Setting up a lab

[vap0r]

I've been into pyrotechnics on an amatuer level for 2 years now. I'm just getting into high explosives. I want to set up a sort of "lab" for making them safely in my garage. Can anyone recommend what I should start off with? I've already got a couple of beakers, a flask, a glass stirring rod, and some other accessories. What do all of you have, and what else are you going to purchase to complete the setup of your lab?

[blindreeper]

I suggest a good spacey lab. Not cluttered. I personally have a wooden cupboard for my chemicals. It has 2 shelves, top for small bottles and powders and the bottom for big things like 4L acetone, KNO3, acids bottles ect.
I also scored a metal, lockable metal cabinet which has all my glass, scale, gloves, glasses, respirator, matches/lighter, fuse ect
A good solid desk/table is essiential for performing synthesis or whatever on.

I have a decent ammount of chems and rarely have to go out and get something new if I want to try a synthesis I "Just saw!"

I think you can;t buy everything you need in a lab at once, it kind of grows, like a garden :)

[xyz]

Now I wonder if we can get the people from one of those "garden makeover" shows like groundforce to start doing labs instead...

[flashpoint]

I'm interested in getting a glassware set, I can get piece by piece at work, but I'd like a whole set, I wonder who sells them, google time i guess...

[Flake2m]

I might setup a decent lab someday when I have enough money to. Labs themselves have also been known to be cash cows...
Anyway as far as I know, make sure that the area your lab is setup is kept fairly clean. A dirty workplace can increase the chance of bad accidents.
If you are really into seting up a lab it migh even be an idea to do a course at a TAFE (in Australia) on laboratory skills and techniques, just so you have the basics.

[flashpoint]

I know its rather childish, but formally Edmund Scientific, has glassware sets...basic labware I do believe. Also I edited to add this in, there is also labx.com that offers glassware I just found this today.

[Anath]

United Glass Tech (http://unitedglasstech.com/) has a nice distillation setup that's fairly cheap, I'd reccomend 24/40 joints.

SciPlus (www.sciplus.com ) also has some interesting stuff.

You can also put the word out if you know any schoolkids that you'll buy glassware for $20 or so, Sometimes it will mysteriously 'appear' ;)

Don't bother buying beakers, I just buy pyrex measuring cups from Kmart, they are cheap and IMHO work better anyway.

Pick up flasks for cheap on eBay, keep an eye out for lab thermometers, a bag of rubber stoppers from a brewery supply shop is always handy. check out the bins at the local Uni. Use an old electric frypan filled with 1" of sand as a cheap hotplate that contains spills. Get a second-hand toaster oven to use as a dessicator. buy every cheap second-hand blender you see. A cheap bar fridge is always handy.

You'll have a great lab in no time :)

[megalomania]

What kind of “kit” were you looking for, because I have yet to see any seller offer more than a set of 10 beakers that is anywhere near economical? Places like Boreal Laboratories offer glassware setups meant to flesh out a complete school lab, of course you have to be a teacher to get the catalog (but not to buy). If small quantities are your thing stay away from Fisher or VWR, they have the cheapest prices only in mega case quantities. In small quantities you will pay through the nose. Ebay or Labx.com would be the first place I would look to build a lab on the cheap. You can’t build a lab all at once through the auction sites though, you have to wait and see what comes available over time.

It has taken me almost my entire life to build my lab. I find things at flea markets, garage sales, and local auctions. When you can’t find what you need at the auctions then you can shop for things specifically at the glassware venders. I suggest www.elementalscientific.net for all your basic labware needs, they are the cheapest on average I have found and one of the few who still sells chemicals to ordinary people. Now if it’s real glassware you want, and by that I mean a set of standard taper glassware to do chemical reactions and distillations (ie. 90% of everything you would want to do) bite the bullet and make the investment over at chemglass.com. Chemglass brand is top notch and the cheapest you can find. Order their free catalog or read it online.

There is a damn good deal going on right now at labx here: http://www.labauction.com/v2/adsearch/Detail3.CFM?adnumb=191416&CatID=165
Current bid is a mere $200 for a complete set, which is about half what I would expect to pay for such a set especially 24/40 taper. Ooh, even a three neck! (banned in California) If I only had the money :(

Now don’t think you need to get all the professional stuff, no indeed. The only thing I would actually advise you to buy is the standard taper kit. Otherwise you can use pickle jars as beakers, wine or beer bottles as flasks, Mason jars as beakers when you need to heat stuff, measuring cups make good, if slightly inaccurate, graduated flasks (instead of a graduated cylinder). You can use an ordinary blowtorch instead of a Bunsen burner. For lab stands you can get steel or aluminum rods at a hardware store and either weld or solder them together. Things like clamps and rings you may be better of buying, and you will need those sooner rather than later.

Save your money for the really important, but somewhat exotic equipment: magnetic stirrer, heating mantle, gram balance, and possibly a pH meter.

Now then, it helps to know what kinds of chemistry you would like to do to choose what equipment you may need. Nothing halts my experiments faster than lacking a bit of equipment.

[Hang-Man]

For those of you just setting up you're lab here are a few of the things I find most useful:
Small, 100 ml beakers
Pipettes (normal and micro)
Scale (0.01g)
Burner (butane rig i sort of made myself. works ok. I need a hot plate...)
Mortar and Pestle
Glass rod
High form, 500mL beakers
250 mL Erlenmeyer flasks for storing liquid chems (acids etc)
Wide mouthed jars for storing powders etc.
Thermometer
A few dozen large test tubes.
Latex gloves
PH strips, (or litmus or Phenolphthalein)

Once you have a lab you may want to check you're yellow pages for a hydroponics store and get some basic chemicals. I find I run through HCl, H2O2, and KNO3 the most. Keep some baking soda on hand for acid spills (if your prone to accidents :rolleyes:) and some salt if, like me, you often use electrolysis (you need to ionize the water) and for gods sake get some decent goggles. Don't eat near you lab and ALLWAYS label your containers.

You may find the following site useful, good glassware kits.
www.thesciencefair.com/Merchant2/merchant.mvc?Screen=CTGY&Category_Code=gla

And for those Canadians, the only good store I’ve found is http://www.escience.ca/home.html they have a large location in the Toronto area, but rather high pricing.

Hope that helps.

On an unrelated topic that does not merit its own post: Why is it that H2O2 accelerates the rate at which HCL eats metals? I’ve never figured it out.

[T_Pyro]

I think basic lab glassware (beakers/test-tubes/measuring cylinders, the works) is easiest to get through auctions/resales etc. That way, you can also save your money for other exotic equipment like ball-mills, weighing scale etc. While just starting out, it's a bit difficult to balance your funds between chemicals and equipment, so I'd suggest using makeshift utensils initially, and slowly acquiring proper lab glassware as you progress.
Though not an integral part of the "laboratory", if you're going to spend most of your time conjuring pyrotechnic mixtures, you'll find a sandbox/sandpit useful for testing out your pyrotechnics compositions safely, and close to your lab. It'll save you the trouble of driving over to the nearest barren ground just to test a mixture.

[Tuatara]

Aside from glassware you'll need somewhere to do your stuff. Thats bench, sink, taps, drain, power, vents. Go scout your local demolition yard for those sorts of things - I scored two proper lab taps for $NZ10 each (the sort with the tall up-and-over standpipe, and a barbed hose fitting on the end). When I built my house I designed in a photo darkroom - it now doubles as chem lab!

I got really lucky with the glassware - the med co my wife was working for decided to quit selling Schott - so I got three carloads for FREE! :D :D :D Favourite pieces would be the 3l round vessel with the 5 hole clamp-on lid, and an all glass burette with a fancy vacuum self-filling thingy designed to sit in a stock bottle. After browsing the online stores I've come to realise I've walked away with about $3k worth of stuff.

[Zeitgeist]

Just don't make the same mistake as me, and assume a big Pyrex pot from the supermarket will survive being put on a gas burner

[frogfot]

By things that you will need in your next experiment. That way you'll have a lab very soon..

On weighting scale subject.. recently got a broken scale for free: 6kg 0,01g. When it's turned on, it shows "overloaded", so I gonna save it until I can fix it.. hope it's not the sensor.. maby somebody got a "magic" solution for this :)

[Zeitgeist]

Just noticed your unrelated topic Hang-Man

I think that the H2O2 is a stronger oxidant than the H+, and the dissolving of any metal is really just redox. I use H2O2/HCl to etch printed circuit boards, but you can leave a board in conc. HCl for a week and nothing happens.

Once it's oxidised, the metal will happily dissolve in the aqueous HCl

[flashpoint]

I appreciate all the help and advice, I think I'm going to work slow, to get up to standard, like you said, I already have a .01g scale, used for weighing something else ;) But I don't do that shit anymore so its free to use...anyhow I'll just check auctions and slowly build from there. What about a good thermometer, I stole one from walmart in the food section, its digital, and I calibrated it and everything but I read not to use those since the probe is metal...any suggestions on a good one? Possibly digital...if not I'm making one at work
:D

[Anthony]

I think a probed thermometer will always be a problem considering the very corrosive chemicals that we usually work with. A solution might be an infra-red electronic thermometer.

I don't see what's wrong with a traditional glass thermometer though. Alcohol filled ones are available from places that sell home brewery equipment amongst other places, for a couple of dollars/pounds.


A hotplate is always useful, even just a kitchen one.

[flashpoint]

Anthony, I have one that uses infrared, I don't know why I didn't think to use it...How accurate are they? My dad uses them at work and I have his at my place...let me know please :) Thanks

[blindreeper]

Those proper lab thermometers are very cheap, I have found them for $1.90 AU alcohol or mercury, they both cost the same. But they break easy :(

[flashpoint]

I have a hard time reading regular thermometers though, that's why I like the digital ones :)

- Jared

[Tuatara]

The accuracy of IR thermometers is somewhat dependant on the material you are measuring. Obviously low emissivity materials produce less IR than high emissivity ones - this is often solved by supplying black paint with the thermometer.

For a thermocouple meter there is no reason why one could not take a piece of 5mm glass tube, melt seal one end, then insert the thermocouple, then seal around the thermocouple with silicone or epoxy. That way you get a nice , inert, accurate digital thermometer.:) It is also possible to by stainless and inconel thermocouple probes.

Ordinary glass thermometers are plenty strong enough as long as you don't use them as stirring rods!:rolleyes: Though I will concede they are hard to read when covered in condensation.

[flashpoint]

Tuatara

Are you talking about using a thermister to read the temperature?

[Tuatara]

No, I'm referring to a thermocouple, which is two dissimilar metal wires bonded together. Heating the bond creates a small voltage between the two wires, dependent on the temperature. Search for 'Seebeck effect' (sp?). Most commonly used is the K type thermocouple,. Thermometers using K type thermocouples are quite cheap.

Some thermocouples:
type T : copper / copper-nickel : up to 350 C
type J : iron / copper-nickel : up to 700C
type K : Nickel-chromium / nickel-aluminium : up to 1200C
type N : nickel -chromium/ nickel-silicon : up to 1250C
type S : platinum-10%rhodium / platinum : up to 1500C
type R : platinum-13%rhodium / platinum : up to 1600C

Thermistors can also be used, but tend to be non-linear, and need calibration as their response depends on their physical dimensions as well as their material properties, whereas the Seebeck effect is only a function of the metals used.

Silicon sensors are also available, but can't be used much above 150C.

[wrench352]

Heres a link to a great site:
International Order of Nitrogen (http://www.nitrogenorder.org/lessons/household.shtml)
Every thing you wanted to know about setting up the homelab but were afraid to ask ;)

Also odd lots of glassware, in various sizes, can be found on Ebay at sometimes good prices.Actually you really can by just about anything on Ebay.I have a real human skull paper weight/candleholder I just got,really sets off the lab,you know.Im hoping to get a hoplate stirrer for my Birthday.10x10 Corning

mmmmmmmmmmmmmmmmmmm,hotplate stirrer
(drools)

[Skean Dhu]

while searching for chems on eBay I stumbled across this
http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&item=2578421348&category=11812
small setup but everyones gotta start somewhere, if I weren't saving up for a computer I'd consider buying one. the keywords were'Laboratory equipment'

"seek and ye shall find"

[vap0r]

this seams like a nice set or starter glass as well. http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&item=2579328892&category=26406

[Skean Dhu]

good thing this guys isn't a chemist, otherwise the price would be considerably higher. you'd be lucky to find 30pcs for that price. especially since most of its for distiilation

[flashpoint]

yeah tell me about it

[flashpoint]

Well..I stooped down and had my sniping ebay program snag it for me...at 148.50 total, I was pissed as it came from 38.00 to that :eek: Good find though, I appreciate it. Now just a few more pieces to collect.

[Chemiboy]

I totaly agree to blindreeper: "I think you cant buy everything you need in a lab at once, it kind of grows, like a garden"
in my country (Austraila) chemicals and equipment are hard to obtain. The chemicals comes slowly to u if u try to look for them, but comes in small quanties and also not very pure.
So i just want to tell every one who is in other countries that u get many chemicals easily, always be against the people that get themselves busted with explosives because, one day ur country will be like Australia.

[Anath]

I'd just like to point out that this statement..

"in my country (Austraila) chemicals and equipment are hard to obtain"

Is factually incorrect. I believe that what the original poster meant to say was.

"in my country (Austraila) chemicals and equipment are hard to obtain, if you are lazy, have a bmx as your sole means of transport, and look 12 years old"

Australia is probably one of the -easiest- civilised countries to obtain OTC chemicals, Pyro supplies (second only to America), and lab grade reagents, equipment & glassware in. It just takes a bit of know-how, (and know-who) and a willingness to get off your arse and have a look around. See Blindreeper's excellent Australian OTC pdf for a (small) example of what you can buy here easily.

Sometimes good suppliers just won't sell dangerous chemicals to little kids.. This is not a bad thing.

[flashpoint]

"in my country (Austraila) chemicals and equipment are hard to obtain, if you are lazy, have a bmx as your sole means of transport, and look 12 years old"

That's got to be the funniest thing I've read, concerning little "KEWLZ". Out of all the Austrailian people on this board, it seems, 99% of them don't have a hard time finding most chemcials...

[metal dragon]

As an Australian I sometimes have trouble finding chemicals but others are easily obtained so it really means where you live, how much cash you got, etc. But some Australians over exaggerate about how hard it is.

[Ammonal]

Well I was nearly going to complain about certain things but since I just ordered a kilo of 98% purity KNO3, and some 50% H2O2, I think living in Australia is tops! :D
And all it took to locate the source was a Google search, maybe I am giving away answers to KEWLS here, maybe not because theyre too preoccupied with whatever it is they waste theyre time on to actually look beyond other peoples sources for things.
Look and ye shall find.

[flashpoint]

they beat off to much to do a search Ammonal :D

[blindreeper]

Only one kg of KNO3? Thats not much, it will go fast!

[Blackhawk]

I'd give my left testical for some KNO3, oh well time will yeild all :( I have ways of getting it, but I will wait, I have so much on my plate ATM anyway, a little wait won't hurt and I learn more in the meantime.

[blindreeper]

Blackhawk, contact me about KNO3 ;)

[Ammonal]

A kg should be enough to do how much fuse? This is my only use for KNO3. Appart from terrorising mailboxes with KNO3/Sugar :P And anyways this is the first place that sold me KNO3, 50% H2O2 (Thanks Blindreeper, I love the Aus OTC PDF) and some Nitric acid no questions asked and I watched the guy burn the reciepts :D Gotta love the business weed growers make!!

[Jackal919]

Here's a handy site for building your lab, http://www.geocities.com/capecanaveral/lab/4444/making_a_small_laboratory.html

[Sparky]

On McMaster's (the university) site I found this:

http://www.science.mcmaster.ca/glass/

Basically the university sells glassware. They also make custom glassware. I don't know if their prices are intended to sell to research labs, so if they are it might not be a feasible source of glassware. Otherwise it could be handy.

[zeocrash]

I'm still in dire need of a proper distillation set up.
I found ebay was not the place to look though as none of the quickfit pieces seem to fit each other. :( ah well if any of the UK members are getting rid of a distillation setup tell me.

[atlas#11]

http://www.freyscientific.com is a great company with a bad site. if you request the catalog you can get evry thing you need except chems, that is unless your a teacher or something. their glass ware is quite cheap and they have it all distillation apparatus, filtering flasks, tubing you name it. as for now i'm still saving up so i'm using one quart mason jars for everything.

[tom haggen]

I'm looking for a complete vacum distillation setup. Included with a condenser, a proper vacum pump, a ring stand, some hoses, and the proper fittings. does anyone know where to find something like this for sale that is fully assembled?

[Mendeleev]

Tom hagen, www.unitedglasstech.com they have a 1 liter vacuum apparatus for $150, but no vacuum pump. I am hoping to buy a 12 liter distillation apparatus from www.unitedglasstech.com with 2 12 liter flasks, a 600 mm Vigreux column, a three-way adapter, thermometer adapter, vacuum adapter, and a 600 mm liebig condenser. This costs about $800 :(. If I decide not to go this way I will place a $600 order at www.elementalscientific.com and have tons of beakers graduated cylinders, meker burner, ringstands and clamps, hotplate/stirrer, and scale deliverd. Could anyone describe to me how effective are the various condensers, like liebig, west, graham, and others? Also do I even need a 600 mm Vigreux column?

[vulture]

A vigreux column is useful if you're separating liquids which have close boiling points and are miscible with eachother. The smaller the difference in boiling point, the longer the Vigreux column should be.

Cooling capacity only matters when doing reflux, to make sure nothing escapes out of your setup.
A liebig cooler is very ineffective, because of laminar flow. The "snake" cooler (alternating bubbles) is quite an effictive reflux cooler. For substances with very low boiling points, Graham or Dimroth coolers should be used.

[Xioa]

Though this is slightly off subject, it's the only thread that i could find that would relate to my question. My lab is pretty ideal for me, the only thing i need is running water in it. Is there a cheap way (installing plumbing is too damn expensive) to get running water into my lab? The lab is seperate from my house and is a good 30 ft from it. Thanks.

[SpiffyVision]

This place also sells beakers and such for a good price http://www.enasco.com/prod/Home

[Mendeleev]

When you say low do you mean like ammonia gas low, nitric acid low, or need liquid nitrogen to make it liquid low? Just as an example what would be the ideal condenser for say nitric acid (bet you never saw that coming ;))?

[grendel23]

A retort can be used to distill nitric, so you don't need an ultra efficient condenser to get good results, I use a 300mm liebig and it works fine.
If you are planning to distill more demanding substances, then a west, graham, or allihn may be a better choice.

[SpiffyVision]

You wouldnt happen to have a picture of your set up, would you grendel?

[ossassin]

Not much has been said about location. It would be hard for me to make a lab inside of my house. Would something in a little shed work? How much ventilation should I have? How do those of you with parents manage to hide everything?

[frogfot]

Xioa, how about leading some cheap garden hose from the house into your lab?

I was also thinking about homemade ventilation hoses made from polyethylene bags. They could be easily fused together by an iron to any diameter..

[vulture]

I was also thinking about homemade ventilation hoses made from polyethylene bags. They could be easily fused together by an iron to any diameter..


You're kidding, right? PE bags have virtually zero resistance against oxidizing acids, especially in vapour form.

[SpiffyVision]

No Vulture, he's not kidding... LETS JUST USE TEFLON BAGS!!!

[T_Pyro]

Then how about HDPE? I've seen some acid/alkali (including conc. acids) resistant HDPE measuring cylinders, but acids in vapour form (especially at high temperatures) are quite different...

[Mendeleev]

Sorry, another sort of newbish question about distillation. See I've been using brainfever's ghetto set up with two beakers which works just fine, but I know little about the real jointed glass set ups, so I was wondering what type of flasks would be best for distilling: round bottom boiling, flat bottom boiling, erlenmeyer, or pear-shaped?

[grendel23]

SpiffyVision,
Here are a couple of pictures of my setup, here (http://www.geocities.com/sulfuric23/glass.jpg) is the overall setup, here (http://www.geocities.com/sulfuric23/head.jpg) is a closer view of the head end, and here (http://www.geocities.com/sulfuric23/tail.jpg) is a closer view of the tail end. Cut and paste URL's into your browser.
What you are looking at is a 2000ml round bottom flask at the hot end, a distillation adaptor with a glass stopper in the unused 24/40 opening at the top and a thermometer in the 10/30 port wrapped with Teflon tape to seal it. Then a 300mm liebig condenser, a 105 degree vacuum adaptor, and a 1000ml flask at the cold end.
For clarity I am not showing some parts, I have a mantle on order to heat the large flask, I am tired of improvised heating setups, I also use a ice water bath around the receiving flask, with a submersible fish tank pump to circulate cold water through the condenser. I also use a piece of Teflon lined vinyl hose to attach the vacuum adaptor to a filter flask set up as a water trap, also in the ice water, then to an old medical vacuum pump that will draw 20" of suck, just about right. I have spent about 6 months collecting bits when I could get a good deal.
Mendeleev, If you are thinking of running vacuum you must use round bottom flasks in perfect condition, no cracks, chips or heavy scratches.

[Blackhawk]

Your pictures don't work for me, not copy and pastable and the page has not exceded it's data limit.

[frogfot]

Vulture, can you define "zero resistance"? (thats sounds as if it was aluminium foil vs pure chlorine..)

We're talking about home lab that will output small ammounts of corrosive/poisonous crap, in small concentrations that is. Most of it can be absorbed by washers/active carbon filters on exit from your apparatus, even in real labs they try to absorb most of dangerous exhaust gases.
After all, who in your negborhood wants a half kg cloud of some toxic/corrosive byproduct gas from your reaction? :p

IMO, as long as PE pipe does not fall apart, it will be suitable for amateur lab.

[Jacks Complete]

frogfot,

he isn't talking about plastic pipe, he is talking about melting plastic bags together! I have no idea how you would ever get a good seal over the dozens of joins you would need?

If you want to do that kind of thing, just buy tumble dryer ducting. At least that won't have holes when you start!

[frogfot]

Ofcaurse I meant bags, a 1 m PE pipe of that diameter would cost me 10-20$!!

Anyway, one can make segments by fusing big PE sheets with hot iron :) it's very easy to make good seal, just have to place some paper between iron and PE, else it will be messy.
The segments can then be "mounted" together by some strong elastic tape..

Yeah.. I never said low-budget would give quality, well enough quality for less than 1$ :)
(gonna try this now..)

EDIT: hihi, that was fun.. :p I realised that tape is much better than iron..
Heres a pipe consisting of two segments:
http://www.geocities.com/frogfot/stuff/ventpipe.jpg

Gonna use it next time I melt candy propellant (paraffine stinks) together with homemade fumehood...

[grendel23]

Blackhawk,
The links I posted work for me if I right click on the links and use "copy shortcut" then paste into the browser address bar. I am using IE, are you using something else?
Is anyone else having problems with these?

[SpiffyVision]

Their working for me, where did you get that setup grendel?

[ossassin]

I have access to a large supply of glassware, and since a few items disappear from the annual inventory anyway, I think I'll add a few of them to my collection. :) Right now I have a 250 mL beaker, a 600 mL beaker, a 100 mL graduated cylinder, 2 glass stirring rods, and various bottles. What would you recommend grabbing? Thanks.

By the way, I'd rather it be something very common like a beaker or a flask. Things like condensing tubes would be missed.

[Mendeleev]

If I had the choice to grab something common, given what you already have, it would either be a larger beaker such as 2-4L or better yet a one liter erlenmeyer flask or one liter flat bottom boiling flask as they can be made into a pretty good distilling apparatus using a rubber stopper and PVC pipe like here http://cavemanchemistry.com/cavebook/chalcohol3.html .

[ossassin]

Good idea, I'll look for some. Any other suggestions? Can strong acids be stored in simple glass bottles? Should I grab a few special ones?

[Mendeleev]

Yeah, all acids except hydrofluoric can be stored in glass, and some in polyethylene coke bottles.

[Bert]

Will using a flat bottomed boiling flask under vacuum lead to an implosion?

[ossassin]

What sort of top would be needed for the bottles? Would plastic be OK? It seems like strong acids would melt that. Some sort of stopper, maybe?

EDIT:
I'm actually there right now, so if someone responds quickly, I'll grab it.

[T_Pyro]

"Plastic" is a very generic term. I've seen some HDPE stoppers which are used to seal 98% H2SO4 and 70% HNO3 bottles. On the other hand, there have been reports by other members about 98% H2SO4 melting their plastic vessels. If you're going to rely on plastic, I'd suggest leaving a small sample of the plastic submerged in a small quantity of the most corrosive (for plastics) reagent you'll be using, for at last a week, and then checking for signs of disintegration.

On the other hand, if you're getting your concentrated acids from a laboratory supplier, you should get them in a glass bottle with a stopper of its own. Why not use that itself? That's what I do.

[ossassin]

Just in case anyone is interested in a follow-up, I had another successful mission today. My haul consisted of a 1000 mL beaker, another 250 mL beaker, an 80 mL beaker, a 40 mL beaker, a 1000 mL earlingmier flask, a 500 mL flask, a 250 mL flask, a 25 mL graduated cylinder, a medium-sized bottle of 95% denatured ethanol (has not been measured yet), an alcohol burner, and a small jar of powdered citric acid. There were plenty of these (http://roguesci.org/megalomania/equip/glassware.html#flask) (#6), but I just didn't have any more room in my bag. What are they, and how valuable would one be to me?

[Bert]

It's a distilling flask, and you wouldn't want one unless you were distilling nitric acid from sulfuric acid and nitrate. And no one here would ever want to do something like THAT.

[ossassin]

:cool: Great! It's rounded at the bottom, so is it safe to heat it over an open flame? It looks like it would be hard to use a hotplate. An oilbath maybe?

[tom haggen]

I just added on to my collection of goodies. To me this seems like an essential piece for my lab. I basically got this so I can work around Nitrogen Dioxide in poorly ventilated areashttp://www.geocities.com/grandpa_jacob/night_vision.html?1075603677388

[tmp]

Someone asked about venting fumes. I found that a window fan
works very well for my chlorate/perchlorate cells. I keep the cell
in front of the fan. The fan, of course, is set on reverse to draw
the air out.

[tom haggen]

I own a glass pitcher that is designed for holding extremely hot liquids. I'm kind of a poor guy so I use this instead of buying nice glass ware. I also have one of those portable stoves with a heating element. I have set the glass directly on the heating element before and it worked pretty good. I was just kind of nervous about setting my glass container directly on the heating element. I could probably use a pot filled with sand instead of setting my glass container on the heating element. But does it really matter since i'm only boiling off water at 100C, or is there a risk of my glass cracking? You would think that there would be some danger when placing and removing the pitcher on and off the heating element, seeing as how glass an metal aren't great friends. However, that's not my concern. My concern is the uneven amount of heat due to the spaces in between the coils. Any advice would be greatly appreciated.

-Tom Hagen

[wrench352]

Hmmm,this would be better in the purifiying sulfuric acid threads wouldnt it?But then youve worn out your welcome there havent you. I had basically answered your question Tom when while searching on the subject so as to avoid giving you bad info,I saw some of your other posts.
If you are too lazy to look this stuff up yourself(I found your answer on this site in about 15 minutes) then you are to lazy to research the hazards associated with whatever it is your cooking up. Blindly endangering not only yourself but whomever is nearby.Im through with you.Hey yall check out his posts here and sci mad. The scariest thing, it looks like he's wants to make NG. :O

[tom haggen]

http://www.roguesci.org/theforum/showthread.php?threadid=1899&highlight=nitric+acid+synthesis Well wrench buddy, I searched and found this post. It sure does talk a lot about what I am getting at, gee what do you know. But what I'm getting at is that I have a glass pitcher, and I know for a fact that I could stick this son of a bitch in a 350F vat of oil with out any problems. You see as I said it will with stand high temperatures. But no one really says anything about placing a glass beaker on a heating element. I thought that thread I found was pretty damm close to figuring out my question too. By the way why would this post belong in the purifying acids section? In my post before yours I said I wouldn't be above 100C, I thought most acids have a much higher boiling point than 100C. Also, you are correct i have definitely worn out my welcome in that thread.

[Mendeleev]

I did some research and boiling flasks are apparently the prefereed choice for distilling. I expected as much, but I am still unclear, as to whether flat bottom flasks can be used for vacuum. I believe Bert also asked this question and did not have it answered. For some reason most of the "ready to go" fully constructed distillation apparati sold from labware suppliers are usually made with round bottom flasks, which in my opinion is a bit inconvenient due to the requirement of a heating mantle as opposed to a hot plate and the inability to use a magnetic stirrer, so why are round bottom preffered? Is it because flat bottom is incompatible in vacuum like Bert said?

[tom haggen]

Heres the flat bottom flask I have been talking about. www.geocities.com/grandpa_jacob/night_vision.html?1075604701466 I found it in my kitchen its for holding extremely hot liquids. Putting it on a heating coil makes me nervous. I think i'm just going to use oil baths with this flask. It can hold 1000ml.

[grendel23]

I am not sure that a flat bottom flask would implode, but the results of such an event when distilling HNO3 under vacuum would be so nasty that I cannot imagine why you wouldn't do everything you can to ensure a safe procedure. I might be willing to try an less than optimum rig at ambient pressure, but not with vacuum.
By the way, they make stir bars for round bottom flasks, you can just put the mantle right on top of the stirrer.
A good distillation setup costs quite a bit, but if you are serious about this hobby, its worth every cent.

[tom haggen]

When it comes to a vacuum in a round bottom flask, The pressure is spread out evenly do to the geometery of the flask. The right angle in a flat bottom flask does not have this same advantage. All of the force is directed right in the corner of the flat bottom flask. Sorry if this is stating the obvious, but its what I do best.

[atlas#11]

tom, If that beaker is pyrex then you shouldn't have to wory about it, if it was flint glass I would keep it under 100C. I use my 1L beakers on a hotplate at 1100 watts without problems when concentrating sulfuric, it all depends on what kind of glass it is. As far as vaccum flasks are concerned, it depends on the thickness of the walls, the desisired pressure, the temperature, etc. United glass tech( http://unitedglasstech.com/)sells there erlenmyer flasks with 24/40 joints for relativly cheap prices and they are suposedly able to withstand quite a vaccume(did you mean flat bottom round flasks?). Currently I am working my ass off to save up for a good distilation app. Think I'll go for the 600mm grahm condenser with 24/40jts. I will get the vaccume adapter so I'll be shoveling horse shit for months to save up that kind of money :mad: .

[Mendeleev]

The vacuum adapters are not at all that expensive, its that damn 12 liter three-neck flask that I'm saving up for.

[tom haggen]

atlas, I think my beaker is pyrex. However, it doesn't really say. I have boiled water with it a few times now just to make sure it is not going to crack. I think its made out of the same glass that people make coffee pots out of.

[atlas#11]

If it's for high temps then no doubt it's pyrex. Mendeleeve, what do you want a three necked flask for? Are you distilling 3 gallons of nitric at a time or what? And where on earth did you find one?

[Jacob Kell]

Can somebody tell me if there exists a simple distillation apparatus, just without a chance of anything getting out? I mean, no holes for termometer, vacuum, with joints that can be hermetically sealed. I need something for concentrating sulphuric acid and making nitric, and I am afraid of fumes, I dont want anything to get out of it. I also live in apartment. has anyone seen such a thing somewhere for sale?

[Jacob Kell]

Can somebody tell me if there exists a simple distillation apparatus, just without a chance of anything getting out? I mean, no holes for termometer, vacuum, with joints that can be hermetically sealed. I need something for concentrating sulphuric acid and making nitric, and I am afraid of fumes, I dont want anything to get out of it. I also live in apartment. has anyone seen such a thing somewhere for sale?

[Jacob Kell]

Can somebody tell me if there exists a simple distillation apparatus, just without a chance of anything getting out? I mean, no holes for termometer, vacuum, with joints that can be hermetically sealed. I need something for concentrating sulphuric acid and making nitric, and I am afraid of fumes, I dont want anything to get out of it. I also live in apartment. has anyone seen such a thing somewhere for sale?

[Aristocles]

Allow me to resurrect this thread... hopefully it doesn't fall into the "necromancy" category ;)

Here's a copy and paste of what I tentatively plan to purchase tomorrow or the next day:

Flask, 3 neck, standard joint, 1000ml, 24/29x3
$29.95 $29.95
Teflon Joint Tape 1/2W x .003 x 260"
$1.50 $1.50
Simple Distillation Kit w/ 1000ml Flask & Hardware
$39.50 $39.50
SUPPORT STAND w/ ROD Cast iron 5" x 8"
$11.20 $11.20
SUPPORT RINGS w/ CLAMP Cast iron 3"
$5.60 $5.60
EXTENSION CLAMP w/ interlocking jaws
$6.31 $6.31
BURET CLAMP Rubber covered jaws One Buret
$4.60 $4.60
Allihn Condenser, 300mm jacket, 24/40 joints
$35.25 $35.25
Buret Class A Teflon Stopcock amber Straight 50ml
$27.95 $27.95


Does this look like a reasonable bare-bones beginning for someone interested in our hobby? I realize that to hyperbolically generalize is silly but just give me your thoughts. I also, full well grasp that our experiments vary greatly but I'm just looking for some rudimentary lab ware.

I have some glass vessels, scales, 'fridge', hotplate, thermometer, funnel, small oven, etc.

[megalomania]

Those prices are quite reasonable. It is hard to quantify what would be useful without knowing what kind of chemical manipulations you intend to do, like you said. Personally I find 3-neck flasks to be of little utility; adapters can always add additional functionality, and the extra openings can be inconvenient when you really need just the one. "Find the glass stopper" is a terrible game we all are forced to play in the lab :(

I used to buy stuff that I thought I needed, but I ended up never using it. I like to ask myself a simple question, "do I have a need for this, or do I just want it?" Do you really need 1000-mL flasks? Can you fit those with your heating mantles? Do you want to make things on that scale? I used to love the big stuff, but now I embrace microchemistry. An experiment works just as well (better usually) at 50 mL than it does at 1000.

I am not saying don't buy the stuff you want, just to stop and mentally picture what you will need. I always close my eyes and try to imagine myself doing a reaction before I do it. I concentrate on the little details, bits of equipment, and reagents, that I need so I can gather them up. If I don't have it, I can't do the reaction. It is better to realize this before you start something than after a reaction is underway. If in your mind you do not use the stuff you want to buy, don't buy it.

[Charles Owlen Picket]

The first time I got a chance to get a decent distillation rig, I bought one that came in a briefcase. I wondered why they thought it needed so much protection but was happy with the price. I realize that it was an attempt at portability but it was still nice to have; in that glass is actually the largest expense of my lab. Although fairly cheap by today's standards; it was only offered in a larger volume level for both receptacles. I thought that if offered between 500ml or a L that it's better to have larger as I would always cut volume but not expand, if I didn't have the size to begin with.

Personally, I never had a big use for 3-neck flasks and since then I heard that a lot of cooks get them set up to speed-up a synth and some jack-offs have put them on a "watch list" of glass materials... At the time I thought: "Good grief! They watch fucking glass now." And bought up all the stuff I needed. I noticed at the time that the less expensive was in a 24/40 format or I would also have bought on a smaller scale.

[Aristocles]

The three-necked flask has been shit canned. Thanks for the help.

I've tried to order but keep getting the answering machine... perhaps not everyone rushes back immediately following Christmas.

To me, the dictum about mentally picturing picture the detailed setup has helped. (Truth be told, the three-necked flask failed- actually it seems superfluous, for my purposes)

[megalomania]

Indeed 3-necks are on the fedgov watch list for Kalifornia, and probably Texass (they watch almost everything now). The strange thing is I don't recall any meth recipes on the Hive that actually used 3-necks, but trying to find logic from fedgov motives is impossible.

I should say it is nice to have a large flask when you need it because it is better to do a reaction in an oversized flask. A flask should be filled to no more than 50% of its capacity for safety reasons.

Personally, I prefer to use silicone grease to seal standard taper joints. It makes for a tighter seal, it helps keeps a joint from getting frozen (stuck forever), and they tend to stay attached better. It also makes for a quicker setup and teardown of glassware, but you will have to wash everything by soaking in a base bath after use. I do vacuum work, so grease is really a requirement for that. I also like to keep a spool of wire and wirecutters handy for securing vacuum and water lines to the appropriate ends. A squirt of acetone in the end of a rubber hose really helps get the sucker slip on (a condenser for example). Keck clamps are also useful... These little incidentals should be factored into a setup because they can save you from breaking expensive glassware.

[Barnacles]

I just ordered a distillation setup, this is what it came with!
I have a few questions! I wish I had thought of before. Is it common for these sets to come with all the stop cocks I will need? And can I heat these flasks with a open flame? for non-flammable- non explosive reactions obviously? and mega maybe there is no reason other than to test the waters of what they can and can't watch without raising a stink. and getting their foot in the door.


1 x 2000ml Round bottom Flask

1 x 1000ml Round bottom Flask

1 x Vacuum (Bent, 105 degree) Adapter

Distilling 3-Way Adapter

1 x 300mm West Condenser

1 x Threaded Thermometer Adapter (w/Nylon bushing top)

1 1 x Full length -10C to +150C Thermometer

1 x Medium Size Kit Stand (5" x 8" Stand, Rod 20" high)

5 x 24/40 Plastic Keck Clamps (to hold together the different units)

1 x Metal Utility Clamp

[megalomania]

You don't have anything on your list that would include a stopcock. They are typically included when a bit of glassware uses them. Typically, but not always.

You can heat your flasks with an open flame, yes.

[Charles Owlen Picket]

-> One note when distilling nitric acid; your "Threaded Thermometer Adapter (w/Nylon bushing top)" will go to shit from heat & fumes. Most everyone's does after about half dozen distillations. When distilling nitric, remember the setting on your heat source and replace the above with a plug of Teflon so it doesn't get messed up.
Most people think they won't distill nitric that often but when you can; you do....The first few months of "new glass" in the period of most intensive use. have fun!

[Barnacles]

Thanks for that, dually( now how do I spell that word again always thought Duelly) noted.

I have a few questions sorry to bog up the thread.

Now that I know that, Wont that be a place that a stop cock could come in handy? Will the nylon melt into the acid causing some unwanted reactions rendering the nitric acid useless for nitrations due to some ultra unstable nitro nylon or something?
Could I just wrap it in Teflon tape to stop that from happening ,but that may affect its temperature taking?\

Right about now I am wishing I spent a bit more time readingg about which would best suit me. But I had finally just put together enough money that I was able to spend on such things for the first time in years so was pretty excited and went ahead and bought it.

PS you must be psychic you read my mind about its purpose.(lol who would think a roguesci'er would want Nitric Acid JK)

PS2 I got it off of United Glass TECH. Gave me free shipping when I asked nice enough, I told them I would upgrade from the 1 literx500ml to the 2000x1000ml for free shipping. That was the setup I was going to buy anyway, but they are really nice definately recommend them <no I am not UGT lackey, Mega can confirm my IP is not from the area of UGT.

[Man Down Under]

Why not replace the nylon with a teflon O-ring? They do make them.

[Charles Owlen Picket]

United Glass are good people; I got some stuff from them also. You know that setting up your lab are YOUR lab concepts in action; if you think a stop cock could be worth the expense rather than a plug or what-have-you, by all means do it. You will know best what has utilitarian value.....to you! You may find that you do somethings on the cheap & others, you put some dollars down to.

My method (which certainly doesn't mean it's a good one) was to get two of everything so if I had breakage, I wouldn't be sidelined. My emphasis went into that concept. In other areas I went cheap. My condensers, let's say, I'd look at using a cheap Clausen or some shit, rather than a high end big-boy. I bought used, a HELL of a lot of times! Any simple shit, I would get those Chinese beakers and flasks; you know what I mean.

[megalomania]

Where do you get your used stuff from, Charles?

I like to use Chemglass products, their prices are the best I have seen for standard taper glassware.

[Charles Owlen Picket]

This is my technique: I have folks I know at the local university. I know students, I hang out in the lab, etc. I also know a guy who is in the chemical business. I hit them up consistently for old stuff. You would possibly be shocked that salvageable glass goes in the dumpster due to the need for spending; in and of itself.

A university (as you may know) has a budget that they MUST spend in order to get next year's at or above the previous level. They NEED to have a need. The trick here is to get a connection.

I won't go into too much detail, but you get the idea. You must cultivate the local resources (even a "community college" - a fucking secondary school) in a manner that allows them to use you as a way to get the stuff from their lab. It's an exercise in creativity... But it can be done. You might even be impressed in the amount of stuff I have gotten. But you need to take the shit with the gold in this as they want it OUT of the lab. Later you can sift through the goodies and keep what you want and shit-can the rest. But you have to clean house for your source.

If you have a connection (close) with someone who either has a chemical business (let's say Water Treatment; that's a gold mine) you let him or her know that you want the chemicals or stuff that they can get but have to order in large volumes. Then you kick them down a few bucks so they can make a large order and save $.

I do the OEM thing a bit. I once got several air-bag units & salvaged about 800gr of azide from them, however it turned out that a bio-lab uses NaN3 for cleaning up and they were getting it for $40 a pound at a purity level that was astounding....close to the cost of an OEM source. But when I need glass there are so many ways to get used stuff that I have to make a decision on what is WORTH buying new. I have a source for cheap (we're talking $8) sep-funnels. They ARE really cheap (Chinese) but they work and have Teflon pet-cocks. A high-end funnel just ain't worth it (to me).

I can go on and on but it's better to PM me if any of you have more involved questions. I don't do anything inappropriate or illegal but I do get some wonderful things that would cost a mint in this manner.

[Aristocles]

Well, I recieved the UPS tracking number today... 'so I guess my shit is in the ether'

Man it was like trying to untie the Gordian Knot to get the stuff ordered from the original place.

I am an impatient bastard.

So I ordered from another place:


http://www.pelletlab.com/p_g_distillation.shtml

I purchased item LB120-1000K

http://www.pelletlab.com/p_g_burette.shtml

I purchased item LB74-50

http://www.pelletlab.com/p_l_support.shtml

I purchased item LB73-20C

http://www.pelletlab.com/p_l_clamps.shtml

I purchased item LB71-1

http://www.pelletlab.com/p_m_thermometer.shtml

The temporary goal will be to distill nitric acid. I am thinking I'll need an aspirator, also...

An interesting hobby... I'll be completely broke within two years from buying glass and chems, OCD does have it's bad side...

[pyromaniac_guy]

did a quick search and haven't seen them mentioned in a while so i figured I'd make a little reminder post. When shopping for new goodies dont forget to browse dovebid.com along with labx and ebay. you normally wont find any 5$ specials, but you might pick up a perfectly good 500 MHz nmr set up for a thousand clams if no one is paying attention....

[Charles Owlen Picket]

Aristocles:
That looks like a good start.
Everyone who spends $ for the glass portion of a lab faces choices as to where and how to spend the real money......What you get from the vacuum is efficiency; that's certain. But it's not mandatory in all situations. An aspirator is cheap but can be a hassle. The choice then becomes one of expense.

I had a chance to get a serious unit. A vacuum / pump that was a lab unit but would cost me 600 bucks. It sold new for over twice that amount. It simply wasn't worth the expense to me. I like getting 1.52 HNO3 but I can live with a few hundred ml here and there; I don't need to make a liter at once. That may be the core of the issue.

[Aristocles]

Well...

I just ordered:

24/40 Vacuum (105 degrees) Adapter - $29.99

24/40 200mm 3-Way Vigreux Distillation Head - $37.50

500ml Corning Brand Erlenmeyer Flask, w/ 24/40 Top - $14.99

Free Shipping...

I am assuming that I will be SOL on the Graham Condenser mentioned in my prior post, as it does not have a ground glass joint at the bottom (where distillate exits). I am trying to figure a way to get a seal between the vacuum adapter and the Graham, that won't be eaten by nitric acid .

Ideas?

[Charles Owlen Picket]

I would Teflon tape the thing to death and let it be. Because you are going to clean up your glass anyway use the Teflon tape as it's cheap (plumbing supply shit) and you just take it apart. I know you want something that would look more professional but whose going to see it? Use the wide stuff.

There ARE urethane stoppers that are acid resistant (not proof) that can work. They will stand up for a long time but the heat gets to them after about a half-dozen distillations or more. You can use urethane for a lot of connections; what's more you can wrap them in Teflon tape and they'll work QUITE well. I have a urethane connection that looks very professional that had held up for a very long time. If you can't get a hold of the stoppers proper; don't fret. Get some skateboard wheels and trim them to size.

Remember you're distilling at about 80-90 C so the glass won't be getting much hotter than that. That's important, as you can use a whole lot of materials that can be covered in Teflon tape that won't melt at that temp. Condenser-wise you really don't need a good one, most anything will do for HNO3. Once I broke a good one I had (don't ask) and I just got a shit-load of sodium glass and made a spiral (like an old-time still!) and my level of efficiency was close to what I had! (I used 1/4" 48" @ 4.5" dia.) Here is where creativity reigns supreme.... the lab layout.

[Aristocles]

Thanks, Charles.

Encouraging and positive... damned good qualities

[megalomania]

There are certain kinds of tubing with excellent chemical resistance you may want to consider using to connect glassware when distilling nitric acid. I just got a new tubing catalog today... Fluran F-5500, Tygon Inert SE - 200, Norprene Chemical Tubing, Tygon Plasticizer Free Ultra Chemical Resistant Tubing, Chemfluor FEP, Chemfluor PFA are just a few that offer outstanding chemical resistance. I saw one type of tubing actually recommend it be cleaned by boiling in nitric acid, but I can't find it now.

You will have to verify which type of tubing can handle hot concentrated nitric acid. I doubt these are hardware store tubings, but an online search should yield some by-the-foot sources. You should not need that much tubing for connecting glassware, keeping in mind these exotic type materials can cost $2-$3 a foot (for small diameter) and >$10/ft (large diameter).