Measurements for Process Control

In 2020 engineers and plant chemists choose from a range of "composition transmitters" that
cover many typical critical measurement needs, leading to substantial improvements in yield,
quality, and cost. This is especially true for applications that are common across the chemical
process industry and that involve single-phase gas or liquid samples. For more complex and/or
multiphase samples, step changes in performance/cost will have made use of analyzer systems
routine across the industry. The increased density of process information resulting from broad
use of analyzers has enabled and stimulated many new process control schemes.
A "composition transmitter" is a device that measures the concentration of an analyte in a process
stream with comparable cost, robustness, and ease of use with current temperature, pressure,
level, and flow transmitters.

1. Developing the Vision

A group of chemists and engineers from industry, academia, and government labs was
challenged with this vision as a part of an NSF/NIST/ATP sponsored workshop on Process
Measurement and Control: Industry Needs held in New Orleans on March 6-8, 1998. Four
potential routes to meet this challenge were identified, and served as the focal points for the
measurement work groups. The reports from the working groups can be found at:
http://fourier.che.udel.edu/~doyle/V2020/Index.html
The views reflected in these more detailed reports have been synthesized to provide a
common view of the major challenges, research objectives, and structural issues that must be
dealt with to achieve the vision.

2. Summary Recommendations
Implement an integrated funding mechanism aimed at invention and development of
integrated sensor and/or micro-fabricated instrument technology and systems that move
toward the "composition transmitter" goal.
Strengthen chemical industry - university - government lab partnerships that are focused on
developing new process analytical chemistry technology.
Develop improved curricula and training for new chemists and engineers and better
continuing education for current employees in the area of process analytical chemistry.
Integrate the vendor community into the effort to define the path to meet critical industry
needs for process analytical technology.
Raise visibility of process analytical chemistry and chemometrics to the academic, industrial
and government lab technical and management communities.
Drive standardization of chemometrics and other key elements of process analytical
chemistry.

3. Critical Needs and Challenges

3.1 Move laboratory detection limits to process analyzers.
Non-routine analytical techniques currently performed in central laboratories represent
the limits of our quantitative knowledge of the process. This information is obtained by
manual sampling, extensive use of highly paid professionals, capital intensive
instruments, and time intensive analytical methods. As these techniques are applied, we
learn more about what is critical for optimization of process operation. For instance, these
techniques are used to provide quantitative and qualitative information on catalyst
poisons. Once a poison is identified, a process measurement is needed to provide input
for the control of the catalyst activity. This requires greater sensitivity and precision in
process analyzers than is available today. In this example and others, extension of current
laboratory capabilities to process analyzers is required to meet constantly more
demanding control objectives. It will also increase substantially the degree of process
understanding that can be obtained by enabling much more detailed characterization of
process dynamics.
3.2 Implement multidimensional analyzers in process applications.
A key strategy used in laboratory instrumentation to increase the amount of information
in a single sample is to run to apply multidimensional or hyphenated techniques (e.g.
GC/MS). This approach can be used in plant laboratories today, but commercial process
analyzers using this approach are not robust enough for widespread use.
3.3 Develop improved sensor based systems for process applications.
In a first order sensor, a small amount of a sensor material is placed on a probe that has a
relatively straightforward read out of the interaction of the material with the analyte. This
concept is attractive, and fits well into the model of the composition transmitter. For
sensors to be broadly useful in process situations, they must be selective for the analyte or
analytes of interest, sensitive, stable over time, and reversible on a time scale faster than
the process dynamics. For the bulk of applications in the chemical industry, the needed
selectivity, sensitivity, stability, and reversibility have not been demonstrated.
3.4 Develop integrated micro-fabricated instrument systems for process
applications.
Micro-fabrication technologies have opened a range of new possibilities for analytical
equipment. The challenge over the next decade is to identify the most promising
approaches and applications, and to identify and apply the resources needed to achieve
the objectives. The revolution that will follow application of these technologies to
analytical chemistry could well provide the critical piece needed for development of a
composition transmitter.
3.5 Provide critical information for control of processes involving complex samples
such as solids, slurries, and other multiphase samples.
Current process analyzer technology often offers multiple choices for compositional
analysis of single-phase gas and liquid samples. However, many chemical processes
involve streams that are not so easy to handle. Current technology does not offer a broad
range of approaches for solids, slurries or other multiphase samples.

3.6 Provide critical information for control of polymer processes.

A large part of the chemical industry involves production of polymer or processing
polymers into formulations or shapes. The product properties that are obtained depend in
detail on the structure and composition of the polymer. Currently full description of the
structure and composition is difficult and time consuming in the laboratory. Since this
information is so difficult to obtain, polymer processes are now controlled using
primarily empirical correlations. In addition, industry standard quality indices are based
on old technology, and dont reflect either polymer structure or customer needs. Today,
laboratory methods are available that can provide a detailed description of the polymer
structure, which can then be used to develop structure/property relationships for the
system. However, these techniques are complex, difficult, and time consuming enough
that this is not always done. Even when these structure/property relationships have been
determined, and potential control measurements identified, technology to reliably
perform these measurements in a process environment is often not commercially
available.
3.7 Provide needed measurements for control of processes based on new process
technology, such as the use of biotech based processes for production of specialty or
commodity chemicals.
The chemical industry is constantly searching for new approaches to production of
products. For example, many chemical companies are exploring catalytic processes based
on enzyme catalysts and fermentation based production of chemicals. These new
processes will raise new challenges in the laboratory and especially in measurements for
process control.
3.8 Reduce resistance to implementation of analyzer systems by plant operating
personnel.
Engineers and operators at chemical plants have a jaundiced view of analyzers. Instead of
recognizing the potential value that the additional information might bring, they often
become concerned with the potential problems that come with analyzers. As chemical
companies deal with competitive pressures by reducing the number of engineers,
mechanics, and operators at typical plants, systems like analyzers that can add
substantially to maintenance loads are looked at with increasing suspicion. Current
analyzer systems often involve complicated application specific sample systems that are
known to be reliability issues and sophisticated instrumentation that requires specialized
training for effective maintenance and support.
3.9 Develop partnerships between instrument vendors and the chemical industry
that enable vendors to see how they can make money in providing improved
products to the industry.
Chemical companies often identify new needs for process measurement and get little
response from vendors. Most of the vendors serving the analyzer and analyzer systems
market are relatively small companies that cannot afford large development investments
without assurances of a market. At the same time, chemical companies find it difficult to
share information about process technology that would allow definition of common
problems with larger market potential. Even some relatively common applications in the
chemical industry might not have the market size required to justify development of a

sensor or analyzer system.

3.10 Optimize placement of sensors and analyzers to provide greatest leverage on
the control of the process.
What an analyzer measures, how well it measures it, where it measures it, and how it is
used by the control system all have an effect on the overall effectiveness of the control
system. Today, intuition, empirical knowledge, or accident has the strongest impact on
determining these factors. Improved communication and understanding between
analytical chemists and engineers could impact this, as well as the development of
appropriate modeling technology.
3.11 Extract the maximum amount of information from the measurement system,
and turning that information to process knowledge and process control actions.
Measurement systems comprising analyzers and temperature, pressure, level and flow
sensors produce a large amount of data. Today we often only use the most obvious data as
information (e.g. specific compositions, pressures or temperatures). If the data for a unit
operation, or perhaps an entire process were looked at as a whole, much more
information about the process might be able to be extracted and turned into knowledge.
3.12 Improve academic standing of chemometrics and process analytical chemistry.
Despite broad interest in the chemical industry, academic attention to the problems of
process analytical chemistry seems to be focused only at a few centers. Academic funding
comes primarily from industry, and focuses on applications. This is especially serious in
the area of chemometrics, where there is little government based funding for data
handling/chemometrics. One result of this funding pattern is an alarming shortage of
academic chemometricians in the U.S. who are needed to train the future implementers
needed by industry. Although chemometric methods have been well proven in selected
academic and industrial research environments, they often suffer from a lack of
acceptance within Chemistry, Chemical Engineering, and Statistics disciplines. This is
very unfortunate, because these areas stand to contribute much to the further development
and implementation of the technology. This situation could be, in part, due to the
relatively limited mathematics and statistics backgrounds of physical scientists.
3.13 Improve the sustainability of chemometrics based analyzers.
The number of successful applications of chemometrics based analyzer systems is limited
by the effort required to sustain and support the application. There are several vendors
that offer packages for calibration and modeling, but the "tools" that are offered for
method implementation, validation, maintenance and diagnostics are very limited. This
has often meant that the user has been required to develop specialty software to properly
and safely implement the technology. When vendors are probed about this, they maintain
that the size of the chemometrics market is somewhat limited and very diversified. This
results in the reluctance of software vendors to develop technology at a price acceptable
to the users.
3.14 Develop improved training on use of process analyzers for all levels of chemists
and engineers.
Analytical chemists and engineers leave school with little common understanding of how
each discipline impacts the other in a chemical plant. Analytical chemistry curricula tend

to emphasize the role of analytical chemists in research support and in development of

new laboratory methods and instruments, while chemical engineering curricula focuses
on use of regulatory measurements (T, P, L, and F) to control systems. The current
challenge is to find ways to operate plants more effectively, requiring engineers and
chemists to work together to understand the process, and to develop and implement
strategies to improve the control. Changes need to be made to both curricula to prepare
new employees to understand the problem more fully and to work together to develop the
improved measurement and control systems. This needs to happen at the undergraduate
and graduate level, and needs to be extended into continuing education programs for
current employees at chemical plants.

4. Research Investments Required to Meet Critical Needs

The time frame, short-term [S], medium term [M] or long term [L] characterizes items in
this list. The urgency of the need and the time necessary to develop and implement
solutions are both considered in the time frame assignment.
4.1 Develop analyzers that move current laboratory capabilities to the process, but
are robust and easy to maintain and support. [S]
Improved analyzers based on molecular spectroscopy.
Faster analyzers based on separations technology.
Analyzers based on use of multidimensional analytical techniques now
used in the laboratory (e.g. GC/MS).
Analyzers based on technology not currently broadly used in the
laboratory (e.g. microwave, acoustics, dielectric relaxation).
4.2 Develop analyzers for complex systems such as mixed solids, polymers, and
multiphase samples. [M]
Technology for characterization of polymers (MW, MWD, branching, etc.)
that is amenable to process analyzers for support of control systems.
Improved structure/property/processing modeling capability, especially for
macromolecular products.
Improved technology for physical and chemical characterization of solids
and slurries.
Sensor concepts that are effective for multiphase systems and solids.
4.3 Develop new approaches to sampling and sample interfaces: [M]
Assure representative samples regardless of sample size.
Reliable degassing and de-bubbling of liquid samples.
Sample conditioning by various techniques (membranes, distillation, etc.).

4.4 Develop needed technology for on-line characterization of new processes used in
the chemical industry, such as biotech based processes. [M]
Process implementation of equivalents to electrophoresis, immunoassay,
and other biological activity sensors
4.5 Develop technology that improves the effectiveness of the measurement system
in implementing the control strategy. [M]
Modeling that enables optimum selection of sampling points and
measurement objectives.
Modeling that extracts maximum information from the ensemble of sensor
systems ("sensor fusion").
Modeling that predicts product properties.
4.6 Develop improved application tools for implementation and support of
multivariate calibrations. [M]
Modular, hierarchical, user-friendly application software interface.
Expert system to guide user through the process
Easier calibration methods
Calibration transfer from the laboratory to plant, and from plant to plant
Improved calibration diagnostics, maintenance, and calibration
maintenance tools.
"Smart" analyzer/sensor systems that have low maintenance requirements
and are self-calibrating and self-diagnostic
4.7 Develop systematic approach for development of new sensor materials. [L]
Fundamental understanding of how sensor material structure affects
selectivity, stability, reversibility, and sensitivity
4.8 Enable the design of micro-fabricated instrumentation systems that address
critical needs in process measurement for modeling and control. [L]
Identification of appropriate application that benefits from microfabricated instrumentation.
Non-fouling micro-sampling systems that yield representative samples
Electronic communication (data and instrument control)
Impact of micro-instrumentation on process modeling, optimization, and
diagnoses

Establish reliability
Micro-scale sensing-control-actuation systems
4.9 Develop low cost approaches to development, manufacture and support of
sensors and micro-fabricated instrumentation systems at appropriate volume levels.
[L]
Modular sensor or micro-fabricated instrument systems.
Modular software for communication, instrument control, and data
reduction.
4.10 Extend theory and develop improved approaches to chemometrics. [L]
Develop more "interactive" algorithms that incorporate prior knowledge in
modeling.
Develop theory of higher order methods.
Develop the theory behind PLS.
Investigate non-stationary, non-linear modeling techniques.

5. How to Get There

5.1 Implement an integrated funding mechanism aimed at invention and
development of integrated sensor and/or micro-fabricated instrument technology
and systems that move toward the "composition transmitter" goal.
An integrated government based funding system that supports both research on all critical
elements of technology needed to meet the goal and all phases of development is needed
if we are to meet the critical needs listed above. The program needs to provide a
mechanism that encourages key participants (National Laboratories, academia, vendors,
and industrial practitioners) to work together, each doing the part that fits their
capabilities best. Research facilities are needed to address problems which may not be
dissertation level material, but are badly needed by industry (e.g., sampling systems).
5.2 Strengthen chemical industry - university - government lab partnerships that
are focused on developing new process analytical chemistry technology.
Provide substantially increased federal funding for centers and projects that involve
partnerships between chemical companies, universities, and government labs. Provide
support for faculty visits and sabbaticals at industrial sites, particularly for analytical
chemistry faculty, and support for chemists in industry to visit universities for extended
periods of time. Encourage industry co-ops for undergraduate and graduate chemistry
students.
5.3 Provide improved preparation for new chemists and engineers, and better
continuing education for current employees in the area of process analytical
chemistry.
Assemble an industry group to define a skill-based definition of expectations of chemists

and engineers at all levels. Use this definition to stimulate funding of curriculum
development by government agencies and universities. Implement improved curricula in
undergraduate, graduate, and continuing education programs.

5.4 Integrate the vendor community into the effort to define the path to meet critical
industry needs for process analytical technology.
Hold Vision 2020 Workshop on Process Measurements aimed at involving and getting
input from the vendor community. Define the components and the interfaces between
academia, industrial users, and vendors. Work with the vendors to identify additional
markets inside and outside of the traditional chemical industry for process analyzers and
chemometrics software. Encourage vendors to develop hardware and software that is
modular and architecturally open in nature. Encourage vendors of process analyzers and
chemometrics software to continue the developments and improvements of their
application interfaces that were evident at the PITTCON 98 exposition.
5.5 Raise visibility of process analytical chemistry and chemometrics to the
academic, industrial and government lab technical and management communities.
Hold workshops and symposia at appropriate venues, particularly at larger national
meetings. Benchmark chemometrics and process analytical chemistry capabilities at
major European and Asian chemical companies. Promote importance of process
analytical chemistry to industry technical and business management.
5.6 Drive standardization of chemometrics and other key elements of process
analytical chemistry.
Support efforts by ASTM Subcommittee E-13.11 on Chemometrics to define and drive
standardization of chemometrics technology, especially in the form of standard reference
data sets and standardized methods and algorithms.
Challenge problems, such as NISTs ANOVA Challenge Problem, need to be designed to
rigorously evaluate new and existing chemometric algorithms. Such challenge problems
should be formulated such that they "push" the abilities of the techniques, define the
limitations of the techniques, and provide a standard comparison between different
techniques.