A traceable technique to calibrate dc current shunts and resistors in the range from 10 μΩ to 10 mΩ

A traceable to dc resistance and dc voltage National Standards measurement technique to calibrate dc current shunts and resistors in the range from 10 μΩ to 10 mΩ has been developed at National Institute of Metrological Research (INRIM) in addition to the primary reference system for low value resistors calibration. This technique is applicable in secondary and industrial metrological laboratories. It is based on a volt-amperometric method, to compare an unknown shunt with a standard one in 1:1 or 1:10 ratios. In the setup are involved: a dc current calibrator and a current generator to supply currents respectively up to 100 A and up to 1200 A, with a switch to reverse the current, two 7 1/2 digit nanovoltmeters (nVs) for the acquisition of the voltage on the standard and under calibration shunts and two Tinsley 100 μΩ and 1 mΩ standard shunts kept in mineral oil and with a cooling system. An optional variation in the procedure that can reduce the measurement uncertainties is discussed. The 2σ relative capabilities of the technique span from 6.0 × 10⁻⁶to 4.6 × 10⁻⁴. Compatibility results with the INRIM reference measurement system for low value resistors calibration are also given.     

FEA calculation of pressure distortion coefficients of gas-operated pressure balances – EURAMET project 1039

Finite element analysis methods were developed and applied to gas piston–cylinder units (PCUs) of piston- and cylinder-floating configuration (2, 5, 10 and 20) cm² nominal effective area, operated in gauge and absolute mode at pressures (0.06–7.5) MPa to determine their zero pressure and pressure-dependent effective areas, as well as pressure distortion coefficients (λ) with associated uncertainties. Real dimensional properties of the PCUs were used. λ were found to be independent of gas (ideal, N₂, He) within the viscous flow model, but strongly dependent on the gap shape, operation mode and elastic properties. Results demonstrate good agreement for λ, with its uncertainty for different PCUs varying between (0.03 and 0.21) × 10⁻⁶ MPa⁻¹ corresponding to maximum relative uncertainties in pressure of (0.07–0.34) × 10⁻⁶.     

Newly developed standard conductance element for in situ calibration of high vacuum gauges

A new leak element, which is named as “standard conductance element (SCE)”, has been developed for in situ calibration of ionization gauges (IGs) and quadrupole mass spectrometers (QMSs). The SCE is made of a stainless-steel sintered filter with the pore size of less than 1 μm. Since the gas flow through the SCE satisfies the molecular flow condition even at the pressure up to 10⁴ Pa, some useful characteristics of molecular flow are available. The SCE is supplied to users with a calibration certificate described its molecular conductance. Users can introduce optional test gases with the known flow rate to their vacuum chamber through the SCE in their laboratories. The overview of the SCE, the calibration method and recommended practices are introduced.     

Characterization of MEMS piezoresistive pressure sensors using AFM

Atomic force microscope (AFM) is adapted to characterize an ultrasensitive piezoresistive pressure sensor based on microelectromechanical system (MEMS) technology. AFM is utilized in contact mode to exert force on several different micromachined diaphragm structures using a modified silicon cantilever with a particle attached to its end. The applied force is adjusted by changing the trigger voltage during each engage step of the probe-tip on the diaphragm surface. The contact force is determined from the force plots obtained for each trigger voltage in advanced force mode. Low force values in the range of 0.3–5 μN have been obtained with this method. This force induces strain on the bridge-arm of the diaphragm where the polysilicon resistor is located. The resultant change in the resistance produced due to varying force/pressure is measured using a delta mode current–voltage (I–V) measurement set-up. The contact mode AFM in conjunction with a nanovoltmeter enables the calibration of very sensitive force sensors down to 0.3 μN.     

1–15,000 Pa Absolute mode comparisons between the NIST ultrasonic interferometer manometers and non-rotating force-balanced piston gauges

The National Institute of Standards and Technology (NIST) Low Pressure Manometry Project maintains and operates primary standard ultrasonic interferometer manometers (UIMs) over the pressure range of 1 mPa to 360 kPa. Over the past decade a new type of customer gauge, the non-rotating force-balanced piston gauge or FPG (model 8601, DH Instruments, a Fluke Company¹) has been introduced to the standards community that covers the range of ≈1–15,000 Pa and is capable of both absolute and differential measurement modes. Since 2002, NIST customers² have requested that four different FPG units be compared to the NIST primary pressure ultrasonic interferometer manometer standards (UIMs). The results of the comparisons were that all four FPG units were within manufacturers stated uncertainty (0.008 Pa + 30 × 10⁻⁶ × P for absolute mode) when compared against the NIST UIMs at pressures between 10 Pa and 15,000 Pa (absolute mode). At pressures between 5 Pa and 10 Pa, the results were generally within manufacturer’s specifications. Below 5 Pa some of the FPG units were outside of manufacturer’s uncertainty specifications. The use of an isolating capacitance diaphragm gauge (CDG) was necessary during the comparisons to prevent humidified gas from the FPG from entering the NIST 160 kPa mercury UIM primary pressure standard. The results of these four different comparison tests will be discussed in detail, along with test conditions, equipment set-up, and test uncertainty analysis.     

Proficiency test for effective area determination of a pneumatic pressure balance in Mexico

A pneumatic pressure proficiency test for effective area determination of a pressure balance was performed among 4 accredited calibration laboratories in Mexico. CENAM provided the reference values (making initial and final calibrations) and was the pilot laboratory. The Mexican Accreditation Entity (ema) collaborated. The participants calibrated, by cross floating, a Wika pressure balance model CPB 5000 with accuracy class 0.015% of the reading in the range 0.7–7 MPa. The calibration pressures were 0.7, 1.4, 2.1 3.5, 4.2, 5.6 and 7.0 MPa. For A₀ and A_e, the normalized error equation was used to compare the results of the laboratories with CENAM’s reference values. The results obtained were satisfactory (E_n did not exceed the compatibility limit, −1 ⩽ E_n ⩽ 1).     

Hamon 10 × 100 MΩ resistor based traceable source for calibration of picoammeters in the range 100 pA–100 nA

This paper describes a measurement method developed at National Institute of metrological Research (INRIM) to calibrate picoammeters in dc current from 100 pA to 100 nA. The current source is based on a traceable to the dc resistance national standard 10 × 100 MΩ Hamon resistor developed at INRIM and on a traceable to the dc voltage national standard high precision dc voltage calibrator. The expanded uncertainties of the method for the calibration of picoammeters span from 9.4 × 10⁻⁴ for the gain of a picoammeter at 100 pA to 4.0 × 10⁻⁴ for the gain at 100 nA. A detailed uncertainties budget at 10 nA level and the results of a comparison with a different technique are also reported.     

Ordinal measurement,preference aggregation and interlaboratory comparisons

The classical problem of a single consensus ranking determination for m rankings of n alternatives has a potential of wide applications in information technologies, and particularly in measurement and instrumentation. The Kemeny rule is one of deeply justified ways to solve the problem allowing to find such a linear order (Kemeny ranking) of alternatives that a distance (defined in terms of a number of pair-wise disagreements between rankings) from it to the initial rankings is minimal. But the approach can result in considerably more than one optimal solutions what can reduce its applicability. By computational experiments outcomes, the paper demonstrates that a set of Kemeny rankings cardinality can be extremely large in small size cases (m = 4, n = 15 … 20) and, consequently, special efforts to build an appropriate convoluting solution are needed. Application of the model to one of practical metrological problems, such as interlaboratory comparisons, is proposed and examined.     

Multiport vector network analyzer calibration using the generalized 3-term error model

A generalized 3-term error model, where only three error matrixes are defined, is proposed for the calibration of n-port vector network analyzer (VNA) with n + 1 measurement channels. In this model, the node is replaced by the complex vector, and correspondingly the branch gain is represented by the complex square matrix. According to this error model, which also obeys the fundamental rules of flow graph, the formula for actual scattering matrix of an n-port DUT can be deduced. Finally, the actual S-parameters of a four-port device can be corrected and they are compared with the measurement results by Agilent VNA E5071B. The good agreement attests the precision of the calibration algorithm.     

Measurement uncertainty estimation of health risk from exposure to natural radionuclides in soil

Cancer mortality risk were estimated due to external exposure to ⁴⁰K in soil. Uncertainty estimation was performed for the risk considered as a measurand. It was presented uncertainty estimation using two methods. One method is based on the Guide to the Expression of Uncertainty in Measurement Framework (GUF) and other represents Monte Carlo method. For the Monte Carlo method, the mean of the obtained distribution that represents mortality cancer risk estimation, due to one year exposure to ⁴⁰K with mean activity concentration of 708 Bq/kg in soil, is 12.9 × 10⁻⁶ with 90% confidential interval (k ≈ 1.64) of (4.7–25.5) × 10⁻⁶. According to GUF the mean value is estimated as 10.9 × 10⁻⁶, with 90% confidential interval of (0.9–20.8) × 10⁻⁶. Uncertainty of assessed risk obtained by numerical simulation is slightly different with asymmetrical boundaries related to the mean value, comparing to the uncertainty estimated using GUF.     

Detection of gas leakage using microcolor schlieren technique

This article presents microcolor schlieren technique for gas leakage detection with medium of liquefied petroleum gas (LPG, 50% C₃H₈ and 50% C₄H₁₀), which can be further applied in pipe gas leakage inspection, e.g. checking gas leakage of condenser and evaporator pipes of air conditioning in the automatic production line. In this work, experiments used microcolor schlieren to observe leaking LPG from microholes with pipes and determined the technical sensitivity, where the microholes were made by using electric discharge machining (E.D.M.). The experimental run conditions are different LPG leaking flow rates integrated with different microhole diameters of 1130, 176, 75, 45.6, 35.32, and 27.5 μm. The results show that present microcolor schlieren can clearly visualize microhole with ?27.5 μm under leaking pressure difference of 5 torr and ?35.32 μm with leaking pressure difference under 1 torr.     

Blow-down calibration of a large ultrasonic flow meter

Oil and gas production industries use large (diameter > 0.8 m) ultrasonic flow meters (USMs) to measure exhaust gas from flare stacks, emissions from smokestacks, flow of natural gas, etc. Since most flow laboratories do not have compressors with sufficient flow capacity (>10 kg/s) to calibrate large flow meters, calibrations are performed using the blow-down method where flow is generated by discharging high pressure tanks, leading to significant flow transients. We used an array of critical flow venturis (CFVs) in a blow-down facility to calibrate a large (D = 89.5 cm) 8-path ultrasonic flow meter. The flow transients associated with the blow-down process caused large spatial and temporal variations in temperature that dominated (40%–67%) the uncertainty budget. Our uncertainty analysis accounts for transient-generated uncertainties and provides guidelines for improving blow-down calibrations of large flow meters.     

INRIM primary standard for microgas-flow measurements with reference to atmospheric pressure

Primary standard flowmeters are developed for the calibration of leak devices used in many applications in which is necessary to detect and quantify gas leakage from a material, a component or a system. At INRIM, a primary standard was designed and realized for the measurement of molar gas flow from 4 × 10⁻¹⁰ mol/s to 2 × 10⁻⁷ mol/s with reference to atmospheric pressure. It is based on the constant-pressure–variable-volume method and is able to work with any tracer gas.     

Accurate determination of spring constant of atomic force microscope cantilevers and comparison with other methods

We present calibration results of commercial AFM cantilevers using the KRISS nanoforce calibrator (NFC) that can determine traceably spring constants with an uncertainty better than 1%, along with the results obtained from other four calibration methods: the dimensional method, the cantilever-on-cantilever method, the Sader method, and the thermal noise method. Two types (contact and tapping mode) of beam-shaped AFM cantilevers with nominal spring constants of 0.9 N m⁻¹ and 42 N m⁻¹, respectively, were investigated in this study. Because of its small uncertainty, the NFC method was used to assess the uncertainties of other four methods through comparisons between values obtained from other methods and those from the NFC method for the same cantilever. Results from other methods were generally in good agreement with those from the NFC method within the uncertainties of other methods claimed in other literatures, but values obtained from the Sader method were differed by up to 40% from the NFC values, which is 2 times worse than the known uncertainty.     

Analysis of pressure distribution for the various gas flow vacuum system in the range from 1 Pa to 133 Pa

The measurement and control of gas flow are critical in many manufacturing processes. Semiconductor manufacturers, in particular, require a number of different process gases for etching, deposition, oxidation, doping and inerting applications. In many of these, as well as other industrial and research processes including measurement of partial pressures with residual gas analyzers (RGAs), calibration of vacuum gauges, and conductance of a conductance-reducer , accurate measurement and stability of the gas pressure within the reaction vacuum chamber is essential. In the present work, pressure distribution in the chamber of a newly developed flow control system was investigated for three gases (Ar, N₂, and He) range from 1 Pa to 133 Pa. For all the gases, the relative deviations in pressure distribution near the gas inlet and outlet were in the range of −1.3% and 1.2% respectively.     

Calibration of linear encoders with sub-nanometer uncertainty using an optical-zooming laser interferometer

The nonlinear errors of high-precision linear encoders were calibrated by using a nanometer-length calibrator that was based on the optical-zooming laser interferometer with an optical frequency comb. A transmission-type linear encoder and a reflection-type linear encoder were calibrated, and the cyclic nonlinear errors were evident. The magnitudes of the observed cyclic errors were 0.1 nm and 0.2 nm, respectively, and the best calibration uncertainties were 0.55 nm (k = 2). A traceable calibration service for linear encoders with the best calibration uncertainty in the sub-nanometer range has started based on this work.     

Measurement of gas flow rate from helium standard leaks

Helium standard leaks are widely used to check and calibrate mass spectrometer leak detectors. Precisely known gas flows are required for measurement of quantities of standard leak rates. A fundamental task of the constructed and presented calibration apparatus is precise measurement of gas leak rate. Thus a primary standard for calibration helium standard leaks in the range from 10⁻¹⁰ to 10⁻⁵ Pa m³/s has been completed at the Laboratory of Vacuum Measurements in Tele & Radio Research Institute.     

Effect of pre-readout annealing treatments on TL mechanism in tellurite glasses at therapeutic radiation doses level

The higher sensitization for thermal annealing on TL mechanism in the region 550–600 °C for 80(TeO₂)–5(TiO₂)–(15 − x) (WO₃)–(x) A_nO_m where A_nO_m = Nb₂O₅, Nd₂O₃, Er₂O₃ and x = 5 mol% has been measured. The behavior of trap centers and luminescence centers has been investigated for tellurite glasses doped with rare earth oxides irradiated at 0.5 up to 2 Gy and annealed at different temperatures in the range 350–700 °C. The behavior of the three types of tellurite glasses is analyzed regarding to their kinetic parameters and luminescence emission which enhance the claim of tellurite glasses for use as TLD material at therapeutic radiation doses.     

Analysis of interlaboratory comparisons affected by correlations of the reference standards and drift of the travelling standards

The paper describes a method for analysing interlaboratory comparison results among accredited laboratories. Interlaboratory comparisons are used in order to achieve or to maintain the accreditation following the ISO/IEC 17025 standard. The used approach permits an evaluation of the reference value and of the degree of equivalence in the cases in which the laboratories participating are mutually dependent and the travelling standards are not stable during the comparison. This approach, as an example, was applied to analyse the SIT (Servizio di Taratura in Italia) interlaboratory comparisons carried out for the pressure quantity in the range from 10 MPa to 100 MPa (gage mode and liquid medium) and in the range from 0.15 MPa to 7 MPa (gage mode and gas medium).