Sciencemadness Discussion Board

1k for new labware, What would you get.

Sedit - 15-8-2010 at 17:52

I know this sounds like one of those "whats your reagents" type of threads but I want to run this to get an idea of how to budget money while trying to build whats needed to perform various operations in a home lab.

If you had 1000 US dollars what would you do with it if you had nothing but improvised equipment.

Seperation funnel is first and formost because thats the one thing that improvised equipment fails at everytime for one reason or another.

So as it stands what would be your choice? Try to keep it small because almost all my experiments are small scale and I have no will to scale up at the moment. This is an important thing to keep in mind for myself.

Arrhenius - 15-8-2010 at 18:38

If you like small scale, buy a ~$300-400 microscale kit (14/20 joints). That'll get you a distillation setup and reflux setup. A vacuum pump ($100 and up). Thermometers (cheap). A balance (a cheap eBay one will do). A Thiele tube for melting points - I think this is something every amateur organic chemist should have, because a melting point is one of the only pieces of data you might reasonably obtain to ID a compound. A hotplate/stirplate & stirbars (expensive). Spend the rest on reagents.

aonomus - 15-8-2010 at 18:41

Well, you might have to be a bit more specific.

- What is 'small scale', 0.1g, 1g, 10g?
- What do you do in terms of average operations? Refluxing, filtrations, separations, extractions?
- What improvised equipment do you have? Non improvised?

For myself, if I had $1kUSD, I would probably invest towards building an 'improvised' (but not really improvised) fume extraction hood, chiller, vacuum system.

If it had to be glassware/labware and not furniture/support equipment:
- Distillation head + RBF + mantle for solvent distillation/prep
- Hotplate + sand bath/heating block for oil-less heating

densest - 15-8-2010 at 18:42

Organic? Inorganic? All of this will have to be used. $1K doesn't go very far for new equipment.

And most important a clean, solid table with a resistant top and place to wash all of this & a set of jugs & cans to dispose of your waste.

Chainhit222 - 15-8-2010 at 22:24

a dry box

and maybe a present for chainhit

can anyone recommend any cheap FTIR's?

[Edited on 16-8-2010 by Chainhit222]

kclo4 - 15-8-2010 at 23:23

Quote:
If you like small scale, buy a ~$300-400 microscale kit (14/20 joints). That'll get you a distillation setup and reflux setup. A vacuum pump ($100 and up). Thermometers (cheap). A balance (a cheap eBay one will do). A Thiele tube for melting points - I think this is something every amateur organic chemist should have, because a melting point is one of the only pieces of data you might reasonably obtain to ID a compound. A hotplate/stirplate & stirbars (expensive). Spend the rest on reagents.


I agree with this strongly.

good advice!

Look in surplus -- if it works, you can get it a lot cheaper!

What to get?

Enantiomer - 16-8-2010 at 01:07

Well, as some other replies have suggested, it does depend on what your objecive is. However, let me offer some input on what someone I know recently spent thier money on . . .

This person had roughly $500 to spend and they decided to go to work on ebay making some purchases (granted, some of these may have been unwise decisions and they may have been able to get more in the end).

They decided to go up to 3000 ml capacity.

Sep funnels (500, 1000, and 2000 ml)

RB flasks (1 3000 ml 3 neck straight necks, 5 X 250 ml single neck, 1 X 500 ml single neck, 1 X 1000 ml single neck - some of this a package deal).

Filter flasks (1 X 1000 ml, 1 X 2000 ml)

Graduated cylyners (1 X 250 ml, 1 X 500 ml, 1 X 1000 ml)

Erlenmyer flasks (2 X 125 ml - happened across in a garage sale)

Condensers (1 X 300 mm west condenser, 1 X 300 mm alihn)

Buchneer funnel (1 X 83 mm coors)

Thermometer (1 X 10 degrees to 260 degrees celcius)

Adapters (1 X claisen head, 1 X 105 degree bent vaccuum adapter, 1 X distillation reciever)

Greeen keck clips (for 24/40) a dozen or so.

Thermometer adapter (1 X)

And this one wierd dessicator apparatus called an abderhalden drying apparatus.

All 24/40 joints

If he had, had another $500 I bet he would have purchased a scale (new) that weighs to a min. 0.01 resolution with as high a capacity as possible for the money (maybe $250).

He might have purchased a magnetic stirrer/ hot plate (these can be expensive new but it is the type of thing it is ok to buy used, if you are careful)

And, if he had, had another $500 he might have purchased a couple pressure equalized addition funnels (say, 500 and 1000 ml), and he probably would have filled in the rb flasks collection (ie - 3 necks for 1000 and 2000 ml, and 2 necks for 1000, 2000 and 3000 ml).

He definitely would have invested in a fume hood (very useful/ necessary) but he would have built his own since this item is extremely cost prohibitive to just purchase as is.

If he had yet another $500 he might have purchased a good millligram scale (0.001 resolution) or even better something with 0.0001 resolution (one tenth of a milligram - adjusting for error, of course).

Overall, if he had, say, $3000 to invest, he's sure he could have had the kind of basic setup that would really be pretty complete (of course there is always more when you start to get into it - electrolytic cells, etc).

None of this counts the cost of materials/ ingredients for experiments (just equipment).

I'm sure there are some people on this board who will kill me for saying this but, please, for the love of God, don't improvise unless you have to. Most real lab ware is easily had at a very cheap price. It is not illegal to own or to purchase (except in a few states, like Texas and mayve California) but you may still want to be careful. Even if you think you will end up with more (bulk wise) by improvising - and you may be right - you are far better off with the real stuff. It is designed for the purpose (interchangeable joints, etc). Be sure you know how to care for your equipment so it doesn't fail/ break on you (know how and why you must grease the joints and what type of lubrication to use given your application).


zed - 16-8-2010 at 11:42

I come up with, buy a Parr pressure reactor on e-bay. They don't come up for bid very often now, but that would be my pick. In the past, I've seen several go in the 500 dollar range.

Then, I'd acquire a microwave oven, to dedicate to chemistry only. And, I'd buy or build a tube furnace. Finally, were there any money left, I'd build a "Sponenberg type" Ball milling machine.

A good fume hood would be nice, and a dry box/glove box would round things out. Mo' money, Mo' money, Mo' money. Oh, and an emergency lab shower. All of that neat equipment, would be of little use to me, if I became a crispy critter.

Better give me more money to play with. How about three thousand total? Since my glassware is basically "zippo", I'd need to upgrade via LabEx auctions.

OK, so...... three thousand wouldn't actually be enough to build a good home lab. But it would get you in the "ballpark".

peach - 16-8-2010 at 17:40

I'd buy this & then that, which I did, about 3 hours ago...



Only kidding, except about me actually buying them. Kidding as to suggesting you should include them in the budget.

To give you a comparison of what I've been working with thus far, in addition to the digital kitchen scales and (when their batteries ran out) a ruler balanced on a pencil with some coins on the other end...


Before the nay saying boots up, you may wish to check the minted weight of a UK penny and compare it to what's on the display. That was the first one I picked up and threw on there. I have owned these for years, they cost about £8.99 from China, I've spilled stuff all over, never even attempted to calibrate them, but there are the numbers.

I chose those pictures quite carefully. That little 'piece of shit', costs next to nothing. The others are £3k new. The 'POS' are so light and small, one of their major downfalls is them falling down the sides of things. The others, that platter it's sat on weighs about half as much as me.

Why those pictures? To graphically illustrate a point. Those cheapo ones are perfectly accurate in the hundred ml's scale, they're dirt cheap, incredibly compact and light, require very little (zero) care to be taken over them and so on (they're pretty much disposable at that price). So why did I just drive for an hour to get the others? Purely because I'm now downgrading, or upgrading if you want, to the 5ml type domain for reactions, so I'm running off the edge of those. But that's an ultra small scale, you won't get that running in normal glass (even normal B14 has issues with it).

The only other major downside to those cheapo scales is the impression they give, particularly to the boys in blue. Although, I'm sure they'd have issues with that balance as well if they were unhappy about something (you're more than welcome to visit, but please knock prior to wrecking the front door... :D).

I have also checked things like 'dividing by eye' with icing sugar when I got bored and found it can be remarkably accurate when done with some care (which that balance it's self requires).

I'm trying to say, sometimes the cheaper things are perfectly good (or even better suited) as part of your $1k budget. For instance, that's a nice balance, but look at the amount of desk space it's taking up; which is, it's self, a highly valuable asset around here. ;)

Here they are playing their part in my caffeine post.


Whilst I was going to reply to you saying your question was a little too diffuse, I think a few of the replies are even more so. It's seems to me that you are probably at the beaker stage (or slightly above) and looking for the first few bits. Some of the recommendations (whilst I do agree they're good to have to hand) are going to perhaps be a bit beyond what you can actually make use of given what you already have, I imagine.

Also, small scale (to me), means a few hundred ml or less, so even a 250ml funnel is big by comparison.

With that said, I entirely agree with Arrhenius and kclo4 with regards to B14. I am now amassing a large collection of B14 because it's so much easier to work with; particularly on experimental (referenceless / instructionless) ideas.

I would also recommend you check out things like Chinese hoteplates. I have had a £750 - 1k plate from IKA, and sold it. This is the first Chinese plate that shows up from some googling. Check them out (MS300?), higher temperatures than an IKA, digital display of the heat and stir parameters. Even has a built in timer, so you can go for some important, brain enhancing beer in the mean time. When I checked the price on these, it was around $150 I think. I would not be surprised if they've simply copycatted the circuit from an IKA.


Forget fume hoods and all that for now. I was on the phone to BOC and Air liqude this afternoon about renting cylinders of corrosive and speciality lab gases. Those gases =/= fume hood, hazmat & respirator, so basic stuff certainly doesn't.

The guy I bought that balance from actually happened to work for Air Products here in the UK, building the 2kT per day liquid oxygen fractional towers for steel refineries and things to generate it on site. The balance came out of their lab. He's now working on some obscure thing for Sellafield to handle nuclear 'liquor' with.

You can even forget about the hotplate to some extent, you can find a counter top hotplate at the tip and (provided it has a dial on it) it won't be a million miles off a commercial plate. You can also use a fridge pump for a fair bit of vacuum work (as I discuss in the video I just made, as I tear two apart to the nuts and bolts level); I'll go a stage further and tell you I still use fridge compressors for some vacuum tasks, despite the fact I now have three laboratory rotary vanes. Cold stirrers you can make from a $2 computer fan, some glue and some magnets.

"A poor workman blames his tools". True to some extent but you also can't do the best possible with the worst available. There's a balance to be struck (ha har :P), and your inventiveness and care plays a big part in setting the tipping point.

If I had to pick a few items off the top of my head;

Clips to hold the glass together (or, !smash!)
A GOOD THERMOMETER! So easily overlooked, so, so, so important
Roll of tinfoil for TP heating

My thinking when replying to this has been to suggest ideas for how you can 'feel your way through', rather than dump a lot of money and then find you can't afford something important, when you could have ignored some of the other items.

For example, you could spend that entire grand on a fume hood. Then have fuck all to put in it.

Here's the B14 3 way vacuum thingy-meh-jiggeroo I have at the moment, which I'm actually about to sell, as I now have multiples of some items.


[Edited on 17-8-2010 by peach]

densest - 16-8-2010 at 18:59

I'd second, third, fourth, whatever the thermometer!! They vary in quality all over the place. If you're not too much of a klutz, get a mercury thermometer. The "mercury free" lab thermometers I've had have all been wildly inaccurate and/or have had permanent bubbles.

On the other hand, the cheap cheap cheap electronic cooking thermometers I've had are all within 1F of correct. As long as 1C or 1F resolution is enough and stainless steel will not be corroded, the one I got for under $10 reads from 0C to 300C (maybe 350, I forget).

And small scale glass is often less expensive, lighter, and, well, smaller which encourages tidy work. And if a reaction does something unexpected, there's far less of a mess.

Chainhit222 - 17-8-2010 at 03:22

Quote: Originally posted by densest  
I'd second, third, fourth, whatever the thermometer!! They vary in quality all over the place. If you're not too much of a klutz, get a mercury thermometer. The "mercury free" lab thermometers I've had have all been wildly inaccurate and/or have had permanent bubbles.

On the other hand, the cheap cheap cheap electronic cooking thermometers I've had are all within 1F of correct. As long as 1C or 1F resolution is enough and stainless steel will not be corroded, the one I got for under $10 reads from 0C to 300C (maybe 350, I forget).

And small scale glass is often less expensive, lighter, and, well, smaller which encourages tidy work. And if a reaction does something unexpected, there's far less of a mess.



bulk reactions are much more fun imo.

peach - 17-8-2010 at 04:19

Quote:
bulk reactions are much more fun imo.


;)

True, until it goes unexpectedly fk'ing mental and ruins everything.

It also starts getting very expensive when working with pricey reagents on things that are still being worked out.

I suppose when choosing glass sizes you really have to have a think about what the intention is. For a lot of the time, if you're working out parameters and looking at how something functions, you'll only be working with tens of ml's. If you're reasonably sure something will work (some guys on here have already done it and the optimizing for you), a few hundred ml's will usually be good. A few hundred ml's is also okay for experimental work if the smaller scale is beyond what you're comfortable handling or capable of accurately measuring (running things at tens of ml's is trickier than it sounds, as is running tens of liters). If you're trying to run up a batch of something, like a solvent or reagent, so you don't have to keep remaking it, a liter or two is good. A few hundred mls often falls into the tangible, human, everyday numbers, so kitchen measuring jars and scales can function reasonably well in the range.
Quote: Originally posted by densest  

On the other hand, the cheap cheap cheap electronic cooking thermometers I've had are all within 1F of correct. As long as 1C or 1F resolution is enough and stainless steel will not be corroded, the one I got for under $10 reads from 0C to 300C (maybe 350, I forget)


I've been using a digital probe to monitor some things as of late.

Shame that it'll only read to 100C, making it not all that useful for distilling heavier things.

I can calibrate the meter this is coming from, which is important.

As you, being an electronic'sy type person, may already realize, measuring temperature, accurately, with digital gear can sometimes be misleading.

A lot of digital temperature sensors have 0.1C increments on the display. However, checking the actual datasheets from the semiconductor guys, the sensing elements often can't manage better than 0.5C, and it's often 1C; with the 0.1C being there to fill up the rest of the display and make it look good.

As with a normal thermometer, I'd certainly recommend giving a digital a dip in some boiling, distilled / deionized water, ice made from the same and perhaps some boiling solvents in between.

My mercury is on the way out after years of loyal service. The bulb has cracked, I have splits, it's dying.

If your columns split, and the glass is still okay, toss the suckers in the freezer for an hour. Take them out and immediately flick the bulb, tap the stick against the side of your pointy finger, or use an electric tooth bursh to vibratorize them. That can rejoin the column. I'm sure a few of you already know that, but I expect a few don't.

Now I have some mercury to amuse the younger generations with (including myself), as it's obviously not something people under the age of about 40 have much first hand experience of with it now having a bounty on it's head in educational establishments.

I just noted densest recommendation of a permanently available, dedicated surface to do this kind of thing on; preferably not in the kitchen (for reasons you're about to see). Moving it round all the time, you'll break it and get so tired moving it you'll never want to do anything.

I won't post these in tour my lab, as I haven't made any effort to actually get things out, I just thought you might like to see the mess.

"Is it... e-vil?"


That's 1" ply, supported in two places along the length and batoned around the edges, painted with polyurethane commercial stuff (I'd recommend epoxy floor paint for resistance and wipeability).


That's why the kitchen sink is a bad idea. Particularly if there's anyone with a pussy in the house; marmalade doesn't like the state of the sink.


You's dern wanna have that on yer freshly installed, solid wood kitchen surfaces! Note the POS scales beside the balance in this and the first photo, for a direct size comparison.


The floor is also a prime target (epoxied, smells amazing, goes off very quickly once mixed, very sticky to put down, very messy if not gloved up and 100% ready to go)...


[Edited on 18-8-2010 by peach]

DDTea - 17-8-2010 at 11:34

My opinion on thermometers: get yourself a mercury one. Alcohol thermometers and the like have caused me non-stop frustration. At higher temperatures especially, they don't expand very linearly--at least, much less linearly than mercury does. What a lot of people don't realize is that thermometers are calibrated to be submerged to a certain depth. You'll see them labeled "partial immersion", followed by the immersion depth, or "total immersion." It makes a difference, especially with those alcohol thermometers at higher temperatures (and by "high," I mean as low as 90-100 C). If you don't do a stem correction, the temperature the thermometer is reading can be off by quite a bit. Save yourself the headache and just buy a mercury thermometer.

Also, whatever scale you get, buy yourself a box of weigh boats and weigh paper. Those small things can make your life a lot easier :)

Not sure if this would fit in your budget, but if you DO plan to work on a microscale, a micropipette is another nice tool to have.

Don't forget some volumetric flasks. Those are absolutely essential.

[Edited on 8-17-10 by DDTea]

psychokinetic - 17-8-2010 at 13:02

Peach - is the tumble dryer for when the ceramic cat gives you sass?

peach - 17-8-2010 at 18:16

Quote: Originally posted by psychokinetic  
Peach - is the tumble dryer for when the ceramic cat gives you sass?


How dare yar sir, how dare yar land lubber! If only marmalade could understand the word virus, she'd nuke you with her neon green lazer eyes.

No, no, no, no, no! NO!

The washing machine is where I do my glass and the dryer is for the anhyrous....

DUH! :P:D

mr.crow - 17-8-2010 at 19:43

Looking good in your lab, peach.

Looks like you've spilled iodine everywhere :( time to get some sodium thiosulfate.

As for thermometers, I want to get a thermocouple probe and seal it in the end of a glass tube. They can withstand the heat of the softened glass.

As for small scale, you can still use 24/40. I have some 50 and 100 mL flasks and a distillation head with built in condenser for that purpose. Less hold up space.

1K For Lab Gear

MadHatter - 17-8-2010 at 19:47

Distillation setup, vacuum pump, centrifuge, high resolution balance, expensive reagents.
You'll eat 1K pretty fast with that combination.

DDTea - 17-8-2010 at 22:24

And more on those sort of "convenience" items that will make lab work more efficient (i.e., less of a headache to do the simplest things):
-Wash bottles for at least Water and Acetone.
-Bottle-top dispensers (to minimize contact with strong acids)

Are you planning to include Personal Protective Equipment in this $1k? If so, I'd suggest the following:
-Nomex lab coat; the flame resistance could really save you one day.
-Face shield, in addition to your regular goggles
-A few boxes of Neoprene gloves, although your hand protection will depend on what you're working with.

peach - 18-8-2010 at 03:42

Quote: Originally posted by mr.crow  

Looks like you've spilled iodine everywhere :( time to get some sodium thiosulfate.


Yep, I have a fair amount of it in sublimated form, so it's extremely easy to get the yellow spots as a grit sized bit or two goes missing.
Quote: Originally posted by MadHatter  
Distillation setup, vacuum pump, centrifuge, high resolution balance, expensive reagents.
You'll eat 1K pretty fast with that combination.


I don't think that's true.

Guys like UGT and Expedi sell distillation setups, new, reasonably cheap. If you're not doing fractional distillations, you can use a fridge pump (I've seen HVAC vacuum pumps on eBay, new and with a buy it now and fifty in stock, for ~$100, and the pressure rating is close to a used laboratory pump, or better).

He's not going to need a high resolution balance for working with a few hundred ml, unless he's a biologist working with enzymes or a chemist specializing in catalysts. I've been using those £8.99 scales for years and they've worked fine.

I don't have a centrifuge (possibly hackaday / instructables material, modify a washing machine drum (tip)? 1krpm? Very tolerant of unbalanced loads, very large OD chamber. Has an element for warming the inside 'water bath', timer, interlocks, fill / drain, etc...).

Expensive reagents... that depends entirely on what he's running in it doesn't it. He could be doing things that require 1p's worth of reagents, or £1k's worth.
Quote: Originally posted by DDTea  

-Wash bottles for at least Water and Acetone.
-Nomex lab coat; the flame resistance could really save you one day.
-Face shield, in addition to your regular goggles
-A few boxes of Neoprene gloves, although your hand protection will depend on what you're working with.


I forgot that one, and it's a very good one, wash bottles.

I wouldn't get the lab coat myself. The face shield is a good idea, better than goggles and the coat IMO. The gloves, yep... that depends what you're doing with them really.

I've seen the really expensive ones from Ansell that are supposedly resistant to the charm of Jesus, but they work by having 5 laminations of varying material (I think). I expect, it would be possible over repeated exposure to different things, to go through all five and that it'd be cheaper and easier to buy some boxes of disposables and get used to which works for which, as they go in the bin.

I'd recommend you grab a pair of these (drain gloves) from the DIY store for the washing up. I've been through a lot of gloves in doing the dishes, these are the way to go (the long sleeves are necessary, or you'll have the wash going down the cuffs as you move the glass around);




[Edited on 19-8-2010 by peach]

iHME - 18-8-2010 at 11:17

My chemresistant gloves are from the harware store. Thick nitrile.
Mine ware sold directly as chemically resistant.
They do stand quite nicely against common acids like nitric and sulfuric.

Sedit - 18-8-2010 at 17:09

Wow thanks for all the replys since im not use to getting so many so quick. It would take a week to get this many replys on a detailed experiment.

@Arrhenius
I have in mind a microscale kit that was in the range of about $250-450 IIRC and it contained the basics such as distilling, refluxing ect with a few different attachments. It also includes a seperation funnel which is a plus.

I honestly can do without the hotplate at the moment because im pretty handy with my hands and make something to suffice for now without forking over serious dough on a hot plate and stirrer. Its no doubt on my ToDo list but for now I would like to focus mostly on glass and apperatus like the melting point apperatus other then reagents.

@aonomus

Sorry if the term small scale confused some but my main objective it to keep MOST operations at a 1 mol scale or below for the sake of saving cost on reagents as I experiment. I do however wish to leave my options open to scale pretty large when desired to ensure I have space for larger reactions when I got the kinks worked out in smaller scales. Id rather do my haphazard form of experimenting at the smallest scale I can get away with yet still be able to isolate whatever i'm working with.
Quote:

What improvised equipment do you have? Non improvised?

All improvised, I have condensers able to reflux I have oilbath/stirrer. Mainly I improvise when I need it and most of the equipment I need I make prior to the experiment adding time and effort into anything. While this is something I truely enjoy I wish to have a setup ready to go when needed since I feel I have reached that point where I wish to focus more on the chemistry itself other then the construction of the materials I need.

Support equipment is a must since I really want a sturdy setup. I want to be able to clamp it and let it be for something without affecting it in anyway.


@Peach

I love the idea of pear shaped flask so when you mentioned you are about to sell that B-14 3 it caught my attention. PM me so we can talk about somethings.




Thank you to all I may not have mentioned. Its something I really want to do and small scale things like epoxide floors and gloves ect... are so cheep in comparison that I am not including them into my budget. I plan on 1k but given my track record of funds I may not get quite that but we will see. Im more then likely cutting myself short and there is talk of padding my wallet well beyond what is going on now so that is indeed a pleasent suprize. Good to know a highschool expelle can still make good money in such a harsh economic times while still getting the respect they deserve.


Cheers everone keep the suggestions comming. I wanted to respond yesterday but yall seemed on a roll and I didn't want to interrupt when everyone was in the zone like that :D

smaerd - 19-8-2010 at 08:51

-I'd finish my chemical storage cabinet($20)
-I'd tile and finish my counter-top($30)
-Fume-hood(need a nice fan, etc)($400?)
-A gas tank and regulator for inert atmospheres($100)
-A Nice PH Meter($100-$200)
-Magnetic Stirrer($50)

The rest I would probably blow on storage bottles, glass-ware, and sillica or alumina for gravity chrom.

Chemicals are important but I need a lab first!

[Edited on 19-8-2010 by smaerd]

Ephoton - 19-8-2010 at 16:44

mag stirr hotplate $250
small glass kit $250
cheap oil vac $150
1L sep $100
alc burner $30
crucible set $50
tongs $15
misc stands and clips ect rest of money.

all found on ebay rough prices.

psychokinetic - 19-8-2010 at 22:38

I didn't realise there was any ambiguity.

Peaches are tasty.

devongrrl - 21-8-2010 at 01:45

I'd have to add a nice vacuum dessicator to the shopping list.
Ziploc bags with CaCl2 or MgSO4 are ok but nothing pulls out moisture like a good vacuum, imho.

Mildronate - 21-8-2010 at 05:16

just look for some closed local lab that will be much cheaper.