Linearity Characterization and Uncertainty Quantification of Spectroradiometers via Maximum Likelihood and the Non-parametric Bootstrap.

A technique for characterizing and correcting the linearity of radiometric instruments is known by the names the "flux-addition method" and the "combinatorial technique". In this paper, we develop a rigorous uncertainty quantification method for use with this technique and illustrate its use with both synthetic data and experimental data from a "beam conjoiner" instrument. We present a probabilistic model that relates the instrument readout to a set of unknown fluxes via a set of polynomial coefficients. Maximum likelihood estimates (MLEs) of the unknown fluxes and polynomial coefficients are recommended, while a non-parametric bootstrap algorithm enables uncertainty quantification including standard errors and confidence intervals. The synthetic data represent plausible outputs of a radiometric instrument and enable testing and validation of the method. The MLEs for these data are found to be approximately unbiased, and confidence intervals derived from the bootstrap replicates are found to be consistent with their target coverage of 95%. For the polynomial coefficients, the observed coverages range from 91% to 99%. The experimental data set illustrates how a complete calibration with uncertainties can be achieved using the method plus one well-known flux level. The uncertainty contribution attributable to estimation of the instrument's nonlinear response is less than 0.025% over most of its range.

Sub-picoliter Traceability of Microdroplet Gravimetry and Microscopy.

Gravimetry typically lacks the resolution to measure single microdroplets, whereas microscopy is often inaccurate beyond the resolution limit. To address these issues, we advance and integrate these complementary methods, introducing simultaneous measurements of the same microdroplets, comprehensive calibrations that are independently traceable to the International System of Units (SI), and Monte-Carlo evaluations of volumetric uncertainty. We achieve sub-picoliter agreement of measurements of microdroplets in flight with volumes of approximately 70 pL, with ensemble gravimetry and optical microscopy both yielding 95% coverage intervals of ±0.6 pL, or relative uncertainties of ±0.9%, and root-mean-square deviations of mean values between the two methods of 0.2 pL or 0.3%. These uncertainties match previous gravimetry results and improve upon previous microscopy results by an order of magnitude. Gravimetry precision depends on the continuity of droplet formation, whereas microscopy accuracy requires that optical diffraction from an edge reference matches that from a microdroplet. Applying our microscopy method, we jet and image water microdroplets suspending fluorescent nanoplastics, count nanoplastic particles after deposition and evaporation, and transfer volumetric traceability to the number concentrations of single microdroplets. We expect that our methods will impact diverse fields involving dimensional metrology and volumetric analysis of microdroplets, including inkjet microfabrication, disease transmission, and industrial sprays.

Demonstration of a laser powder bed fusion combinatorial sample for high-throughput microstructure and indentation characterization.

High-throughput experiments that use combinatorial samples with rapid measurements can be used to provide process-structure-property information at reduced time, cost, and effort. Developing these tools and methods is essential in additive manufacturing where new process-structure-property information is required on a frequent basis as advances are made in feedstock materials, additive machines, and post-processing. Here we demonstrate the design and use of combinatorial samples produced on a commercial laser powder bed fusion system to study 60 distinct process conditions of nickel superalloy 625: five laser powers and four laser scan speeds in three different conditions. Combinatorial samples were characterized using optical and electron microscopy, x-ray diffraction, and indentation to estimate the porosity, grain size, crystallographic texture, secondary phase precipitation, and hardness. Indentation and porosity results were compared against a regular sample. The smaller-sized regions (3 mm × 4 mm) in the combinatorial sample have a lower hardness compared to a larger regular sample (20 mm × 20 mm) with similar porosity (< 0.03 %). Despite this difference, meaningful trends were identified with the combinatorial sample for grain size, crystallographic texture, and porosity versus laser power and scan speed as well as trends with hardness versus stress-relief condition.

Scatter Corrections in X-Ray Computed Tomography: A Physics-Based Analysis.

Fundamental limits for the calculation of scattering corrections within X-ray computed tomography (CT) are found within the independent atom approximation from an analysis of the cross sections, CT geometry, and the Nyquist sampling theorem, suggesting large reductions in computational time compared to existing methods. By modifying the scatter by less than 1 %, it is possible to treat some of the elastic scattering in the forward direction as inelastic to achieve a smoother elastic scattering distribution. We present an analysis showing that the number of samples required for the smoother distribution can be greatly reduced. We show that fixed forced detection can be used with many fewer points for inelastic scattering, but that for pure elastic scattering, a standard Monte Carlo calculation is preferred. We use smoothing for both elastic and inelastic scattering because the intrinsic angular resolution is much poorer than can be achieved for projective tomography. Representative numerical examples are given.

The Influence of X-Ray Computed Tomography Acquisition Parameters on Image Quality and Probability of Detection of Additive Manufacturing Defects.

X-ray computed tomography (XCT) is a promising nondestructive evaluation technique for additive manufacturing (AM) parts with complex shapes. Industrial XCT scanning is a relatively new development, and XCT has several acquisition parameters that a user can change for a scan whose effects are not fully understood. An artifact incorporating simulated defects of different sizes was produced using laser powder bed fusion (LPBF) AM. The influence of six XCT acquisition parameters was investigated experimentally based on a fractional factorial designed experiment. Twenty experimental runs were performed. The noise level of the XCT images was affected by the acquisition parameters, and the importance of the acquisition parameters was ranked. The measurement results were further analyzed to understand the probability of detection (POD) of the simulated defects. The POD determination process is detailed, including estimation of the POD confidence limit curve using a bootstrap method. The results are interpreted in the context of the AM process and XCT acquisition parameters.

Influence of Wind Tunnel Test Duration on Wind Load Factors.

A method is presented for calculating the uncertainty associated with the estimation of peak pressure coefficients from wind tunnel test records of various lengths and how this uncertainty influences design wind effects. The proposed method is applicable to any type of structure and any type of civil engineering aerodynamic testing facility, including large-scale facilities. As an example of the application of the method, an investigation is presented of time series belonging to five categories of pressure coefficients implicit in Chapter 27 of the ASCE 7-10 Standard. The results of the investigation show that, for typical civil engineering wind tunnels, estimated design wind effects based on tests with durations as low as 10 s, corresponding to prototype durations of less than 6 min, are larger than their counterparts based on tests with 100 s duration by only approximately 5%. The proposed method provides useful indications on minimum lengths of pressure records to be measured in wind tunnels.

Recent and Current Wind Engineering Research at the National Institute of Standards and Technology.

This paper briefly reviews recent and current National Institute of Standards and Technology (NIST) research aimed at improving standard provisions and advancing structural design practice for wind loads. The research covers: (i) New wind speed maps for the conterminous United States; (ii) Risk-consistent estimation of wind load factors for use with the wind tunnel procedure; (iii) Modern peaks-over-threshold approaches to estimation of peak wind effects; (iv) User-friendly procedures for the database-assisted design of rigid and flexible structures; (v) Novel approaches to codification of pressures on cladding and components; (vi) Modern modeling of synoptic storm planetary boundary layers and its implications for super-tall building design; (vii) Computational Wind Engineering (CWE); (viii) Tornado climatology and development of tornado-resistant design methodologies; (ix) Joint climatology of wind speeds, storm surge and waves heights, and estimates of their combined effects on structures.

Algorithm for rapid determination of optical scattering parameters.

Preliminary experiments at the NIST Spectral Tri-function Automated Reference Reflectometer (STARR) facility have been conducted with the goal of providing the diffuse optical properties of a solid reference standard with optical properties similar to human skin. Here, we describe an algorithm for determining the best-fit parameters and the statistical uncertainty associated with the measurement. The objective function is determined from the profile log likelihood, including both experimental and Monte Carlo uncertainties. Initially, the log likelihood is determined over a large parameter search box using a relatively small number of Monte Carlo samples such as 2·104. The search area is iteratively reduced to include the 99.9999% confidence region, while doubling the number of samples at each iteration until the experimental uncertainty dominates over the Monte Carlo uncertainty. Typically this occurs by 1.28·106 samples. The log likelihood is then fit to determine a 95% confidence ellipse. The inverse problem requires the values of the log likelihood on many points. Our implementation uses importance sampling to calculate these points on a grid in an efficient manner. Ultimately, the time-to-solution is approximately six times the cost of a Monte Carlo simulation of the radiation transport problem for a single set of parameters with the largest number of photons required. The results are found to be 64 times faster than our implementation of Particle Swarm Optimization.

Experimental and statistical methods to evaluate antibacterial activity of a quaternary pyridinium salt on planktonic, biofilm-forming, and biofilm states.

Robust evaluation and comparison of antimicrobial technologies are critical to improving biofilm prevention and treatment. Herein, a multi-pronged experimental framework and statistical models were applied to determine the effects of quaternary pyridinium salt, 4-acetyl-1-hexadecylpyridin-1-ium iodide (QPS-1), on Streptococcus mutans in the planktonic, biofilm-forming and biofilm cell states. Minimum inhibitory and bactericidal concentrations (MIC and MBC, respectively) were determined via common methods with novel application of statistical approaches combining random effects models and interval censored data to estimate uncertainties. The MICs and MBCs for planktonic and biofilm-forming states ranged from 3.12 to 12.5 µg ml-1, with biofilm values only ≈ 8 times higher. Potent anti-biofilm activity and reactive structural features make QPS-1 a promising antibacterial additive for dental and potentially other biomedical devices. Together, the experimental framework and statistical models provide estimates and uncertainties for effective antimicrobial concentrations in multiple cell states, enabling statistical comparisons and improved characterization of antibacterial agents.

Comparison of One-Dimensional and Volumetric Computed Tomography Measurements of Injected-Water Phantoms.

The goal of this study was to compare volumetric analysis in computed tomography (CT) with the length measurement prescribed by the Response Evaluation Criteria in Solid Tumors (RECIST) for a system with known mass and unknown shape. We injected 2 mL to 4 mL of water into vials of sodium polyacrylate and into disposable diapers. Volume measurements of the sodium polyacrylate powder were able to predict both mass and proportional changes in mass within a 95 % prediction interval of width 12 % and 16 %, respectively. The corresponding figures for RECIST were 102 % and 82 %.

Estimating peaks of stationary random processes: a peaks-over-threshold approach.

Estimating properties of the distribution of the peak of a stationary process from a single finite realization is a problem that arises in a variety of science and engineering applications. Further, it is often the case that the realization is of length T while the distribution of the peak is sought for a different length of time, T 1 > T. Current methods for estimating peaks of time series have drawbacks that motivated the development of a new procedure, based on the peaks-over-threshold method, an advantage of which is that it often results in an increased size of the relevant extreme value data set compared with epochal procedures. For further comparison, the translation approach depends upon the estimate of the marginal distribution of a non-Gaussian time series, which is typically difficult to perform reliably. The epochal procedure for estimating peaks combined with Best Linear Unbiased Estimates (BLUE) of the Gumbel parameters was found to depend, in some cases very significantly, upon the number of partitions being used. The proposed procedure is based on a Poisson process model for the thresholded pressure coefficient y, with threshold u. The estimated peak depends upon the choice of the threshold. However, unlike for the choice of the number n of partitions for the epochal procedure, a criterion is available that allows the analyst to make an optimal choice (according to a chosen metric) of the threshold value. Two versions of the proposed new procedure have been developed. One version, denoted by FpotMax, includes estimation of a tail length parameter with a similar interpretation to the generalized extreme value distribution tail length parameter. The second version, denoted by GpotMax, assumes that the tail length parameter vanishes, resulting in a tail of the Gumbel distribution type.

Development of two fine particulate matter standard reference materials (<4 µm and <10 µm) for the determination of organic and inorganic constituents.

Two new Standard Reference Materials (SRMs), SRM 2786 Fine Particulate Matter (<4 µm) and SRM 2787 Fine Particulate Matter (<10 µm) have been developed in support of the US Environmental Protection Agency's National Ambient Air Quality Standards for particulate matter (PM). These materials have been characterized for the mass fractions of selected polycyclic aromatic hydrocarbons (PAHs), nitrated PAHs, brominated diphenyl ether (BDE) congeners, hexabromocyclododecane (HBCD) isomers, sugars, polychlorinated dibenzo-p-dioxin (PCDD) and dibenzofuran (PCDF) congeners, and inorganic constituents, as well as particle-size characteristics. These materials are the first Certified Reference Materials available to support measurements of both organic and inorganic constituents in fine PM. In addition, values for PAHs are available for RM 8785 Air Particulate Matter on Filter Media. As such, these SRMs will be useful as quality control samples for ensuring compatibility of results among PM monitoring studies and will fill a void to assess the accuracy of analytical methods used in these studies. Graphical Abstract Removal of PM from filter for the preparation of SRM 2786 Fine Particulate Matter.

Absolute calibration of a variable attenuator using few-photon pulses.

We demonstrate the ability to calibrate a variable optical attenuator directly at the few-photon level using a superconducting Transition Edge Sensor (TES). Because of the inherent linearity of photon-number resolving detection, no external calibrations are required, even for the energy of the laser pulses, which ranged from means of 0.15 to 18 photons per pulse at the detector. To verify this method, calibrations were compared to an independent conventional calibration made at much higher photon fluxes using analog detectors. In all cases, the attenuations estimated by the two methods agree within their uncertainties.Our few-photon measurement determined attenuations using the Poisson-Influenced K-Means Algorithm (PIKA) to extract mean numbers of photons per pulse along with the uncertainties of these means. The robustness of the method is highlighted by the agreement of the two calibrations even in the presence of significant drifts in the optical power over the course of the experiment.Work of the United States Government. Not subject to copyright.

Traceable localization enables accurate integration of quantum emitters and photonic structures with high yield.

In a popular integration process for quantum information technologies, localization microscopy of quantum emitters guides lithographic placement of photonic structures. However, a complex coupling of microscopy and lithography errors degrades registration accuracy, severely limiting device performance and process yield. We introduce a methodology to solve this widespread but poorly understood problem. A new foundation of traceable localization enables rapid characterization of lithographic standards and comprehensive calibration of cryogenic microscopes, revealing and correcting latent systematic effects. Of particular concern, we discover that scale factor deviation and complex optical distortion couple to dominate registration errors. These novel results parameterize a process model for integrating quantum dots and bullseye resonators, predicting higher yield by orders of magnitude, depending on the Purcell factor threshold as a quantum performance metric. Our foundational methodology is a key enabler of the lab-to-fab transition of quantum information technologies and has broader implications to cryogenic and correlative microscopy.

Milk and serum standard reference materials for monitoring organic contaminants in human samples.

Four new Standard Reference Materials (SRMs) have been developed to assist in the quality assurance of chemical contaminant measurements required for human biomonitoring studies, SRM 1953 Organic Contaminants in Non-Fortified Human Milk, SRM 1954 Organic Contaminants in Fortified Human Milk, SRM 1957 Organic Contaminants in Non-Fortified Human Serum, and SRM 1958 Organic Contaminants in Fortified Human Serum. These materials were developed as part of a collaboration between the National Institute of Standards and Technology (NIST) and the Centers for Disease Control and Prevention (CDC) with both agencies contributing data used in the certification of mass fraction values for a wide range of organic contaminants including polychlorinated biphenyl (PCB) congeners, chlorinated pesticides, polybrominated diphenyl ether (PBDE) congeners, and polychlorinated dibenzo-p-dioxin (PCDD) and dibenzofuran (PCDF) congeners. The certified mass fractions of the organic contaminants in unfortified samples, SRM 1953 and SRM 1957, ranged from 12 ng/kg to 2200 ng/kg with the exception of 4,4'-DDE in SRM 1953 at 7400 ng/kg with expanded uncertainties generally <14 %. This agreement suggests that there were no significant biases existing among the multiple methods used for analysis.

Uncertainties in RECIST as a measure of volume for lung nodules and liver tumors.

PURPOSE: The authors wish to determine the extent to which the Response Evaluation Criteria in Solid Tumors (RECIST) and the criteria of the World Health Organization (WHO) can predict tumor volumes and changes in volume using clinical data. METHODS: The data presented are a reanalysis of data acquired in other studies, including the public database from the Lung Image Database Consortium (LIDC) and from a study of liver tumors. RESULTS: The principal result is that a given RECIST diameter predicts volume to a factor of 16 or 10 for the two data sets, respectively, by examining 95% prediction bounds and that changes in volume are predicted only little better: to within a factor of 7 for the liver data. The WHO criteria reduce the prediction bounds by a factor of 1.3 in all cases. Also, the RECIST threshold of 10 mm to measure a nodule corresponds to a transition zone width of a factor of more than 2 in volume for the nodules in the LIDC database. CONCLUSIONS: While the RECIST diameter is certainly correlated with the volume, and similarly for changes in these quantities, the use of the diameter introduces additional variation assuming volume is the quantity of interest. Exactly how much this reduces the statistical power of clinical drug trials is a key open question for future research.

Wind Load Factors for Use in the Wind Tunnel Procedure.

A 2004 Skidmore Owings and Merrill report (in Simiu E. (2011) Design of Buildings for Wind, Appendix 5, Wiley, Hoboken, NJ) notes that the ASCE 7 Standard (American Society of Civil Engineers (2002) ASCE 7-02, Reston, Va) is incomplete insofar as it provides no guidance on wind load factors appropriate for use with the Standard's wind tunnel procedure. The purpose of this paper is to contribute to such guidance. Based on a classical definition of wind load factors as functions of uncertainties in the micrometeorological, wind climatological, aerodynamics and structural dynamics elements that determine wind loads, the paper presents a simple, straightforward approach that allows practitioners to use appropriate wind load factors applicable when those uncertainties are either the same as or different from those assumed in the development of the ASCE 7 Standard. Illustrations of the approach are presented for a variety of cases of practical interest. In estimating design wind loads, the various uncertainties should not be accounted for in isolation, for example by specifying peak pressure coefficients with percentage points higher than those corresponding to their expected values. Rather, to achieve risk-consistent designs, the uncertainties should be accounted for collectively, in terms of their joint effect on the design wind loading. The design wind effect is equal to the estimated expectation of the peak wind effect times a load factor that, in most cases, is not significantly different from the load factor explicitly or implicitly specified in the ASCE 7 Standard. Notably, the load factor is not affected significantly by errors associated with interpolations required in typical Database Assisted Design applications. However, if the available wind speed records are several times shorter than, say, 20 to 30 years, the wind load factors increase by amounts of the order of 15 %.

National Institute of Standards and Technology measurement service of the optical properties of biomedical phantoms: Current status.

The National Institute of Standards and Technology (NIST) has maintained scales for reflectance and transmittance over several decades. The scales are primarily intended for regular transmittance, mirrors, and solid surface scattering diffusers. The rapidly growing area of optical medical imaging needs a scale for volume scattering of diffuse materials that are used to mimic the optical properties of tissue. Such materials are used as phantoms to evaluate and validate instruments under development intended for clinical use. To address this need, a double-integrating sphere based instrument has been installed to measure the optical properties of tissue-mimicking phantoms. The basic system and methods have been described in previous papers. An important attribute in establishing a viable calibration service is the estimation of measurement uncertainties. The use of custom models and comparisons with other established scales enabled uncertainty measurements. Here, we describe the continuation of those efforts to advance the understanding of the uncertainties through two independent measurements: the bidirectional reflectance distribution function and the bidirectional transmittance distribution function of a commercially available solid biomedical phantom. A Monte Carlo-based model is used and the resulting optical properties are compared to the values provided by the phantom manufacturer.