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Loosening frozen ground glass joints

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Philip Henderson

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Aug 19, 1999, 3:00:00 AM8/19/99
to
Prior to me wasting my time be trying something that won't work, are there any
recommendations on loosening a "frozen" ground glass joint? While cleaning up
my lab, I found an old sample contained within a glass 500 mL rb flask with
a 24/40 stopper that won't budge. The small amount of sample inside is
acidic, but fairly innocuous, not combustable, and not a peroxide former.
The Chemist's Companion recommends a solution of 10 parts choloral hydrate,
5 parts glycerine, 5 parts water, and 3 parts conc. HCl. yummy.
A quick google web search yielded one reasonable hit for a commercial
detergent called "Haemo-sol" which is "unsurpassed in its ability to loosen
barrels of syringes that have become stuck, as well as 'frozen' stopcocks
and ground glass joints."
Any experience with these? Anything better? Perferably, I'd like to use
something more elegent than a hammer.

--
Phil Henderson drp...@fast.net
------------------------------
It's not the Y2K bug that has me worried ... it's the Y2Kooks!

Eric Lucas

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Aug 19, 1999, 3:00:00 AM8/19/99
to
Heating with a heat gun might do it. It will both soften any grease on
the ground glass, and differentially heat (and thus expand) the female
part of the joint. If the stopper has either a pennyhead or a hex head,
a little persuasion applied with an adjustable wrench might help. Wrap
the head in electrical tape to cushion the points of contact, and apply
very gentle force to the wrench.

Eric Lucas

Uncle Al

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Aug 19, 1999, 3:00:00 AM8/19/99
to
Philip Henderson wrote:
>
> Prior to me wasting my time be trying something that won't work, are there any
> recommendations on loosening a "frozen" ground glass joint? While cleaning up
> my lab, I found an old sample contained within a glass 500 mL rb flask with
> a 24/40 stopper that won't budge. The small amount of sample inside is
> acidic, but fairly innocuous, not combustable, and not a peroxide former.
> The Chemist's Companion recommends a solution of 10 parts choloral hydrate,
> 5 parts glycerine, 5 parts water, and 3 parts conc. HCl. yummy.
> A quick google web search yielded one reasonable hit for a commercial
> detergent called "Haemo-sol" which is "unsurpassed in its ability to loosen
> barrels of syringes that have become stuck, as well as 'frozen' stopcocks
> and ground glass joints."
> Any experience with these? Anything better? Perferably, I'd like to use
> something more elegent than a hammer.

1) First shot is to cool the thing in the freezer overnight, then
take a propane torch and "warm" around the outside of the joint fast,
then PULL! (furnace gloves help).

2a) Second shot is to infiltrate 1% Dawn diswashing liquid in water
into the room temp joint. If you see dribble into the interface wet it
as much as you can, then ultrasonicate. Pull.

2b) Second shot is as (2a), but with WD-40 instead of the aqueous
detergent. Depends on personal aesthetics.

3) Decide which you want more, the stopper or the RB, then...

--
Uncle Al Schwartz
http://www.mazepath.com/uncleal/
http://www.ultra.net.au/~wisby/uncleal/
http://www.guyy.demon.co.uk/uncleal/
http://uncleal.within.net/
(Toxic URLs! Unsafe for children and most mammals)
"Quis custodiet ipsos custodes?" The Net!

Dr. Henry

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Aug 19, 1999, 3:00:00 AM8/19/99
to
Trying the Coke first is recommended in the Corning Guide to
Glassware. It is actually "soft drink" now, but in older versions
they really did recommend Coke. All the other recommendations
are worth trying after that. Soak it in Coke at least overnight. I once
had one that loosened after two days (and two refills).

--

Dr. Henry Boyter, Jr. Ph.D. Chemist

The opinions of Dr. Boyter are provided for informational
purposes only and should not be used as advice. No
warranty or expression of professionalism is implied.

***************


Philip Henderson wrote in message ...


Prior to me wasting my time be trying something that won't work, are there
any
recommendations on loosening a "frozen" ground glass joint? While cleaning
up
my lab, I found an old sample contained within a glass 500 mL rb flask with
a 24/40 stopper that won't budge. The small amount of sample inside is
acidic, but fairly innocuous, not combustable, and not a peroxide former.
The Chemist's Companion recommends a solution of 10 parts choloral hydrate,
5 parts glycerine, 5 parts water, and 3 parts conc. HCl. yummy.
A quick google web search yielded one reasonable hit for a commercial
detergent called "Haemo-sol" which is "unsurpassed in its ability to loosen
barrels of syringes that have become stuck, as well as 'frozen' stopcocks
and ground glass joints."
Any experience with these? Anything better? Perferably, I'd like to use
something more elegent than a hammer.

--

SNUMBER6

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Aug 20, 1999, 3:00:00 AM8/20/99
to
>From: drp...@fast.net (Philip Henderson)

>Prior to me wasting my time be trying something that won't work, are there
>any
>recommendations on loosening a "frozen" ground glass joint?

Years of experience, and attempts at all thoughts and ideas from forums much
larger than this one I have concluded that the following are the best methods
in fact the only methods that work ... the last is absolutely foolproof ...

1) Prayer - Which faith matters not but it must be fervent without any "damns"
in the prayer body no matter how hard it is ... Atheists can pray to God-Not
and agnostics to Maybe-God but prayer is necessary.
2) Voodoo - I know some consider this a prayer but the animal innards and the
blood and the feathers etc. are far beyond a mere prayer ... Of course after
hours of trying to loosen it ... you may look like a Zombie ... but that is not
enough ....
3) Soak in all the elements Air Earth Fire AND Water ... If you are trying to
find Phlogiston ...forget it your textbook is too old ...
4) The foolproof method ... accidentally let it fall from the sink to the
floor, the first bounce will loosen the stopper and it will gently fall off ...
the second bounce will shatter the flask though ...

In the Village ....
I am not a number ... I am a free man !!!!

Ron Michalak

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Aug 20, 1999, 3:00:00 AM8/20/99
to
1st attempt: heat gun
2nd attempt: propane torch
3rd attempt: waste glass receptacle
Philip Henderson <drp...@fast.net> wrote in message
news:drphil-1908...@maxtnt07-abe-157.fast.net...

> Prior to me wasting my time be trying something that won't work, are there
any

Trevor Calder

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Aug 20, 1999, 3:00:00 AM8/20/99
to

Philip Henderson wrote in message ...
>Prior to me wasting my time be trying something that won't work, are there
any
>recommendations on loosening a "frozen" ground glass joint?

I've used a couple of things in the past.

First, soak it in Coke. The idea is that as the liquid seeps into the joint,
the bubbles loosen the joint. It sounds good, and gives an excuse for buying
Coke on the lab budget.
Actually you can use any fizzy drink - I just like Coke.

If that doesn't do it, there is one method almost certain to work.
Try everything you can think of, and when that doesn't work give it to some
one else - but you have to be very careful and say these words:

"This joint is frozen solid - nothing will free it."

It'll be free in a couple of minutes.

Frank Martin

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Aug 20, 1999, 3:00:00 AM8/20/99
to
We used to use a very small flame in the centre of the stuck assembly while
applying a slight twist and a greater pull to each end. A bit of tapping
with a piece of hardwood before the above procedure can help too.
Depending on the nature of the muck entrapped, some solvent such as kerosine
will often work its way into the part and loosen it.
You might consider giving it to the local glassblower to fix.


Philip Henderson <drp...@fast.net> wrote in message
news:drphil-1908...@maxtnt07-abe-157.fast.net...

> Prior to me wasting my time be trying something that won't work, are there
any

Max

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Aug 20, 1999, 3:00:00 AM8/20/99
to
I've yet to see a frozen joint that won't budge with a
little "persuesive" use of a heat gun. The differential heating makes
the thing pop out rather easily.

M


In article <drphil-1908...@maxtnt07-abe-157.fast.net>,


Sent via Deja.com http://www.deja.com/
Share what you know. Learn what you don't.

mge...@rocketmail.com

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Aug 20, 1999, 3:00:00 AM8/20/99
to
We used to have a multi-clawed device called an "Easy Out". One set of
claws were fastened around the stopper and another, stationary, set held
the lip of the female standard taper. Once the contraption was
correctly positioned, a few turns of the screw to which the
stopper-holding claws was attached popped the stopper free.

It was a rather clunky looking apparatus and was the origin of the
unflattering phrase "she's got a face like a busted Easy Out."

frigger

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Aug 20, 1999, 3:00:00 AM8/20/99
to
On Thu, 19 Aug 1999 20:02:26 -0400, drp...@fast.net (Philip Henderson)
wrote:

>Prior to me wasting my time be trying something that won't work, are there any
>recommendations on loosening a "frozen" ground glass joint? While cleaning up
>my lab, I found an old sample contained within a glass 500 mL rb flask with
>a 24/40 stopper that won't budge. The small amount of sample inside is
>acidic, but fairly innocuous, not combustable, and not a peroxide former.
>The Chemist's Companion recommends a solution of 10 parts choloral hydrate,
>5 parts glycerine, 5 parts water, and 3 parts conc. HCl. yummy.
>A quick google web search yielded one reasonable hit for a commercial
>detergent called "Haemo-sol" which is "unsurpassed in its ability to loosen
>barrels of syringes that have become stuck, as well as 'frozen' stopcocks
>and ground glass joints."
>Any experience with these? Anything better? Perferably, I'd like to use
>something more elegent than a hammer.


If the flask contains a lot of volatile solvent which might make the
use of a heating gun dangerous, here is something you can try that
will sometimes work.

Put the flask in a shallow beaker or some other container and put it
in the sink. Set the faucet to drip and make sure the drip lands on
the female lip. Leave this for a few days. This works on the same
principal as Chinese water torture, each drop applies a small force
which over time can loosen the stopcock.

Michael Hinsberg

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Aug 20, 1999, 3:00:00 AM8/20/99
to
Uncle Al wrote:

>
> Philip Henderson wrote:
> >
> > Prior to me wasting my time be trying something that won't work, are there any
> > recommendations on loosening a "frozen" ground glass joint? While cleaning up
> > my lab, I found an old sample contained within a glass 500 mL rb flask with
> > a 24/40 stopper that won't budge. The small amount of sample inside is
> > acidic, but fairly innocuous, not combustable, and not a peroxide former.
> > The Chemist's Companion recommends a solution of 10 parts choloral hydrate,
> > 5 parts glycerine, 5 parts water, and 3 parts conc. HCl. yummy.
> > A quick google web search yielded one reasonable hit for a commercial
> > detergent called "Haemo-sol" which is "unsurpassed in its ability to loosen
> > barrels of syringes that have become stuck, as well as 'frozen' stopcocks
> > and ground glass joints."
> > Any experience with these? Anything better? Perferably, I'd like to use
> > something more elegent than a hammer.
>
> 1) First shot is to cool the thing in the freezer overnight, then
> take a propane torch and "warm" around the outside of the joint fast,
> then PULL! (furnace gloves help).
>
> 2a) Second shot is to infiltrate 1% Dawn diswashing liquid in water
> into the room temp joint. If you see dribble into the interface wet it
> as much as you can, then ultrasonicate. Pull.
>
> 2b) Second shot is as (2a), but with WD-40 instead of the aqueous
> detergent. Depends on personal aesthetics.
>
> 3) Decide which you want more, the stopper or the RB, then...
>
> --
> Uncle Al Schwartz
> http://www.mazepath.com/uncleal/
> http://www.ultra.net.au/~wisby/uncleal/
> http://www.guyy.demon.co.uk/uncleal/
> http://uncleal.within.net/
> (Toxic URLs! Unsafe for children and most mammals)
> "Quis custodiet ipsos custodes?" The Net!

Suspend the flask upside down in a sonic bath with the stopper suspended
above the bottom of the bath. Sometimes the stopper will fall out after
5 - 10 minutes of sonication.

--
Michael Hinsberg
Hinsbar Laboratories, Inc.
http://www.hinsbarlabs.com

Bill Walker

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Aug 20, 1999, 3:00:00 AM8/20/99
to
I'll use a solution of water/glycerin, perhaps with addition of a quat. to wet
the glass surface and draw the liquid into the joint and lubricate the glass
sufaces prior to extraction.
Heat before/after/during this process from a heat gun/burner/plasma torch can
sometime help.
Thick rubber gloves and a strong arm can pursuade it to give by visciously
ripping it out with a little twisting.
Try doing the old tie a string between the stopper and the door and slamming
it.... (I'm not exactly kidding here)
One thing I've had great success with is clamping the bottom part to a ring
stand, then fastening the jaws of a second clamp to the top part, pulling the
back part of the clamp up the ring stand so that it's at an angle, and then
tightening the screw so that the jaw part is drawn upwards as the screw is
tightened onto the ring stand. Sort of like a lever lifting the upper part out
of the joint.
Sonicators work well sometimes, as do the usual witches brew cocktails of cola,
phosphoric acid, dilute HF, detergents, surfactants, etc.

Luck and patient persistence are key factors.
I've been known to keep bits of stuck together stuff around for months to give an
occasion tug at, and sometimes after vigorously working at the problem the stuck
piece suddenly falls out almost by itself just as I'm about to abandon it
again... witchcraft, baby.

Sell your soul to Satan maybe?

How 'bout this:
Mail me your glassware, and I'll mail you the reactions I can't get to work...

Bill


Philip Henderson wrote:

> Prior to me wasting my time be trying something that won't work, are there any
> recommendations on loosening a "frozen" ground glass joint? While cleaning up
> my lab, I found an old sample contained within a glass 500 mL rb flask with
> a 24/40 stopper that won't budge. The small amount of sample inside is
> acidic, but fairly innocuous, not combustable, and not a peroxide former.
> The Chemist's Companion recommends a solution of 10 parts choloral hydrate,
> 5 parts glycerine, 5 parts water, and 3 parts conc. HCl. yummy.
> A quick google web search yielded one reasonable hit for a commercial
> detergent called "Haemo-sol" which is "unsurpassed in its ability to loosen
> barrels of syringes that have become stuck, as well as 'frozen' stopcocks
> and ground glass joints."
> Any experience with these? Anything better? Perferably, I'd like to use
> something more elegent than a hammer.
>

-log(on)

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Aug 20, 1999, 3:00:00 AM8/20/99
to

Trevor Calder <trevor...@THISiinet.net.au> wrote in message
news:7pi7tm$8sd$1...@inet-1.pnu.com...

>
> Philip Henderson wrote in message ...
> >Prior to me wasting my time be trying something that won't work, are
there
> any
> >recommendations on loosening a "frozen" ground glass joint?
>
> I've used a couple of things in the past.
>
> First, soak it in Coke. The idea is that as the liquid seeps into the
joint,
> the bubbles loosen the joint. It sounds good, and gives an excuse for
buying
> Coke on the lab budget.
> Actually you can use any fizzy drink - I just like Coke.
>
>
Agreed. Learned this trick in undergrad school. In addition, if it is a
stopper that is frozen, after soaking, gently tap the head of the stopper
with another similarly sized glass stopper. Never failed, never broken.
stan


Little Steve

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Aug 20, 1999, 3:00:00 AM8/20/99
to

I have some more less than sensible suggestions which still work
though...

1>We heat with a heat gun or blow torch, maybe try keeping the stooper
head cold while doing this then it shrinks whil the neck widens.
However I usually take a hammer, yes a hammer, and use the handel, the
wooden bit, to make taps on the stopper. I usually tap it not directly
on bu sweeping the hammer up the flask in an attempt to knock the
stopper out. Usually works and does not break the flask.

2>Do no try if you have nasty things like 400ml TFA and such in the
flask. heat. Yep heat the flask, even in an isomantle. Maybe even go
as far as refluxing the thing. Watch the pressure build, watch the
stopper fly. Suggest something to catch the stopper though <g> If the
entire flask explodes then at least you can rest assured the stopper
would not have come out anyway as the pressure will take the easiest
way out.

3>One glass cutter. One piece of wood. Score edge, snap off neck.

4>Table. Smash neck off table. Or if you think you can waste the flask
and recover the product, a stirrer rod through the bottom of the flask
is always a good move.

5>Dont do this but im including it just cos it amused me. Another girl
at work saw me doing the sweeping hammer action, which has worked
every single time for me, and thought she'd do it for a stuck stopper.
Except she did not notice I was using the soft wooden handle and
sweeping up into the stopper. You should have seen her face when she
took the metal pole from a clamp stand and hit straight at the
stopper, removeing the upper 3/4 of the flask in the process.

heat gun almost always works. heat gun plus some gentle tapping always
works. Smashing stuff is a last resort and one not to allow the bosses
to see.

Little Steve

Daniel E. Macks

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Aug 20, 1999, 3:00:00 AM8/20/99
to
Eric Lucas <eal...@worldnet.att.net> said:
: Heating with a heat gun might do it. It will both soften any grease on

: the ground glass, and differentially heat (and thus expand) the female
: part of the joint. If the stopper has either a pennyhead or a hex head,
: a little persuasion applied with an adjustable wrench might help. Wrap
: the head in electrical tape to cushion the points of contact, and apply
: very gentle force to the wrench.

Or if the stopper is hollow and you're willing to sacrifice it but not
the stuff in the flask, score and break off the top bulb, then punch
through the lower surface with a nail or wide-bore needle. The rest of
the stopper can then be chiseled out of the joint. With a septum over
the top before breaking into the flask itself, the contents won't
escape or contact air/chemist/etc. Like when I discovered a stuck-shut
flask of a bunch of Tf2O left in my fridge by the previous lab
occupant.

dan
--
Daniel Macks
dma...@a.chem.upenn.edu
dma...@netspace.org
http://www.netspace.org/~dmacks


Phil Henderson

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Aug 20, 1999, 3:00:00 AM8/20/99
to
Thanks to all who took the time to post. I loosened the frozen glass
stopper today by using a combination of ideas from the posts. I had tried
a heat gun without any luck prior to posting to the group. I don't have a
torch available and wanted to avoid the ideas that used chemicals (not
that i'm chemophobic, but I was *cleaning up* the lab afterall)

Today I put the flask in the freezer for an hour (thanks, Al), then
blasted the flask neck with a heat gun, and finally used a 3/4" wrench on
the stopper which indeed had a penney head (thanks, Eric) to gain a bit of
leverage.

I had no doubt that there would be a good number of varied responses to
this post. Thanks again.

Rodger Whitlock

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Aug 20, 1999, 3:00:00 AM8/20/99
to
[snippage not noted]

Uncle Al <uncl...@hate.spam.net> wrote:
>Philip Henderson wrote:
>>
>> ...are there any recommendations on loosening a "frozen" ground glass >> joint?

> 2a) Second shot is to infiltrate 1% Dawn diswashing liquid

> 2b) Second shot is as (2a), but with WD-40 instead of the aqueous


>detergent. Depends on personal aesthetics.

To which I will add, based on experience from the halcyon days of youth:

2c) A few drops of glycerin on the joint, then wait a week or two for it
to infiltrate.


Allan Adler

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Aug 21, 1999, 3:00:00 AM8/21/99
to

I've been following this thread for a while and, before I offer the
crackpot idea that just occurred to me, let me admit that I don't
know beans about this problem. Here is the crackpot idea: when you
have a glass with some water in it and wet your finger and run it
around the rim, you make the glass vibrate at a certain frequency.
The frequency depends on the height of the water, so it must really
be the air column, I guess, but I'm sure the glass vibrates too.
So the crackpot idea is to take the bottle, wet your finger and
rub your finger around the edge trying to induce vibrations that
will cause the stopcock to realign itself, then try to pull it out.

This crackpot idea has been brought to you courtesy of

Allan Adler
a...@altdorf.ai.mit.edu

****************************************************************************
* *
* Disclaimer: I am a guest and *not* a member of the MIT Artificial *
* Intelligence Lab. My actions and comments do not reflect *
* in any way on MIT. Morever, I am nowhere near the Boston *
* metropolitan area. *
* *
****************************************************************************

Ziwcam

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Aug 22, 1999, 3:00:00 AM8/22/99
to
I was almost hoping you wouldn't be able to open your flask for a while, just
so that I could continue to read the myriad of strange yet seemingly useful
ideas that were coming out of this group. But I'm glad your problem is solved.
:-)
-Ziwcam

CLee751159

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Sep 6, 1999, 3:00:00 AM9/6/99
to
One method I didn't see is to tap the stopper against the side of an
old-fashioned ceramic or pottery lab sink - one that has a nice ring to it.

Regards


>Prior to me wasting my time be trying something that won't work, are there

David Elliott

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Sep 7, 1999, 3:00:00 AM9/7/99
to
I've had some success removing ground glass stoppers using an ultrasonic
bath. I suspend the flask so the ground glass joint is immersed upside down
in soapy water. I turn the bath on and wait. Capillary action allows the
water to
wick its way between the ground glass surfaces, while cavitation from the
ultrasonic
bath, (in conjunction with gravity) usually does the trick, allowing the
stopper to fall out.
Good Luck!

CLee751159 wrote in message
<19990906154620...@ng-fj1.aol.com>...

dewit...@gmail.com

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Jan 11, 2019, 2:23:29 PM1/11/19
to
Don't forget rotation is optimal for removal. As such superglue can be your friend with a taper with preapplied superglue to mount the i.d. of the stopper-joint- which might be accessible either sacrificial or otherwise (scoring with a dremel diamond disk if possible). Taper insert can be anything around. The taper is your rotational handle obviously. Heating and cooling are risky but in the most simple of situations.
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