JJay - 19-8-2021 at 17:26

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.

Texium - 19-8-2021 at 17:44

What were you using to clean up the borohydride?

JJay - 19-8-2021 at 19:14

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]

JJay - 20-8-2021 at 13:26

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 - 20-8-2021 at 13:46

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 - 21-8-2021 at 10:58

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.

DraconicAcid - 21-8-2021 at 11:14

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).

JJay - 21-8-2021 at 13:56

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.


charley1957 - 8-10-2021 at 08:33

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.

arkoma - 10-10-2021 at 10:48



PGM extraction.jpg - 1.4MB

Hopeful platinum group metal extraction with boiling Aqua Regia and ground up roasted cat converter honeycomb.

Texium - 10-10-2021 at 14:14

Nice! I like your fume hood :P

arkoma - 11-10-2021 at 12:04

Quote: Originally posted by Texium  
Nice! I like your fume hood :P


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.............:D

arkoma - 13-10-2021 at 09:06

Phenol from salicylic acid. No short path condenser but this adapter seems to be working well.



phenol.jpg - 1.2MB

j_sum1 - 31-12-2021 at 21:28

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.

DraconicAcid - 31-12-2021 at 23:04

Made some copper and iron acac complexes.

B(a)P - 1-1-2022 at 01:59

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!

S.C. Wack - 1-1-2022 at 14:33

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 - 1-1-2022 at 15:34

Quote: Originally posted by B(a)P  

Is that Diggers?

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]

Rainwater - 1-1-2022 at 20:05

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.

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j_sum1 - 5-1-2022 at 20:32

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.

j_sum1 - 9-1-2022 at 00:50

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.

AvBaeyer - 9-1-2022 at 19:41

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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