水三相点瓶的国际比对介绍

本文介绍了在1994～2000年间不同国家实验室参加的由国际计量局BIPM组织的水三相点瓶的国际比对.比对结果表明,不同国家实验室所使用的水三相点瓶多数情况下在±0.1mK范围内一致.     

EURAMET.T-K7 Key Comparison of Water Triple-Point Cells

The results of a EURAMET key comparison of water triple-point cells (EURAMET.T-K7) are reported. The equipment used, the measuring conditions applied, and the procedures adopted for the water triple-point measurement at the participating laboratories are synthetically presented. The definitions of the national reference for the water triple-point temperature adopted by each laboratory are disclosed. The multiplicity of degrees of equivalence arising for the linking laboratories with respect to the ??mother?? comparison CCT-K7 is discussed in detail.     

Doping Experiments in Mercury Triple-Point Cells

Mercury is one of the fixed points that can be obtained with higher purity, and it also can be measured with high accuracy; this turns impurities into one of the dominant sources of uncertainty. This article summarizes the first steps that CEM has carried out to start an exhaustive study of the influence of impurities on the triple-point-of-mercury temperature by means of doping experiments. The basis to choose the doping elements are stated, the procedure to dope the cells is described together with the careful performance of the weighing of the alloy components, and the results obtained for Zn and Ag are also shown.     

Isotopic Composition of Water Used in Triple-Point Cells

Isotopic analysis of the water used in KRISS triple point of water (TPW) cells was performed by three separate laboratories. The δD and δ ¹⁸O isotopic composition of six ampoules, made from two TPW cells, were analyzed by isotope ratio mass spectrometers. The analysis data showed that δD and δ ¹⁸O were − 62.17‰ and − 9.41‰ for the KRISS-2002-Jan cell, and − 36.42‰ and − 4.08‰ for the KRISS-2005-Jun cell. The temperature deviation of the triple point of water for these cells calculated from Kiyosawa’s data and the definition of the TPW were + 45.07μK for the KRISS-2002-Jan cell, and + 25.49μK for the KRISS-2005-Jun cell. The KRISS TPW temperature was + 92μK higher than the CCT-K7 KCRV after correcting for the deviation of the isotopic composition from Vienna Standard Mean Ocean Water.     

Effect of Impurities on Water Triple-Point Cells

Water triple-point cells are the basis for the definition of the kelvin and for the realization of the International Temperature Scale of 1990. The temperature differences between the cells are mainly caused by impurities arising in the cell water from the dissolution of the cell envelope (borosilicate glass or quartz). In order to investigate the effects of such impurities on the realized triple-point temperature, water triple-point cells doped with known amounts of Si and Na impurities ( \(0.1\,{\upmu }\hbox {mol}{\cdot }\hbox {mol}^{{-1}}\) to \(1\,{\upmu }\hbox {mol}{\cdot }\hbox {mol}^{{-1}}\) of Si and \(0.2\,{\upmu }\hbox {mol}{\cdot }\hbox {mol}^{{-1}}\) to \(2\,{\upmu }\hbox {mol}{\cdot }\hbox {mol}^{{-1}}\) of Na) were manufactured at VSL by adding gravimetric mixtures of a Si standard reference material and ultra high-purity water to the cell high-purity water. Water samples were taken from the manufactured cells, partitioned into three samples, and distributed to different laboratories for isotope and impurity analysis (inductively coupled plasma mass spectrometry, ICPMS). The results of two independent ICPMS analyses were compared with impurity calculations based on the gravimetric data of the prepared mixtures and manufactured cells. One undoped cell manufactured by UME and one undoped cell manufactured by VSL were intercompared at both VSL and SMD to demonstrate the equivalence of the manufacturing processes of UME and VSL. The triple-point temperatures realized by the doped cells and the undoped cell manufactured by VSL were measured at SMD. The results showed that, in doped cells, the equilibration time after the last freezing is directly dependent on the impurity concentration, and the temperature depression of doped triple-point-of-water cells is significantly greater than the values predicted by Raoult’s law for an ideal dilute solution.     

Investigation of the Parameters of Sealed Triple-Point Cells for Cryogenic Gases

An overview of the parameters of a large number of sealed triple-point cells for the cryogenic gases hydrogen, oxygen, neon, and argon is given that have been determined within the framework of an international star intercomparison to optimize the measurement of melting curves as well as to establish complete and reliable uncertainty budgets for the realization of temperature fixed points. Special emphasis is given to the question, whether the parameters are primarily influenced by the cell design or the properties of the fixed-point samples. For explaining surprisingly large periods of the thermal recovery after the heat pulses of the intermittent heating through the melting range, a simple model is developed based on a newly defined heat-capacity equivalent, which considers the heat of fusion and a melting-temperature inhomogeneity. The analysis of the recovery using a graded set of exponential functions containing different time constants is also explained in detail.     

Long Term Performance of Mercury Triple-Point Cells Realized at NIS-Egypt

The triple point of mercury is one of the defining fixed-points of the International Temperature Scale of 1990 (ITS-90). Its value was assigned to be 231.3456 K (?38.8344 °C) by ITS-90 and has a unique importance since it is the only fixed-point suggested by ITS-90 between 0.01 °C and ?190 °C. The thermal metrology laboratory of the National Institute for Standards has chosen, several decades ago, to realize this fixed point through batch of thermometric cells. In the present work, four cells, composing the batch of reference, are inter-compared. The results of these inter-comparisons, over a period of time that may reach a dozen of years, showed the excellent reliability of these cells. One cell of the batch, that is constructed thirty years ago, is still able to materialize a fixed point with an expanded uncertainty of 0.44 mK.     

Isotope and Impurity Content in Water Triple-Point Cells Manufactured at NMi VSL

The isotopic and impurity content of 15 water triple-point cells, manufactured at NMi VSL in the past three years, were investigated. The isotopic analyses were performed on water specimens sampled at three different stages of the manufacturing process. This allowed us to separate and quantify the influence of the source water and of the manufacturing process (distillation, degassing) on the final isotopic composition of the water in the cells. Inductively coupled plasma mass spectrometry (ICPMS) was conducted on selected water samples to investigate the potential contamination of the source water during the manufacturing process, and to evaluate the impact of impurities on the water triple-point temperature. The temperature differences among the manufactured cells were measured, and correlations between the observed differences and the results of isotope and chemical analysis were studied.     

Progress Towards the Determination of the Relationship of Triple-Point Temperature versus Isotopic Composition of Neon

Following the finalization of the work performed to establish the triple-point temperature versus isotopic composition relationship for protium (Metrologia 42, 171 (2005)) adopted into the ITS-90 definition by the International Committee for Weights and Measures (CIPM) in 2005, and a preliminary exploration of the variability in the triple-point temperature of neon gas samples arising from differences in isotopic composition (Anal. Chem. 77, 5076 (2005)), this article reports further progress toward the determination of a similar comprehensive relationship for neon, to be included in a future revision of the Technical Annexe to the ‘mise en pratique’ of the kelvin. This progress article mainly concerns a set of gas samples used for the neon triple-point measurements during CCT-K2, and subsequently, others for which the isotopic compositions were recently measured. Recent high accuracy measurements of the corresponding thermal data are now available for many of these samples, but not yet for all of them.     

The Impact of Isotopic Concentration,Impurities, and Cell Aging on the Water Triple-Point Temperature

In 2005, the National Institutes of Standards and Technology (NIST) and Fluke’s Hart Scientific Division initiated a study to validate the isotopic correction algorithm applied to the realization temperature of triple point of water (TPW) cells. Additionally, the study quantified the impact of water sample impurities on the TPW cell realization temperature. For this study, eight TPW cells containing water of the same nominal isotopic concentration as Vienna Standard Mean Ocean Water (VSMOW) were used. Five of the cells were manufactured with fused-quartz envelopes and the remaining three with borosilicate envelopes. One TPW cell of each type was uniquely designed so that water samples could be periodically removed to analyze the isotopic composition and to monitor any changes in water purity with time and thereby correlate changes in composition with changes in realization temperature. The borosilicate TPW cells gave an average drift of −13 μK · yr⁻¹ and the more stable fused-quartz TPW cells gave an average drift of −2 μK · yr⁻¹.     

不同来源的水三相点容器的比对

本文介绍了水三相点在开尔文热力学温度和ITS-90国际温标中的重要地位.重点介绍了麦克劳式水三相点容器内冰套的冻制方法及水三相点的复现.同时,NIM与ISOTECH同种结构的水三相点容器进行比对.比对结果表明,不同来源的水三相点容器复现的水三相点值在±0.04mK范围内一致.     

4种不同水源的水三相点容器的比对

为了研究水源对水三相点温度的影响,采用4种不同的水源并按照相同的制作工艺研制高质量的水三相点容器.同时,将这些容器进行了比对实验.比对结果表明:这些不同水源的水三相点容器复现的水三相点值在±0.02 mK范围内一致.故推断出水源对水三相点温度的影响很小.     

Comparison at NMIJ/AIST of the Triple Point of Neon Using Different Sealed Cells

At the National Metrology Institute of Japan (NMIJ), the triple point of neon was measured using an NMIJ sealed cell, NMIJ Ne-5, and a modular sealed-cell model, Ec2Ne, made by the Istituto Nazionale di Ricerca Metrologica (INRiM) in Italy, and the results were compared. The melting curves obtained with the NMIJ Ne-5 cell show narrow widths (0.1 mK) over a wide range of the inverse of the melted fraction (1/F) from 1/F = 1 to 1/F = 10, which is consistent with a previous report. On the other hand, the width of the melting curves obtained with the Ec2Ne cell is 0.15 mK from 1/F = 1 to 1/F = 10. The liquidus point T _tp estimated by the melting curves from F ~ 0.35 to F ~ 0.85 using the NMIJ cell is 0.05 mK higher than that using the Ec2Ne cell. The difference does not agree with the results obtained in an assay of the isotopic concentration from samples of the original Ne sources. The origin of the discrepancy has not been clarified yet.     

膨胀阀对陈列柜内温度分布影响的对比实验研究

对热力膨胀阀和电子膨胀阀控制下陈列柜内的温度分布做了实验研究。结果表明，在热力膨胀阀控制下，陈列柜内的温度分布情况与电子膨胀阀相差不大。在目前的实际应用中，热力膨胀阀基本能满足一般客户对陈列柜的使用要求，没有必要大规模进行电子膨胀阀的替代。     

Study on the Difference Between the Triple-Point Temperatures of ^{20}Ne and ^{22}Ne Using Sealed Cells

At the National Metrology Institute of Japan (NMIJ), the triple points of \(^{20}\) Ne and \(^{22}\) Ne were realized using modular sealed cells, manufactured by the Istituto Nazionale di Ricerca Metrologica (INRiM) in Italy to measure the difference of the triple-point temperatures of \(^{20}\) Ne and \(^{22}\) Ne. Standard platinum resistance thermometers (SPRTs) were used that were calibrated by NMIJ on the International Temperature Scale of 1990 (ITS-90). In previous reports, sealed cells of \(^{20}\) Ne and \(^{22}\) Ne were mounted one at a time in a cryostat and their triple points were realized in separate cool-downs (the single-cell measurement). In this study, first, the triple point was realized using the single-cell measurement for \(^{20}\) Ne and \(^{22}\) Ne cells. Second, the \(^{20}\) Ne and \(^{22}\) Ne cells were mounted together on the same copper block and their triple points were realized subsequently one after the other in the same cool-down of the cryostat (the double-cell measurement). The melting curves observed by the single-cell and the double-cell measurements were almost identical for each cell. The difference of the triple-point temperatures between the two cells, \(^{22}T -^{20}\!T\) , was estimated, not only using the subrange of SPRTs defined in the ITS-90 from 13.8033 K to 273.16 K (subrange 1) but also that defined from 24.5561 K to 273.16 K (subrange 2). The difference in \((^{22}T-^{20}\!\!T)\) between the subranges 1 and 2 is within 0.06 mK, which is caused by the subrange inconsistency in the ITS-90. The standard uncertainty in \((^{22}T-^{20}\!T)\) due to the subrange inconsistency is estimated to be 0.017 mK. After correction for the effects of impurities and other isotopes in the \(^{20}\) Ne and \(^{22}\) Ne cells, the difference in the triple-point temperatures between pure \(^{20}\) Ne and pure \(^{22}\) Ne is estimated to be 0.146 64 (5) K on subrange 1, which is consistent within the uncertainty with the former studies. When \(^{22}T-^{20}\!T\) for pure \(^{20}\) Ne and pure \(^{22}\) Ne is estimated on subrange 2, \(^{22}T-^{20}\!\!T\) becomes 0.146 60 (5), which agrees very well with the former reports of INRiM evaluating \(^{22}T-^{20}\!T\) on subrange 2.     

水声材料小样品声学性能不同测试方法比较

介绍了水声材料声学性能的3种不同的测试方法,通过对同种样品的性能测试,分析了不同测试方法的优缺点。结果表明,与行波法相比,脉冲法和驻波法测试可靠性较高。     

Reference Viscosity of Argon at Low Density in the Temperature Range from 290 K to 680 K

An all-quartz oscillating-disk viscometer of very high precision was used to measure the temperature dependence of the viscosity of argon in the limit of zero density. The measurements were based on a single calibration value at 298.15 K, which was calculated theoretically using an accurate ab initio pair potential for argon and the kinetic theory of dilute gases. The uncertainty of the experimental data is conservatively estimated to be 0.15 % temperature increasing to 0.2 % 680 K. The new data, as well as viscosities determined in 2007 at the National Institute of Standards and Technology in the range from 200 K to 400 K, agree excellently within ±0.1 % theoretically calculated viscosity of argon at zero density. On the contrary, the widely accepted viscosity data recommended by Kestin et al. (J Chem Phys 56:4119, 1972) deviate by as much as 0.9 %     

空气中氮气或氩气浓度对锆粉尘层着火温度的影响

为了探索抑制锆包壳剪切过程中锆粉着火的方法,采用粉尘层最低着火温度测定仪、红外热成像仪、真空手套箱等测定了不同粒径的锆粉尘层在空气和含不同浓度氮气、氩气的空气中的最低着火温度和火焰温度。结果得出:锆粉的中位粒径从2.4 μm升至71.7 μm,粉尘层最低着火温度从200 ℃升至390 ℃,表明粒径越小的锆粉着火敏感性越高;4种粒径的锆粉燃烧火焰最高温度都在1 776～1 913 ℃范围内,锆粉粒径较大时,燃烧的剧烈程度较低;氮气或氩气体积分数从60%～65%升至70% 85%时,锆粉尘层最低着火温度升至400 ℃,表明空气中高浓度的氮气或氩气对锆粉燃烧有抑制作用,且浓度越高,抑制作用越强,锆粉粒径越小,抑制效果越好。氩气的抑制效果强于氮气。