National Metrology Institutes Research Articles

Experimental installation of a reference source of low currents for calibration of electrometers

Today, there is great scientific interest in the possibility of implementing reference sources of low currents based on single-electron pumps using the single-electron tunneling effect and the modern definition of the SI system. However, the practical use of this effect in everyday metrological practice has not yet reached the stage of widespread use. Typically, for routine calibration work in laboratories, either mass-produced instruments (low current sources and meters, electrometers) are used, which are calibrated against higher standards, or specially designed precision current sources. The article describes a reference installation developed on the basis of the VNIIFTRI, where in the mode of generating ultralow currents the principle of forming a linearly increasing voltage on a reference capacitor is used. A simplified block diagram of the reference setup is shown. Issues of practical adjustment of modern electrometers are considered. The generalized results of participation in international comparisons on low currents EURAMET.EM-S44 “Comparison of ultra-low DC current sources” conducted by national metrological institutes in 2018–2020 are presented. The results of a metrological study of the calibration factor Q and an example of calculating the uncertainty budget of measurements carried out at the VNIIFTRI as part of these international comparisons are presented. The research described in the article to increase the accuracy of measurements of small and ultra-low currents of this level has valuable practical significance in the field of electrical measurements, in aeroionometry and metrology of ionizing radiation.

International comparisons in the field of measurement of specific adsorption of gases and specific surface area of solids: the optimal amount to ensure calibration and measurement capabilities

Indicators of the accuracy of measurements of the most important characteristics of the structure of porous and dispersed materials - specific adsorption of gases, specific surface area, specific pore volume and pore size – are considered. The performance of sorbents, catalysts and membranes in the chemical and petroleum industries, including the purification of substances and materials, depends on the values of these characteristics. It has been established that for mutual recognition of national standards and certificates of calibrations and measurements of porosity characteristics of solid substances performed by national metrological institutes, it is required to organize and successfully participate in three international key comparisons under the auspices of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology of the International Bureau of Weights and Measures. The results of the participation of national metrology institutes and designated organizations of Germany, China, Japan, Brazil, Turkey and Russia in three international key comparisons in the field of measurements of specific adsorption of gases (nitrogen, argon, krypton) and specific surface area of solids (zeolite, silicon oxides and aluminum) are presented. Carrying out the optimal number of comparisons makes it possible to register in the Key Comparison Database of the International Bureau of Weights and Measures the measuring and calibration capabilities of the national metrological institutes of the participating countries for various matrices in a wide range of measurements of specific adsorption of gases 0.001–25 mol/kg and specific surface area of solids 0.1–1500 m2/g. Based on the results of these three international key comparisons, 18 of broad calibration and measurement capabilities of the Russian participant, the D. I. Mendeleev Institute for Metrology, were entered into the Key Comparison Database; two of these items are currently undergoing examination, including reference materials produced by this institute. A comparative analysis of the results of measurements of the specific surface area of solids using nitrogen and krypton as adsorbates was performed. It has been established that the uncertainty of the measurement results of the specific surface area is significantly less in the case of using krypton as an adsorbate with a specific surface area of less than 1 m2/g, which is due to the higher values of the relative pressure of krypton compared to nitrogen. The use of calibration and testing laboratories in Russia of certified reference materials of sorption properties presented in the Key Comparison Database of the International Bureau of Weights and Measures will ensure metrological traceability in the field of measurements of porosity characteristics.

Survey of bidirectional transmittance distribution function measurement facilities by multilateral scale comparisons

In recent years, a growing demand for the capability of performing accurate measurements of the bidirectional transmittance distribution function (BTDF) has been observed in industry, research and development, and aerospace applications. However, there exists no calibration and measurement capabilities-entry for BTDF in the database of the Bureau International des Poids et Mesures and to date no BTDF comparison has been conducted between different national metrology institutes (NMIs) or designated institutes (DIs). As a first step to a possible future key comparison and to test the existing capabilities of determining this measurand, two interlaboratory comparisons were performed. In comparison one, five samples of three different types of optical transmissive diffusers were measured by five NMIs and one DI. By specific sample choice, the focus for this study lay more on orientation-dependent scatter properties. In comparison two, where one NMI, one DI, one university, and three industrial partners investigated their measurement capabilities, the dependence on the orientation was not assessed, but two additional samples of the same material and different thickness were measured. Results of the two comparisons are presented, giving a good overview of existing experimental solutions, and showing specific sample-related problems to be solved for improved future BTDF measurements.

Proficiency testing for event-specific quantification of genetically modified maize MON87427: Performance assessment based on the metrologically traceable reference values as assigned values

The Asia Pacific Metrology Program and the Accreditation Cooperation joint Proficiency Testing (PT) program for the quantification of genetically modified maize MON87427 was organized by the National Institute of Metrology, China, to enhance the measurement accuracy and metrological traceability in the region. Certified reference materials were employed as test samples; metrologically traceable certified reference values served as PT reference values (PTRVs) for evaluating the participants' results. The consensus values obtained from the participants were higher than the assigned values, potentially due to the systematic effects of DNA extraction process. The participants' relatively poor overall performance by the ζ-score compared with z-score demonstrates their need to thoroughly investigate quantification bias to elevate the measurement capability of genetically modified (GM) content and deepen their understanding of uncertainty estimation. This program confirmed the importance of using metrologically traceable reference values instead of consensus values as PTRV for reliable performance assessment.

Characterization of calibration solution certified reference material for polycyclic aromatic hydrocarbons by exact matching isotopic dilution mass spectrometry: a case study from the Brazilian Metrology Institute

Abstract Recertification is a common practice in National Metrology Institutes whenever advances are made in certified reference material (CRM) characterization procedures, which play a key role in metrological traceability. This article compares measurements of 16 priority polycyclic aromatic hydrocarbons (PAHs) in toluene by gas chromatography isotopic dilution mass spectrometry (IDMS) using either an calibration curve or the exact matching approach. The multi-point IDMS calibration curve was used on the original CRM certification and the exact matching approach was carried out on its recertification. The measurement uncertainties by exact matching approach (0.3%–1.0%) were approximately 5 times smaller than those obtained using the calibration curve (1.5%–4.4%) for all PAHs, reducing the uncertainty component due to characterization of PAH CRM. This new characterization study added reliability, increased accuracy and reduced the measurement uncertainty of the Inmetro CRM, with metrological traceability to the International System of Units. The exact-matching isotope dilution is an important technique to value assign organic compounds in CRMs, an action that consolidates the chemical metrology in the Brazilian Metrology Institute.

State primary standard of the unit of wave resistance in coaxial waveguides GET 75-2023

The issues of measuring the wave resistance and complex reflection and transmission coefficients of devices operating at ultrahigh frequencies in coaxial waveguides are considered. Measurements of these parameters are important in the development and production of communication and information transmission systems, radar and radio navigation systems. In order to ensure the uniformity of measurements, reproduction and transmission of wave resistance units and complex reflection and transmission coefficients to measuring instruments with coaxial connectors of type 1 mm in the frequency range 0.01–67 GHz, the state primary standard of the unit resistance in coaxial waveguides GET 75-2023 has been approved. It includes means of reproducing the unit of wave resistance, complex reflection coefficients, a comparator and comparison standards in a coaxial path with a cross section of 1.0/0.434 mm with a connector of type 1 mm. The expressions for calculating the parameters of coaxial waveguides with bimetallic conductors are refined. The technical characteristics and results of metrological studies of GET 75-2023 are presented. The results of the research confirmed the high accuracy of GET 75-2023, which has comparable metrological characteristics with the standards of national metrological institutes of other countries.

Rola i znaczenie cyfrowych mostków impedancji we współczesnej metrologii

The article presents current trends in impedance metrology of the highest accuracy. Attention was paid to digital non-quantum impedance bridges, which have been developed in many European National Metrology Institutes over the last decade. Particular attention in the article was devoted to the digital impedance bridge currently being developed at the Central Office of Measures in Warsaw. The conceptual diagram, system implementation and the progress of work related to the development of this bridge and its implementation in the near future into the national measurement system are presented as well.

A 10 V Transfer Standard Based on Low-Noise Solid-State Zener Voltage Reference ADR1000

Voltage standards are widely used to transfer volts from Josephson voltage standards (JVSs) at national metrology institutes (NMIs) into calibration labs to maintain the volts and to transfer them to test equipment at production lines. Therefore, commercial voltage standards based on Zener diodes are used. Analog Devices Inc. (San Jose, CA, USA), namely, Eric Modica, introduced the ADR1000KHZ, a successor to the legendary LTZ1000, at the Metrology Meeting 2021. The first production samples were already available prior to this event. In this article, this new temperature-stabilized Zener diode is compared to several others as per datasheet specifications. Motivated by the superior parameters, a 10 V transfer standard prototype for laboratory use with commercial off-the-shelf components such as resistor networks and chopper amplifiers was built. How much effort it takes to reach the given parameters was investigated. This paper describes how the reference was set up to operate it at its zero-temperature coefficient (z.t.c.) temperature and to lower the requirements for the oven stability. Furthermore, it is shown how the overall temperature coefficient (t.c.) of the circuit was reduced. For the buffered Zener voltage, a t.c. of almost zero, and with amplification to 10 V, a t.c. of <0.01 µV/V/K was achieved in a temperature span of 15 to 31 °C. For the buffered Zener voltage, a noise of ~584 nVp-p and for the 10 V output, ~805 nVp-p were obtained. Finally, 850 days of drift data were taken by comparing the transfer standard prototype to two Fluke 7000 voltage standards according to the method described in NBS Technical Note 430. The drift specification was, however, not met.

Precision of diamond turning sinusoidal structures as measurement standards used to assess topography fidelity

In optical surface metrology, it is crucial to assess the fidelity of the topography measuring signals. One parameter to quantify this is the small-scale fidelity limit T FIL defined in ISO 25 178-600:2019. To determine this parameter, sinusoidal structures are generated, where the wavelengths are modulated according to a discrete chirp series. The objects are produced by means of ultra-precision diamond face turning. Planar areas and regions with slopes below 4° could be produced with form deviations of ≲10 nm. An initial estimate of the cutting tool’s nose radius resulted in a deviation that caused the ridges of the structures to be too narrow by approximately 150 nm, while the trenches were too wide. At the bottom of narrow trenches, deviations are observed in the form of elevations with heights of about 20 to 100 nm. The measurement standard investigated in this study has also been used to characterise optical instruments in a round-robin test within the European project TracOptic, which requires precise knowledge of the geometry of all structures. The geometry of the topography, cosine structures superimposed with form deviations, was measured using the Met. LR-AFM metrological long-range atomic force microscope of the German National Metrology Institute.

Development of an insulin-like growth factor-1 certified reference material by SI-traceable isotope-dilution mass spectrometry

In this study, an insulin-like growth factor-1 (IGF-1) certified reference material (CRM) was developed by the National Institute of Metrology (NIM), and two different principles for evaluating the IGF-1 CRM were established. After optimisation of the acid hydrolysis conditions (110 °C, 36 h), quantitative determination of peptide purity, and chromatographic separation and mass spectrometric detection, amino acid analysis-based high-performance liquid chromatography combined with isotope-dilution tandem mass spectrometry (AAA-HPLC-IDMS/MS) and peptide analysis-based HPLC-IDMS/MS (Peptide-HPLC-IDMS/MS) were used for certified value assignment; the results obtained were 136.28 and 135.01 μg/g, respectively, which were in good agreement. These results were subjected to the normal distribution test, outlier test, and method consistency test. The homogeneity and stability of the reference materials were also examined, and the uncertainty introduced in the experimental process was calculated. The final certified value was (136 ± 15) μg g−1 (k = 2). The CRM was found to be stable for at least six months when stored at −70 °C and for 7 d when stored at higher temperatures (−20 °C, 4 °C, 25 °C, or 40 °C). The CRM is expected to be used as a primary calibrator for quality control in biopharmaceutical production and clinical diagnostics.

MSL goniospectrophotometer measurement model

Measurements of both hemispherical reflectance and the bidirectional reflectance distribution function (BRDF) are of interest to a wide range of industries including computer graphics, remote sensing, lighting design, and cosmetics. The scale of directional reflectance is often realised at national metrology institutes using goniospectrophotometers, and by integrating BRDF measurements made over the hemisphere, the scale of hemispherical reflectance can also be realised. This paper describes the measurement model for BRDF and hemispherical reflectance using the MSL goniospectrophotometer, which uses rotation stages to adjust the angle of the sample. The measurement model is applied to measurements of a white Spectralon sample and a white ceramic tile to demonstrate the performance of the instrument. The relative standard uncertainty in the BRDF of a white Spectralon sample at 550 nm is less than 0.1% for in-plane measurements, while the relative standard uncertainty in the hemispherical reflectance of a white Spectralon sample at 560 nm is 0.27%.

Circular Section Metal Wall Cut-Off Wave guide Accurate Calculation when used as a Standard Attenuator

In this paper, the mathematical analysis is carried out from many angles, so that the theoretical calculation problem of the circular metal wall cut-off wave guide used as a premary attenuation standard is completely solved, and the Chinese national standard of the attenuation quantity is established. The benchmark was completed by the Chinese National Institute of Metrology (NIM) with an accuracy of 5×10-5; Reach the international advanced level. The calculation accuracy provided in this paper is 10-6~10-7. This is a good example of a project combining theory and practice.

Multi-kilowatt cw laser power measurement comparison between national standards

We present here the first comparison between National Metrology Institutes of high accuracy continuous wave optical power measurements in the kilowatt regime. The National Institute of Standards and Technology (NIST) performed measurements with a power meter relying on photon momentum. The Physikalisch-Technische Bundesanstalt (PTB) performed measurements with a modified off-the-shelf thermal power meter. The non-absorbing photon momentum measurement approach permits the two power meters to measure the same laser beam optical path simultaneously, resulting in a direct comparison of the meters supported by an optical system to accommodate differences in instrument settling times. The results show agreement within the expanded uncertainties for each instrument. NIST and PTB illustrate a degree of equivalence of 0.49% with an expanded uncertainty of 1.37% (k = 2) for an average result across all power levels.

Air kerma reference field with high energy photons using a 15 MeV electron beam from a clinical linear accelerator.

In the medical and nuclear fields, there are environments where exposure to photons with energies above several MeV can result in problems. The National Metrology Institute of Japan has developed a high-energy photon field using a 15 MeV electron beam of a clinical linear accelerator with a copper target and an aluminium filter unit to facilitate dosimeter calibration in terms of air kerma. To determine the air kerma rate, the energy fluence distribution at a reference point was calculated, and both calculations and experiments evaluated the effective energy and spatial dose distribution. Moreover, to validate the air kerma measurement, two commercial cavity chambers were calibrated in a developed photon field. The results obtained exhibited a 4% difference compared with those in a Co-60γ-ray reference field.

Modern components of activities and models of national metrological institutes

Economies and societies are constantly changing and developing, so national metrological systems also need changes and adaptation to modern conditions. National Metrological Institutes (NMI), as one of the main elements of the national metrological infrastructure, are responsible for the development and maintenance of national standards, conducting scientific research in the field of metrology. There are significant risks due to the lack of an effective metrology infrastructure at the national level. The article analyzes the main modern components of NMI activities and offers options for models of NMI functioning depending on the existing metrological infrastructure, taking into account various risks of the operation of such infrastructure.

Design and implementation of a kind of high precision temperature compensating system for silicon-on-sapphire pressure sensor

In order to reduce the temperature effects on the testing accuracy of the silicon-on-sapphire high-temperature large-range pressure sensor, a miniaturized portable silicon-on-sapphire pressure sensor temperature compensation system is designed and implemented after solving the following three issues: temperature compensation structure design, temperature compensation circuit fabrication, and temperature compensation algorithm implementation. The simulation results indicated that the temperature of the test circuit part of the package structure is close to 30 °C at an ambient temperature of 30 °C, with the sensor sensitive element at 250 °C working temperature and 28 MPa ultimate pressure. Regarding to the problem of large sensor drift in high-temperature environments, a temperature compensation algorithm combining least squares and Lagrange interpolation is designed based on the input and output characteristics of the sensor. The algorithm improves the computational efficiency while also increasing the hysteresis error and nonlinear deviation of the sensor to 0.028%. The test results of the NIM (National Institute of Metrology, China) show that the measurement accuracy of the sensor is higher than 1‰ FS within −20 °C to 140 °C and higher than 3‰ FS within 140 °C to 250 °C.

Final report for SIM.QM-S12: supplementary comparison for trace elements in natural water

Main textThe SIM Supplementary Comparison SIM.QM-S12 for Trace Elements in Natural Water was undertaken to assess and demonstrate the analytical capabilities of national metrology institutes (NMIs) and designated institutes (DIs) of SIM members (or other regions) for the accurate determination of trace elements in natural water at µg/kg levels.Evidence of successful participation in formal, relevant international comparisons is needed to document calibration and measurement capability claims (CMCs) made by NMIs and DIs.Seventeen NMIs and DIs participated. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of arsenic, cadmium, lead and antimony in a natural mineral groundwater that was spiked with the respective elements. A variety of instrumental techniques including inductively coupled plasma mass spectrometry (ICP-MS), isotope dilution ICP-MS (ID-ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), electrothermal atomic absorption spectrometry (ETAAS) and hydride generation flame atomic absorption spectrometry (HG-FAAS) were used by the participants for the determination.The NIST decision tree was used to assign the SCRV estimate for the proposed measurands and to calculate the degrees of equivalence of each national measurement standard following the IAWG Guidance on Using NIST Decision Tree for Comparison Reporting from 30 June 2023.Successful participation in SIM.QM-S12 demonstrates measurement for determination of elements in water matrices. Considering the IAWG Core Capability Matrix, this material falls into the matrix challenge called "Water/aqueous", which corresponds to the CCQM amount-of-substance category fresh water, and so will support CMCs for the metalloids and semi-metals at mass fraction levels below 50 µg/kg (As and Sb measurements) and transition elements at mass fraction levels below 50 µg/kg (except Hg) (for Cd and Pb measurements).To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Final report, ongoing key comparison BIPM.QM-K1, ozone at ambient level, comparison with NIM, Oct 2023

Main textAs part of the ongoing key comparison BIPM.QM-K1, a comparison has been performed between the ozone national standard of China maintained by the National Institute of Metrology (NIM) and the common reference standard of the key comparison, maintained by the Bureau International des Poids et Mesures (BIPM). The instruments have been compared over a nominal ozone amount fraction range of 0 nmol mol−1 to 500 nmol mol−1.To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Subsequent bilateral key comparison study - organic solvent calibration solution - gravimetric preparation and value assignment of aflatoxin B1 (AfB1) in acetonitrile (ACN)

Main textThe original CCQM-K154.b comparison was coordinated by the Bureau International des Poids et Mesures (BIPM) and the Chinese National Institute of Metrology (NIM) on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA) and/or have participated in the BIPM's Mycotoxin Metrology Capacity Building and Knowledge Transfer (MMCBKT) project as part of its "Metrology for Safe Food and Feed in Developing Economies" Capacity Building Programme.Gravimetrically-prepared solutions having an assigned mass fraction of specified organic analytes are routinely used to calibrate measurement processes for the quantification of the same analytes in matrix samples. Appropriate assignments of the property value and associated uncertainty of calibration solutions thus underpin the traceability of routine analysis and are critical for accurate measurements. Evidence of successful participation in relevant international comparisons is needed to document calibration and measurement capability claims (CMCs) made by national metrology institutes and designated institutes. In total, eleven NMIs/DIs participated in the Track C, Model II, Key Comparison CCQM-K154.b [Gravimetric preparation and value assignment of aflatoxin B1 (AfB1) in acetonitrile (ACN)] for emerging areas of global interest and innovation. Participants were requested to gravimetrically prepare calibration solutions and value assign the mass fractions, expressed in mg/kg, of aflatoxin B1 (AfB1) in the acetonitrile (ACN) solution. Study samples, with assigned values and associated uncertainties were prepared by the comparison participants and sent to the coordinating laboratory for comparison. The Key Comparison Reference Values (KCRVs), calculated form values measured by the coordinating laboratory based on calibrations obtained from independent gravimetrically prepared calibrant solutions, agreed with participants reported values, within their stated uncertainties.AfB1 was selected to be representative of polar aflatoxins. Aflatoxins are a class of mycotoxins generally produced by fungi of the genus Aspergillus. It was anticipated to provide a challenge representative for the gravimetrical preparation and value assignment of calibration solutions in the mass fraction range of 2 mg/kg to 50 mg/kg of mycotoxins with broadly similar structural characteristics.In the original study CCQM-K154.b, nine participants of the MMCBKT programme were provided with a stock solution having a known AfB1 mass fraction and expanded uncertainty to use to gravimetrically prepare and value assign a calibration solution. Three NMIs/DIs also participated using their own calibration solutions. The use of in-house solutions required anadditional capacity to undertake a fit-for-purpose purity assessment. NIM was the only NMI participating using both the MMCBKT based and their own in-house assigned solutions in order to connect the two different groups.It was decided to propose separate KCRVs for each of the two ampoules provided by the participating NMIs/DIs based on the AfB1 mass fraction. This allowed participants to demonstrate the efficacy of their implementation of the approaches used to gravimetrically prepare calibrations solutions and to assess the AfB1 mass fraction.The majority of the AfB1 mass fraction KCRVs (wKCRV) for CCQM-K154.b spanned a mass fraction range of 2.02 mg/kg to 31.57 mg/kg. The relative expanded uncertainties U(wKCRV) ranged from 0.69 % to 2.93 %. Inspection of the degree of equivalence plots for the AfB1 mass fraction assignments in CCQM-K154.b indicated that there was an excellent agreement of results. Solely, the AfB1 mass fraction assignments of the INRAP (Institut National de Recherche et d'Analyse Physico-Chimique, Tunisia) did not agree with the KCRVs. It was found that the samples were altered as a result of an acid contamination.The INRAP has produced a new batch of AfB1 calibration solution using the AfB1 stock solution originally provided to MMCBKT participants to be able to demonstrate the efficacy of their implementation of the approaches used to gravimetrically prepare calibrations solutions and to assess the AfB1 mass fraction. The BIPM organized the present subsequent bilateral comparison CCQM-K154.b.1 to assess the new batch of AfB1 calibration solution of the INRAP. Inspection of the degree of equivalence plots for the AfB1 mass fraction assignments indicated that there is an excellent agreement of the INRAP results for CCQM-K154.b.1.To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Final report of APMP.AUV.V-S1: supplementary comparison on calibration of laser tachometers using mechanical generators

Main textThis is the final report for APMP supplementary comparison APMP.AUV.V-S1 in the area of 'vibration' (quantity of rotational speed). The aim of this comparison was to compare primary measurements of rotational speed in the range from 10 r/min to 99 999 r/min. Two Metrology Institutes from APMP have participated in the comparison with National Institute of Metrology, P.R. China as pilot lab. Both laboratories used mechanical generators as standard equipment and provided their calibration results, which were all consistent within their declared expanded uncertainties for the measurement results except for 10 r/min. Both participants contributed to the SCRVs calculated for thirteen rotational speed comparison values. NMC was not consistent within their declared expanded uncertainties at 10 r/min. Further improvements of their calibration devices and uncertainty evaluations will provide more accurate and reliable measurement results in the future.To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.The final report has been peer-reviewed and approved for publication by the CCAUV, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).