Sciencemadness Discussion Board

Beginning. well. I suppose that'd be where I'm stuck.

nyx - 2-10-2006 at 13:18

Okay. Where. to. begin. ...

I've got hundreds of bits of glassware. Don't know what most of it is. I think I've got everything BUT erlenmeyer flasks and plain old beakers. Testtubes, i guess some sorts of condensers, bulbs with 1, 2, and 3 necks, connection pieces, filter funnels, filter bulbs? they look like the funnels.. only spherical, tiny bottles, a graduate or two, and assorted miscellany that defies easy description.

And my favorite new addition, an NMR spectrometer. snagged it at a college auction. No clue if it works or how it works or what it's good for if it does work. but it seemed like a fun gamble. It's big and heavy and has neat little dials and knobs. Who wouldn't want it for only 25 bucks?

Some digital analytical balances (I think accurate to 0.000 g) No idea if they're calibrated right or if that matters much at this stage.

Some melting point aparati. No clue how or if or what they do either.

Now, after senselessly amassing all of this, I feel as though I really owe myself to start getting my hands dirty.

So that leaves me wondering where to begin.

I'm currently in an apartment.

The only available 'lab space' here would be my walk-in closet, which conveniently has it's own sink, and offers a benefit of being right next to a shower should that for some reason be needed. I suppose I could connect a vent tube to the ventilation fan in the bathroom for a sort of fume hood, but I don't know if that'd be safe or useful for much. I don't even know where the ventilation goes.

Also rather important, I lack a general knowledge of chemistry beyond what I vaguely remember from freshman highschool, which I'm trying to remedy, though I'd feel more comfortable with the concepts with a little experimentation rather than reading. Most of the books I've found are either more overly theory oriented than I'm able to deal with quite yet, or so much the opposite that I'd not be terribly comfortable doing what they offer, at least not in an apartment with no ventilation or a clue of what I'm doing. They also often call for chemicals I don't have or know where to find.

Any suggestions? I'm just a tad overwhelmed at what to begin with. My interest at this point is mostly general. And in general, there seem to be quite an awful lot of different ways to go from here.

Thanks in advance

12AX7 - 2-10-2006 at 13:46

Well then. Start by eating the stuff in your cupboard that's in glass jars. Now you have some cheap glass suitable for like, beakers. Not good glass, it'll crack if you try to heat it much (microwave is -generally- okay, but be careful), especially externally, but chemically it's basically as good as borosilicate.

There's a lot of things you can do with beakers. Synth various compounds from household (and hardware store) chemicals. Grow crystals. Watch reactions, figure them out. Generally build the skill of practical chemistry. Then you could start distilling things with your column, extractions, more complicated processes with your fancy-shmancy equipment. Use a milk jug or something to ferment a sugary solution and distill your own alcohol...for fuel, of course! So on and so on. Check out member websites for ideas maybe. For the time being you can stay away from some of the more insane projects.. :)

Tim

making sodium acetate

Magpie - 2-10-2006 at 15:24

Here's something you can do without any special glassware (although a magnetic stirrer is quite handy). I.e., making sodium acetate from vinegar and sodium bicarbonate.

I used a large pickle jar to do the neutralization reaction, leaving a lot of freeboard as copious amounts of CO2 are generated. Then as each batch appeared neutralized I checked its pH with pH paper looking for about an 8 or a little more (see MSDS for pH). I accumulated the batches in a large Corning casserole (high freeboard is again good to minimize spatter). The casserole is heated at simmer on the kitchen stove all the while. Eventually you end up with a gravy-like slurry of mostly sodium acetate containing just a little water. Sometimes kitchen equipment is the best. ;) (But good thing my wife was away. :o )

So this is pretty much beginning preparatory chemistry showing you a neutralization reaction with gas evolution, and evaporation of a salt to near dryness. I will place the final slurry in my drying oven to finish the drying process.

Now from here I intend to go on to, as Tim says, the insane part, i.e., making glacial acetic acid from the sodium acetate. For this I will use a distillation set-up with gas tight fittings (tapered glass), bunsen burner, sulfuric acid, and do it in my hood, just in case. But you can stop at making sodium acetate, as you wish.

This is a common occurence for the home chemist (at least for me), that is, making your reagents. I do this for several reasons: (1) cheaper, (2) use OTC starting materials, (3) keeps me off lists, (4) sometimes its the only way to aquire the reagent, (5) can be quite challenging, (6) can be fun, and (7) you learn a lot of good basic chemistry.

Ooops. My wife just came home. She said that you are not supposed to place a ceramic casserole on a glass top stove. :o

sodium acetate.JPG - 64kB

The_Davster - 2-10-2006 at 16:04

Yeah, stovetops and glass vessels are a no-no, the temp gradient can be too high for the glass to take. Learned this the hard way..by loosing almost 2L of satuated KClO3 solution....around a pound of chlorate went allover the stove.

hinz - 2-10-2006 at 16:52

What kind of NMR is it? One of those old 60MHz ones, or a new 300MHz? You're quite lucky to get one, try to get it working. Then you can eighter sell it for a lot of money at ebay or you can do some freaky things in organic chemistry because you don't have to believe in reactions published in books. Instead you can cook on your own, modifying already known reactions and look what happens.
Did you get the accessory like the RF generator, detector and the measure computer, too? If yes, then assemble it and look if it's working, please take a photo I'm just curious

Magpie - 2-10-2006 at 17:34

Rogue, my understanding is that the ceramic casserole is OK for the regular electric element stove use, but that using them on a glass-top stove can damage the stove top. Can scratch it I think. This is why you're not supposed to use cast iron frying pans either. But if you are careful and don't slide these across the surface I'd think that there would be no problem. The stove is new and we are just getting use to it.

12AX7 - 2-10-2006 at 18:04

I find it ironic that the kitchen's "Pyrex" (in quotes as a figure of speech) measuring bowls are specifically labeled "not for stovetop or lab use". Pyr my ass!

Carefully on low heat, it works fine anyway. :D :P

Would be a damn shame to lose a couple quarts of electrolyte or other solution though.

Tim

Elawr - 2-10-2006 at 18:06

I'd have to agree about the ceramic cookware on the stove top. Last night I was messing around in the basement with a hotplate. Had some NaSO4(H2O) heating in a ceramic pan, which shattered as the last of the salt's water of hydration boiled away. Sure do hate it when that happens!

nyx - 2-10-2006 at 19:04

Thanks for the advice so far. Kind of amuses me that I have to make beakers out of pickle jars when I have all this other fancy-schmancy stuff laying around. Time to eat more PB and pickle sandwiches, I suppose.

Hinz: it's one of the 60hz ones. it's a Hitachi R-1200. So far as I can tell, it has everything except the oscillioscope, not that I'm an expert on this or anything. The one I have looks like this picture minus the doohickey on the sidetray : http://www.cas.astate.edu/draganjac/NMRInstr.html

Could I add almost any oscilloscope in it's place, or does it need this particular one? Don't have one on hand in any case, but I'll see about finding one at some point.

Didn't come with any manuals or anything either. just a big note labeled "SURPLUS." I plan on contacting someone in the science dept at the college to see if anyone knows anything about a manual for it laying around collecting dust in someone's office or the like. Or maybe someone around there knows details about the machine itself and can offer some advice.

Magpie - 2-10-2006 at 20:43

My assertion that Corning ceramic cookware can be used on the stovetop is not completely true. It seems that only Corning Corelle Visions has that capability. It is no longer in production but still likely available at yard sales and Goodwill.

I'm glad I didn't take that sodium acetate to dryness.

YT2095 - 3-10-2006 at 11:11

if it`s of any help to anyone, I do similar also when my wife is away, we have a Gas cooker/hob.
I have a large stainless steel bowl and in the bottom of that I put in well washed and dried Silver sand to a depth of about 3cms.
I rest my glassware snugly on the sand and proceed as normal.
slower heating time and cooling time (idea for large crystals too), with the added bonus that if the glass ever broke, the stainless steel would buy me enough time to deal with it.
and if it`s not corrosive, you can still salvage your chems from the glass and sand.

perhaps Someone here may find this tip helpfull :)

Diacetyl tartaric acid esters of mono and diglycerides?

nyx - 5-10-2006 at 03:38

Anyone know much about this? There's about a dozen 50lb boxes of the stuff in the dumpster behind my work.

I grabbed a couple, thinking it might be something I can play with for awhile. I mean, hey, a few hundred pounds of free chemicals.

About all I can find that makes much sense to me at this stage is that it's used in bread making as a dough conditioner. Smells kind of like an acid, I think.