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cmos6667
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[*] posted on 14-4-2015 at 10:28
Glassware question


Hi folks,

I'm overwhelmed :(
Where do you buy your glassware?
How many of which flasks do you suggest? Which volumes?
Do I choose just one filter flask (for vacuum filtration) that is 1000 ml or do I choose different sizes?
For recrystallization, I get that I use a small beaker for little amount of solvent to boil, but what's the situation with other things?
Does anyone sell a set from say Simax or Pyrex or Schott?

Sorry for the many questions but like I said, this is a bit overwhelming when you don't have that much money to spend :(
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ISCGora
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[*] posted on 14-4-2015 at 10:41


What is your budget?
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cmos6667
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[*] posted on 14-4-2015 at 10:51


I think about €1000, but that's including chemicals and electronics (laboratory balance, aquarium, vacuum sucker, uv lamp etc)

I intend to make perfume like compounds and maybe also toy around with polymers

[Edited on 14-4-2015 by cmos6667]
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ISCGora
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[*] posted on 14-4-2015 at 11:12


Well all depends on your plans I guess.I had pretty much same budget as you only it was just for glasswear.I bought a condenser400mm maybe 2 1000ml RBF
and 1 RBF 500ml,1 Erlenmeyer 1000,Distillation adapter,thermometer adapter with -20C/+350Cthermometer.vacuum take of adapter,maybe 5 beakers 1000ml ,2x500ml,250 and one of 50ml,3 neck round bottom flask 1000ml,some glass stoppers 2 crystallizing dishes 1000ml,pipettes pretty much all I upgraded a bit lately got a Separatory funnel 1000ml and also 50 test tubes 30mmX250 .(all with joints)

But with your plans I dont think you would need half of this stuff.Also it was pretty hard finding any glasswear sellers in my country I thought I could try buying from other places like US but shipping cost were huge and finnaly after 2 months of research I found some people and got all this under 1150e.
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MrHomeScientist
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[*] posted on 14-4-2015 at 11:24


The way I built my lab was to look up experiments I wanted to try, then buy all the equipment and chemicals for that particular experiment. That way, you don't end up with stuff you never use. Do this as your interest develops and soon you'll have a very well-stocked lab. Since you're interested in organic chemistry, round bottom flasks, a heating mantle, and a reflux setup would probably be good to have. I don't do much organic, but that seems to be common in most procedures. Besides that, general lab necessities include a balance with at least 0.1g precision, a hot plate / stir plate, beakers and flasks of various sizes (50mL - 1000mL), filter paper & funnels, spatulas or powder scoops, and lots of empty bottles. Check eBay for lots of glassware, or Dr. Bob here on the forum for his great deals and large stock. Look for his thread stickied at the top of the page.
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[*] posted on 14-4-2015 at 11:26


1000 ml is about the largest you would want in any of the glass commonly used. I guess mainly for holding whatever while you divy it up into smaller reaction vessels.

I sort of believe it is better to have two of each of the larger sizes mainly in-case one breaks.

For vacuum filtration's a 1000 ml filter flask, and 90ish mm Buchner funnel work well together. You also need a smaller 500ml filter flask to act as a "trap" or use a proper trap, and keep the 500ml for a spare.

Beakers, flasks, RBFs, graduated cylinders are relatively inexpensive in the 50 - 500ml sizes, and I believe you can never have too many. For a good starter set I would say 4 of each size is a good inventory (50 - 100 - 250 - 500ml)

Something to consider is ground glass joins vs. rounded edge, and rubber stoppers, connections...
For the few dollars saved, rubber is a pain in the butt. You are ALWAYS adapting something to work. Go for the ground glass... 24/40 is pretty much the most common size.

There are lots of starter sets around but most have stuff that you will never use, and some are just plain junk glass, Like the Amazon sets on line... JUNK!

I have two suggestions. Dr. Bob is a member here, and he is the most helpful fella you would ever want to run across. I would U2U him with a "wish list", and see how far he can help. He sells some used, and some new glass, and all of it is a BARGIN!!!

Second suggestion is Ebay, and Deschem. I ordered my first set (still unused) from them, and I could not be happier. I bought a 24/29 complete set up (picked out piece by piece), and all the beakers, ect I could ever use.
Total cost was under 250.00USD, free shipping, and a 10% discount simply because I asked.
For 1000.00 Eu you can set yourself up very well.

Look for used stirrer plates on Ebay, and the like to save a bundle. Same for almost all your electrical equipment.

There are a few threads on this site that show how to build some equipment, and some explain how to re-purpose everyday items for lab use.

Keep reading here, and your list will narrow down what you really have to buy vs. what you may THINK you need





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ISCGora
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[*] posted on 14-4-2015 at 11:58


Yeah,also don't forget to buy right hot plate/stir plate for right voltage in your country.In Europe it is 220V 50/60Hz and 24/40 far as I know are mainly used in US in Europe 24/29 is more common.
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szuko03
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[*] posted on 14-4-2015 at 12:15


I just started this process myself. The first items I plan on purchasing are basically all the pieces to be able to run a distillation at both 100mL and 1000mL volumes because I figure I will want to be able to do micro as well as full scale. Obviously I do not intend on buying two of everything but rather the boiling flasks etc needed.

For chemicals all the "basic" things in very small quantities just to produce a small library of reactants. Once I get all that stuff I plan on buying a college lab book and picking up my studies where i left off.

I already have a cheap scale and plan on getting a cheap heating/stirring unit for now.

The way I see it is getting a lab is basically a collection, there is no need to rush in and potentially waste money. Find out what you want to do and order based on that, or just get what would be considered necessities. Thats just me though. Also it fits what i have to do because my budget comes in 100 dollar chunks.

[Edited on 14-4-2015 by szuko03]




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[*] posted on 14-4-2015 at 12:48


When I first started out, I thought that it was good to get a lot of big glassware. I thought that 250 mL vessels were the smallest necessary and 24/40 jointed glassware was small enough to be used for anything. It turns out that isn't true at all. Quite often, you end up needing to do stuff on a smaller scale, and even when it's not absolutely necessary, it's still just as fun and equally rewarding as performing large scale syntheses. I would suggest not getting the stuff that ISCGora suggests, as it's all very large scale oriented and quite inflexible. Start with a good set of beakers, but get a couple extra 100 and 250 mL ones. Same goes for flasks. A 500 mL filtering flask is probably best if you're only getting one. 24/40 distillation setups are good, but like I previously said, they're less flexible and efficient than a good 14/20 kit (which is something I really want to get at some point)



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ISCGora
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[*] posted on 14-4-2015 at 13:07


I never said he should do what I did like.I said in that post:

"Well all depends on your plans I guess."


:)

[Edited on 14-4-2015 by ISCGora]
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[*] posted on 14-4-2015 at 13:59


I started last year, not in an organised way,
all of my glassware is via eBay, almost all 'used', some individual pieces, some in large (very) mixed job lots.
often one or two pieces in a job lot can justify the total cost and I got lots of interesting glassware.
nett result ... GBP500 on equipment (including hotplate, thermometers, scales, pumps, etc.)
I have ended up with several joint sizes, which is a nuisance ... beginners oversight :)
including a very cute 10/19 distillation kit and accessories
small size is cute, takes less space and encourages minimal use of chemicals (cheaper and less waste)
but more expensive than the common (European) 24/29 equivalents

I suspect that you will be doing steam distillations for essential oils etc.
there are several choices of 'complete' borosilicate 3.3 "distillation kit" on eBay,
stands and clamps are essential, I discovered. (I'm looking for cheap 10/19 keck clips :(
I found it very frustrating to wait for the piece that I forgot or didn't know I needed
so I think that a Chinese eBay kit is an easy start, and any part can later be 'upgraded' if needed.
I have some Chinese glassware, not as good quality as Quickfit
but perfectly usable and MUCH cheaper

I have not bought a complete eBay Chinese distillation kit,
my opinion is just based on a few random pieces that I have.

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Etaoin Shrdlu
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[*] posted on 14-4-2015 at 14:01


Quote: Originally posted by cmos6667  
I intend to make perfume like compounds and maybe also toy around with polymers

Kindred spirit!

You're going to want a scale, hot plate, thermometer, test tubes, flasks, beakers, reflux condenser, and distillation setup at least. Addition funnels and separatory funnels are nice to have, as are glass dropper bottles for solutions or liquid reagents you use frequently. Graduated cylinder will be practically necessary, graduated pipettes are good but less crucial. Get set up for vacuum filtration if you can. Parafilm is great for closing test tubes temporarily or lining caps that might otherwise get attacked by solvent. If you start working with bromine or iodine you may want teflon tape as well. Don't forget boiling stones. Buying containers to store products in beforehand is a Good Thing To Do.
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cmos6667
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[*] posted on 17-4-2015 at 13:11


Thank you all for your answers, they've been very helpful!
I found glassware all together for around 100£, now all I'm missing is that thing you attach to the bridge to attach vacuum...
Any idea on what it's called and how much it should cost?
Apcpure calls it "bends with vacuum", but it costs more than 20£, which sounds ridiculous considering I'm getting a Dimroth condenser for the same price
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Sulaiman
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[*] posted on 17-4-2015 at 13:21


Vacuum adapter? https://www.google.co.uk/search?q=vacuum+adapter&es_sm=9...
or
receiver adapter? https://www.google.co.uk/search?q=receiver+adapter&es_sm...

[Edited on 17-4-2015 by Sulaiman]
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cmos6667
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[*] posted on 17-4-2015 at 13:35


Ahhhh thank you very much :)
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cmos6667
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[*] posted on 29-4-2015 at 09:11


Another two things:

What's a reliable balance (I suppose around .1g accuracy) brand? for around 100€
Is there any digital melting point apparatus available for less than 200€?
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[*] posted on 29-4-2015 at 21:07


Quote: Originally posted by cmos6667  
<snip> What's a reliable balance (I suppose around .1g accuracy) brand? for around 100€<snip>

Werll, mine is similar to this one but goes to 300g with a precision of 0.01.
At a similar price point there are many to choose from. http://www.dx.com/s/digital+scale
I haven't calibrated it / tested it so I don't know if its accuracy is as good as its precision. But it does the job for me rather well and cost next to nothing.
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[*] posted on 29-4-2015 at 21:55


Cheap and sufficiently precise scales cost around 10-20$. Although they don't have the declared precision on all wights, but they can definitely measure few grams very precisely. Make sure you don't buy the cheapest one, because they don't even have the declared accuracy because of temperature drift, time drift and other problems.
My last one is http://www.globalsources.com/si/AS/Shenzhen-Big/600884525326... and they are doing really well, though it probably will measure 30.00 grams weight as 30.05 or something, but who cares? It will still be 0.01 g precise if you tared it with 25-35 g weight first.

Now my question: why should I need a crystalization dish?
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cmos6667
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[*] posted on 30-4-2015 at 06:42


Crystallization dishes are better because they are low in form and heavier than beakers
The crystals are bigger because they dont transfer as much vibration to the content
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[*] posted on 30-4-2015 at 11:14
I have developed a standard response to this question:


It all really depends on your budget and what kind of experimentation you plan to do.

Some of the bare necessities:

1. A decent 0.01g (or better) scale. You can't do much if you can't weigh anything out!
2. Graduated cylinders. For the same reason as #1.
3. A device for heating and stirring - essential for solution preparation. Even a $20 Walmart hotplate, and a glass rod for stirring will be fine to start. Magnetic stirring and a set of various bars is really nice if you have the cash.
4. Vessels you can heat. A lot of great packs of beakers and Erlenmeyer flasks can be found online. It is good to get a variety of sizes, but double up on the ones in the 300-600ml range since you will probably use these the most. Get Erlenmeyer flasks with stoppers for oxidation sensitive things or stinky solvents.
5. A 1ml class A pasteur pipette and bulb. This is the best $5 you will ever spend. Coupled with the scale, it is an incredibly useful analytical tool for taking the density of liquid solutions, assessing gravimetrically the solubility of compounds, etc.
6. A partial immersion thermometer, and some closed-end capillaries to go with it. Melting point is also critical in assessing what you have and how pure it is. You can get a thiele tube if you want but a well-stirred oil or water bath works just as well.
7. A decently-sized (~100mm) porcelain buchner funnel, filter flask, and water aspirator. Waiting hours for things to fall through coffee filters is annoying, and will ruin compounds that you want to prepare anhydrous, or those that react with oxygen (which there are a surprising number of). Sometimes you can get the vacuum tap on the funnel and use a regular erlenmeyer to catch the filtrate. Don't bother with a hand pump for vacuum. They suck.
8. Storage. I started with cheap canning jars. Freund Container and Specialty Bottle are great places to get lots of containers for both solids and liquids.

You will find that there will be lots more incidental things you need to make your life easier - spatulas, funnels, a mortar and pestle, a torch, pH paper, a burette, wash bottles, a sep funnel, syringes, pipettes and droppers, test tubes, etc. I would suggest buying these as you see fit. Skip the expensive stuff to start - I still use plastic spoons from the grocery store and funnels from the auto parts store even though I have glass ones... simply because glass is expensive, fragile, and not always necessary. If you buy the stuff as you need it, you will eventually end up with a well-stocked lab.

You may have all of that already though. The next step starts getting expensive, and that is the distillation stuff. This level gets ugly on the budget really fast.

The best way to start is to pick up a kit. Cheap Chinese distillation kits are worth it. You will break things. Everyone tells themselves that they are not like the others and they will be very careful, all the time... me included. I still have a glassware graveyard full of newbie mistakes. I would be much more angry if the broken crap wasn't cheapie glass from China! Shatter your glass, not your bank account. The worst part about Chinaware is that it takes like 15 days to ship.

I currently have all 24/40 stuff. 24/29 is also common in Chinese glass. I started with 19/22 because I was being cheap... I ended up selling it shortly thereafter because the stuff was just too small to be useful for anything involving large amounts of solvents or purifying OTC chems, and 19/22 was hard to find apparatus for.

Get a kit corresponding to what your budget allows. A simple 500ml distillation kit with a 300mm leibig will suffice for most purposes. Keep in mind that if you break just one piece, the whole thing is unusable until you get the replacement part - hence the beauty of bigger kits where you get multiple condensers, extra flasks, and extra adapters. This is also why it is nice to go with Chinese glass to start. Getting one with a Vigreux column enables you to fractionate better and you will be able to do a lot more with your kit. Again, get the biggest one that still fits your budget with some wiggle room for incidentals. I would also suggest picking up at least one multi-neck flask.

Keep in mind that you need to figure out:

1. A heating system for the boiling flask. You can use a hotplate/oil bath/water bath heating system for the flask (which suck!), with a lab jack (or wood blocks, as I used to do...) so you can remove it from heating if you need to. You will be unable to stir unless the hotplate has a magnetic stirrer. A heating mantle is better, but you will also need a variac to control the temperature. A 1000mL heating/stirring mantle is ideal for amateur scale stuff; I have two of them. Unfortunately they are also very expensive.
2. You will need the ability to circulate water through the condenser - It can be a hose on a water tap or a pump in a bucket. Keep this in mind when you make your budget list. A pump is a lot more expensive than 10 feet of vinyl tubing from the hardware store.
3. Invest in good quality clamps and stands (which are annoyingly expensive!) or you will be like me and break a bunch of glass trying to use homemade ones, and end up buying them anyway.
4. Finally, consider building a fume hood. You may have been able to get away with it up until this point, but boiling stuff inherently involves fumes - potentially unhealthy, flammable, etc. Now is the time to invest in something that could save your life/house or prevent you from working outside all the time.

And then there is the miscellaneous junk like joint grease, boiling chips, keck clips, thermometer O-rings, storage flasks with stoppers, addition funnels, flask brushes, claisen and thermometer adapters, extra stoppers, etc. I won't even get started on chroma columns, microscopes, gas washing, etc.

I do have a lot of ace/wilmad/kimble/kontes/kimax/pyrex/chemglass stuff but almost all of it is used and was purchased on ebay. I am just now getting to the point where I can justify the purchase of expensive stuff because I am dealing with some pretty nasty chems, airless chemistry, etc. I wouldn't worry about glass quality since it's all 3.3 boro glass, Chinese or not, and almost every Chinese place I have bought from will refund for any defect or breakage in shipping.

Anyway, on top of all of that are the chemicals. If you need OTC sources for chems, I can definitely point you in the right direction.

eBay is the greatest place to get stuff, and Amazon after that. I can point you toward my favorite sellers if you're interested.

I realize that was a bit of a ramble, but I hope it helps a little. If you have any questions about something specific, I will be glad to help!

[Edited on 30-4-2015 by Praxichys]




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