Sciencemadness Discussion Board - Latest chemical order?

A really nice one would be thorium violurate

I think that too

, but no more violuric acid, i used all.

woelen - 6-9-2021 at 00:17

I actually do have some thorium metal, but I never did any experiments with that. It was donated to me, more than 10 years ago and I put it on my website:

https://woelen.homescience.net/science/chem/compounds/thoriu...

I will not break this sample. Although it is not really nice looking, it is interesting to have around. Only years, after I received the sample, I began to realize how rare this must be.

vano - 6-9-2021 at 00:21

Quote: Originally posted by Fery

Here in CZ I was able to buy thoriated tungsten welding electrodes (TIG), they contain upto 4% of ThO2, but W must be dissolved first to obtain ThO2. Nobody uses these electrodes today because of choices of less toxic compounds available. The shop offered me a discount and they found 2 more electrodes in stock so they contacted me later whether I wouldn't like to buy also these extra electrodes which were not listed in eshop (I added to cart all pieces available in their eshop system so they correctly presumed I would like to buy everything they have).

I have lots of Czechoslovakian chemicals, almost all is analytical reagent, maybe they also produced uranium and thorium salts for analytical chemistry. In those days, their salts were not considered as dangerous.

vano - 6-9-2021 at 00:23

I actually do have some thorium metal, but I never did any experiments with that. It was donated to me, more than 10 years ago and I put it on my website:

https://woelen.homescience.net/science/chem/compounds/thoriu...

I will not break this sample. Although it is not really nice looking, it is interesting to have around. Only years, after I received the sample, I began to realize how rare this must be.

Yes, some compounds are better stored than used. I think so because it has a different charm.

woelen - 29-10-2021 at 07:08

I purchased an ozone generator tube, with a separate adjustable power supply (3 ... 40 W high frequency high voltage) and a separate quartz tube for conversion. A little air pump (5 liter per minute) is delivered with the ozone generator, but I'll probably not use that. I have an oxygen generator, which can generate 1 liter per hour at 93% O2, or 2 liter per hour at 70% O2.

The tube apparently is designed for a somewhat higher flow of 5 liter per minute, but probably lower flows will work as well, if you crank down the power output of the high voltage generator.

With the ozone I want to do interesting experiments. Only small amounts of ozone can be made with this device (max 3 grams per hour, according to specification, but I do not believe that figure). Probably less than 1 gram per hour, but it should be enough for small scale ozone experiments.

CharlieA - 29-10-2021 at 15:23

......

With the ozone I want to do interesting experiments. Only small amounts of ozone can be made.....

Please keep us posted; I am sure that your experiments will be very interesting.

itsallgoodjames - 3-11-2021 at 16:17

My chemcraft order has arrived!
50g iodine
10g HgCl2
100g NaI
100g sodium metal

CS2 ?

soreff - 9-11-2021 at 11:35

Can anyone suggest a supplier of CS2 that will ship small quantities
(around 10ml - 100ml) to individuals in the United States? I'd like to
grow sulfur crystals by slow evaporation, and, as far as I know, CS2
is a much better solvent for S8 than anything else. Yeah, I know it is
carcinogenic - I'd be doing the evaporation outside.

itsallgoodjames - 9-11-2021 at 11:43

Can anyone suggest a supplier of CS2 that will ship small quantities
(around 10ml - 100ml) to individuals in the United States? I'd like to
grow sulfur crystals by slow evaporation, and, as far as I know, CS2
is a much better solvent for S8 than anything else. Yeah, I know it is
carcinogenic - I'd be doing the evaporation outside.

Provided you don't mind buying 500ml, chemsavers has it.

If you want a smaller quantity, it may be best to message mario840 or chemship1978. They're both from Poland (if I recall correctly), but shipping of 100ml probably won't be too expensive.

The main danger of CS2 isn't that it's carcinogenic, it's the flammability. CS2 is very volatile, and it's vapors have an autoignition point of around 100ºC.

timescale - 9-11-2021 at 11:57

Can anyone suggest a supplier of CS2 that will ship small quantities
(around 10ml - 100ml) to individuals in the United States?

Chemsavers lists CS2 on their website, but when I asked about it I was told it's on the "only real labs with commercial addresses can buy" list.

LabDirect is the only domestic seller I know of: https://www.labdirectllc.com/product/CS2/107

soreff - 9-11-2021 at 11:58

Quote: Originally posted by itsallgoodjames

Many Thanks!

Best wishes,
-Jeff

woelen - 12-12-2021 at 11:19

I ordered 4 small bottles of CH2Cl2 (4 x 500 ml), now that it still is possible to obtain this. It looks like the sale of DCM to private individuals is going to be forbidden in the EU. De oplosmiddelspecialist in the Netherlands already does not sell it to belgian residents anymore, and sale to dutch residents seems to be limited to 300 ml.
I do not use DCM a lot, with these 4 bottles I will have enough for many years to come. DCM is not something you can easily make at home, making it is much harder than making chloroform. That's why I ordered it.

yobbo II - 16-12-2021 at 10:27

You can purchase DCM + Methanol paint remover, 5L, in car accessory shops for about 30 Pounds in the UK.
It is for 'professionial' use only.

Yob

aab18011 - 17-12-2021 at 06:44

New chemical shipment came in last week,

-500g of an old phenol bottle from TCI that is easily 8 years old but still unopened (was cheap as hell, but I need some ideas on what to do with it)
-50g of Oleum (30%)
-100mL THF
-250mL of EtOH (99.99% food grade and kosher, who knew it would or could be kosher)
-50g of Sn
-100g of Sodium Azide
-250mL of Bromobenzene
-50mL of Acetic anhydride
-250mL of 38% H2O2
-100g of NaNO2
-75g of Iodine (elemental)

Also, LabDirect is the best place to go in my opinion. I have dealt with others but Richard C. (The owner) is a great guy and actually loves hobby chemistry. He has frequently given me discounts and will always help you find the right price. I usually email him with a cas number and the use for it. Usually if its water sensitive I tell him and he will find a cheap supplier. He has even helped me reduce the price of overseas stock. Im 100% sure you can find a cheap CS2 supplier through him.

[Edited on 12-17-2021 by aab18011]

[Edited on 12-17-2021 by aab18011]

yobbo II - 21-12-2021 at 16:47

In relation to dichloromethane, this stuff contains it.

https://www.ebay.co.uk/itm/384345107507?hash=item597cc0ec33:...

Langlow strip away pro.

Yob

MidLifeChemist - 1-1-2022 at 19:37

Hot Xylene should also work, and it is easy to get

B(a)P - 20-1-2022 at 13:21

2100 L of argon!

CharlieA - 20-1-2022 at 14:34

It seems to me that the volume of that cylinder is somewhat less than 2100L. Is that the volume that the argon would have at 1 atm Pressure? I'm just confused (not that is an unusual state for me!)

B(a)P - 20-1-2022 at 14:58

Quote: Originally posted by CharlieA

It seems to me that the volume of that cylinder is somewhat less than 2100L. Is that the volume that the argon would have at 1 atm Pressure? I'm just confused (not that is an unusual state for me!)

You are correct, it is a D size cylinder. It holds compressed argon that is the equivalent of 2100 L at STP.

pantone159 - 20-1-2022 at 15:21

Bromocresol purple, powder, water soluble, 1g.
'Bromothymol blue', Na salt, powder, WS, 5g.
Fructose, purified, 25g.
D-glucose, anhydrous, reagent grade, 100g.
Lithium chloride, granular, lab grade, 100g.
Oxalic acid 2-hydrate, crystal, ACS, 125g.
Phenol red, Na salt, WS, indicator powder, O.R., 5g.
Sodium phosphate, dibasic, anhydrous, ACS, 100g.
Sodium tungstate, granular, reagent grade, 25g.
pH paper, 1-12, #50.

I suspect that my 'bromothymol blue' is actually bromophenol blue. When I dissolve some of this in water, it makes a rather strange and interesting colored solution. When I look though a large thickness of solution, the color is red. But looking at a small thickness, the color is green instead. (And little bits of the solution that dry on the sides of the vial are blue.) This optical behavior seems to be characteristic of bromophenol blue, but not of bromothymol blue.

I intend to prepare some pH buffers to evaluate which compound this really is, the yellow-blue transition point is different by about 3 pH units between the two.

Bedlasky - 20-1-2022 at 20:42

Bromophenol blue should be blue in water. Bromothymol blue green. Bromothymol blue in conc. HCl should give red colouration (at least according to wiki).

pantone159 - 21-1-2022 at 07:05

I think I have the sodium salt of whatever indicator I have, so it is, I believe, in a concentrated solution at the midpoint of the color change, so green. (Sort of, the same green solution is actually red if you look through a thick section of the solution. It is rather interesting.) With much more dilution with H2O I get a slightly greenish yellow solution.

I do see a color change at very low pH: A 2.7 mol/kg solution of HCl gave a red-orange color, very distinct from the yellow color, and a 2.0 mol/kg solution of H2SO4 also gives a red-orange color, perhaps not as strong colored as the HCl one. In both of these cases, some solid precipitate seems to form.

I wondered about the wikipedia notes on the red color, I find no other references besides that photo, and the red color change is disputed in the wikipedia talk section. But my indicator does indeed change to a reddish color at pH < 0.

I think I will try and prepare a pH 5.4 solution. Bromophenol blue and bromocresol blue should be fully blue at this pH, while bromophenol blue should be fully yellow.

The wikipedia entry for bromophenol blue states the following, which is consistent with my indicator:
In solution at pH 3.6 (in the middle of the transition range of this pH indicator) obtained by dissolution in water without any pH adjustment, bromophenol blue has a characteristic green red colour, where the apparent colour shifts depending on the concentration and/or path length through which the solution is observed. This phenomenon is called dichromatic color.[7] Bromophenol blue is the substance with the highest known value of Kreft's dichromaticity index.[8] This means it has the largest change in colour hue, when the thickness or concentration of observed sample increases or decreases.

[Edited on 21-1-2022 by pantone159]

pantone159 - 2-2-2022 at 12:34

I conclude that my indicator is indeed bromothymol blue, as claimed by the seller, and not bromophenol blue, as I had suspected.

I prepared some pH buffer solutions, using preparations from CRC handbook, to cover the range of bromothymol blue, bromophenol blue, and bromocresol green, and added some of the indicator to each. The colors observed match that for bromothymol blue, and not the other two indicators.

The actual vs expected result for these indicators:
pH actual bromothymol blue bromophenol blue bromocresol green
< 3 yellow yellow yellow yellow
3.0 yellow yellow yellow [edge] yellow
3.8 yellow yellow green [mid] yellow [edge]
4.6 yellow yellow blue [edge] green [mid]
5.4 yellow yellow blue blue [edge]
6.0 yellow (slt green?) yellow [edge] blue blue
6.8 green green [mid] blue blue
7.6 blue (slt green?) blue [edge] blue blue
9.2 blue blue blue blue

However, a strong solution of this indicator does show the dichromatic effect which is very pronounced for bromophenol blue. The second photo shows the indicator solution in transmitted light: When looking through a thick portion of the solution, the color is red. But when looking at a thin portion, i.e. the meniscus at the surface, the color is green. My photo is not great but the different colors are visible.

ave369 - 13-2-2022 at 09:36

Recently, my age-old interest in ferrates was piqued by a recent purchase: a mixture of potassium permanganate and sodium ferrate. This mixture is sold OTC in my country because pure potassium permanganate is a listed chemical.

The product looks like a gray powder (sodium ferrate) with purple-black crystals (potassium permanganate). It does not appear possible to physically separate them. Upon dissolving, it forms a reddish-purple solution, purpler than pure permanganate but redder than pure ferrate.

If sulfuric acid is added to the solution, oxygen is evolved, and the color shifts to pure permanganate purple as the ferrate decomposes.

I've performed some experiments with this mixture. It does oxidize CoCl2 to Co2O3 and Cl2. It also precipitates barium ferrate with a soluble barium salt, but I failed at isolating barium ferrate because I tried to use a fritted glass filter and the gel-like precipitate clogged it.

Herr Haber - 2-3-2022 at 07:48

2x 500ml Butyric acid repackaged from HDPE to 1L glass bottle.

The place stinks, I feel like going out for a walk...

Fery - 2-3-2022 at 21:27

Trash away the old plastic bottles. I repackaged butyric acid from plastic to glass few years ago and put the bottle outside of house as I was curious how long it will last to lose the stinky smell... it lasted for few months for butyric acid and more than 1 year for valeric acid. Plastic is good for transport (glass is fragile) but for storage you did well with repackaging into glass. Storage of phenylacetic acid the same - very bad stinky scent in whole house when it was in original plastic container... problem disappeared when stored in glass.

woelen - 21-4-2022 at 01:00

I purchased material for making a good quantity of bromine very cheaply:
- 1 lb of KBrO3, see here: https://www.ebay.nl/itm/125184055068
- very cheap 48...49% HBr from here: https://www.laboratoriumdiscounter.nl/nl/waterstofbromide.ht...

Especially the latter is a really good price. I received my order with the HBr from laboratoriumdiscounter, and it is a high quality product. It is nearly colorless, which is quite unique for HBr. Usually, the stuff is yellow, piss-colored, but this only has a very weak yellow color.
I intend to carefully mix the KBrO3 and HBr, making Br2, without any other stuff in it (especially no chlorine, which may lead to BrCl-impurity). The Br2 then can easily be distilled off.

Making Br2 is very simple with this. I'll mix appr. 250 grams of KBrO3 with the liter of HBr, which will produce Br2 and leaves a slight excess of HBr in solution. The Br2 can be distilled off into a little concentrated H2SO4, which makes it dry. The Br2 then again is distilled off from the H2SO4, leaving pure and dry Br2. In this way, I will have appr. 700 grams of pure bromine, which is around 230 ml of bromine.

The liquid from which Br2 initially is distilled will have KBr (and a little HBr and probably also some remains of Br2, bound as Br3(-)). This liquid can be boiled down to drive off the last remains of HBr and Br2 and leave 170 to 180 grams of KBr behind, which also is useful.

ManyInterests - 22-4-2022 at 05:49

I've ordered potassium chloride (because I can't get any from sodium free salt lately), Resorcinol, and 28% ammonium hydroxide. While I do want to make my own ammonium hydroxide, I want some ready before I make my first synthesis.

woelen - 13-5-2022 at 13:40

I purchased material for making a good quantity of bromine very cheaply:
- 1 lb of KBrO3, see here: https://www.ebay.nl/itm/125184055068
- very cheap 48...49% HBr from here: https://www.laboratoriumdiscounter.nl/nl/waterstofbromide.ht...

Warning: Do not buy the KBrO3 from that first seller. It is fake. It is not KBrO3. I think it simply is expensive KBr. It dissolves very easily in water and when a drop of aqueous HClO4 is added, you get a white precipitate (must be KClO4), and when a strong oxidizer is added to the acidified solution, then Br2 is produced. I asked either a refund, or a shipment of real KBrO3. The seller seems to be chinese. The object location is in Bulgaria, but probably the material is shipped from some warehouse, which is done more and more by chinese sellers.

The HBr from the second link is good stuff, that company definitely is trustworthy.

I get the impression that buying things from eBay has become more troublesome the last two years or so. I already buy from eBay from 2005 or so, many chemicals, and many electronics parts, but my last three purchases all were fake or crap (one crap electronic device, an ozonizer, which was totally bogus, crappy Cu(OH)2, which was anything but Cu(OH)2, and now this failure with KBrO3). All items were from chinese sellers, but in the past, I also purchased many things from chinese sellers and always had good, or at least decent experiences. But things have changed . . .

Edit(woelen): I was offered a refund by the seller, or a reshipping of another parcel. I chose a refund. After accepting the offer of a refund, I received it just a few hours later. So, at least the seller recognized the error and did his best to keep me happy.

[Edited on 14-5-22 by woelen]

Texium - 13-5-2022 at 16:19

That's a bummer. I guess you could always go the oxidizer+sulfuric acid+KBr method if you're stuck with that stuff. I like to do that with hydrogen peroxide as the oxidizer since it's cheap (for me) and clean, though I know it's harder to get in Europe, so probably not a viable option for you.

SWIM - 13-5-2022 at 17:51

It's really strange all the bogus Ebay products.
Don't know if other countries are different but here in the US a bad Ebay products can be returned within a certain time period with the seller forced to pay the shipping for return. (Or at least could a couple of years ago. I quit selling there because they kept changing their rules to my disadvantage)

This even happens with good products if the buyer insists they are bad. Sometimes the generous policy is used to screw the seller, but I found this to be very rare in my hundreds of ebay sales. Most people are honest, even if they're buying stuff I'm pretty sure is being used for illegal purposes. If anything the shady buyers were more honest.
Anyway, with this policy selling bogus products only pays off if the seller doesn't complain to Ebay before the time window for complaining is up. I find it surprising that this happens enough to pay off for the crooked seller.
Maybe the seller you bought from got screwed by his source? Testing your wares is problematic unless you're buying bulk (or very conscientious).
I myself wound up with egg on my face a few times when I sold second hand chemicals that must have been improperly stored and had deteriorated.
(Some protease inhibitors and a couple of items that can't tolerate California summers unless in a refrigerator at least.)

I tested what I could; but if it's a closed container you hate to open it for testing if opening it may lead to degradation or contamination.
I finally disposed of a number of valuable but 'iffy' used chems as I just couldn't stand the possibility that I might screw up somebody's reaction that they put a lot of effort and expense into because I was unknowingly peddling junk.

Keras - 14-5-2022 at 00:42

All items were from chinese sellers, but in the past, I also purchased many things from chinese sellers and always had good, or at least decent experiences. But things have changed . . .

IMHO, you just had a stroke of luck. I shun Chinese products like hell. And it’s getting worse with the Covid.

Laboratorium Discounter is great, though. They’re a bit—how to put it mildly—messy in their organisation: their lead times are usually way too optimistic, especially for compounds they don’t stock like phosphorus pentoxide, and I once ordered calcium hypochlorite and got sodium nitrate instead! :p—but they’re otherwise very fair priced and reliable.

As for making bromine, I’m surprised you don’t use a simpler method. I just tried KI + sodium percarbonate. For some reason, it didn't work. It must probably be carried out in an acidic solution. I’ll redo the experiment later. However, I substituted sodium percarbonate for Oxone, and it instantly oxidised I⁻ into solid I₂, so I think you can obtain Br₂ very neatly by dropping an Oxone solution into a KBr solution.

[Edited on 14-5-2022 by Keras]

Texium - 14-5-2022 at 07:40

so I think you can obtain Br₂ very neatly by dropping an Oxone solution into a KBr solution.

I would expect so. It would be very similar to the sulfuric acid + hydrogen peroxide method.

woelen - 14-5-2022 at 10:06

I know other methods of making Br2, but with cheaply available HBr and cheaply available KBrO3 things get really easy. Of course, I can use other oxidizers, but first I'll see whether I get another shipment from that chinese seller (or get a refund).

Keras - 14-5-2022 at 22:36

Quote: Originally posted by Texium

so I think you can obtain Br₂ very neatly by dropping an Oxone solution into a KBr solution.

I would expect so. It would be very similar to the sulfuric acid + hydrogen peroxide method.

Well, Oxone is basically a Caro’s acid salt, so yes, that’s the same.
Oxone is cheap too. I don’t remember how much I paid for it but it was quite low.

What I don’t understand is why sodium percarbonate didn’t work. I added a very few crystals of TsOH to the mix, and sure the brown colour appeared immediately, but then after a swirl or two the mixture became clear again. I’ll retry using citric acid to neutralise the sodium carbonate.

Keras - 15-5-2022 at 00:29

Okay, so I redid the experiment with sodium percarbonate using citric acid. Dissolved a few milligrams of KI into 2 mL or so of water, added a few milligrams of citric acid. When everything had dissolved, added small portions of sodium percarbonate → solution became yellow then brown then with added KI a lot of I₂ crystals formed. So this procedure works with iodine, and probably with bromine too, provided you operate in acidic solution (strong acid not needed).

[Edited on 15-5-2022 by Keras]

Tsjerk - 15-5-2022 at 06:30

Doesn't citric acid react with iodine/bromine?

Keras - 15-5-2022 at 07:14

Quote: Originally posted by Tsjerk

Doesn't citric acid react with iodine/bromine?

Apparently not? I didn't assay the crystals, though, but they seem to be perfect iodine at first sight.

Boffis - 15-5-2022 at 07:55

Quote: Originally posted by Tsjerk

Doesn't citric acid react with iodine/bromine?

Apparently not? I didn't assay the crystals, though, but they seem to be perfect iodine at first sight.

Oh yes it does, the product is pentabromoacetone which is produced almost quantitatively and is used as a means of analysis for citric acid. I have some papers somewhere on the reaction if you are interested.

Keras - 15-5-2022 at 08:08

Quote: Originally posted by Boffis

Yes, please

This document (p.3, first §) suggests otherwise, though.

[Edited on 15-5-2022 by Keras]

woelen - 13-6-2022 at 11:11

I purchased 1 liter of 30% NaClO3 (pure, no NaCl in the mix, just water). This is within the EU-rules and sale of such solutions is allowed. I intend to try making concentrated solution of NaClO4 with this. I have a PbO2 electrode and do not want to spend that on making NaClO3 from NaCl (this corrodes the anode more than I like) and with this NaClO3-offer I just can buy this liquid, stick in the electrode and make NaClO4. The solution of NaClO4 then can be mixed with conc. HCl to make quite pure HClO4 (at least good enough for experiments in making salts of transition metal complexes). It's good to see that there are suppliers who are willing to sell stuff like NaClO3 to private individuals in such a way that it is inside the EU-regulations and on the other hand is easy to purify and to use in experiments.

Herr Haber - 13-6-2022 at 11:54