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Author: Subject: new toys
JJay
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[*] posted on 30-4-2017 at 13:36


I needed something for preparing analytical solutions and weighing samples for microscale experiments, and the price was unbeatable. I am sure I could get another decimal point of precision out of a much more expensive setup, though.

As much as I like using a power drill with a dimmer switch for stirring mixtures, I don't think that's a good idea with ether (or even acetone really), so I recently ordered a JJ-1 mechanical stirrer: http://cnjinyi17.en.made-in-china.com/product/WvCQrFMlEDVR/C...

Mechanical-Stirrer-JJ-1.jpg - 19kB

I've sunk an obscene amount of money into mechanical stirrers, so I hope this one will do what I want and have few problems.




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XeonTheMGPony
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[*] posted on 1-5-2017 at 11:05


just scored 2 pounds of mercury! some in the form of beautiful mercury displacement relays!!!! Will post porn shots of it when I get home!

Best part is only cost 20 bucks Canadian, was doing a job at an old medical building and figured I'd ask the head maintenance guy if they had any!

Pics as promised

did a ruff weigh and I deff have 2 or so pounds !


Mercury 1.jpg - 354kB Mercury 2.jpg - 298kB Mercury 3.jpg - 102kB

I'm not going to kill the Displacement relays! I'm going to make them new coils and use them suckers!

[Edited on 1-5-2017 by XeonTheMGPony]
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Funkerman23
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[*] posted on 1-5-2017 at 20:20


Quote: Originally posted by JJay  
I needed something for preparing analytical solutions and weighing samples for microscale experiments, and the price was unbeatable. I am sure I could get another decimal point of precision out of a much more expensive setup, though.

As much as I like using a power drill with a dimmer switch for stirring mixtures, I don't think that's a good idea with ether (or even acetone really), so I recently ordered a JJ-1 mechanical stirrer: http://cnjinyi17.en.made-in-china.com/product/WvCQrFMlEDVR/C...
Mc Master carr has the ready made one here: https://www.mcmaster.com/#chucks/=17g1k6t I've shopped around and save for a a dollar or so, these things are set in price. Failing a chuck, the old standby of automotive jubilee hose clips and a length of rubber tubing might work but that can be a PITA.


I've sunk an obscene amount of money into mechanical stirrers, so I hope this one will do what I want and have few problems.
At some point you may find that the included chuck does not work well with different diameter stirr rods. There is a Mixer chuck available from a number of sources that will solve this problem permanently but is around 100 USD. I don't know what wattage you have as I have a 100 what one. Same JJ1 stirrer.

[Edited on 2-5-2017 by Funkerman23]




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JJay
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[*] posted on 3-5-2017 at 19:03


I finally got my JJ-1 stirrer, and it looks very nice. It comes with a very sturdy collapsible stand and some clamps, as well as two stainless stir paddles. The included chuck is a collet chuck and is designed to work with a single diameter stir rod... it would be nice to hook a small Jacobs chuck up to it, but collet chucks are more durable and hold the shaft straighter (so I guess that is why they designed it with a collet chuck).

Mine was sold as 40 watts but it looks the same as the 100 watt ones, so I really don't know. I think 40 watts should be sufficient for most purposes.

I am going to get it set up and take some pictures.

[Edited on 4-5-2017 by JJay]




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JJay
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[*] posted on 3-5-2017 at 19:55


Here is my humble small-scale reaction apparatus. It still needs a fume hood, an argon tank, a thermometer tube, and a temperature controller

IMG_20170503_194803[1].jpg - 470kB




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JJay
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[*] posted on 9-5-2017 at 22:44


I got some 300 mL crucibles. I would like to point out that javener2010 is an *excellent* seller - shipping was fast, the price was the best on eBay, and the crucibles were packed like they were shipped by Deschem.

IMG_20170509_223734[1].jpg - 430kB




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Funkerman23
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[*] posted on 10-5-2017 at 13:24


Quote: Originally posted by JJay  
Here is my humble small-scale reaction apparatus. It still needs a fume hood, an argon tank, a thermometer tube, and a temperature controller


If I may: what size flask and mantle are you using in that set up? And where did you find the mantle?




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XeonTheMGPony
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[*] posted on 10-5-2017 at 15:21


Well my toys from deschem arrived and got to say they look much better then the last order and very well don ground joints!

My lab safety partner was diligently watching my unpacking and ready to attack the foam if it made any dangerous moves!

P6100299.JPG - 1.3MBP6100300.JPG - 1.3MB
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Eyeborg
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[*] posted on 10-5-2017 at 16:38


I got an older Fisher Thermix 310T hot plate stirrer of eBay rather recently.

http://www.ebay.com/itm/182545765277?_trksid=p2057872.m2749....

Got a pretty good deal for it, $26 and ~$10 shipping.
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JJay
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[*] posted on 10-5-2017 at 17:01


Quote: Originally posted by Funkerman23  
Quote: Originally posted by JJay  
Here is my humble small-scale reaction apparatus. It still needs a fume hood, an argon tank, a thermometer tube, and a temperature controller


If I may: what size flask and mantle are you using in that set up? And where did you find the mantle?


3000 mL. It's a Glas-Col fabric mantle. They are all over eBay.

The hardest piece to obtain was the 1L pressure-equalizing addition funnel.






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JJay
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[*] posted on 18-5-2017 at 19:35






IMG_20170518_193255[1].jpg - 476kB




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tsathoggua1
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[*] posted on 3-6-2017 at 08:35


Another trick to avoid sparks is to use a hand-drill, since they rely on gear wheels and hand cranking rather than an external energy source there is no motor wiring to arc. And they can take any reasonable size of stirring rod.

And as it happens the neck portion of many of them happens to fit conveniently into a standard sized two-pronged lab glass clamp. Not exactly cutting edge, but it is handy to have the option when doing things that need stirring, especially when there is something extremely flammable present, or ferromagnetic materials present that would preclude stirring (such as nickel catalysts, Fe, Raney cobalt etc.) For the likes of reductions involving nickel catalysts and hydrogenation at STP using the likes of Ni2B/borohydride it fits the requirements pretty well.

Just had a water aspirator vacuum arrive yesterday, for when the more powerful electric vac pump is overkill and today, a big bag of stainless steel keck clips to replace the plastic ones that with the exteption of perhaps 3 or at most, 4, all died horribly after being used to secure joints of a still being used for distillation of ICl.

[Edited on 3-6-2017 by tsathoggua1]
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Magpie
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[*] posted on 3-6-2017 at 09:21


Quote: Originally posted by tsathoggua1  
Another trick to avoid sparks is to use a hand-drill, since they rely on gear wheels and hand cranking rather than an external energy source there is no motor wiring to arc. And they can take any reasonable size of stirring rod.


Perhaps it would not be too difficult to provide a belt drive to the drill. Then place the motor in a more protected area.

Quote: Originally posted by tsathoggua1  

... and today, a big bag of stainless steel keck clips to replace the plastic ones that with the exteption of perhaps 3 or at most, 4, all died horribly....


Where do you buy ss Keck clips?

Edit: Nevermind. A few years ago I searched all over for ss clips. Now I see they are available through Walmart :o

[Edited on 3-6-2017 by Magpie]




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tsathoggua1
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[*] posted on 3-6-2017 at 11:35


Bought a big bag of them on ebay. Not sure how many there actually are but certainly enough to last a while. Those plastic ones were awful. Alright for a few uses but some chemicals, most notably iodine monochloride and trichloride ripped them to pieces. They quite literally crumbled away when lightly touched into powder and small plastic chunks about the size of a BB.

I think I'll end up electroplating them in something highly resistant to most attack, such as iridium, perhaps, or if I can't get sufficient iridium salts then nickel as second choice. Ir, IIRC, is only attacked by molten, fused alkali metal hydroxides, halogens at elevated temperatures and fused cyanide melts. And plenty things will have a go at ordinary stainless given a chance.

Walmart? from what I read of that place, that does surprise me. Although we haven't got walmarts in the UK.
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Magpie
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[*] posted on 3-6-2017 at 12:37


My problem with the old Delrin clips was melting when I would do high temperature disitillations, etc. Then I bought ptfe clips and haven't melted one since. They are expensive, however, but so is a failed synthesis.

What you have read about Walmart is likely true. Amazon is going to slay them all however. They have 30,000 employees in Seattle and want to build to 100,000. They are ruining the Seattle real estate market.

https://www.google.com/aclk?sa=L&ai=DChcSEwiruoKLwqLUAhU...

[Edited on 3-6-2017 by Magpie]




The single most important condition for a successful synthesis is good mixing - Nicodem
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tsathoggua1
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[*] posted on 3-6-2017 at 13:17


Yeah in the end, using PTFE tape to wrap stoppers (didn't have any fluorocarbon grease) was the only thing that didn't end up as crumbly powder or cement-ified slag on contact with the vapors from the iodine monochloride. Definitely not something I'd wish to inhale.
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tsathoggua1
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[*] posted on 5-6-2017 at 01:35


Bought a 150ml glass syringe, for dispensing nasty things that would eat plastic/rubber or cause it to burst into flames. Worked a treat for bottling my iodine monochloride without it escaping (a few drops did, but nothing my gas mask wouldn't handle)

A 100-pack of melting point tubes. Need to get a Thiele tube as well, new 1l sep funnel, a new fritted Buchner, going to get a few different sizes of the latter plus some filter papers for my ceramic type non-fritted buchners and some celite.

Also, seen some long, tall and narrow fritted Buchners on ebay that I like the look of, would be quite convenient for vac filtrations, going to bag a few in different sizes.

Bought a shitton of small test tubes (50 of them) and a 1.5l flat-bottom conical vacuum filter flask.

Contemplating, if I have enough money left over after going lab-shopping, getting myself a kilo of boron, as a replacement for the lead that is currently inhabiting the heating chamber of my molten metal bath, mainly due to the toxicity of lead and the quite obvious fuming at higher temperatures, it was enough to quite quickly produce a fair bit of white lead slag
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JJay
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[*] posted on 19-7-2017 at 22:04


I bought most of the materials I need to make a recirculating aspirator and an amateur fume cabinet. I still haven't decided exactly what I am going to use for the sash, but I'll have a look around when I go back to the home improvement store for PTFE tape and plaster. Polycarbonate would be nice....



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[*] posted on 20-7-2017 at 05:24


Polycarbonate is great stuff for impact and strength, but it gets hazed by chemicals quickly. For use with chemicals, I would stick with plexiglas, which is more chemical resistant (but still attacked by many chemicals.)

PS, If you want long, tall glass frit funnels, I have lots of them, tell me what you are looking for, and I can find some.
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JJay
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[*] posted on 20-7-2017 at 06:48


Oh, cool. I might be interested in those. I've been looking in particular at how to safely filter out salts when making organometallics. My one fritted funnel broke a couple of weeks ago while it was sitting in a box, so I have actually been looking for a new one.... I guess I'll have to see what you have :)



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[*] posted on 20-7-2017 at 15:37


My latest purchase was a soxhelt extractor (well 2, because one came broken), a hotplate stirrer aaaand benzyl alcohol.
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tsathoggua1
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[*] posted on 20-7-2017 at 23:07


I'd be interested in tall thin fritted buchners myself.
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JJay
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[*] posted on 21-7-2017 at 00:10


It's not pretty, but here's my recirculating aspirator almost ready for action. I'm curious about how strong of a vacuum it will pull.

IMG_20170721_000300.jpg - 76kB

[Edited on 21-7-2017 by JJay]




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JJay
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[*] posted on 28-7-2017 at 18:02


I recently obtained a bundle of ceramic paper.

s-l1600.jpg - 59kB

The quality of it seems to vary, with some sheets being in perfect shape and others seeming fragile, being ripped and perforated. It was dirt cheap though. I wish I had some way to stitch the sheets together....




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[*] posted on 28-7-2017 at 19:11


JJay,

Re.: Your recirculating aspirator system.

In the event that your home-built aspirator system does not meet your needs, have you considered buying a used commercial system such as those offered by Cole-Parmer and similar? They can seem pricey but are worth every dollar. I bought one several years ago on ebay and it is a lab workhorse for filtration and distillation.

AvB
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