A facile NMR method is reported for analysis of ammonia from the electrochemical reduction of nitrogen, which compares a calibrated colorimetric method, a calibrated 1H NMR method and two 1H NMR direct measurements using external reference materials. Unlike spectrophotometric methods, 1H NMR requires less bench time and does not require separation of ammonia from the electrolyte. A novel approach to the problem of radiation damping in NMR measurements considered the specific role of hardware tuning. Radiation damping is suppressed improving signal-to-noise ratio and detection limit (1.5 µg L-1). The method is demonstrated to be effective for the analysis of ammonia from direct electrochemical nitrogen reduction in KOH, and from lithium-mediated nitrogen reduction in a non-aqueous solution. An uncertainty budget is prepared for the measurement of ammonia.

A metrologically consistent procedure for assessing the detection limits of activity measurements for gamma-ray emitters with high-resolution spectrometers using the LSQ method is described and tested. As the input to the assessment, besides the measured contents of the spectral channels, the results of the peak analysis, i.e., the indication and its uncertainty, are used. The unfolding of the spectral region of interest into its components corresponding to the peak representing the indication and its background allows us to take into account the uncertainty budget, describing the uncertainty of the indication and the shape of the corresponding peak, making possible to include these sources of uncertainty in the calculation of the decision threshold. To assess the detection limit, the variance of the indication is calculated as a function of the indication itself, while considering the relative uncertainty of the conversion factor. The variance of the indication observed is approximated by a polynomial of the second order of the indication, thus making it possible to calculate the detection limit analytically. The method was tested on measured spectra using the empirically determined spectral shape of the peak representing the indication. It was shown how the empirically determined shape of an isolated and expressive peak close to the peak representing the indication can be used in the calculation of the decision threshold and how the presence of a peak overlapping with the peak representing the indication affects the decision threshold and the detection limit. It is explained that besides the counting statistics, the sources of uncertainty due to the shape of the peak representing indication also contribute to the decision threshold. However, to the increase of the detection limit over the decision threshold, besides the counting statistic, only the uncertainty of the conversion factor contributes. It is shown that in the presence of the indication, the decision threshold and the detection limit can be used to quantify the comparison between the observed value and the true value of the measurand with a predetermined quantity value in terms of the probabilities of making errors of the first and second kind. The application of the decision thresholds and detection limits to a conformity assessment is proposed.

Measurements of particulate organic carbon (POC) in the open ocean provide grounds for estimating oceanic carbon budgets and for modelling carbon cycling. The majority of the published POC measurements have been collected at the sea surface. Thus, POC stocks in the upper layer of the water column are relatively well constrained. However, our understanding of the POC distribution and its dynamics in deeper areas is still modest due to insufficient POC measurements. Moreover, the uncertainty of published POC estimates is not always quantified, and neither is it fully understood. In this study, we determined the POC concentrations of samples collected in the upper 500 m during an Atlantic Meridional Transect and described a method for quantifying its experimental uncertainties using duplicate measurements. The analysis revealed that the medians of the total experimental uncertainties associated with our POC concentrations in the productive and mesopelagic zones were 2(±2) mg/m 3 and 3(±1) mg/m 3, respectively. In relative terms, these uncertainties corresponded to ∼12% and ∼35% of POC concentrations, respectively. We modelled the POC uncertainty in order to identify its main causes. This model however could explain only ∼19% of the experimental POC uncertainty. Potential sources of the unexplained uncertainty are discussed.

The structural collapse of a street lighting pole represents an aspect that is often underestimated and unpredictable, but of relevant importance for the safety of people and things. These events are complex to evaluate since several sources of damage are involved. In addition, traditional inspection methods are ineffective, do not correctly quantify the residual life of poles, and are inefficient, requiring enormous costs associated with the vastness of elements to be investigated. An advantageous alternative is to adopt a distributed type of Structural Health Monitoring (SHM) technique based on the Internet of Things (IoT). This paper proposes the design of a low-cost system, which is also easy to integrate in current infrastructures, for monitoring the structural behavior of street lighting poles in Smart Cities. At the same time, this device collects previous structural information and offers some secondary functionalities related to its application, such as meteorological information. Furthermore, this paper intends to lay the foundations for the development of a method that is able to avoid the collapse of the poles. Specifically, the implementation phase is described in the aspects concerning low-cost devices and sensors for data acquisition and transmission and the strategies of information technologies (ITs), such as Cloud/Edge approaches, for storing, processing and presenting the achieved measurements. Finally, an experimental evaluation of the metrological performance of the sensing features of this system is reported. The main results highlight that the employment of low-cost equipment and open-source software has a double implication. On one hand, they entail advantages such as limited costs and flexibility to accommodate the specific necessities of the interested user. On the other hand, the used sensors require an indispensable metrological evaluation of their performance due to encountered issues relating to calibration, reliability and uncertainty.

BACKGROUND: Magnetic resonance (MR)-guided radiation therapy provides capabilities to utilize high-resolution and real-time MR imaging before and during treatment, which is critical for adaptive radiotherapy. This emerging modality has been promptly adopted in the clinic settings in advance of adaptations to reference dosimetry formalism that are needed to account for the presence of strong magnetic fields. In particular, the influence of magnetic field on the uncertainty of parameters in the reference dosimetry equation needs to be determined in order to fully characterize the uncertainty budget for reference dosimetry in MR-guided radiation therapy systems.
OBJECTIVE: To identify and quantify key sources of uncertainty in the reference dosimetry of external high energy radiotherapy beams in the presence of a strong magnetic field.
METHODS: In the absence of a formalized Task Group report for reference dosimetry in MR-integrated linacs, the currently suggested formalism follows the TG-51 protocol with the addition of a quality conversion factor kBQ accounting for the effects of the magnetic field on ionization chamber response. In this work, we quantify various sources of uncertainty that impact each of the parameters in the formalism, and evaluate their overall contribution to the final dose. Measurements are done in a 1.5 T MR-Linac (Unity, Elekta AB, Stockholm, Sweden) which integrates a 1.5 T Philips MR scanner and a 7 MVFFF linac. The responses of several reference-class small volume ionization chambers (Exradin:A1SL, IBA:CC13, PTW:Semiflex-3D) and Farmer type ionization chambers (Exradin:A19, IBA:FC65-G) were evaluated throughout this process. Long-term reproducibility and stability of beam quality, TPR 10 20 ${\\mathrm{TPR}}_{10}^{20}$ , was also measured with an in-house built phantom.
RESULTS: Relative to the conventional external high energy linacs, the uncertainty on overall reference dose in MR-linac is more significantly affected by the chamber setup: A translational displacement along y-axis of ± 3 mm results in dose variation of < |0.20| ± 0.02% (k = 1), while rotation of ± 5° in horizontal and vertical parallel planes relative to relative to the direction of magnetic field, did not exceed variation of < |0.44| ± 0.02% for all 5 ionization chambers. We measured a larger dose variation for xy-plane (horizontal) rotations (< |0.44| ± 0.02% (k = 1)) than for yz-plane (vertical) rotations (< ||0.28| ± 0.02% (k = 1)), which we associate with the gradient of kB,Q as a function of chamber orientation with respect to direction of the B0 -field. Uncertainty in Pion (for two depths), Ppol (with various sub-studies including effects of cable length, cable looping in the MRgRT bore, connector type in magnetic environment), and Prp were determined. Combined conversion factor kQ × kB,Q was provided for two reference depths at four cardinal angle orientations. Over a two-year period, beam quality was quite stable with TPR 10 20 ${\\mathrm{TPR}}_{10}^{20}$ being 0.669 ± 0.01%. The actual magnitude of TPR 10 20 ${\\mathrm{TPR}}_{10}^{20}$ was measured using identical equipment and compared between two different Elekta Unity MR-Linacs with results agreeing to within 0.21%.
CONCLUSIONS: In this work, the uncertainty of a number of parameters influencing reference dosimetry was quantified. The results of this work can be used to identify best practice guidelines for reference dosimetry in the presence of magnetic fields, and to evaluate an uncertainty budget for future reference dosimetry protocols for MR-linac.

The ISO/IEC 17025 standard requires that all significant contributions have to be propagated to the measurement uncertainty, including also sampling uncertainties. We evaluated soil sampling uncertainties for gamma-ray spectrometry by using in-house and split-sample methods. By in-house method, the sampling uncertainty was determined by comparing standard deviations of measurement results and average analytical uncertainty. With split-sample method, it was calculated using between-sample and between-analysis variances. If analytical uncertainty is reliably determined, the in-house method is recommended because fewer measurements are needed.

161Tb has potential applications in targeted radionuclide therapy and nuclear forensic science. However, the half-lives of 161Tb in previous studies show a discrepancy. In this study, 161Tb samples were produced by irradiating 160Gd2O3 with thermal neutron flux. A series of procedures were applied to extract a pure 161Tb solution and three solid samples were prepared. The half-life of 161Tb has been measured with a high-purity germanium (HPGe) detector. The time-dependency of the 161Tb activity was followed by assessing the count rate of their characteristic gamma-ray emissions at 48.9 keV and 74.6 keV over a period of 33-43 days. The experiment and uncertainty budget are discussed in detail. Different uncertainty propagation equations were applied for random uncertainties, medium-frequency deviations and potential systematic errors. The result for the 161Tb half-life of 6.967 (11) d was determined by the weighted mean of half-lives from three samples, which confirms that the half-life is longer than the of the current evaluated half-life of 6.89 (2) d. From all available quoted experimental values, a recommended half-life of 6.934 (14) d was determined by the power-moderated method (PMM). Based on recent four published half-life values, a half-life of 161Tb of 6.9582 (33) d was determined by the PMM analysis.

Since both size and shape of nanoparticles are challenging to be quantitatively measured, traceable 3D measurements are nowadays an issue. 3D nanometrology plays a crucial role to reduce the uncertainty of measurements, improve traceable calibration of samples and implement new approaches, models, and methodologies in the study of the nanomaterials. AFM measurement of nanoparticles with unusual shape represent a non-trivial challenge due to the convolution with the finite size of the tip. In this work, geometric approaches for the determination of critical sizes of TiO2 anatase bipyramids and nanosheets are described. An uncertainty budget is estimated for each nanoparticle size with the aim of assessing the different sources of error to obtain a more reliable and consistent result. The combined standard uncertainties are respectively less than 5% and 10% of the dimensions of bipyramids and nanosheets. Due to the stability and monomodal distribution of their critical sizes, bipyramids and nanosheets are suitable to apply as candidate reference materials at the nanoscale. Moreover, quantitative measurements of shape and texture descriptors are discussed in order to understand the quality of the synthetized batch.

OBJECTIVE: The aim of this study is to reduce the uncertainty associated with determining dose-to-water using an amorphous silicon electronic portal imaging detector (EPID) under reference conditions by developing a direct calibration formalism based on radiochromic film measurements made within the EPID panel and detailed Monte Carlo simulations. To our knowledge, this is the first EPID-based dosimetry study reporting an uncertain budget METHODS: Pixel sensitivity and relative off-axis response were mapped by simultaneously irradiating film contained within the imager panel and acquiring an EPID image set. The detector panel was disassembled for the purpose of modeling the EPID in detail using the EGSnrc DOSXYZnrc usercode, which was in turn used to calculate dose-to-film in the EPID and dose-to-water in water conversion factors RESULTS: A direct comparison of the two correction methodologies investigated in this work, the previously established empirical method and the proposed simultaneous measurement approach involving in-EPID film dosimetry, produced an agreement with an RMS deviation of 1.4% overall. A combined standard relative uncertainty of 3.3% (k = 1) was estimated for the determination of absorbed dose to water at the position of the EPID using the proposed calibration methodology CONCLUSIONS: This work describes a direct method of calibrating EPID response in terms of absorbed dose to water requiring fewer measurements than other empirical approaches, and without 2D spatial interpolation of correction factors.

OBJECTIVE: Modern radiotherapy modalities, such as Intensity-Modulated Radiotherapy and Volumetric Modulated Arc Therapy involve complex dose delivery. The dose delivery is complex as it involves beam modulation, hence, manual dose calculations for these techniques are not possible. Film dosimetry is commonly used method of dose verification for these modalities because of the advantages associated with it. The quantification of uncertainty associated with a film dosimetry system under clinical use becomes important for accurate dosimetry. The spread in the distribution of the pixel values (PV) of the irradiated film contributes to the uncertainty. The probability distribution (PD) of the PV was studied for the clinical photon beam energies of 6, 10, and 15 MV.
METHODS: Gafchromic EBT3 film and EPSON 10000XL flatbed scanner were used for this purpose and using the resulting PD, the uncertainty budgets for these energies in the red, green and blue color channels were estimated.
RESULTS: The PV of exposed films for the energies studied follows t-distribution, the sum of the squares of the deviation of the measured data from the fitted value was of the order of 10-7, this indicates the goodness of fit. The \"t\" value corrected combined standard uncertainty (CSU) at 1σ confidence level for exposed film and dose measurement at 200 cGy were 1.42%, 1.48%, and 1.63% and 1.99%, 3.23%, and 5.08% for 6, 10, and 15 MV energies, respectively, in the red colour channel.
CONCLUSIONS: In the case of the limited number of measurements of a quantity, the SU values must be corrected using the \"t\" value to get the correct CSU.