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5
Process Measurements Division
SUMMARY
The Process Measurements Division’s (PMD’s) mission of disseminating national
measurement standards for thermodynamic parameters and conducting relevant measurement
science research fits well with national priorities and NIST focus areas. The PMD provides
essential calibration services in fundamental parameters that support many sectors of the U.S.
economy as well as facilitating international commerce. It conducts research that is directly
aligned with NIST and national priorities. The PMD’s research includes projects that support
the Department of Homeland Security (microsensor chemical detectors), the climate-change
research community (spectroscopy and gas properties), the biopharmaceutical industry (gold
nanoparticle reference materials), and developers of the hydrogen economy (hydrogen gas
data and flow-rate calibrations and standards). In those areas for which the PMD maintains
U.S. national standards and provides measurement services, it is preeminent among national
metrology institutes; the division is an important national resource. The overall mood of the
PMD staff appears to be positive, with researchers dedicated to maintaining and enhancing
the international stature of the division.
RESPONSE TO RECOMMENDATIONS FROM THE PREVIOUS REPORT
The panel’s 2007 report1 contained nine specific recommendations for the Chemical
Science and Technology Laboratory. Those recommendations are reprinted below; each is
followed by the panel’s current assessment of the PMD’s response to the recommendation.
1. The set of criteria known as 5+1 for ensuring that the research projects are
aligned with the mission of NIST and the laboratory should continue to be used.
The CSTL leadership should link its more basic research investments to the
potentially important measurement-related outcomes that are envisioned to result
from CSTL research.
The PMD recognizes the need to spend more effort on this issue. The
plasma processing project is a key example.
2. The CSTL leadership should put more effort into communicating to the staff the
rationale for resource allocation between new initiatives and established
programs, some of which produce revenues through standard reference materials
(SRMs). One example is the current focus on nanoscience and nanotechnology,
which competes with established metrology.
1
National Research Council, An Assessment of the National Institute of Standards and Technology
Chemical Science and Technology Laboratory: Fiscal Year 2007. Washington, D.C.: The National Academies
Press, 2007, pp. 1-2.
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The PMD has effectively transitioned several of its programs to the
bioengineering arena.
3. CSTL should continue its practice of cross-pollinating research planning teams
with individuals from different divisions as new initiatives are developed.
The PMD has been participating in cross-divisional planning related to the
focus in the biosciences area, and this participation has increased
somewhat. Recently, the chief of the PMD has been tapped to coordinate
the activity that NIST is planning and implementing in the area of carbon
mitigation. This cross-divisional activity involves the Process
Measurements Division and the Analytical Chemistry Division within the
CSTL and several other divisions within NIST and other laboratories.
4. There is a sense that a greater fraction of research is being directed at
computation than at experimentation and instrument development. The CSTL
leadership should examine this trend to assess its impact on future capabilities of
the laboratory.
The PMD seems to have a good balance between modeling and
experimentation. It has automated one of its measurement laboratories
(Thermometry Laboratory) with impressive success. This is a good
example of using modern computer techniques to save labor and improve
efficiency, and it should be examined for other measurement laboratories.
5. CSTL should consider special efforts, such as interdivisional seminars and study
groups, to generate more interest in interdisciplinary projects and to avoid
redundancy in research projects across divisions.
This remains an area for improvement within the PMD. It is a challenge,
common to many technical organizations, to motivate researchers to
participate in technical activities that are not closely tied to their personal
areas of expertise and activity, but PMD management should continue to
try to find ways to expand the technical interactions of its researchers.
6. The CSTL leadership should carry out its planned efforts to communicate to the
staff the incentives for disclosing intellectual property and applying for patents.
The PMD seems to be doing a good job in this area.
7. The ratio of Ph.D. scientists to technical and office support staff appears to be so
high that the Ph.D. scientists are often required to perform a technician’s work to
accomplish a task. Besides serving as a barrier to the recruitment of outstanding
scientists, this imbalance reduces the research productivity of the scientists.
CSTL leadership should assess the ratio of support staff to Ph.D. scientists in
terms of its effect on recruitment and productivity.
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This ratio of support staff to PhD scientists is an obvious problem in the
PMD. NIST is a very high-level intellectual organization, and therefore it
is a common practice within NIST to strive for intellectual flexibility by
focusing its hiring efforts on PhDs. It is also difficult to gain funding for
established standards activities. However, considerable efficiencies could
be realized with more support personnel, and improved basic research
would be realized.
8. It is not clear that the laboratory [the CSTL] has developed guidelines for
replacing scientists in critical areas who retire or leave the laboratory for other
reasons. The laboratory should develop a strategic plan to address recruitment
issues and identify areas of opportunity and areas of concern.
The PMD seems to be doing a good job in this area.
9. The CSTL should increase efforts to make its scientists more visible in their
respective scientific communities.
Many of the top PMD scientists seem to have good external recognition;
however, the PMD recognizes this as an area to be improved.
TECHNICAL MERIT
The Process Measurements Division is composed of five groups: Fluid Metrology,
Process Sensing, Thermometry, Pressure and Vacuum, and Nanoscale and Optical Metrology.
The division seeks to improve the realization of U.S. national measurement standards for
temperature, fluid flow, liquid volume and density, pressure and vacuum, humidity, and
airspeed. The PMD also seeks to develop the science to support new or improved
measurements and standards technologies, with an emphasis on industrial process
applications. The division provides access to these standards by providing instrument
calibration services, SRMs, and standard reference data.
Overall, PMD staff are of very high quality, very sophisticated in their methods, and
positive in their attitude about NIST and their work.
In the division’s measurements groups, most activities are among the best in their
field, and they produce the secondary calibration tools and standards that are recognized as
the best. These secondary standards are used by other nations for primary calibrations. The
measurement groups have responded well to market needs, and their facilities allow the
attainment of the highest standards of calibration to take place.
The pressure measurements team produces methods and standard calibration services
for pressures down to 10–7 pascals (Pa). Methods for pressures as low as 10–11 Pa should be
provided, because the semiconductor and solar energy processes frequently work in those
pressure realms.
An example of work that the PMD has done very well is the pressure transfer
standard. The PMD developed a transfer standard package (TSP) with high stability to be
used as a way of comparing the performance of primary pressure standards from NMIs
around the world. Typically, the TSPs use pairs of resonance silicon gauges, which are based
on microelectromechanical systems technology; a temperature-controlled enclosure (based on
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a commercially available cooler with an incorporated thermoelectric cooling unit); support
electronics; and customized software. The PMD developed a modification of the TSP as a
prototype to provide NIST pressure traceability for the Army Primary Standards Laboratory
(APSL) for pressures of up to 130 kilopascals (kPa). For its needs, the APSL requires a
reliable barometric-pressure range instrument that is stable to within 50 ppm over a period of
1 year. This is to support calibrations for a wide range of precision pressure equipment―the
most stringent requirement is the calibration of aircraft instrumentation calibrators. The PMD
reports that, based on its experience with distributing TSPs internationally, the long-term
calibration stability of this prototype will meet or exceed the Army requirement. The PMD
expects these transfer standards, with their demonstrated stability, to remain within Army
requirements for several years before they would be returned to the PMD for recalibration.
This work is highly innovative, and the stability and precision of the standards are impressive.
The Thermometry Laboratory has undergone major renovations and is very
impressive. The laboratory has been automated using LabView® software. The automation
project was a pilot to see whether or not this approach would be useful, and it turned out to be
a greater success than the PMD had expected. With the new system, several calibrations can
now be carried out at the same time using far less technical staff time. Since tasks associated
with calibration activities lend themselves well to automation, the PMD is concentrating on
automation in this context at the moment. This example demonstrates that the automation of
tasks that are repetitive and must be done in a particular way increases the efficiency of the
laboratory and its staff. Other measurement laboratories should consider implementing this
automation, using the same software and hardware platforms.
The sapphire high-temperature measurements pursued by the PMD are much needed
by industry; the tool geometry specifications have been established by working with the end
users. This is an example of a program that is well aligned with the NIST mission and should
be completed. The program could have more impact and should be reviewed internally to
ensure that it is staffed at a level sufficient to achieve its potential for impact.
The plasma processing effort is a technically solid program; however, the customer
base has evaporated. This program should be refocused and better aligned with the NIST
mission. There does not seem to be an established methodology to evaluate and eliminate
programs within the PMD. It is recommended that the PMD management team establish such
an evaluation program. This would make the program direction choices easier to implement.
Industry focus has been shifted away from semiconductors (a heavy emphasis in the
past) into light-emitting diodes, the Smart Grid, and carbon cap-and-trade (energy-related)
programs and the associated technologies.
The work involving quasi-spherical resonators to provide an atomic standard of
pressure is impressive. The goal of the research involved here is to develop an accurate
primary standard for pressure in the range of 0.3 megapascals (MPa) to 7 MPa, which is based
on fundamental physical properties of helium and the use of quasi-spherical resonators.
Using quantum mechanical theory, it is possible to predict the polarizability of helium, with
agreement among all predictions of a few parts in 107. Quasi-spherical resonators have been
developed that use acoustic and microwave resonances to measure the dielectric constant of
helium from measurements of the microwave resonance frequencies of the cavity. Helium
was used initially, but impurities in the helium presented a problem. Argon was then used,
followed by the use of a mix of helium and argon. The approach of using quasi-spherical
resonators has revolutionized the realization of pressure standards. Moreover, NIST and other
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NMIs are using these cavities to determine imperfections in the internationally accepted
temperature scale—the International Temperature Scale of 1990, or ITS-90.
The PMD is pursuing measurements for biopharmaceutical manufacturing, the
objective of which is to develop standards and measurement tools to enable better
comparability and more efficient science-based manufacturing of biological products. The
manufacturing of protein drugs is expensive and inefficient; inadequate metrology results in
high costs for these drugs. The researchers are using the technique of electrospray-differential
mobility analysis to measure protein aggregation. The electrospray process, used in the past
for separating gold nanoparticles of very precise dimensions, is now being used successfully
in this new context. The team is using a technique that was employed for one type of particle,
and bringing it into a biological application is commendable. This is a good example of
transforming a program with less than good support into a program in a new arena (the
biological arena) that is of interest today, and an arena in which it is good for NIST to be
involved—one in which standards are anticipated to be increasingly important.
Protein aggregation can decrease the safety and efficacy of protein therapeutics (a
category of biotechnological drugs), and the adsorption of protein therapeutics to
bioprocessing materials used in the production, storage, and delivery may also contribute to
this problem. A technique for surface analysis, x-ray photoelectron spectroscopy (XPS), is
being used to attain elemental information on all of the elements on a sample (except
hydrogen and helium). The objective of this work is to provide protein adsorption data,
measured on materials commonly used in bioprocessing, to address these issues. Using this
technique and the fact that there are surface interactions with proteins mean that the
researchers have to understand how the particle changes with time. This is more complex
than a mere physical measurement; the standard has to be understood.
The biological work of the PMD is impressive, and it is good for NIST to be doing
work in the biological arena.
If a process is changed in biological and semiconductor processes, the process needs
to be recertified. In the semiconductor manufacturing arena, the copy exact processes are
well understood, and they assist in the scaling-up processes and the transferring of complete
fabrication rules to new facilities. The ability to do this is based on well-understood
metrology methods and standards, many of which are directly traced to early work at NIST.
The division should explore ways to increase work directly related to methods and standards
that are directly applicable to drug manufacturing in order to enable the cost-effective scale-
up of processes.
In performing the chemical sensor work being pursued in the PMD, the researchers are
very clever about how they extract data and carry out sophisticated analysis. The technology
involved emphasizes the integrated, multidisciplinary approach, which has become more of a
trend in this group. In order to realize the impact of technologies such as chemical sensors,
there is a demand on many disciplines that must be carefully integrated to ensure success. It
is encouraging to see the multidisciplinary approach―using a variety of technologies to
deposit the sensory materials, using outside sources effectively, employing the properties of
these materials by using rapid thermal cycling to achieve chemical fingerprints in a novel
way, and taking the data and using computer modeling and analysis to extract data in a unique
way. In addition, the background materials chosen are appropriate. This is an exciting
technology, and the division should actively pursue external partners. It is encouraging that a
research license already exists with an external company.
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The work using calibrated nozzles for fluid-flow metrology is very good. It is elegant
in its simplicity and precision, and this is a technology that is clearly appreciated by the
international community. Other countries come to this group to have their standards certified
as well.
In 2007, division researchers produced 68 publications, gave 56 talks, and had 7
patents pending, with 29 division staff members holding professional committee assignments
and 2 holding editorships of professional journals. In 2008, division researchers produced 83
publications, gave 48 talks, and had the same 7 patents pending, with 28 division staff
members holding professional committee assignments and 2 holding editorships of
professional journals.
The Department of Commerce Silver Medal Award is the second-highest honor
awarded by the department. It is bestowed for exceptional performance characterized by
noteworthy or superlative contributions that have a direct and lasting impact within the
department. One was awarded to division personnel both in 2007 and in 2008.
INFRASTRUCTURE
Of the Process Measurements Division laboratories visited by the panel, differences
between the old and new buildings are apparent; however, even in the old buildings, no staff
members complained about their space, so space does not appear to be a problem. There is a
fair amount of aging equipment (old power supplies, for example), however. A review of
capital equipment should be undertaken with an eye to ensuring that the most efficient and
safest equipment is provided. NIST hosts numerous visitors from many countries, and the
appearance of being state of the art is important.
As noted above, the automation of the Thermometry Laboratory is an impressive
achievement. This involved the use of LabView® to fully automate calibrations, which, prior
to automation, were tedious, time-consuming, and required considerable manpower. The
automation of this laboratory should be a model for automating other measurements
laboratories that have similarly routine (although important) measurement requirements.
Moreover, there should be cross-pollination between the groups to avoid unnecessary
duplication of efforts in laboratory automation. Considering that the PMD is looking at
automating laboratories, the need for computer and automated equipment would be a good
investment of resources.
The Pressure Laboratory is a state-of-the-art facility. There is a measured, large
improvement in the accuracy of pressure measurements with the new facility.
With the recent rise in interest within the federal government in hydrogen as a
potential part of the future U.S. energy landscape, NIST is anticipating that it may be
expanding its role in hydrogen-related standards development. The PMD is designing a new
facility for hydrogen-related activities. The safe handling of high-pressure hydrogen gas is, of
course, a key consideration as plans for the facility move forward. Accordingly, the PMD is
taking a careful, step-by-step approach in designing and planning for the new facility.
Although it is not currently a certainty that hydrogen will become a more significant part of
the future infrastructure of the United States or that hydrogen-related activities at NIST will
increase significantly, the PMD is planning the new facility with an eye to the possibility that
hydrogen may eventually be used there.
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The current approach to safety is to initially qualify the new facility’s operation for
pressures of up to 6,000 pounds per square inch (psi), while also considering the requirements
associated with the handling of high-pressure hydrogen. Initial activities will involve the use
of argon or nitrogen, followed by the use of methane. Government efforts to use hydrogen as
a fuel for vehicles may lead to the facility’s being used to study the effects of transient flows
on the response of typical flow meters, and the development of standards that account for
transients. Currently, standards of this type are not available, although many realistic, real-
world gas flows involve large transients. The PMD is planning to put as much of any
combustible material as possible outside the building. This is a sound element in an approach
to safety planning for this facility.
There is a critical need for full-time technicians, especially in those areas where
measurements and calibrations are intense. In an effort to strive for intellectual flexibility,
hiring at the PMD typically favors PhDs rather than technicians. Moreover, the way in which
new funding comes into the PMD does not generally support the established standards
activities, and the division does not have a method for keeping those activities’ funding at a
healthy level as compared with funding for high-profile research areas. The PMD, in concert
with its NIST leadership, needs to specify the ways in which NIST evaluates and values the
long-standing standards activities of the PMD. There does not appear to be a strategy for
maintaining the ranks of technicians at a healthy level. The addition of a few technicians
would probably greatly improve the productivity of the most senior professional staff―taking
advantage of the investment that the PMD has made in them. Therefore, there should be more
technicians to improve the efficiency of the entire technical staff. There are many examples
of PhD-level personnel doing routine functions, and the addition of more technicians would
free the PhD-level staff to perform more PhD-level work.
OBJECTIVES AND IMPACT
The PMD should consider and investigate media opportunities to publicize the
usefulness of its capabilities. Many more potential users of PMD services and products would
come forward if they knew more about what the PMD has to offer. In addition, industry
would probably take more advantage of PMD capabilities if the cycle time for standards work
were shorter. Also, the division is slow when it comes to developing a new process for a
standard, which inhibits industry with respect to using PMD services. Finally, the PMD
should continue to check for and evaluate new technologies that may be coming in the future
and should plan for how its capabilities would properly address them.
CONCLUSIONS
Overall, PMD staff are of very high quality and very sophisticated in their methods,
and they evince a positive attitude about NIST and their work. Among the PMD’s
measurements groups, most activities are among the best in their field, and these groups
produce the secondary calibration tools and standards that are recognized as the best.
The automation of the Thermometry Laboratory, using LabView® software, is an
impressive accomplishment. Other measurement laboratories should consider implementing
this automation, using the same software and hardware platforms, and there should be cross-
pollination between the groups in order to avoid unnecessary duplication of efforts. Since the
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PMD is looking at automating laboratories, computer and automated equipment would be a
good investment of resources.
Methods for pressures as low as 10–11 Pa should be provided by the PMD, because the
semiconductor and solar energy processes frequently work in those pressure realms.
PMD management should establish an evaluation methodology and program to
facilitate the elimination of programs when they are no longer effective in meeting the PMD
and NIST missions. The plasma processing effort is an example of PMD management’s
recognition of this need.
The sapphire high-temperature measurements pursued by the PMD are much needed
by industry. The program could have more impact and should be reviewed internally to ensure
that it is staffed at a level sufficient to achieve its potential for impact.
The PMD has transitioned several programs to the bioengineering arena very well. It
is good for NIST to be doing work in the biological arena, where standards are anticipated to
be increasingly important. The PMD should explore ways to increase work directly related to
methods and standards that are directly applicable to drug manufacturing in order to enable
the cost-effective scale-up of processes.
The PMD should consider and investigate media opportunities to publicize the
usefulness of its capabilities. Many more potential users of PMD services and products would
probably come forward if they knew more about what the division has to offer. Industry
would probably take more advantage of PMD capabilities if the cycle time for standards work
were shorter. Also, the PMD is slow when it comes to developing a new process for a
standard, which inhibits industry with respect to using PMD services. The PMD should
continue to evaluate new technologies that may be coming and plan for how its capabilities
would address them.
Although many of the PMD’s top scientists seem to have good external recognition,
the division should continue its efforts to make its scientists more visible in their scientific
communities. It is a challenge to motivate researchers to participate in technical activities that
are not closely tied to their personal areas of expertise and activity, but PMD management
should continue to try to find ways to expand the technical interactions of its researchers.
With increased interest within the federal government in hydrogen as a potential part
of the future U.S. energy landscape, NIST is anticipating an expanded role in related
standards development. Although these possibilities are not a certainty, the PMD is planning
ahead for a facility to accommodate the safe handling of high-pressure gases, with an eye to
the possibility of eventual hydrogen use. The panel thinks that the careful, step-by-step
approach being taken by the PMD in designing and planning for the new facility is sound.
There is a critical need for full-time technicians, especially in those areas where
measurements and calibrations are intense. The addition of a few technicians would greatly
improve the productivity and efficiency of the entire technical staff.
A review of capital equipment should be undertaken with an eye to ensuring that the
most efficient and safest equipment is provided.
32