An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2009 (2009)

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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. 25 

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. 26 

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 27 

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 28 

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. 29 

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. 30 

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 31 

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