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Rich_Insane
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Registered: 24-4-2009
Location: Portland, Oregon
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Hey guys.
I'm just setting up my lab -- on an extremely tight budget.
I just bought 2 lbs of 99% KNO3 and 500 g of Ca(NO3)2 (Calcium nitrate for nitric acid production)
Can anyone recommend a nice source of acids, namely sulfuric. I am reluctant to buy it from the hardware store, I would like it very pure so nothing
blows up in my face.
I also want to purchase methanol. i can find acetone, toluene, xylene, kerosene, and naphtha at ACE hardware..... but no methanol. And methanol is
especially important to me. As is HCl which I have found in 31% concentration at ACE hardware as muriatic acid.
I have checked Acros for cyclohexanol (an alcohol I may be using -- I would only need 1 L).... it is quite expensive on my standards. I am looking in
the $10-15 range..... laugh if you would like.
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Phosphor-ing
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Methanol can be distilled from gas line antifreeze/ water remover product called "Heet".
"The nine most terrifying words in the English language are: 'I'm from the government and I'm here to help.'" -Ronald Reagan
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gnitseretni
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Does it need to be distilled? I thought it was already relatively pure methanol. I use it as is to make methyl nitrate and never had a problem.
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woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
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I just received a really cool set of chemicals for just GBP 24:
- 160 grams of RuO2
- 150 grams of CsAl(SO4)2.12H2O
Both chemicals usually are MUCH more expensive, so I was quite happy with the materials. The RuO2 is an active catalytical chemical (e.g. when added
to bleach, the bleach at once starts bubbling, giving off oxygen). Another interesting property is that it dissolves in HCl easily, giving a deep
red/brown solution, and when zinc is added to such a solution a deep blue solution is obtained of a Ru(2+)-species.
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Klute
International Hazard
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Registered: 18-10-2006
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You are forming RuCl3.3H2O by adding it in HCl; I work with this compound all day long at work! You can form some nice complexes with RuCl3, complexes
with benzene, p-cymene, etc This can be used to as starting material for much more complexes, notably complexes containing Ru-C bonds.. Let me know if
you want some procedures!
\"You can battle with a demon, you can embrace a demon; what the hell can you do with a fucking spiritual computer?\"
-Alice Parr
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woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
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Klute, are you sure about the making of RuCl3 by adding RuO2 to HCl? I tried it, but my RuO2 does not dissolve at all, not even on careful heating of
the suspension of RuO2 in conc. HCl. Maybe my RuO2 is calcined and more inert than yours. I also have a book, which states that RuO2 is not attacked
by acids.
How does your RuO2 look like? Mine is a black powder with a slight bluish hint, but calling it dark blue would be misleading.
If I, however, add the RuO2 to bleach, then part of the bleach decomposes, giving oxygen, and then I get a dark green and clear solution. The RuO2
fairly easily dissolves in the bleach. When I add this green solution to conc. HCl, then a very deep red solution is obtained (and chlorine is
produced). When I add zinc to that deep red solution, then I obtain a beautiful blue solution, which is air-sensitive (on contact with air, a
yellowish solution is obtained).
If you can give more information on RuO2 and the Ru-complexes you mentioned, then that would be very nice.
[Edited on 29-7-09 by woelen]
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JohnWW
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I think that Klute is likely to be right about RuCl3, because Ru(III) compounds, homologous to those of Fe(III), or at least "high-spin" ones with
relatively weak ligands, are energetically favored due to having five unpaired 4d electrons, one in each 4d orbital. Ru(II) compounds would be liable
to oxidation by air.
Higher-valent Ru compounds, including the (VIII) tetroxide, RuO4 (obtainable by heating in oxygen), are much more easily obtained than those of Fe (of
which ferrates (VI) are obtained only with strong alkaline oxidants, and perferrates(VII) and FeO4 are still unknown AFAIK although might just be
obtainable by high-voltage electrolysis of supercooled alkaline ferrate(VI) solution).
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Klute
International Hazard
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Registered: 18-10-2006
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Well, I use RuCl3 everyday, not RuO2, but considering the colour ou describ and the relative sensitivity of this oxide, I'm pretty sure this is what
you are forming.
If you heat the chloride with cyclohexadiene (either 1,3 or 1,4) in aq. EtOh, you get [RuCl2(benzene)]2 dimer, a brick red powder insoluble in most
solvents, I use this compound as precrusor for Ru-C complexes, by adding a bidendate ligand such as a phenylpyridine, you get a N-Ru bond and a
cycloruthenation reaction between the ortho H of the phenyl ring, by C-H activation. The reaction is done in acetonitrrile, the benzene is replaced by
3 molecules of acetonitrile.
You can also form a arene complexe using phellandrene, this compound is much more stable and the arene is very hard to remove.
\"You can battle with a demon, you can embrace a demon; what the hell can you do with a fucking spiritual computer?\"
-Alice Parr
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woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
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Ah, I see, you already start from hydrated RuCl3. That is different from my situation. I start with the ruthenium(IV) oxide, which I first need to
dissolve in bleach. When this is done, then it can be reacted with hydrochloric acid to give the material you mention.
When the solution is reduced with zinc and the resulting liquid is allowed to stand for an hour or so, then the result is really nice. The blue
ruthenium(II) species is very easily oxidized by oxygen from air.
After one day of standing, all of the liquid has turned yellow.
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Jor
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Posts: 950
Registered: 21-11-2007
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250g phosphorus pentoxide
250g sodium dithionite
100mL 55% hydrazine hydrate
25g vanillin
150g MnSO4.H2O
about 20g sodium nitroprusside
200g silicagel
50 K-ferricyanide
100g K-ferrocyanide
Still to come:
-100g tin(II)chloride
-10mL trifluoroacetic anhydride
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Bikemaster
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Where did you find you phosphorus pentoxide....i never see any where, where they was selling it.
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Jor
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Posts: 950
Registered: 21-11-2007
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Well... I bought it from Acros  Just like the hydrazine hydrate, and many of my
chemicals.
I dont buy directly, but via a local chemical supplier. I know him for long enough, I have a business relation, so he will order many things (except
CWC-chems, severe poisons as cyanide, arsenic and thallium compounds, and some others). So I virtually have access to most chemicals, also things like
chlorosulfonic acid, sulfuryl chloride, oleum, phosphorus, perchloric acid, etc. but I don't need these at the moment.
My only irritation is is that I can't buy thionyl chloride, wich I REALLY want so bad.
Try to find a local supplier buying from the big companies.
Where do you live? If you live in Europe, I have an interesting supplier for you, he sold me some sodium hypophosphite (100g) and phosphorus pentoxide
(130g) for fair prices.
[Edited on 20-10-2009 by Jor]
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Bikemaster
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Sadly, i don't live in europe, i live in canada...
Did you ever think about synthesis the thionyl chloride? I think just just need sulfur, chloride, sulfur trioxide (maybe olem will do) and the right
condition.
thanks
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Bikemaster
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Sadly, i don't live in europe, i live in canada...
Did you ever think about synthesis the thionyl chloride? I think just just need sulfur, chloride, sulfur trioxide (maybe olem will do) and the right
condition.
thanks
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Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
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Mood: Chemistry: the subtle science.
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| Quote: |
I have an interesting supplier for you, he sold me some sodium hypophosphite (100g) and phosphorus pentoxide (130g) for fair prices.
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Jor, you ****! 
The single most important condition for a successful synthesis is good mixing - Nicodem
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devongrrl
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Posts: 91
Registered: 28-7-2009
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Mood: Nucleophilic
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HCl & CH3COOH
2.5 ltrs of each
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aonomus
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Posts: 361
Registered: 18-10-2009
Location: Toronto, Canada
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Mood: Refluxing
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Hmm, last order was a small one,
250g FeCl3 * 6H2O
500g NaSO4 anhyd
250g CaCl2 anhyd
2.5kg NaCl
Once all the labware is gathered, then I can do derivatives of benzoic acid and salicylic acid for fun...
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woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
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Mood: interested
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My last order was
100 grams of Nd2O3
100 grams of Te (powder)
120 grams of La2(CO3)2
100 grams of Y2O3
some dyes (rhodamine B, methylene blue, malachite green)
I also ordered some non-chemical stuff
4 schottky diodes 1N5820
several coils with thousands of turns
a few xenon U-shaped discharge tubes
a few 1 F capacitors (so-called goldcaps)
some very high efficiency LED's (13000 mcd, 19000 mcd and even a few 40000 mcd LED's)
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aonomus
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Posts: 361
Registered: 18-10-2009
Location: Toronto, Canada
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So this is a little bit of a necro, but the thread is not that old. I just spent 2 days on and off distilling 1L of 'methyl hydrate' (claimed 99.9%
methanol), but about 100mL remained before the temperature started to rise enough to justify chucking the remainder (ie: some sort of impurity that
started to distill off at a higher temperature). I got probably about 800mL methanol, as pure and crystal clear as can be.
Also, my last order (spread out between a few sources):
Potassium hydroxide, 500g
Ferric chloride*5H2O, 500g
Potassium nitrate, 500g
Alum, 500g
Sodium sulfate anhyd., 500g
Oxalic acid, 100g
Ethylene glycol, 500mL
Sodium thiosulfate*5H2O, 500g
Sodium borohydride, 50g
Sodium chloride, 2.5kg
Ferrous sulfate, 100g
Boric acid, 100g
Benzoic acid, 100g
Sodium bisulfate, 100g
Sodium metabisulfite, 100g
Sodium iodide, 100g
Oh, and not shown here, but gotten, obtained, or made/purified from OTC stuff.
3kg NaOH pellets from Home Hardware, no aluminum flakes, just pure pellets (for $21! I was amazed I even saw it, I was tempted to grab more, but that
would look suspicious)
1kg activated carbon
1L mineral oil for heating baths
~500g MgSO4 anhyd. from calcined epsom salts
~300g Na2CO3 anhyd. from calcined baking soda
[Edited on 21-11-2009 by aonomus]
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a_bab
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Posts: 458
Registered: 15-9-2002
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Mood: Angry !!!!!111111...2?!
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This is so sad, aonomus.
Where I live, sodium hydroxide flakes runs for around 2 dollars/kg. You can buy the entire stock and nobody would raise an eye.
On the other hand, when I bought some 5 packs of sodium metabisulphite (100 grams each), I did get a raised eyebrow. Later at home I realized it was
meant to be used on some 2000 liters of wine. Oh well...
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aonomus
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Posts: 361
Registered: 18-10-2009
Location: Toronto, Canada
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Mood: Refluxing
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I live in Toronto, and I had to go to a suburb farther away just to find anything pure and not padded for your own safety....
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carbonfeind
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200ml glyoxal
100g hydroxylamine sulfate
100g lead acetate
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Jor
National Hazard
Posts: 950
Registered: 21-11-2007
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Last 2 months I obtained some more reagents:
-250g phosphorus pentoxide
-100g potassium ferrocyanide
-50g potassium ferricyanide
-25g vaniline
-100mL 55% hydrazine hydrate
-250g sodium dithionite
-100g MgSO4.7H2O
-200g silicagel, powdered
150g MnSO4.H2O
-50g KCN (finally, I can make those lovely CN-complexes, I am currently working on K2[Ni(CN)4)]. I had 5 grams already, but now I have more).
-10g NaN3
-10ml trifluoroacetic anhydride
-100g SnCl2.2H2O
-150g pure zinc powder
-15g of sodium nitroprusside, Na2[Fe(CN)5NO].2H2O, wich are beautiful very large crystals (a few are about 1cm long).
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woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
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Mood: interested
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Again, I also have purchased some interesting things:
More opamps, capacitors, diodes, transistors and other electronics goodies. I also purchased a few IN14 and IN3 nixie tubes and high voltage driver
IC's for them, just for the fun of it. Lovely retro stuff  I can make a clock of
these IN14's, but I also consider making a digital readout with them for a digital multimeter circuit, using high precision opamps like the LME 49710
opamps for the preamp section (max. voltage offset just a few tens of microvolts without offset balancing) and standard integrating AD-converter
circuits for the readout. It would be lovely to have a high-precision digital meter using really high-quality components, while have a retro sixties
readout.
I also purchased a few new and rare chemicals for very low prices (shutdown of supplier, I purchased some remaining chems for highly reduced prices):
- 100 grams of I2O5
- Barium metal (a single stick for my element collection, sample is appr. 100 grams)
- 100 ml of diacetyl. This stuff looks like liquid chlorine, including the yellow/green vapor, but it is not really toxic and has the nice smell of
butterscotch when highly diluted.
And finally, I was given 100 grams of LiAlH4 in a sealed metal can, which has a little plastic bag inside. I did not yet open the can, because I have
no direct use for this compound. I myself would never have purchased this (it is very expensive, but also rather dangerous to handle), but it was
given to me by the same supplier, for free because he had no use for it anymore. If anyone of you has some nice inorganic experiments in mind with
this compound, then it would be nice to know of them. For the time being I'll keep it in its metal can, safely sealed, keeping the material fresh.
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mr.crow
National Hazard
Posts: 884
Registered: 9-9-2009
Location: Canada
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Mood: 0xFF
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- 50g sodium metal
- 0.5g platinum wire
- 5g palladium
- 1g of gold
Nice little collection
Not much in terms of reagents recently, maybe during the spring when I can do some more experiments.
Woelen,
I love IN14 tubes, I have a clock I put together from a kit that uses those and it looks really nice.
I also have a bag of 100 IN3 tubes from Russia and most of them are worthless. The light always comes from a corner instead of the center of the
plate. Horrible soviet quality.
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