Essentially, the experiment consists
of a small amount of sample material being placed on a platinum filament
which is then inserted into an IR cell. The cell can be evacuated and filled
with gas at a pressure of choice. The filament is then heated to
a desired temperature causing flash pyrolysis of the material.
While the sample is being heated and is decomposing, the decomposition
products are detected by the rapid-scan FTIR spectrometer. These
products give not only decomposition mechanism information, but sometimes
kinetic data. This provides information which has been traditionally
elusive; namely, the initial products of decomposition of fast burning
and energetic materials such as rocket propellant ingredients and explosives.
Application of T-Jump Experiment:
In the field
of combustion, the chemistry in the thin zone at a burning surface has
long defied experimental description because a complex heterophase, nonequilibrium
reaction network exists over a very short short length and a steep temperature
gradient. We develop new techniques to stimulate the burning surface
of solid materials, and outline the reaction networks for the first time.
Various methods are used for fast, controlled heating of small amounts
of material coupled with real-time detection of the chemistry by rapid-scan
FTIR spectroscopy. The choice of materials is based on the practical
importance of the decomposition mechanisms and products. They include
polymers, gas generators, explosives, and rocket propellants.
Projects within the group are tailored to each student's interest in technique
design, synthesis of model compounds, fast decomposition studies, and data
analysis techniques.
A special IR cell (as shown below)
must be employed in order to perform the T-jump experiment in an oxygen
free environment at a desired pressure. The "Brill Cell", as it has
come to be called, satisfies these requirements. It is essentially
an aluminum pressure cylinder (A) with IR transparent windows (Zinc Selenide)
on either end. Phenolic curtains (B) are used to maintain an
IR transparent gas purge between the windows and the cell compartment sides
of the IR spectrometer (in this case a Nicolet Model 800 bench, C).
Three ports are fitted to the cell. One port (D) serves as both the
control gas inlet and the pressure gauge (E) port. Another serves
as a gas bleed-off (F). The last is the inlet into which the probe
containing the fillament and sample is inserted (G). The stage onto
which the cell is placed is designed to direct the beam path directly above
the probe's filament.
The pyroprobes
we use (as shown below) are made by CDS Analytical (. They are essentially
a coaxial bar (H) with the inside conductor and insulation recesed about
2 inches and a "top" and "bottom" window cut from the outside conductor.
This allows a Platinum filament (I) to be attached to the inside conductor
on one end and the outside conductor at the tip, thus closing the circut.
The other end contains leads (J) which are connected to the power source
inside an insulating handle. The probe is fitted with a gas sealing
ferrul (K) which makes the pressure seal with the probe port in the Brill
Cell and a nut (L) used to tighten the probe into place. A plastic
fitting (M) further to the rear of the probe holds the probe tightly in
the abovementioned handle and prevents it from turning freely.
Before the experiment a very small amount of material is placed on the
filament. The probe is then carefully inserted into the Brill
Cell and the experiment conducted.