国际90温标关键比对3的评述

1998年BIPM温度咨询委员会 (CCT)组织了从氩三相点到铝凝固点 90温标定义固定点的复现值的国际比对 ,称为CCT关键比对 3。中国计量科学研究院作为中国国家实验室参加了这一比对 ,给出了全部 8个定义固定点的复现值。本文通过对已公布的结果进行分析和评述 ,使国人了解国际ITS 90温标复现情况的现状 ,以及我国在此次比对结果中的位置 ,进而指导我们今后进一步提高ITS 90复现和维护水平。     

新型水三相点瓶与国家基准水三相点瓶的比对

2002年11月由国际计量局组织的水三相点瓶的国际关键比对（简称CCT－K7），中国计量科学研究院研制出新型结构的水三相点瓶，本文详细介绍了新型水三相点瓶，并将其与国家基准水三相点瓶进行了比对，同时，给出了比对结果。     

0-5kN-10kN力值国际关键比对的评述

从1999年起，国际计量局（BIPM）质量及相关量咨询委员会（CCM）组织了0-5kN．10kN（CCM．F-K1）、0-50kN-100kN（CCM.F-K2）、0-500kN-1000kN（CCM．F-K3）和0-2MN．4MN（CCM．F．K4）等4个量程的力值国际关键比对，旨在保证世界各国间力值的准确一致。中国计量科学研究院作为中国国家实验室参加了全部4项力值国际关键比对。介绍了CCM．F-K1．a0-5kN．10kN力值国际关键比对的比对方法和比对结果，对提高我国力值计量领域的研究水平，以后组织或参加力值国际和国内力值比对及进行各实验室问能力验证具有一定的指导意义。     

铝凝固点及银凝固点容器国际关键比对评述

介绍了国际计量局（BIPM）温度咨询委员会（CCT）关键比对4即铝凝固点及银凝固点容器国际比对。采用固定点容器直接比对的形式进行，共11个国家实验室参加了该项比对，介绍了比对的组织、比对过程、实验方法以及参考值的选取，同时给出了比对结果及比对等效图。     

新型水三相点瓶与国家基准水三相点瓶的比对

2 0 0 2年 1 1月由国际计量局组织的水三相点瓶的国际关键比对 (简称CCT -K7) ,中国计量科学研究院研制出新型结构的水三相点瓶。本文详细介绍了新型水三相点瓶 ,并将其与国家基准水三相点瓶进行了比对。同时 ,给出了比对结果。     

传递水三相点容器在国际计量局的比对

国际计量局作为主导实验室组织了由20个国家计量标准实验室参加的CCT-K7水三相点容器国际关键比对.按照比对协议,参加者均选择了1个校准的传递容器送到国际计量局与两个共同的参照容器进行比对.介绍了国际计量局的比对,包括:冻制方法、实验装置、测量步骤、比对结果及相应的不确定度评定.比对结果表明:多数水三相点容器在0.15 mK范围内一致.     

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.     

水三相点瓶的国际比对介绍

本文介绍了在 1 994～ 2 0 0 0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。     

黏度量值第二次国际关键比对(CCM.V-K2)

黏度量值国际关键比对由国际计量委员会（CIPM）的质量及相关量咨询委员会（CCM）下属的黏度工作组（WGV）组织实施,每4年进行1次。由于完全符合“国家计量标准和国家计量院开具的校准证书的互认协议”（MRA）,关键比对具有很大的权威性,参加单位均为各国最高计量研究机构。     

直径测量国际比对中标准器和测量方法的统一与讨论

国际比对是国际计量局的重要工作任务之一,比对项目由国际计量局的各个专业咨询委员会确定.由于直径尺寸是精密制造业中一项关键的测量内容,国际计量局长度咨询委员会(BIPM CCL),将"直径标准尺寸"列为长度国际关键比对项目(包括内直径和外直径测量).参加比对的实验室为12个国家的计量院.关于直径标准器(环规和塞规)和测量问题等,参加比对的实验室进行了长时间的讨论,最终确定了比对标准器规格尺寸、测量位置、温度修正以及测量和评定方法.     

Isotopic Effects on the Temperature of the Triple Point of Water

An investigation into the effects of isotopic composition on the triple point temperature of water has been carried out at the National Institute of Metrology (NIM), China, since redefinition of the kelvin with respect to Vienna Standard Mean Ocean Water (V-SMOW) was officially proposed by the Consultative Committee for Thermometry (CCT) in 2005. In this paper, a comparison of four cells with isotopic analyses and relevant results corrected for isotopic composition, employing the isotope correction algorithm recommended by the CCT, is described. The results indicate that, after application of the corrections, the maximum temperature difference between the cells drops from 0.10 mK to 0.02 mK and that these cells are in good agreement within 0.02 mK. Also, temperature deviations arising from isotopic variations fall in the range from −55.9 μK to + 40.7 μK. We consider that the distillation temperature and degassing time of the production procedure lead to isotopic variations.     

Isotopic Correction of Water-Triple-Point Cells at NMIJ

The twenty-one participating laboratories in the international key comparison of water-triple-point cells (CCT-K7) can be classified into three groups: two laboratories that corrected the effect of the isotopic composition of water, four laboratories that had information on the isotopic composition but did not correct the effect, and the remaining laboratories that had no information. There were significant differences in the realized national standard for the triple point of water (TPW) between those laboratories that applied the isotopic correction and those that did not. The isotopic correction is now considered essential for the triple point of water. Since the National Metrology Institute of Japan (NMIJ) did not apply the isotopic correction and estimated large uncertainties at the time of the CCT-K7 comparison, we subsequently developed new cells for the TPW to improve the reliability and to reduce the uncertainty of the realization as a national reference. The isotopic compositions of seven cells were analyzed, and a chemical impurity analysis of one cell was performed. The good consistency among seven cells was shown in the results obtained when the isotopic correction was applied to the realized temperatures measured experimentally. The expanded uncertainty of the new national reference of NMIJ is estimated to be 49 μK (k = 2), and as a result of this improvement, the expanded uncertainty for calibrating a water-triple-point cell is 80 μK. The previous reference of NMIJ, reported in CCT-K7 to have an expanded uncertainty of 302 μK, is 42 μK lower than the new one. The new reference value is within the uncertainty of the previous national reference, and the new uncertainty is completely covered by the previous uncertainty. Furthermore, the new reference of NMIJ shows good agreement with the national references of the six laboratories able to apply isotopic corrects to their results for CCT-K7. These facts confirm the validity and the linkage to the CCT-K7 of both the previous and the new national references of NMIJ.     

Analysis of the Comparison of TPW Realizations in Europe in Light of CCT Recommendation 2 (CI-2005)

Three comparisons of different triple-point-of-water (TPW) realizations in Europe have been organized under the auspices of EUROMET (EUROMET Projects 278, 549, and 714). Thirty European national metrology institutes were involved in these three comparisons that took place from 1994 to 2005. The aim of these successive projects was to assess the uncertainties associated with the practical realization of the triple point of water in Europe. Fifty-four TPW local cells were compared to a traveling standard cell (ref 679) circulated with an isothermal enclosure. The same equipment was used for the three projects, and LNE-INM regularly checked the stability of the TPW standard cell. Recently, LNE-INM has devoted efforts to bring the French standard at the triple point of water into close agreement with CIPM Recommendation 2 (CI-2005). The isotopic fractionation between water and ice when the cell is in use was experimentally studied. Several new TPW cells delivered by the manufacturer with water samples were added to our batch of reference cells. A French laboratory analyzed the isotopic compositions of these samples. These actions allow the French national definition of temperature at the triple point of water to be changed. A new temperature was associated with TPW cell 679 in agreement with the CIPM recommendation. In this presentation, the latest TPW cell measurements carried out by LNE-INM are presented. The results from EUROMET Projects 278, 549, and 714 are investigated in light of these changes.     

Implementing a New Group of TPW Cells as National Standard: Impact on Calibration Services

The definition of the kelvin is based on the triple-point temperature of highly pure water having the isotopic composition of ocean water (more specifically, the isotopic composition is equivalent to that of VSMOW). Belgian national metrology realizes the triple point of water (TPW) as the mean of temperatures measured in three sealed cells. In order to take into account the isotopic composition effect on TPW temperature, the ensemble of cells was replaced in 2006. Three new cells, with isotopic analysis of the contained water, were bought from different manufacturers. The new group of cells was compared to the old TPW national realization in order to quantify the effect of moving towards a new reference. Two different standard thermometers were used in all the cells to take 10 daily measurements on two different ice mantles. The measured resistances were corrected for hydrostatic head, self-heating, and isotopic composition (when available) before calculating the difference. A difference of about 87 μK was found between the old and the new national references. This difference is transferred to customers’ thermometers and cells through calibrations, and the change has to be documented in each new calibration certificate. An additional consequence of the new ensemble cell implementation is the significant reduction in the spread of deviations of individual cells from the mean temperature. The maximum difference between two cells of the ensemble is 96 μK for the old reference cells and 46 μK for the new reference cells corrected for isotopic composition effects.     

高准确度水三相点容器

水三相点的高精度复现及准确测量是保证国际温标ITS-90实施的关键。水三相点容器内高纯水的同位素组成会影响复现的水三相点温度值。为了提高水三相点复现水平,减小氢氧同位素的影响,研制了带有氢氧同位素分析的石英及硼硅玻璃高准确度水三相点容器。为了评价容器的性能,开展了硼硅玻璃和石英水三相点容器的比对。实验结果表明:同位素修正前,石英玻璃和硼硅玻璃水三相点容器复现的水三相点在0.058mK范围内一致;同位素修正之后,容器之间的差异在0.017mK范围内一致。采用高准确度水三相点容器复现水三相点的扩展不确定度为0.066mK(k=2)。     

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.     

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.     

VSMOW Triple Point of Water Cells: Borosilicate versus Fused-Quartz

To investigate an ideal container material for the triple point of water (TPW) cell and to reduce the influence to the triple-point temperature, due to the deviation of the isotopic composition of the water, both borosilicate and fused-quartz glass shelled TPW cells with isotopic composition substantially matching that of Vienna Standard Mean Ocean Water (VSMOW) were developed and tested. Through a specially designed manufacturing system, the isotopic composition, δD and δ¹⁸ O, of the water in the TPW cell could be controlled within ±10‰ (per mil) and ±1.5‰, respectively, resulting in control of the isotopic temperature correction to better than ± 8 μK. Through an ampoule attached to the cell, the isotopic composition of the water in the cell could be individually analyzed . After manufacture, the initial triple-point temperatures of the two types of cell were measured and compared to assess the quality of the cells and manufacturing process. Cells fabricated with the new system agree within 50 μK. Two innovatively designed borosilicate and fused-quartz TPW cells were made, each with six attached ampoules. One ampoule was removed every 6 months to track any changes in purity of the water over time.     

液氮冻制冰套法对水三相点温度的影响

介绍了液氮作为冷却剂在水三相点容器内冻制冰套的方法。利用该方法同时在两个不同真空度的水三相点容器内分别冻制冰套。通过实验，研究了此方法对所复现的水三相点温度的影响。实验结果表明：冻制过程中产生的应力以及开始生成的小冰晶引起水三相点温度偏低；并且，其对水三相点温度的影响随着水三相点容器内真空度的降低而增大。随着应力慢慢消除，小冰晶逐渐长大为大冰晶，所复现的水三相点值逐渐回升并趋于稳定。因此，为了高精度复现和准确测量水三相点，采用该冻制方法时，必须将冰套老化至少5天以后，才可以消除其对水三相点温度的影响。     

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.