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Figure 7 (ALL FIGURES ARE COURTESY OF THE AUTHORS.)
Single sensor or sensor array? Single dielectric spectroscopy sensors can yield a large amount of information about a particular sample. However, in some
cases it is important to sense multiple analytes simultaneously. An array can be constructed in which each sensor has a different
functional material placed on its surface (see Figure 7). Each functional material is chosen based on known properties of
sensitivity or selectivity. Dielectric sensors have been fabricated to sense many volatiles, dissolved chemicals, and solids
in a heterogeneous medium. Analytes studied using dielectric sensors include toluene and ethanol (38), n-octanes, 1-proponal,
ethylacetate, n-hexanes (39), a wide variety of toxic chemical warfare and industrial agents ranging from nerve agents to
rocket fuel and many volatile organic compounds (40), and varying polarity hydrocarbons, aromatics, polar volatile organic
compounds (41). This wide variety of chemical sensing capabilities is accomplished by using an equally varied number of polymer
bases above the dielectric sensor electrodes. When constructing an array of chemically sensitive dielectric sensors, the electric
field excitation frequency also can be tuned to target a dielectric relaxation process that is unique to a specific analyte.
In the process of designing a new sensor that can detect a specific analyte, one method to choose which polymer substrate
to use is to determine the chemical solubility of the analyte in the polymer (42). A wide variety of chemicals and solvents
can be sensed once the solubility of each analyte is known. Dielectric sensors can be quickly designed by simply studying
the solubility of each analyte of interest into each polymer matrix that is used. By using other tuning parameters of dielectric
sensors (e.g., the the electric field excitation frequency) and the electrode geometry, dielectric sensors can be designed
for both selectivity and sensitivity to many analytes of interest on a single substrate.
Real-time or not? Real-time measurements in a process may be required if the result of those measurements are used to control another step in
that process in a time-sensitive manner. Depending on how quickly events occur within the process, measurements may need to
be taken very quickly and coarsely or more slowly and rigorously. For example, if moisture must be known before entering a
drying cycle, real-time operation implies that the measurement is performed before the material enters the drying cycle. Continuous
measurements imply real-time measurements when each measurement must be performed at a sufficient rate so that information
about the process is not lost. While dielectric relaxation processes can vary widely from many seconds to less than a nanosecond,
faster relaxation processes are typically used to achieve real-time operation in a process.
Conclusion
Dielectric spectroscopy is a promising technology that has found uses in many fields and is now being realized as a useful
tool for the pharmaceutical industry. This paper discusses a number of versatile adaptations made possible by advances in
electrode materials, fabrication techniques, and measurement systems. Presently, dielectric spectroscopy offers process analysts
a wide variety of options, much like an advanced tool, where parameters can be tweaked as desired to implement a "tailor-made"
process control solution. For instance, the measurement frequency can be changed to optimize measurements for slow bulk process
or for fast intermolecular interactions. Similarly, changing the structural properties of electrodes such as coating of sensor
heads can result in improved sensitivity to a particular analyte, or, changing the physical spacing between electrodes can
selectively measure specific regions in a sample. Dielectric measurements can be made in a noncontact, nondestructive mode;
therefore, measurement instrumentation is relatively easy to integrate at different stages of the process. Measurement time
issues not withstanding, a process engineer could chose to obtain data at an early stage of the process and implement a feed-forward
control system with the same ease as more conventional feedback-based control. Further, for industrial dielectric measurements,
the frequency range is generally below 100 MHz; therefore, instrumentation required for such measurements is relatively inexpensive
and does not have signal integrity issues associated with high frequency instrumentation. Dielectric spectroscopy has been
widely investigated for measurement of pharmaceutical properties; however, majority of the work has been focused on establishing
the feasibility of this technology at a laboratory level. Further work, more inline with the PAT initiative, will focus on
identifying specific process needs and customizing sensor designs and circuitry.
A. Mathur is a graduate student at the Sensors, Energy, and Automation Laboratory, Department of Electrical Engineering, University of Washington, Seattle.
Articles by A. Mathur
K. Sundara-Rajan is a PhD candidate at the Sensors, Energy, and Automation Laboratory, Department of Electrical Engineering, University of Washington, Seattle, tel. 206.351.8101.
Articles by K. Sundara-Rajan
G. Rowe
G. Rowe is a PhD candidate at the Sensors, Energy, and Automation Laboratory, Department of Electrical Engineering, University of Washington, Seattle
Articles by G. Rowe
A. V. Mamishev
A. V. Mamishev is an associate professor at the Sensors, Energy, and Automation Laboratory, Department of Electrical Engineering, University of Washington, Seattle.
Articles by A. V. Mamishev
Survey
How does your company apply quality-by-design (QbD) principles to manufacturing processes?
To all processes for both new and legacy products
19%
To all process for new products only
14%
To select process for new products only
24%
To select processes for both new and legacy products