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aonomus
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[*] posted on 18-10-2009 at 19:52
Starting glassware and reagents?


So first a bit of background on me (first post), I'm a undergrad at the University of Toronto studying chemistry & biology, and I've been working with electronics for some time now, so I already have a little bit of glassware for preparing circuit board etchants, etc.

I've been wanting to do some experiments such as making ferrofluid via different methods, maybe the occasional organic experiments as well (and a home made fume hood would be well in order for that then). Also some preparatory things such as mixing up circuit board etchant, or distilling large amounts of water to wash things, and maybe distilling plant oils (orange oil, lavender, etc) for soaps?

I have a few questions regarding glassware, reagents/chemicals, and most importantly legal implications before I take the plunge and start collecting more equipment/chemicals/apparatus and running experiments.

Glassware
To start off I'm wondering if this list of glassware is a bit much, or ok. Everything is pyrex unless listed otherwise (or its obvious).

General
Beakers: 50mL, 150mL, 400mL, 3x 600mL, 1000mL
Erlenmeyers: 125mL, 250mL, 500mL, 1000mL
Graduated cylinders: 500mL (HDPE), 10mL, 50mL
Filtration: 1L filtration flask, Buchner funnel, stopper. Vacuum aspirator and gauge
Distillation: 1L RBF, 500mL RBF, distillation head, thermometer + adapter, condenser, vacuum adapter
Other: Watchglasses, funnels, stir rods, 250mL sep. funnel

Equipment/apparatus
Heating (gas): bunsen burner, striker, gas regulator, crucible, clay triangle or wire gauze
Handling/prep: crucible/beaker tongs, cork rings (for RBFs), mortar & pestle
Storage: various jugs, bottles, and jars, either as glass or HDPE
Other: homemade stir plate, stir bars, clamps, rings and retort stand(s), soap and brushes, plastic buckets and carboys

General safety: lab coat, gloves, goggles, full face shield, eye wash
Fire safety: sand bucket, ABC fire extinguisher

Reagents and chemicals
My next question is about reagents in different categories:

Should I stock up small amounts of different reagents such as oxidizers/reducing agents, and only purchase larger quantities for syntheses of things I want to make in larger scale? I already store small quantities of things in 20mL scintillation vials so I don't have too many bulk chemical jars sitting around.

Another factor is solvents, I've read the Ontario fire code which sets limits on the volume of solvents inside dwellings and other safety standards ( see: http://www.e-laws.gov.on.ca/html/revokedregs/english/elaws_r... section 4.12.1 onwards), but should I try and obtain a flammable solvent storage cabinet to store everything and vent it?

What about acid and base storage? I should be able to get HCl, H2SO4, NaOH/KOH, NH4OH/NH3(aq), and I know not to store them next to each other, but what is a reasonable storage method? HDPE bins inside a cabinet, or a cabinet with trays underneeth all the bottles incase of breakage?

Legal
And the last but most important question is regarding legal issues. Does anyone on this forum reside around Toronto, or Ontario, Canada in general and have experience setting up a home lab? What are the laws regarding this? I've been browsing quite a few threads before finally posting this, so I've seen some general guidelines so as not to run afowl of the law...

- Keep everything labelled, stored properly, keep MSDS for *everything* on hand
- Safety equipment present and clearly accessible
- Keep a detailed log book of everything you do, including basic things
- A fuzzy area for me: avoid having restricted precursor chemicals (I know of the DEA list I, but not of its Canadian counterpart). The only reason why I say its fuzzy is because there was a post about a RCMP list restricting things like sodium bicarb, and Al foil, and generalist things such as benzene, etc... (thread here)

Being able to fulfill *all* the requirements of the fire code (secton 4.12) would be tough, so I'm wondering how far I should go before the effect of diminishing returns kicks in.
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marklar
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[*] posted on 21-10-2009 at 12:14


Glassware
What type and length of condenser do you have?

Where did you buy your glassware? I bought most of mine from a local manufacturing company called DIMA Glass. Their prices are totally reasonable for the quality, their selection is decent and the shipping fee is usually only about $20.

I don't see any pipettes on your list. Which reminds me, I need to buy some. Have you dealt with Indigo Instruments? I also need to get stands and clamps. I was thinking of setting up a lab frame, but it's definitely pricey.

One thing that you totally lack is a hot plate stirrer. Buy one! It may seem expensive at first, especially when you're looking at the bill, but life is easier with stir bars. And boiling chips!


And NO, you can never have too much glassware. At least that's my opinion.


Chemicals
Now with regards to storing reagents. I think it's totally up to you. Personally, I try to only purchase enough for a single procedure. I've been screwed over by this a few times, especially when attempting something for the first time, but I think I'd rather be ticked off about running out of solvent versus having my basement explode in a chemical fire. The more you have on hand, the greater the risk during an accident.

If you're scaling up, I think it's best to go all out in safety equipment. A flammable, ventilated storage cabinet sounds awesome.


Legal
I think that RCMP list is a "watched list". I mean, come on, I can go out to RONA and pick up half the things just by looking at the FIRST AID label. Don't even get me started with Acetone and Muriatic acid!

It's probably safe to assume that the feds are looking for people trying to buy AR grade potassium nitrate or isosafrole.

[Edited on 21-10-2009 by marklar]

[Edited on 21-10-2009 by marklar]
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aonomus
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[*] posted on 21-10-2009 at 14:57


The condenser is a 20cm Liebig condenser, 24/40 taper. I ordered mine from United glass technologies from the US. Their prices, with shipping, are better than DIMA glass or local retailers for certain items, however I'm taking a gamble on the quality. It should arrive in a few days, so we'll see how that goes.

Last time I spoke with a few people and they said DIMA glass doesn't want to deal with small orders, has this changed? My university gets deals on glassware from DIMA in big lots, but otherwise their prices are higher. On the bright side, DIMA glass sells round bottom blanks and other glassblowing pieces, so round bottom flasks could be made cheap if I really want to build an annealing oven...

I will be getting clamps, but I've thought about making the stands myself either using wood or concrete for the bases.

As for pipettes, I have no volumetric ones, only a box full of Pasteur pipettes that I use. Its somewhat on my list but not a terribly high priority, since I can measure out volumes into a graduated cylinder and pasteur pipette the contents, etc (I find this useful since if you have to add something dropwise, no sense in holding the volumetric pipette for a few minutes, not to mention its easier to clean stuff from graduated cylinders).

In terms of a hot plate, I have a dual-burner electric hot plate, but I've found it always generates hot spots, and is lacking. Indeed the price tag is high, so I'll have trouble justifying it. It might be on my 'second round' list, since one of the first reasons why I'm getting the quickfit glassware is to make distilled water in bulk, cheap, and some of the other experiments I had initially planned don't need the heating and stirring simultaneously. I also plan to build a stir plate (no heating) from scratch just so I don't need to monopolize my time with a glass rod stirring all day.

I was at work today (lab assistant for my uni) and I looked at how the flammables cabinets are made. They appear to have some sort of fiberglass matt, and are double walled. They also had quite thick paint to prevent metal on metal sparking during closing, and had a (barely functional) piping system to extract fumes.

Without breaking the bank the best I could probably do is a small office cabinet, lined with fiberglass mats somewhat thickly, and ventilate using a pipe + fan. The general idea is to prevent the buildup of solvent fumes in an enclosed area, so drawing sufficient air through any cracks in the cabinet should keep the area clear of solvent fumes.

I don't plan on scaling up, but even 2.5L - 4L jugs of solvents start to add up quickly. Not to mention that in terms of scaling up, some solvents I simply *don't* want to store and buy in bulk (ie: diethyl ether or THF that can over time form peroxides if you aren't careful and don't store over KOH).

Edit: I just remembered the lab tech that I work for said something about renovations during the summer, and that they'd be throwing out some equipment, which might even include a flammable safety cabinet (which otherwise cost quite alot). I should commence begging no? :D

[Edited on 22-10-2009 by aonomus]
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worldspawn
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[*] posted on 23-10-2009 at 10:06


marklar = worldspawn
I didn't change the default password and used one of those 10-min email websites. *sigh*



Other than charging a fee for orders less than $50, DIMA seems willing to ship to any "business". Just say your X from Y's Homoeopathic Healing & Supplies. Or whatever! You get the point. And yeah, they ship to residential addresses, they did for me.

And, omg, YES! I envy you. Circle the garbage bins at uoft like a vulture. So far I've begged every semester at my college to buy equipment or be told whenever something gets thrown out. I'm always told "we use everything until it's unusable." I know someone who rescued a rotovap and a industrial mantle, among other things, from being sacrificed to the garbage dump gods.



Not too sure about your lab applications, but what have you done for a fume hood? After being told NO from the parents (housing is expensive in Toronto, but you know that,) when I asked if I could use the dryer exhaust, I've had to do pretty much anything outside. Which is totally bad practice and absolutely does not feel right. Chemistry is supposed to be done in concrete rooms with tiny windows and humming fluorescent lighting.

Anyway. :P That means my chemistry season is pretty much over, especially with all the rain we've been getting in Toronto!

Which makes me think. I mean, in chemlab we vacuum distilled dilute H2SO4 into pretty pure stuff. (Don't ask.) Those vapours were nasty! So when we did our work under the fume hood, it got sucked up and pumped into the air outside. I understand gas diffusion, but is that any different from simply doing it in your backyard? The building we worked in was only 1 story tall, which leads me to think the vents were on the roof. (I never spotted anything protruding way up into the air.)



I despise having anything shipped a long distance. I haven't found anyone suppliers locally in Toronto though. Then again, that's because I haven't looked close enough. I really should crack open the yellow pages or visit one of the libraries downtown.

www.stobec.com - surplus chemicals, never dealt with these guys yet, Quebec
www.acamchem.com - chemicals, expensive, but they have a wide range, Quebec

www.cole-palmer.ca - they have everything, unfortunately that doesn't include anything deemed toxic, their prices are high

www.boreal.com - aimed at teachers, seem pretty expensive, Ontario
www.indigo.com - kinda gimmicky, but their lab equipment is cheap, Ontario
www.dimaglass.com - glassware, Ontario


Otherwise, as you obviously know, anything can pretty much be had from a hardware store. Tubing, pumps, solvents, etc.




BTW, your Red Alert tesla coil video is totally awesome!

[Edited on 23-10-2009 by worldspawn]
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aonomus
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[*] posted on 23-10-2009 at 11:19


In terms of ventilation, I do plan on building a proper fume hood and epoxy coating the insides thoroughly, and venting to the backyard. I've noticed that all the piping and ductwork for fumehoods and solvent cabinets are sealed with fireproof compounds, but I'm a little worried about metal ducts reacting with the compounds. Any thoughts as to what duct material to use? Aluminum ducts probably cost more, but might passivate (or already be such due to the oxide coating), whereas steel ducts will rust under acid fumes. Plastic duct = fire hazard, so thats already out of the question.

I've also tracked down a hotplate/stirrer that seems cheapish, so I'm going to order that, and the rest of the glassware. I should have pretty much everything I'd need to run most reactions necessary at that point.... but most will have to wait until fume hood + flammables cabinet get built/acquired.

I have somewhat resolved myself with having to spend a fair bit of money at this, knowing that it will last longer than $100 jeans that some people waste money on.
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[*] posted on 23-10-2009 at 11:57


Cool worldspawn, another Torontonian :)

I always look for junk when they throw stuff out. Once there was a huge pile of circuit boards with 3 profs in lab coats and white hair picking them apart like vultures. I also scored an Apple IIe that was broken for 20 years before I fixed it. Someone else said they found an x-ray power supply there.

There was a box of old glass in a basement and I picked up a 1L filter flask, thats about it.

Active Surplus used to have some really nice glass a year or 2 ago, but its all been sold and now they just have beakers.

Getting a real hotplate/stirrer is really useful. Just don't buy one from the States or UPS will ding you $95 :mad: I always look for Canadian sellers now
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[*] posted on 23-10-2009 at 12:03


Quote:
I'm a little worried about metal ducts reacting with the compounds. Any thoughts as to what duct material to use?
My hood exhaust duct is the "Aluminum Film Laminate" flexible duct sold in hardware stores. I worried about halogen and acid fumes destroying it, but it lasts for a few years before needing replacement and it's cheap, and the duct is accessible for easy replacement if need be. I've used it with Br2, Cl2, NH3, HCl, HBr, and other nasties in the hood without problems. But I almost always use a water or caustic trap on the exit tube from reaction vessels to keep the fumes out of the blower, which isn't cheap.

In professional labs I've worked in the blowers usually gave up long before the ductwork.
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aonomus
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[*] posted on 23-10-2009 at 12:28


It makes more sense to try to trap the corrosive or toxic fumes if you can. I usually try to run the output of a reaction into a tube or jar with a bubbler, or packed with the appropriate chemical. (eg: drying a HCl solution, take the output and run it through a big Na2CO3 tube)

In other cases, recovering the corrosive/toxic fumes can be useful, say if the reaction evolves ammonia gas, bubble it into water, or condense it. I think its safe practice to take a gas inlet adapter and connect it to a bubbler, or at least a trap incase the reaction goes runaway. Depends on the reaction, but my main concern is over things like HCl, NH3, Cl2, O3, NOx, SOx. Considering that the fume hood output will be from a basement going to a ground level output, perhaps its best to scrub the exhaust so that the grass near the outlet doesn't die (or the cement doesn't corrode).

As for the hotplate, I was looking at ebay, and getting shipping via USPS, so I shouldn't get dinged too hard. It will be cheaper even after customs, before getting a hotplate locally sadly. My guess is alot of labs in the US are closing down and liquidating assets.
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[*] posted on 23-10-2009 at 14:21


Ah yeah, Active. It came up in a conversation with a friend last December. So I phoned them up and was told they get glassware every now and then. I asked what that meant and the guy on the other end said every four months or longer. :D Awesome! That 70cm graham condenser I'm looking for might ONLY take a few decades to come.

Thanks a ton for the duct info entropy. That stuff is sold everywhere here. I can't wait until the semester ends, I have a sweet project for the break.

Ah, and if you still haven't committed to buying anything as of yet aonomus, there's always:
http://www.labequip.com/itemcatalog/category.html
And a quick search on labx yielded:
http://www.labx.com/v2/adsearch/detail3.cfm?adnumb=399410
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aonomus
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[*] posted on 26-10-2009 at 08:35


I'm starting to wonder now how good an idea saving up some money further down the road and getting smaller 14/20 glassware would be? The 500mL/1000mL scale is for preparing stuff as I need it such as acids, or other reagents, so its starting to look like a better idea if I want to do microscale organic chem.
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[*] posted on 28-5-2010 at 15:49
RCMP List


I know I am digging up an old thread.

I all to well know about the RCMP List.
I have a copy of it.
A lot of what is on it is a joke.
The list looks like it was made up from what things that have been found in lab busts.

Quote: Originally posted by marklar  
Glassware
What type and length of condenser do you have?

Where did you buy your glassware? I bought most of mine from a local manufacturing company called DIMA Glass. Their prices are totally reasonable for the quality, their selection is decent and the shipping fee is usually only about $20.

I don't see any pipettes on your list. Which reminds me, I need to buy some. Have you dealt with Indigo Instruments? I also need to get stands and clamps. I was thinking of setting up a lab frame, but it's definitely pricey.

One thing that you totally lack is a hot plate stirrer. Buy one! It may seem expensive at first, especially when you're looking at the bill, but life is easier with stir bars. And boiling chips!


And NO, you can never have too much glassware. At least that's my opinion.


Chemicals
Now with regards to storing reagents. I think it's totally up to you. Personally, I try to only purchase enough for a single procedure. I've been screwed over by this a few times, especially when attempting something for the first time, but I think I'd rather be ticked off about running out of solvent versus having my basement explode in a chemical fire. The more you have on hand, the greater the risk during an accident.

If you're scaling up, I think it's best to go all out in safety equipment. A flammable, ventilated storage cabinet sounds awesome.


Legal
I think that RCMP list is a "watched list". I mean, come on, I can go out to RONA and pick up half the things just by looking at the FIRST AID label. Don't even get me started with Acetone and Muriatic acid!

It's probably safe to assume that the feds are looking for people trying to buy AR grade potassium nitrate or isosafrole.

[Edited on 21-10-2009 by marklar]

[Edited on 21-10-2009 by marklar]
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