Date: Tue, 5 Jan 2010 14:10:24 -0500
Reply-To: DCHAS-L Discussion List <DCHAS-L**At_Symbol_Here**LIST.UVM.EDU>
Sender: DCHAS-L Discussion List <DCHAS-L**At_Symbol_Here**LIST.UVM.EDU>
From: ILPI <info**At_Symbol_Here**ILPI.COM>
Subject: Re: Unknown Hazardous Chemical
In-Reply-To: <2317fc9b1001051051x60e6949awa8d296232181e682**At_Symbol_Here**>

For chlorinated materials, the isotope pattern is key.  Is it possible for you to post the spectra somewhere so we can see it?  If you don't have any way of doing that yourself, you can email them to me and I'll post them in a temporary directory where others on the list can look at them.

Rob Toreki

On Jan 5, 2010, at 1:51 PM, Andrew Gross wrote:

First off I would like to thank everyone for their time and thoughts
to our mystery, which as of now remains a mysery.

We ran GC and it is not in our library.  I'm hoping someone might be
able to help with some new information.

ion 91 is the strongest peak
ion 61 is apx 75% of ion 91
ion 45 is apx 50% of ion 61.

the peaks were very light so we are extending run time to see if we
can generate more peaks.

we ran ph on all samples.  5 of the 7 are ph 12, 2 of the samples are
ph 7.  The two that are ph 7 are obviously the most concentrated based
on the odor that rushes at you when you open the jar.

Thanks for your continued help,

Andrew Gross

On Mon, Jan 4, 2010 at 11:41 AM, Clark, Richard C <rcclark**At_Symbol_Here**> wrote:
Just got back to work this morning after a week's vacation and read the
postings related to this problem.

The chlordane speculation merits comment.  I was the works chemist for
Velsicol at Marshall, IL just before the plant closed in the late 70's.
That was the only site in the world that manufactured chlordane; Velsicol
also manufactured hexachlor at another site (Tennessee, I think).  Chlordane
is a polychlorinated dicyclopentadiene and had lots of by-products;
hexachlor was hexachlorocyclopentadiene made by a different process and was
much purer.  Chlordane was so heavy that it could only be shipped in 30-gal.
drums.  It was diluted by reformulators with kerosene (5-10% chlordane, I
think).  The kerosene-chlordane mixture could be dispersed in water with the
aid of detergent to make an emulsion for field spraying and termite
treatment.  With the closure of the Marshall, IL plant, acquisition of
Velsicol by Great Lakes Chemical (now part of Chemtura), and environmental
issues, chlordane manufacture was never re-started.  This might explain the
age of the drums.

Chlordane is an impure mixture containing numerous chlorination byproducts
of cyclopentadiene and dicyclopentadiene.  The EPA published a GC-MS study
of it ca. 1976 in Analytical Chemistry which revealed dozens of compounds..
Velsicol had no idea of that complexity; we were using packed column GC
technology for process control.  I'm not sure that GC-MS will be useful for
identification given the mixture of kerosene and chlordane. That would be an
identification nightmare.

Chlordane yellows with age.  The green flame is from the Bielstein test for
chlorine.  The emulsion of the kerosene mixture is cloudy-white.  While the
initial boiling point may be 27=B0C, the boiling point may rise quickly above
100=B0C.  An ASTM distillation will give some idea of that.  Infrared
spectroscopy of the distillation fractions (10% volume cuts) should show a
mixture of saturated hydrocarbons and chlorination of saturated and
unsaturated hydrocarbons.  I'll be surprised if you can take the
distillation to a dry point before the flask contents start to smoke;
chlordane will likely break down before it distills.  If the low boiling
components are chlorinated by-products, they won't flash.

Hope this helps (and my memory isn't too inaccurate).

Rick Clark
Sr. Research Chemist
Curwood, Inc.

From: DCHAS-L Discussion List [mailto:DCHAS-L**At_Symbol_Here**] On Behalf Of
List Moderator
Sent: Monday, December 28, 2009 11:38 AM
To: DCHAS-L**At_Symbol_Here**LIST.UVM.EDU
Subject: Re: [DCHAS-L] Unknown Hazardous Chemical

From: Andrew Gross <gross.drew**At_Symbol_Here**>
Date: December 28, 2009 12:02:48 PM EST
Subject: Re: [DCHAS-L] Unknown Hazardous Chemical

Hi Everyone,
My lab recieved a sample from a power plant that they do not know what
it is and wish to have it identified.  I am trying to ID it because
until I have a better idea it is on hold for all testing (read on to
find out why).  I'm hoping for some thoughts.
Sample is liquid in appearance, but lighter then di-chloromethane.  I
think it is actually an oil of some kind.  It is transparant yellow
and some say it smells like kerosene.
It forms a white emulsion when mixed with water.
There is no flash point.  On closed cup method it flames out below
25C.  It does not ignite when exposed to direct flame.  However it
boils around 27C.
Exposed flame turns green (like copper flame), vapors also turn flame green.
When dried, it turns to a waxy white translucent crystal.  My closed
cup flame is still green meaning it is contaminated by the vapors.
Vapors in small quanteties (under hood) cause nausea, light headedness
and confusion.
pH is 6ish (litmus paper) although client claims it to be caustic.
All PCB analysis came up negative.
The exposure effects are why all tests are on hold till we have a
better idea as to what were dealing with as well as the remaining
tests for my department involve reacting with acid and pumping
nitrogen through it.
Thoughts, ideas, experiences?  Client has 5 unidentified drums of this
stuff and has no idea what it is.  We need to identify but I am not
going to put anyone in danger until I know more about it.
Andrew Gross

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