The volumes of two 1 kg silicon spheres, AVO28-S5 and AVO28-S8, fabricated from a 28Si-enriched crystal were measured to determine the Avogadro constant by the x-ray crystal density method in the International Avogadro Coordination Project. The volumes were determined from diameter measurements of the two spheres using a laser interferometer with a flat etalon. In the diameter measurement, the sphere was placed between the two flat etalon plates. The gaps between the sphere and the etalon plates and the distance between the etalon plates were measured by phase-shifting interferometry with optical frequency tuning. The apparent volumes of the 28Si spheres were determined from the diameter measurement in many directions with relative combined standard uncertainties of 5.0 × 10−8 and 4.4 × 10−8 for AVO28-S5 and AVO28-S8, respectively. The effect of the surface layer on the diameter measurement was evaluated on the basis of the results of characterizing the sphere surface. By taking into account the effect of the surface layer, the silicon core volume excluding the surface layer and the actual volume including the surface layer were also determined. Details of the interferometer, data analysis and the uncertainty in the measurement are described.
The CCT has completed the guide summarizing the uncertainties in the realization of the SPRT subranges of ITS-90 between the triple point of neon (24.5561 K) and the freezing point of silver (961.78 • C). This article identifies aspects of standard platinum resistance thermometry where either data or models are lacking and further research is required. In the calibration of SPRTs, the two main concerns are the need for data on liquidus slopes for the different impurities in the fixed points and improved understanding of the impact of the thermal environment of the fixed point on the realized temperature. In the use of SPRTs, the two largest sources of uncertainty are Types 1 and 3 non-uniqueness and oxidation. The causes of Type 3 non-uniqueness are not yet understood, especially at low temperatures, and there is a paucity of data for the high-temperature subranges. In respect of oxidation, there is a need for validation of the models developed in the 1980s, especially in light of the reduced partial pressure of oxygen used in modern SPRTs. A range of other effects including vacancy effects in SPRTs, isotopic effects in fixed points, and improved statistical methods are discussed.
The impurity effect on fixed-point temperature realization by thermal analysis has been assessed. For such an assessment, the following actions were conducted: (1) the fabrication of aluminium point cells using 6N or higher-grade aluminium samples from different sources (manufacturers), (2) temperature measurements during solidification and thermal analyses based on freezing curves obtained from the measurements, (3) direct cell comparison among cells of different nominal purities and (4) calculation of the departure of the freezing point from the ideally defined freezing point by applying the sum of individual estimates (SIE). Two aluminium point cells were prepared in action (1) using 6N-grade and one cell using 6N5-grade aluminium samples. To realize a fixed point using the cells, a fixed-point furnace was developed and evaluated. Temperature measurements in action (2) were conducted at different rates of solidification and in accordance with the one using the liquid–solid interface technique. Gradients of freezing curves were derived in the thermal analysis, and from their dependence on the rate of solidification, the impurity effect was evaluated. Indirect cell comparison was also derived using the difference in the gradients. It was found that the indirect cell comparison was in satisfactory agreement with the direct cell comparison, which was obtained from action (3). It was also found that the departure of the thermal analysis from the SIE obtained from action (4) was within the uncertainty. This fact may imply a possible application of thermal analysis for estimating the effect of impurities in the realization of the aluminium point, especially for 6N-grade aluminium fixed-point cell as used in the present study.
Working Group 3 of the Consultative Committee for Thermometry is responsible for recommending methods to assess uncertainties in contact thermometry. Accordingly, it has now completed a guide summarizing the uncertainties in the realization of the standard platinum resistance thermometer subranges of ITS-90 between the triple point of neon (24.5561 K) and the freezing point of silver (961.78 • C). The document provides guidance to assess the uncertainties of both SPRT calibrations and temperature measurements. The document describes all known sources of uncertainty and influence variables, identifies key references in the literature that discuss, model or evaluate each effect, gives an indication of the typical magnitudes of the uncertainties, and provides propagation laws. This article is an overview of the guide emphasizing aspects that may be different from common practice, which includes: associating all uncertainty terms with a physical cause to ensure they can be propagated and to prevent double counting; uncertainty due to the oxidation state of the SPRT; uncertainty due to the isotopic composition of fixed-point substances; uncertainty due to impurities in fixed-point substances; and uncertainty due to nonuniqueness of the SPRT interpolations. The article gives a graphical summary of the total uncertainties in ITS-90 over the SPRT temperature range.
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