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Loptr
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[*] posted on 25-6-2015 at 06:23


Quote: Originally posted by Praxichys  

I am still looking into the reflux condenser compatibility. I think I will use teflon tape as padding in the joint to help with potential thermal expansion issues.
[Edited on 25-6-2015 by Praxichys]


If you used teflon tape that didn't allow the joints to seat all the way, it should allow for some thermal expansion to occur within the female joint, and hopefully enough to not break the male. You might want to attempt a test run to make sure.. :)
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[*] posted on 25-6-2015 at 07:14


Quote: Originally posted by Tdep  
Thallium! Very interested in what you get up to with that. Thallium cacodylate?? Or perhaps complete hair loss is trendy over there? Good luck with whatever is planned
Why so upset about thallium? I read about people experimenting comfortably with mercury or lead and their salts and these are of similar toxicity as thallium. Others play around with phosgene and derivates (di- and triphosgene), or with white P. All of them equally toxic and dangerous.

Of course, you have to be careful with thallium, but at least it is not volatile at all, not in its salts, nor as the free element. You have to be careful not to get a Tl-containing solution on your skin, and not to inhale dust or droplets of a bubbling solution of a Tl-salt. If a little amount of a solution of a Tl-salt is spilled on your skin, then simply quickly rinsing away with water removes the risk. Just do not allow it to act upon the skin for minutes.
I think that experimenting with solutions of Tl-salts is not more dangerous than experimenting with solutions of Hg-salts or Pb-salts. The latter two are more common and hence sound less scary.

The reason why I purchased a little Tl2O3 is that chemistry of thallium is only marginally known and I hope to find a few interesting things about its chemistry.




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[*] posted on 25-6-2015 at 14:16


I found this company that sells fused quartz glassware with standard joints. They also have an (American) Amazon page.

You can make triphosgene using dimethyl carbonate. This book written by member len1 goes into details. Looks like nasty shit. Washing the glass with acetone causes residue to revert to normal phosgene.




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[*] posted on 25-6-2015 at 18:31


Quote:
Quote: Originally posted by woelen  
Why so upset about thallium? I read about people experimenting comfortably with mercury or lead and their salts and these are of similar toxicity as thallium. Others play around with phosgene and derivates (di- and triphosgene), or with white P. All of them equally toxic and dangerous




Upset? No, excited is a much better word. It's interesting, I actually have an Exam in 20 hours where I'll have to compare the toxicity of thallium, Mercury and lead (environmental chemistry). There really isn't much day to day exposure to background levels of thallium, unlike Mercury and lead (depending on how much fish you eat) and it's mainly known for killing people, much in the same way arsenic sort of developed a reputation as a murder weapon. So you're right, comparable toxicity but definitely screams death to many a chemist.

Give me a few years and this hopefully will be my career path, heavy metals in the environment.

Also, I believe pre 1970 there was no cure for thallium poisoning, now Prussian Blue is used. Took quite a while to find an effective treatment.

Any oxidation states with colour though? You've always presented such wonderful colour changes of metal chemistry in your website, think you will be able to that with thallium?

[Edited on 26-6-2015 by Tdep]
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[*] posted on 30-6-2015 at 03:15


Well you're in the right location for that career Tdep
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woelen
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[*] posted on 7-7-2015 at 23:21


Quote: Originally posted by Tdep  
[...]Any oxidation states with colour though? You've always presented such wonderful colour changes of metal chemistry in your website, think you will be able to that with thallium?

I have done a first few experiments with the thallium oxide to get a feeling of its properties. I'll summarize a few for the interested people:
1) Tl2O3 is a dark brown powder, like dark chocolate.
2) Tl2O3 dissolves in acids very easily. If you add it to e.g. 20% HCl, then you hear a soft hissing noise and then it is dissolved. The solution is colorless and contains Tl(3+) ions. The sulfate, nitrate and chloride all are soluble, I tried all of them.
3) Tl(3+) is very easily reduced to Tl(+). An example is addition of acidified sulfite (or SO2) to a solution, containing Tl(3+) ions. Reduction is fast and complete. When this is done in a solution of Tl2O3 in dilute HCl, you get a white precipitate of TlCl, which is formed as soon as SO2 is added.
4) Tl(+) is very easily oxidized to Tl(3+). E.g. adding H2O2 to an acidic solution, containing Tl(+) leads to formation of Tl(3+). On addition of a base, brown Tl(OH)3/Tl2O3.xH2O precipitates.
5) Tl(+) forms a nice yellow precipitate of TlI with iodide ions. The yellow solid looks like sulphur, not like the very bright yellow of PbI2. It really is hard to distinguish powdered TlI from powdered sulphur.
6) Most special is addition of a solution of NaIO4 to a solution with Tl(+). This forms a snow-white fine crystalline precipitate of TlIO4, which however, after 5 minutes or so becomes yellow and after a quarter of an hour it is brown. Tl(+) resembles K(+) and hence forms the nearly insoluble TlIO4. This compound contains a reductor and oxidizer in the same compound and these react with each other. The Tl(+) is oxidized to Tl(3+), while the IO4(-) is reduced (probably to IO3(-) and O(2-) and maybe part of it is reduced to I(-)). The brown color then most likely is caused by formation of basic thallium(III) compounds.
7) Tl(+) forms a pale yellow solution with nitrite ions, which decomposes on acidification. Probably this is a complex ion.
8) Alkalies do not precipitate Tl(+), they do precipitate Tl(3+) as a dark brown precipitate. A nice effect is created when a solution of Tl2O3 in an acid is reduced (e.g. with SO2), then made alkaline and then H2O2 is added. On addition of H2O2 the colorless solution becomes brown and turbid at once.

More experimenting will follow and when I have collected more interesting results, I will make a write-up with pictures.




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[*] posted on 31-7-2015 at 04:06


Not chemicals. But I am now the proud owner of some 24/40 glassware with flasks up to 1L.
It's not a great photo: I just snapped it in poor light conditions with the first thing available.
Mantle will arrive soon.

Now I am only a magnetic stirrer, a furnace, a fume hood and a couple of bottles of acid away from a properly stocked lab.

2015-07-31 18.13.36a.jpg - 311kB
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[*] posted on 1-8-2015 at 00:55


3 kg of potassium sulfate and 3 kg of calcium nitrate, very impure (fertilizer grade) at a local hardware store. Sitting side by side in plastic bags on the same shelve, begging to be bought and made into KNO3 :)
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[*] posted on 1-8-2015 at 09:45


Bought glacial Acetic Acid today... Not bad quality, technical grade, and surprisingly it only cost me like 2 or 3 bucks for a liter of it. I'm using it on some zinc carbonate that have been laying on the shelf for quite a while.
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[*] posted on 6-8-2015 at 07:42


My now long awaited package just arrived.

Apart from some Salts like Manganese Chloride or Sodium Sulfite that I need was a bottle of Benzene
which is like the best, some LiAlH4 and lot's of other stuff.
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[*] posted on 30-8-2015 at 19:46


I found a great score at the antique fair today. A large fishersci hotplate stirrer for $35! Also a 2L filter flask for $10 with a dead mouse inside. The seller said it was from someone's basement and he sold over 40 beakers and flasks that day.



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[*] posted on 30-8-2015 at 20:45


Dang it! I never find used glassware with dead things inside :(

I bought an electrical stove to replace my alcohol camping stove in my experiments... And seems I'm up to a rather good start with a beaker full of manganese dioxide cracking over it and making THE mess....
I also bought a MFRC522 nfc reader and a couple tags, I'll try to dump the tags used in the local public transportation and then I'll have more the a copy of my personal card so I don't have to walk every time I forget the original one... And maybe I'll expose some design flaws and get free bus rides to all the members of the local hackerspace.
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[*] posted on 31-8-2015 at 05:28


disregard , post .Thanks

[Edited on 31-8-2015 by skip]
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[*] posted on 31-8-2015 at 09:42


Just ordered some polyethylene glycol brake fluid and fumed silica. Any guesses on what I'm making? ;D



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[*] posted on 31-8-2015 at 23:50


I usually buy from a Russian supplier "AntrazoXrom". They sell reagents and glassware by mail order (though the notorious Mail of Russia is known for breaking glassware en route, so if I need a lot, I travel to Moscow in corpore with a duffel bag). My most current order was a fresh supply of filter paper, litmus and universal indicator, and two new beakers to replace the one I broke recently.

Of course, many things I have here are extracted or synthesized from stuff bought in our town stores such as hardware, gardening, etc. That's the very essence of survivalist chemistry - being able to do stuff with things you can find at the nearest ruins.

[Edited on 1-9-2015 by ave369]




Smells like ammonia....
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[*] posted on 14-9-2015 at 22:58


I ordered a single chemical now, rubidium nitrate 100 grams.

This was a very good offer, 100 grams for just over 70 euros! You can find it on the onyxmet.com website. Select english language and the currency of your choice (at top right of webpage) then search for "rubidium".

In the last few months I discovered more and more that rubidium and cesium are much more interesting than I thought some time before. It is remarkable how many special anions can be stabilized in the solid form with rubidium and cesium ions. I have experimented with TeCl6(2-), TeBr6(2-) and SeBr6(2-), some time ago with chloro-complexes of Sb and I intend to experiment with special alums of titanium, vanadium and chromium, stabilized with rubidium or cesium. Many very special chemicals can be isolated, while this cannot be done with potassium ions or sodium ions. More on this will follow soon on my website.




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[*] posted on 22-9-2015 at 02:21


Went to my Vintner ( Oh I love that word, never heard that one before looking it up in a dictionary ) for the annual talk on how well our Wine is doing. We thought of making some Spirits this year, too since we recently aquired a small field with some pear trees. So I went to my Vintner and asked him what additional chemicals we would need that don't belong to winegrowing and he told me that we needed conc. Sulphuric Acid for it and gave the the Adress to a shop that sells food grade 96% Sulphuric Acid. So I went there today and nearly bought the whole shop since the have a freaking lot of stuff all for agricultural stuff, everything is food grade and very pure and really cheap. Just bought a 1 kg Bottle of Copper Sulphate for around 15 $, a bottle of Sulphuric Acid ( 1L ) for around 14$ and some Citric Acid togehter with some glassware.

If it wasn't only 1 kg minium sizes I'd buy more, all the stuff like pure Vitamins, Tartaric Acid, Malic Acid, Sodium Hydroxide standart Solution, Indicator Solutions and lot's and lot's more. I even saw a bottle of Methanol but it was mixed with something else so not pure.

I'll keep that shop in mind, really usefull !
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[*] posted on 22-9-2015 at 07:08


1. A Buchner set for vacuum filtering. Now I can finally experiment with solid ferrates!
2. A set of spare rubber bungs.
3. New test tubes. Including the tiny Ulengut test tubes which will be useful for microchemistry.
4. Potassium iodide and salt of hartshorn. And a huge fresh supply of KOH, once again for ferrate syntheses which gobble this alkali like popcorn!

[Edited on 22-9-2015 by ave369]




Smells like ammonia....
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[*] posted on 2-11-2015 at 01:18


Yesterday bought a bottle of argon and a regulator. Also some more NaOH and some gypsum.
Today I had 100g of sodium arrive, 115g of Ca, 100g of CaF2 and 10 grams of alizarin.


I have also located a cheap OTC source of manganese sulfate. I might start using that for making sulfuric acid instead of copper sulfate. Especially useful if I can recycle the MnO2 byproduct by bubbling some SO2 through it. Even without that extra step, it is looking cheaper than the CuSO4 route. And if the recylcing works efficiently I will have a workable route from garden sulfur to concentrated acid.

Anyway, the CaF2 is a slag fluidiser for a titanium thermite. The gypsum is also for that thermite and some others. Alizarin just looks like fun but also useful for identifying cations -- if I can get it to work. I understand that it is a wee bit finicky.
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[*] posted on 2-11-2015 at 01:45


I bought some 91% sodium bisulphate at Wally World. I don't have any specific plans for it, but I never seem to have any when I need it.

I also went to the brewing supply store and was very disappointed at the poor selection of chemicals available and the lack of expertise among the staff. I asked if they had any potassium bicarbonate and was told that potassium carbonate is the same thing!

Oh and I bought two 500 watt immersion heaters, which together provide enough heat to boil 15 liters of water.

Next I'm thinking about hitting up pottery stores to see if I can find any dichromate.
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[*] posted on 3-11-2015 at 10:09


I bought a pound of sodium silicate off eBay... not terribly exotic, really only noteworthy because of the free surprise the supplier decided to throw in: a matching Lucky Charms (TM) spoon and cereal bowl!



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[*] posted on 4-11-2015 at 02:12


112gms KOH



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[*] posted on 4-11-2015 at 03:46


Quote: Originally posted by j_sum1  
Yesterday bought a bottle of argon and a regulator. Also some more NaOH and some gypsum.
Today I had 100g of sodium arrive, 115g of Ca, 100g of CaF2 and 10 grams of alizarin.



did you get the sodium and calcium from onyxmet.com ??
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[*] posted on 4-11-2015 at 04:41


Why. However did you guess?
All four were from there. My problem is that I have more on my wish list than I can afford.
And I have more projects waiting for me to have some time in the lab than I have time in the lab.

Let me add concerning onyxmet, service was great! Shipping from Poland took less than a week. And I was able to pay directly to an aussie account without paypal fees or currency exchange fees.
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[*] posted on 6-11-2015 at 22:57


Quote: Originally posted by j_sum1  
Why. However did you guess?
All four were from there. My problem is that I have more on my wish list than I can afford.
And I have more projects waiting for me to have some time in the lab than I have time in the lab.

Let me add concerning onyxmet, service was great! Shipping from Poland took less than a week. And I was able to pay directly to an aussie account without paypal fees or currency exchange fees.


call it intuition ;P considering the only other easy place to get sodium in aus would be from eBay/argent scientific (same person), and the sodium he gets is from onyxmet. how was customs concerning shipping?
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