09-12-03 01:43
No 458496
swim feels like a very much worried citizen, so he told me to ask: what can be done about potential peroxide formation around the cap of a waste container that could contain diethyl ether?
perhaps further explanation is necessary. swim had attempted to obtain diethyl ether by means of distilling a mixture of conc. H_2 SO_4 and Et OH, but for various reasons botched the synth. in an attempt to be environmentally conscious and low-key, the waste from the failed distillation was stored, rather than diluted and dumped. the volume of stored conc. H_2 SO_4 and Et OH is approximately 2L, 1L in each of 2 1L apothecary jars (tops sealed with vacuum grease in the joint).
swim has related to me that there are small accumulations of white solid around the jar tops' undersides which he suspects to be peroxides. swim also has serious concerns about the detonation properties of such peroxides, especially when viewed in light of the jar contents (sulfuric acid + explosion = double + bad). the estimated time elapsed since storage is ~2 months.
swim thinks this may all bee overreaction, as since the synth was botched, there shouldn't bee that much Et_2 O afoot. this may bee completely wrong, and more experienced bees can feel free to make suggestions along this line.
that said, what options does swim have? ideally, swim would like to find a way of fixing this problem without transporting the jars (explosion and successive corrosion in transit would be really bad) off-site. swim read a post about shaking with a solution of ferrous sulfate to remove peroxides, but this doesn't solve the problem of actually opening the container (the scary part). any suggestions that don't involve "call the bomb squad" (a.k.a. hazmat/fire dept. ppl) would be helpful, but if that's the only route, swim's a swimming up shit creek.
exit stage left bereft of all but a bass clef, i manifest zest
(Newbee)
09-13-03 03:58
No 458779
I may be crass, but me and my buddies would probably wrap the bottles with tape, take 'em out in a field somewhere, put 'em in a pot, and shoot their heads off with a bb gun. Since its only ethanol and acid, you could dilute and neutralize, then dump them where they lie with a clear conscience. Shame to waste good alcohol like that...
(Hive Addict)
09-24-03 07:54
No 460674
Do not follow the tape suggestion. I will get the lit you need.
NA 1:7
(Hive Addict)
09-24-03 11:46
No 460704
A) what is the ratios of the acid, the alc.? was the alcohol everclear and the acid "drain opener"?
B) what was the method of distillation, and why is it thought to have failed?
C) Where are the jars stored, any light or sun hitt them at all? ANY ventilation, and how full are the containers also how long have they been languishing there?
D) Is the white solid on the outside, inside, or both?
E Was the solution added while hot and then the cap/top put on?
F) Anything in those jars before you put the failed project solution in?
give details and accurate ones at that, so that you give a better picture of the situation.
the big concern would be a notable drop in the level of solution with the white precipitate forming afterwards.
NA 1:7
(Newbee)
09-24-03 23:29
No 460805
A) what is the ratios of the acid, the alc.? was the alcohol everclear and the acid "drain opener"?
>>the acid is concentrated H_2 SO_4 (98% i believe, NOT drano) and the alcohol is ethanol 95% (NOT everclear).
B) what was the method of distillation, and why is it thought to have failed?
>> swim's method of distillation was as follows: take 50 mL of ethanol, put it in a 500 mL RBF, add 150 mL of conc. sulfuric via addition funnel, then bring it up to ~135 degrees centigrade. hold it here and add ethanol to the mixture at the rate it is condensing. this went wrong b/c swim didn't have enough condensing power to condense all the ether that formed, thus the configuration had to be shutdown (lots of ether vapors = hella explosive). the contents (a dark brown-black mixture of ethanol and sulfuric acid) were then stored. a number of other unsuccessful variations on this occurred until it was done successfully, so there's extra waste lying around (to the tune of 2L).
C) Where are the jars stored, any light or sun hitt them at all? ANY ventilation, and how full are the containers also
how long have they been languishing there?
>> they're stored in a metal cabinet, so they do not regularly get hit by any light. however, the temperature control is somewhat poor, and this concerns me. if you read the above post, it says that there are 2 1L apothecary jars, each with approximately 1L in each (i.e. they're full, with only ~200 mL air space in each). it's also stated in the first post that they've been there for ~2 months.
D) Is the white solid on the outside, inside, or both?
>> it's on the inside, underneath the top to the apothecary jars. it's a white crustiness and it's creeping into the seal that the tops make with the jar (ground glass).
E Was the solution added while hot and then the cap/top put on?
>> no, it was allowed to cool to room temperature before storage.
F) Anything in those jars before you put the failed project solution in?
>> the jars were empty before any of this failed result went into them.
give details and accurate ones at that, so that you give a better picture of the situation.
the big concern would be a notable drop in the level of solution with the white precipitate forming afterwards.
>> i haven't noticed a drop, so i'd imagine that would mean that not very much ether (or whatever) could have evaporated and formed peroxides. the downside is that i hadn't marked the sides of the containers after pouring, so i'm not certain. i guess that'll teach me to mark fluid levels on sides of containers, it's a damn good way to determine if things have been evaporating.
thx x
exit stage left bereft of all but a bass clef, i manifest zest
(Moderator)
09-26-03 02:53
No 461100
If any of you Brainiacs had used the search engine properly, you'd have found quite a bit of information on removing peroxides from ethers yourself, without calling the hazmat team
There are other applicable posts to find, but one old thread should bee enough for such lazy bees see Post 174898 (LaBTop: "Re: Grignard Startup", Methods Discourse), Post 174921 (lugh: "Re: Grignard Startup", Methods Discourse) & Post 174986 (Scooby_Doo: "Re: Grignard Startup", Methods Discourse) 
Chemistry is our Covalent Bond
09-27-03 06:15
(Rated as: insignificant)
(Moderator)
09-27-03 23:49
No 461379
Karma is given by moderators of the forum involved, obviously you haven't read that particular information
Staff has many more things to do than answer redundant questions by newbees who get themselves into difficulties by beeing unprepared for their actions, it's clear you think otherwise 
SWIL's best post concerning this problem seems to bee MIA 
Those comments weren't just addressed to you, but to all of those posting in this thread, so perhaps you need to rethink your response If you had read the applicable sections in Vogel's and other sources of information available here, you would know that peroxides aren't very dangerous while in solution, which should suggest a simple and obvious answer to your concerns about that precipitate You need to gently invert the bottle to dissolve the potentially dangerous material and get it away from the opening, then treat it to remove any peroxides 
If you have no faith in your ability to carry out such a task manually, you could rig means for doing this behind a blast shield, if you want to spend the money, or use a tool sold for the use of handicapped people to get a little distance between you and the bottle while inverting it 
There are other possible solutions, whatever you decide to do, don't bee in a hurry, unless you're putting out a fire
Chemistry is our Covalent Bond