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Author: Subject: Bad days in the lab or with glassware?
JJay
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[*] posted on 28-12-2016 at 17:31


After distilling some water, I noticed that my favorite 3L flask is developing some nasty scratches, some of which are in an ugly pattern that looks like star cracking. I'm not ready to throw the flask away yet, but I'd be a little concerned to put it under vacuum or use it at high temperatures.

Looks like I will need to pick up a new flask pretty soon... I wonder if I should get one with four necks. I could use an overhead stirrer, reflux condenser, addition funnel and thermometer simultaneously that way, but I find that I rarely require such a complex apparatus, and I could probably get away with using a Claisen adapter on one neck....




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[*] posted on 29-12-2016 at 13:46


First time ive had glassware delivered broken. I think from now on im going to try much harder to find galssware already in the USA instead of having it ordered from China. Because not only does it take about a month, but you could get something like this, which totally bummed me out today when it came. I was really lookin forward to my first pressurized funnel. And now its here and its shit.


br.jpg - 104kB
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[*] posted on 29-12-2016 at 14:58


I hate to say it, but that's why chinese glass is cheap. I see teaching labs complain about the scratching and star cracks in glassware that otherwise gets nearly 20 years of use.
I find it hard to do repairs because there is a difference in the borosilicate batches that china uses compared to the material from European and American suppliers.
That said there are also differences between modern batches and old stocks of glass that I've had difficulty using; and old, I mean older than 40 years.

Support your local glass blower, the difference in price is buying you a reliable service.
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JJay
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[*] posted on 29-12-2016 at 16:43


Some Chinese glass is good; some isn't. I have literally knocked pricechopper2011's flasks from a tabletop onto concrete without damage. I have seen American glass implode under vacuum and crack spontaneously for no apparent reason... there are many factors that affect quality....

When I ordered my addition funnel, it arrived broken twice due to shoddy packaging. When I finally received the funnel, though, it was like unwrapping a Ming vase. I am sure it will last a very long time if treated properly.

I imagine I'll go through the same ordeal with my reflux condenser, but I'm also sure I'll end up with one that will last 20 years.

For every item in those American-made sets that have lasted 20 years, how many got smashed when a spatula was dropped placed on top of them in the chemistry drawer or when they were placed on a cold tabletop after heating? Not every microchip ends up in a server, and not every adapter should handle boiling sulfuric acid... I'd bet you could drop kick a lot of ancient Chinese earthenware (or for that matter, 100 year-old china teacups) across the garage without any damage, but for every piece like that, there were hundreds more that have shattered.

China has subsidized shipping policies that I believe provide insurance, so shippers don't necessarily have a financial interest in supplying the best packaging.

[Edited on 30-12-2016 by JJay]




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Texium (zts16)
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[*] posted on 29-12-2016 at 21:51


I have wondered if some of the older pieces of glassware that I own have survived for decades of use by natural selection of a sort. Maybe that the flasks that made it to me are more well-annealed and even than their compatriots that broke over the years.

It's an interesting thought, not sure if there's any truth to it though.




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JJay
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[*] posted on 29-12-2016 at 22:47


Quote: Originally posted by zts16  
I have wondered if some of the older pieces of glassware that I own have survived for decades of use by natural selection of a sort. Maybe that the flasks that made it to me are more well-annealed and even than their compatriots that broke over the years.

It's an interesting thought, not sure if there's any truth to it though.


Well, you could always do a controlled experiment to find out!




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[*] posted on 28-1-2017 at 09:15
bad day


A nice sunny morning, and I finally felt fit enough to distill some EtOH today :)

took almost 2 hours to set up (I'm not that fit yet)

the still ran long enough to get c20ml of distillate from 1.4l in the pot, then it stopped ...

my cheap hoplate melted it's internal thin pvc insulated ac input wires :(

... then it started to rain on my outdoor workspace :mad:



on the brighter side, the heating element for my diy 500ml 250W mantle arrived today :)
... now looking for tin cans .....




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[*] posted on 28-1-2017 at 09:44


@Sulaiman I bought one of the 250ml liners, but I didn't think about the fact they're meant for 240 Vac... Then my poorly constructed heating mantle (not much insulation) meant only 20 out of the 65 watts made it into the flask. Not to mention the major electricution hazard from my poor wiring.:D
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[*] posted on 28-1-2017 at 10:18


IF you can find a mains transformer of required VA (i.e. 250 VA in this case)
that has dual 110 Vac primaries, you can use it as step=up transformer,
a 110:110 Vac isolation transformer of half of required VA also works.




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[*] posted on 28-1-2017 at 10:34


That's what I was thinking but unfortunately I don't have the right transformer, it's back to the oil bath for now:)
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[*] posted on 28-1-2017 at 12:11


Last time I ordered glass from china, give or take a couple, 100 pieces or thereabout, every last bit arrived wrapped and packaged perfectly, even surrounding the condensers in blocks of something tougher than styrofoam but of a similar foamed plastic nature over the coolant inlet/outlets. Entire lot all packed up individually, and the dead-space in the crate filled with soft packing. Not a scratch on any of it. Only thing not to survive was a 100ml 2-necked flask, and that was my own fault, after having used it and dropping the damned thing. Empty at the time, thankfully.
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[*] posted on 1-2-2017 at 10:05
beginner experience


So i recently sent a bit of Propionyl Chloride to another member here. I have a bottle of this stuff and am saving it for something particular so i hadnt really dealt with it yet. I have never dealt with this chemical but i did have a tiny bottle of Acetic Anhydride once that i was told was kind of similar. So all i did was, i took the bottle of prop chloride and poured it into a graduated cylinder to measure it. Within seconds i couldnt even breathe and my eyes were hurting cuz of how strong this stuff is. It fumes a little and is extremely pungent. I thought it would be bad like dealing with hydrogen chloride but i think this was worse. IT was just really strong. Thats the last time i do that without a respirator and goggles.
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[*] posted on 1-2-2017 at 10:25


I had a similar experience when I bought tetralin without thoroughly researching it beforehand. Wasn't aware it had such a strong, nauseating (to me) smell. Transferring it from the jug it shipped in to several glass bottles was not a fun experience.
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JJay
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[*] posted on 1-2-2017 at 17:51


Ever open a bottle of bromine? :D



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[*] posted on 28-2-2017 at 03:39


I had a close call with some nitrocellulose I was storing in my gun safe, I placed it in the ammunition compartment a long time ago and forgot about it.

it's summer here and the part of the house where I keep my safe gets quite warm and fluctuates a bit which sped up the breakdown of the guncotton (it was neutralised and washed thoroughly before storage)

When I opened the ammo compartment to grab some primers I immediately smelled NO2 and saw a layer of rust on the latch (PANIC!)

Luckily, it doesn't look like my rifles were attacked but I'll give them a good clean and oil tonight anyway, just to be sure.

Below are some pics of the offending guncotton, the jar lid that the NO2 ate through and the damaged latch and primers.

Only powders, primers and ammo will be stored with the firearms from now on.

DSC_3227.jpg - 1.9MB DSC_3226.jpg - 2.7MB

DSC_3219.jpg - 1.6MB DSC_3232.jpg - 2.6MB

DSC_3233.jpg - 2.3MB
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[*] posted on 17-3-2017 at 16:12


Not lab related but certainly a bad day and chemical related. I recently moved into a new place and the previous owner had apparently spilled a whole jug of laundry detergent under the washer and dryer. I literally had to scrape lint, dust and pube encrusted soap off the floor with a chisel. Today my fingers are super dry and sting like crazy. Not fun.



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[*] posted on 23-3-2017 at 13:26


While on my accident streak I had an accidental detonation. I was trying to make nitrite by the reduction of nitrate with sodium sulfide... Again, and it detonated spraying sulfur smelling goop on windows and walls, luckily it did this relativly safely outside so no real damage was done, it didnt even crack the crucible but i think it is time to give up on this synthesis.

Im going to try the electctrolytic oxidation of ammonia instead. :(
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[*] posted on 1-10-2017 at 07:15


I've been doing some experiments with corn syrup and have managed to get it everywhere and all over everything. It doesn't take too much to clean it up, but it has a tendency to cement stuff to the countertop. Most things I've been able to dislodge, but one petri dish was so firmly stuck that it broke rather than come loose. There's still glass glued to the counter top that I haven't been able to get loose :(



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[*] posted on 2-10-2017 at 12:13


Im was finally sucessful with the nitrite but i broke my glass thimble placing it in the sink on top of the drain so it fell over...

Here is another one: :(
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[*] posted on 13-11-2017 at 09:23


Sort of a cross-post, but I thought it belonged here too.

Last night I was doing an experiment on making boron from boric oxide, by mixing the crushed oxide with Mg powder and heating in a small propane furnace. Just a few minutes into heating, I was poking at it with a graphite rod to try mixing things around. It suddenly reached the activation temperature and I was met with a wooshing sound, a blinding white light, and very hot boron flying out of the furnace. While I was right next to it. The tabletop was scorched in several places and my shirt now has a burn mark on it. Luckily, I was doing this outside and was wearing a face shield and welding gloves. I should have also been wearing my welding jacket, apparently. That really surprised me because the reaction shouldn't produce any gas, so I don't know why it would "explode" like that. Always be prepared for the worst!

The upside is it looks like this method worked beautifully, and I have lots of black B powder drying on the filter paper now. Should make for a fun YouTube video!
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The Volatile Chemist
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[*] posted on 18-11-2017 at 21:09


Well I guess I don't have too much to complain about, but I dirtied half my glassware for a phenolphthalein synth that failed simply because I neglected to add sulfuric acid. I did get a very little product in solution, which was a nice proof of concept, however, and I also silenced a nagging that I'd had, that sulfuric acid, when used as a catalyst in reactions involving the release of water, could hardly be necessary. So, all in all, not too bad, but I have to prep some phthalic anhydride all the way from di-n-butylphthalate, so it'll be a while before I can retry the experiment.



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[*] posted on 19-11-2017 at 18:11


I attempted to look at your write-ups, but both links gave me an "account suspended" screen. What am I doing wrong? (I will admit in advance to being severely computer-challenged.):D
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[*] posted on 19-11-2017 at 18:53


Quote: Originally posted by CharlieA  
I attempted to look at your write-ups, but both links gave me an "account suspended" screen. What am I doing wrong? (I will admit in advance to being severely computer-challenged.):D


You normally get that when the person stops paying for the server. In this case i had a peek at the history and I think it never got passed the under construction stage.

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[*] posted on 20-11-2017 at 06:09


I recently broke my liebig condenser. Was a very sad day. With this recent unfortunate event, my ongoing project has come to a halt and I am forced to wait patiently by the mailbox for its replacement to come.
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The Volatile Chemist
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[*] posted on 20-11-2017 at 09:23


Quote: Originally posted by NEMO-Chemistry  
Quote: Originally posted by CharlieA  
I attempted to look at your write-ups, but both links gave me an "account suspended" screen. What am I doing wrong? (I will admit in advance to being severely computer-challenged.):D


You normally get that when the person stops paying for the server. In this case i had a peek at the history and I think it never got passed the under construction stage.


Well if you look long enough back you'd find it did indeed have a website there - though you'd need to look at the ptp.x10.mx link for that. I just use it as a placeholder for the moment, until I have something to actually put there. These days I don't really do big writeups. But when I make some progress on a PDF of amateur-accessible syntheses and the characterization of compounds, I'll put it up there along with the indices.

Ironically, when you checked, the website had just gone suspended. It should be unsuspended now (free host, just have to make sure I log in monthly).

[Edited on 11-20-2017 by The Volatile Chemist]




My write-ups are on here...
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