Sciencemadness Discussion Board - My starting equipment/chemicals so far

My starting equipment/chemicals so far

Schleimsäure - 31-8-2014 at 13:38

Good evening everyone,

since the beginning of the year I have rediscovered my hobby from youth - experimental chemistry. Unfortunately I gave up at the age of 14 and even opted out chemistry at secondary school.

Now, at 36 it comes all back and I even watch Organic Chemistry lessons on youtube. https://www.youtube.com/watch?v=Ig3ok5KbfTo

However, I collect equipment and chems for 3/4 of a year now. Especially chems are not that easy to get in Germany.

I had some luck and got 30 banana boxes full of equipment of a defunct lab, mostly glassware for 450 EUR. There were 10 unused Dimroth condensers or 15 new 1l threeneck RBF's in it for example, so I could get most money back in through ebay. It was all NS29, but there was no claissen adapter and no vacuum adapter, which I purchased just recently. The stirrers in the package were from the 80's without heating, so recently got me one used Heidolph magstirrer/heater for EUR 70.

With chems I got lucky one time, getting two big boxes of chems for 200 EUR from a young chemist, including Diethylether, MeOH in 2,5l VWR bottles. Dichromate 500g, 1l 99,9% Benzene ultrapure from VWR :cool:

, H2O2 30% from FisherScientific, but also not so much needed stuff like 2 kg succinic anhydrid or 1,5kg Aluminiumnitrate nonahydrate.

Until now I could only make simple synthesis, as there are still some simple things missing (pumps, pvc-tube, one more stand) which I will aquire shortly. I made some Nitrobenzene, Mercury II oxide from elemental Mercury, Copper II- oxide, or Sodium acetate, all reactions which do not require refluxing, destillation etc.

As I have already spent like net 1.500 EUR I am looking for the best buck with the rest I need.

I was looking on http://www.lambdasyn.org/ for example for synthesis I can perform until I have my stuff complete finally.

My knowledge in chemistry was very low and is now, with repeating some basic stuff and hearing some OC, mediocre at best. I've got an MBA (shame on me) and my brother suggested to study chemistry at an Open University course, "Fernstudium". Two things, I believe it's not possible, only directly at a University and I can't leave my job, second I am 36.

As I can't wait to make further synthesis, maybe one can suggest some interesting synthesis without destillation from the following educts, oxidizers, reduxers:
(all I can do for now is mixing, heating and cooling (thermometers of all kind), filtering, a vaccume exsiccator without vacuum

Solvents:
Acetone
Benzene
Chloroform
Trichlorethylene (only 300ml)
Ether
2-Propanole
DCM
MeOH
Xylene

Acids and bases(organic and inorganic):
Phthalic Acid
Succinic anhydride
H2SO4 96%
HCL 37%
HNO3 65%
GAA (99,5)
H3PO4 85%
Boric Acid 99,5
KOH
NaOH
AL(OH)3
Ca(OH)2
Formic Acid 85%
Ammonia 25%
HF 10-20% technical
Citric Acid
Urea acid

Chems/elements/Organics of all kind:
KNO3
Red Phosphorus
Mercury
Pot. Metabisulfit
Ferrum powder
Aluminum powder
Magnesia powder
Fe2O3; Fe3O4
Na2O3S2 5xH2O
SrCO3, BaCO3
ZnO
Potassiumdichromate
KMNO4
Benzaldehyde
Ammoniumchloride
Sulfur
Nitroethane
Coppersulfate 5*H2O
Calciumcarbide
Benzene
Borax
Urea
K2CO3
NaSO4
MGSO4
Na2CO3; NaHCO3
Li2CO3
Potassiumiodide
Glycerol, 99,5%
Silversulfate (what to do with 250g Ag2SO4 p.a.?

EDTA sodium salt
KCL
MnO2

Self synthezised in small amounts: Nitrobenzene, HgO, Sodium acetate, CopperII-oxide.

Probably one could suggest something useful for later synthesis with full equipment (as the 25g of HgO I made to make later the II-chloride for amalgamation of Al for example).

Sorry for the long text, for wrong English nomenclature and thank you for consideration.

[Edited on 31-8-2014 by Schleimsäure]

aga - 31-8-2014 at 14:02

Welcome.

Your English is Perfekt.
(Mein Deutsche ist noch nicht gut genug)

What do you Want to Learn, or make ?

Nitrobenzene and Mercury II Oxide seem strange things to make for a beginner.

But then, i am a beginner too, so what would i know !

Schleimsäure - 31-8-2014 at 14:11

Thanks for the welcome!

At first I was eager at the usual stuff, anorganic, some pyro. But after deeper digging Organic Chemistry seems to be much more rewarding.

Well I'm not a full blooded beginner, since I made experiments from age 11-14.
Make no mistake, I had/have a good amount of respect, especially handling HgO, but with 36 years you are not as light minded as with say 16 or so, meaning I take all necessary care when it comes to T+ stuff.

I will finish my basic chemistry book, atomic model, chemical bindings etc. and am now looking for a good OC book.

P.S. Your German sentence was -almost- perfect, though I know it's not easy to learn)

[Edited on 31-8-2014 by Schleimsäure]

Schleimsäure - 31-8-2014 at 14:43

And in what exact field in OC, which is crazy big, to specialize at some point, I have no clue yet.

plante1999 - 31-8-2014 at 14:53

Quite neat stuff, wonder how you managed that out. I would like to add something in German, but I just started learning

.

I always reccomend Inorganic chem, as it is quite easy to make deductions in reaction pathway etc.

Making acetanilide from your chemicals could be an objective for a two week work in your home lab with a regular full time ocupation.

aga - 31-8-2014 at 15:16

Quote: Originally posted by Schleimsäure

German sentence was -almost- perfect, though I know it's not easy to learn

Damn right !

German is harder than Chemistry for sure.

I'm a total Chemistry Noob, with 7 monats experience.
47 years old.

Schleimsäure - 31-8-2014 at 15:27

Quote: Originally posted by plante1999

Quite neat stuff, wonder how you managed that out. I would like to add something in German, but I just started learning

Ja, I put some effort in finding sources, but even the acquisition makes fun. Wo ein Wille ist, ist ein Weg!

Acetanilide? From a quick search the usual way is with acet anhydride, which I do not possess (will get that too somehow eventually).
The other compound, aniline would be no problem, from benzene/nitrobenzene.
Or is there another path to acetanilide with my chemicals?

Schleimsäure - 31-8-2014 at 15:32

Quote:

Damn right !German is harder than Chemistry for sure.

*Laugh*

Nice to see that I'm not the only "oldie" with my almost 37 years.

plante1999 - 31-8-2014 at 17:26

You can make acetic anhydride with sulphur, an halogen and anhydrous sodium acetate, which can be made with sodium carbonate and vinegar (Or diluted glacial acetic acid).

Schleimsäure - 1-9-2014 at 10:39

Quote: Originally posted by plante1999

You can make acetic anhydride with sulphur, an halogen and anhydrous sodium acetate, which can be made with sodium carbonate and vinegar (Or diluted glacial acetic acid).

Thank you. Chlorinating the sulphur to S2CL2. I would still need PVC tubes for the washing bottle(s), tubes and pump for my reflux condenser etc. Will do that when I have all stuff toghether. An interesting synthesis with some steps and surely not too easy.

With the sodium acetate I made 2 runs a month ago. In the first I simply collected the trihydrate (I used a cooking pan, because of the wide surface). In the second run I heated much longer, but the acetate went partly into greyish hard clots. The acetate should have melted and recrystalize again. Don't know what went wrong and discarded the batch. Also the ACS grade GAA I found a little to good for a third run.
I can get the trihydrate, pharma grade for 15 EUR per kilo, which is not cheap but still ok:
http://www.ebay.de/itm/Natriumacetat-Trihydrat-reinst-Ph-Eur...

Or the anhydrate for 10 EUR/500g, not as pure:
http://www.ebay.de/itm/Natriumacetat-wasserfrei-Lebensmittel...

By the way I have a question concerning the quality grades:

In German there are in decending quality:

roh (auch crudum, crd.)
technisch
zur Synthese
rein
reinst
zur Analyse (auch p. a. = pro analysi oder analysenrein)

meaning

crude
technical
for synthesis
pure
purest
p.a. pro analysis

What would be the corresponding terms in English? (I know p.a. should be ACS and crude and technical should be the same).

[Edited on 1-9-2014 by Schleimsäure]

Brain&Force - 1-9-2014 at 11:20

Quote: Originally posted by Schleimsäure

By the way I have a question concerning the quality grades:

In German there are in descending quality:

roh (auch crudum, crd.)
technisch
zur Synthese
rein
reinst
zur Analyse (auch p. a. = pro analysi oder analysenrein)

meaning

crude
technical
for synthesis
pure
purest
p.a. pro analysis

What would be the corresponding terms in English? (I know p.a. should be ACS and crude and technical should be the same).

Purest, I think, would be reagent grade. "For synthesis" is probably lab grade. The Sciencemadness Wiki has information on chemical grades:

http://sciencemadness.wikia.com/wiki/Chemical_grades

Schleimsäure - 1-9-2014 at 13:13

Thank you, this is helpful.

Fantasma4500 - 1-9-2014 at 13:46

try extracting abit of highly concentrated nitric acid, using sulfuric acid and potassium nitrate, then extracting it with DCM
i would reccomend you to get hold of some benzyl alcohol however, im not much into organic chemistry but still has found it to be quite interesting

you could perhaps try melting together P with S in a test tube, with butane as protective 'atmosphere'

for destillation you can try to get hold of a simple glass destillation bridge, ebay.de gives a handful of results if you translate it into german ofcourse

one advice: control Capitalization in chemical formulas, it just looks alot nicer writing MgSO4 than MGSO4, for instance, keep the individual elements in mind when writing up chemical formulas

potentiall you could decant off acetic anhydride from H2SO4 and corrosponding acetate, decanting as in just pouring the liquid layer off, but you must use excess sodium acetate for this

you could try melting KNO3 together with iron powder, when you get it to react it can and may melt steel, potassium ferrate should be formed, when remainings are dumped into water it gives off a purple colour, if you can isolate ferrate then you are pretty well going

perhaps try to make some manganese salts..
also if you can -- get some 30% HCl, it doesnt fume as violently as 37% HCl, so its alot easier to work with

plante1999 - 1-9-2014 at 14:57

Dont take me wrong Antiswat, but acetic anh. can't be made that way, and most prep you reccomend are not good for various reason for a novice.

Schleimsäure - 1-9-2014 at 15:11

90-99% HNO3 was on my agenda anyway from sulfuric and KNO3.

Thanks for the advice, MGSO4 was a typo I have overlooked. Will keep that in mind.

I have really massive glassware still from the big package I bought, 40 cm Liebig condensers, Graham condensers, Dimroths. Just didn't manage yet to get all "small parts" together. But I'm almost there.

Attached some pictures of the treasure before I sorted it out. Also a Soxhlet and some special made stuff from the former phosphate factory lab.

Thank you for the hints, many things I can do until then.

Texium - 1-9-2014 at 15:30

Quite the treasure indeed! I recently had the opportunity to look through a similar lot. It was amateur chemist's heaven!

I assume that you're planning on selling some of that equipment, and if you want to, feel free to advertise your items on the Sciencemadness Wiki Marketplace. It hasn't been used yet, but now would be a great time to start using it.

Schleimsäure - 1-9-2014 at 15:49

Quote: Originally posted by zts16

Quite the treasure indeed! I recently had the opportunity to look through a similar lot. It was amateur chemist's heaven!

Just yesterday I emailed someone on ebay local ads who sells some 450 (!) boxes of lab equipment, mostly from former GDR. Make no mistake this is abolutely high quality glass from Jena, where Borosilicate was invented I think.
Of course I will only look for the stuff I still miss, if he lets me.

As for selling. I already sold much on ebay, but have still considarable amounts left. What shall I do with 50 beakers for example?
But sending glassware by post is really annoying, 2 convolutes I sold had some broken glass despite diligent packaging. Btw I live in Berlin.
Otherwise I would be very happy to help someone out.

[Edited on 1-9-2014 by Schleimsäure]

aga - 1-9-2014 at 16:07

WOW.

Schleimsäure - 1-9-2014 at 16:18

Quote: Originally posted by aga

WOW.

I can tell you. Former Eastern Germany is a heaven for amateur chemists. First, you have many older people still in posession of such lots. Secondly, there are still abandoned factories who ran into bankruptcy end of 90's to mid 2000's, with storage rooms full of chemicals. Together with friends I look for them.

Chemical industry was one of the biggest industries of former GDR.

Currently I try to locate thisone:

And believe me, I have absolutely no monetary motive.

[Edited on 2-9-2014 by Schleimsäure]

plante1999 - 3-9-2014 at 06:59

Don't forget to report your experiments over here!

If you got things to sell, you can make a thread on the Reagent and Apparatus sub forum.

Things like benzene are very hard to get, and not that dangerous, pretty sure many would be glad to be able to get some reagents like that, if you have too much of them.

Schleimsäure - 3-9-2014 at 12:37

Quote: Originally posted by plante1999

Don't forget to report your experiments over here!

If you got things to sell, you can make a thread on the Reagent and Apparatus sub forum.

Things like benzene are very hard to get, and not that dangerous, pretty sure many would be glad to be able to get some reagents like that, if you have too much of them.

Of course, will do.

Benzene I got just a 1l bottle. These hard to get chems I do not have in much surplus neither unfortunately. If I can find the above mentioned storage room, I could provide a lot. Though I think I would have to be careful when it comes to German law.

But the guy with the 450 boxes of equipment replied.
The amount of glassware, mechanical and electrical chemistry hardware is amazing.
He sent me a link with pictures.

http://www.labofix.de/

If you click through the numbers on top, you will see the pictures.

This piece alone is priced at EUR 1600 in used condition (looked it up), don't know what he would charge.

I mean with these things he got you can set up a pro laboratory.

Price indication for the stuff I initially requested I will receive in the next mail from him. I can imagine it's rather cheap, especially when bought en mass.

If it's really a bargain, I will ask in the subforum you mentioned if somebody else is interested.

Maybe, if many will come together and we buy a very large lot, the overall price will be very good.

Only problem is distribution, especially glassware. Or sending to US, Australia. Maybe for someone in Europe it's worth a trip to Berlin and we could go there togehter. It's about 100 km's from Berlin and I plan to go there in late september by car (assuming price is good).

[Edited on 3-9-2014 by Schleimsäure]

aga - 3-9-2014 at 12:59

The Sheer Volume of equipment is incredible !

Yes, i would love to have the opportunity to Play with it all.

As a Business Proposal, it would not be worth the Investment in Time or Money.

To identify, catalogue, describe and photograph everything would take a very long time, and a space where that could be done.

After that you would have to Sell it.
As Used equipment you would have to Clean anything Nasty out of it, which would involve even more Time and money.

For these reasons, this Lot of equipment has probably been trashed.

For the same reasons, it is unlikely that it is worth anybody's Time to Buy it all.
Sadly it will all get trashed, as that will be the most economical way to dispose of it.

It is still the most Amazing Discovery of used lab equipment i have ever seen.

Schleimsäure - 3-9-2014 at 13:07

Quote: Originally posted by aga

The Sheer Volume of equipment is incredible !

Yes, i would love to have the opportunity to Play with it all.

As a Business Proposal, it would not be worth the Investment in Time or Money.

To identify, catalogue, describe and photograph everything would take a very long time, and a space where that could be done.

After that you would have to Sell it.
As Used equipment you would have to Clean anything Nasty out of it, which would involve even more Time and money.

For these reasons, this Lot of equipment has probably been trashed.

For the same reasons, it is unlikely that it is worth anybody's Time to Buy it all.
Sadly it will all get trashed, as that will be the most economical way to dispose of it.

It is still the most Amazing Discovery of used lab equipment i have ever seen.

Absolutely, but I do not have business intentions anyway.

He put that in "ebay Kleinanzeigen", some kind of local ebay where people put all kinds of garage shop items in. That's why I hope I get a heating mantle 1000ml, vigreux colonne, some 2 and 3 neck RBF's (he has even 6l flasks), dripping funnel with pressure balance and some other small things for like 50 bucks, which would be insanly cheap.