Comparison of the extrapolation precision of sequential and conventional standard addition calibrations

The precision of extrapolation for comparable cases of sequential standard addition calibration (S-SAC) and conventional standard addition calibration (C-SAC) are compared for various ratios of target analyte concentration and solution mass of the unknown solution to the standard solution. In addition the difference between homoscedastic and heteroscedastic analyser behaviour has been assessed. Whilst the precision of C-SAC is superior under most practical conditions it is not significant until the concentration of target analyte in the standard solution is less than ten times that of the unknown. The difference in extrapolation precision between C-SAC and S-SAC shows very little dependence on whether analyser behaviour is homoscedastic or heteroscedastic, or on the mass ratio of the unknown solution to the standard solution.     

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.     

Simple apparatus to measure Seebeck coefficient up to 900 K

An apparatus for measuring Seebeck coefficient (S) has been designed that allows measurement of S from room temperature to 900 K. It is constructed from readily available equipment and instrumentation with parts that can be easily fabricated. The details of instrument fabrication, sources of errors, method of calibration, typical measurement in test sample are described. We report the Seebeck coefficient measurement of Ca-cobaltite (Ca₃Co₄O₉) a p-type thermoelectric material. The obtained results from the fabricated setup are well matched with the reported and standard instrument data with standard deviation of ±3%.     

一种便携关节式坐标测量机结构参数标定的优化采样策略

利用高斯—牛顿法求解便携关节式坐标测量机的标定参数时,其参数的可辨识性与Jacobin矩阵的条件数有关,而Jacobin矩阵的条件数决定于标定采样点的坐标。因此,必须对参数标定的采样策略进行优化。以锥孔标准杆件标定法为例,提出一种优化的采样策略来增大各个关节取值范围从而使条件数最小化。经实验验证,采用这种优化的采样策略标定提高了测量系统的精度。     

Improving integrity of on-line grammage measurement with traceable basic calibration

The automatic control of grammage (basis weight) in paper and board production is based upon on-line grammage measurement. Furthermore, the automatic control of other quality variables such as moisture, ash content and coat weight, may rely on the grammage measurement. The integrity of Kr-85 based on-line grammage measurement systems was studied, by performing basic calibrations with traceably calibrated plastic reference standards. The calibrations were performed according to the EN ISO/IEC 17025 standard, which is a requirement for calibration laboratories. The observed relative measurement errors were 3.3% in the first time calibrations at the 95% confidence level. With the traceable basic calibration method, however, these errors can be reduced to under 0.5%, thus improving the integrity of on-line grammage measurements. Also a standardised algorithm, based on the experience from the performed calibrations, is proposed to ease the adjustment of the different grammage measurement systems. The calibration technique can basically be applied to all β-radiation based grammage measurements.     

考虑测量参照物误差对VAMT1Y并联机床的运动标定仿真

采用间接测量对 VAMT1Y并联机床进行标定仿真时 ,需要引进标准测量参照物对动平台的位姿进行测量 ,但参照物本身可能存在一定的尺寸误差 ;另外间接测量时要不断变换标准测量参照物的位置 ,又会引进位置误差。为便于解决实际问题 ,将上述误差和待标定的机床的几何误差综合考虑对机床进行了标定仿真。仿真结果表明 ,适当地考虑一些测量系统的误差并不会影响最终的标定效果     

全蒸发技术在铀同位素丰度测量上的应用

采用全蒸发技术、离子流强度积分的方式 ,用多接收器热表面电离质谱计测量铀同位素丰度。全蒸发技术可克服质量分馏效应带来的测量误差 ,而直接实现准确测量。开发了用于全蒸发技术的测量软件 ,对影响测量结果的因素 ,诸如分析用样量、信号损失与试样残留等进行了研究。最后得出在铀同位素丰度比为 0 1～ 10的范围内 ,95 %的置信水平下 ,该方法的相对扩展不确定度为0 10 %     

Offline and online strategies to improve pose accuracy of a Stewart Platform using indoor-GPS

The pose accuracy of a robot manipulator may be improved by assessing and correcting systematic errors. Both offline and online strategies can be considered. To date, there has not been a solution for the online pose error correction of parallel manipulators. Moreover, offline strategies using indoor-GPS as reference measurement system have not yet been investigated. In this paper an optimization-based kinematic calibration method and an online correction technique are proposed and implemented for a low-cost Stewart Platform. In both cases, an indoor-GPS system was used as reference measurement equipment. Performance of both strategies are compared to a kinematic calibration method based on direct parameter measurement. Pose errors are evaluated for each strategy using a robotic total station. Performance of the optimization-based calibration and the online correction technique were similar and better than the direct parameter measurement calibration. Both techniques resulted in average pose errors less or equal to 0.3 mm and 0.05°. The proposed strategies may be adapted to other similar parallel manipulators and are applicable to large sized equipment.     

Automatic calibration system for polygon mirrors

An automatic calibration system of polygon mirrors is described. This system consists of the four subsystems: a precise rotary mechanism, a rotary magnetic scale for angular standard, a special photo-electric autocollimator which enables dynamic measurement, and a mini-computer system which controls the compiling and handling of data. The basic principle of the system depends on the self-checking method, so that both the polygon mirror and the standard rotary scale are calibrated simultaneously. A time-conversion method is adopted to detect slight angular difference with high resolution. By way of an example, the calibration of a 12-sided polygon is described. The results obtained are as follows: (1) The calibration can be done automatically in a short time without skill, except for the manual operation of setting a polygon relatively for the magnetic scale; (2) 95% confidence interval of instrumental error calibrated on the system is within $\text{±0.07}$ seconds of arc.     

Traceable calibration of transfer standards for scanning probe microscopy

A Metrological Atomic Force Microscope (MAFM) has been constructed for the traceable calibration of transfer standards for scanning probe microscopy. It uses optical interferometry to generate image scales with direct traceability to the national standard of length. Three interferometers monitor the relative displacements of the AFM tip and sample in the x, y and z directions and the interferometer data is used directly to construct 3D images of sample surfaces. Traceable dimensional measurement of surface features may then be derived from the image data. This paper describes the MAFM instrument and presents a measurement uncertainty budget. Examples are given of measurements of pitch and step height on calibration transfer standards for scanning probe microscopy.     

铜合金表面元素的飞行时间二次离子质谱微区原位分析

铜合金中含有Pb、Sn、Zn、Ni等元素,其分布和相对含量对铜合金的性能具有重要影响。本工作采用飞行时间二次离子质谱（TOF-SIMS）法对铜合金标准样品GBW02137和GBW02140的表面进行了微区原位分析;采用束斑直径约5 μm的一次离子束轰击500 μm×500 μm区域内的混合固体合金样品,实现了Cu、Pb、Ni、Sn和Zn元素的表面成像,并测量了各元素在铜合金样品表面的分布情况;利用标样校准法对GBW02137、GBW02140中的⁶⁴Zn/¹²⁰Sn、²⁰⁸Pb/¹²⁰Sn值进行相对含量分析。实验结果表明：TOF-SIMS法可用于铜合金中Cu、Pb、Ni、Sn和Zn等元素的表面成像和相对含量测定;采用标样校准法进行相对含量分析时,测得的⁶⁴Zn/¹²⁰Sn相对误差小于5.1%,RSD优于2.5%,²⁰⁸Pb/¹²⁰Sn的测量相对误差较大,接近27%,但其RSD仍低于5%。     

Influence of flow disturbances on the performance of industry-standard LNG flow meters

In the last decade significant progress has been achieved in the development of measurement traceability for LNG inline metering technologies such as Coriolis and ultrasonic flow meters. In 2019, the world's first LNG research and calibration facility has been realised thus enabling calibration and performance testing of small and mid-scale LNG flow meters under realistic cryogenic conditions at a maximum flow rate of 200 m³/h and provisional mass flow measurement uncertainty of 0.30% (k = 2) using liquid nitrogen as the calibration fluid. This facility enabled, for the first time, an extensive test programme of LNG flow meters under cryogenic conditions to be carried out to achieve three main objectives; the first is to reduce the onsite flow measurement uncertainty for small and mid-scale LNG applications to meet a target measurement uncertainty of 0.50% (k = 2), the second is to systematically assess the impact of upstream flow disturbances and meter insulation on meter performance and the third is to assess transferability of meter calibrations with water at ambient conditions to cryogenic conditions. SI-traceable flow calibration results from testing six LNG flow meters (four Coriolis and two ultrasonic, see acknowledgment section) with water in a water calibration facility and liquid nitrogen (LIN) in the LNG research and calibration facility under various test conditions are fully described in this paper. Water and LIN calibration data were compared and it was observed that the influence of removing the meter insulation on mass flow rate measurement accuracy can be more significant (meter error > ±0.50%) than the influence of many typical upstream disturbances when the meter is preceded by a straight piping length equal to twenty pipe diameters (20D) with no additional flow conditioning devices, in particular for ultrasonic meters. The results indicate that the correction models used to transfer the water calibration to cryogenic conditions (using LIN) can potentially result in mass flow rate measurement errors below ±0.5%, however, the correction models are specific to the meter type and manufacturer. This work shows that the target measurement uncertainty of 0.50% can be achieved if the expanded standard error of the mean value measured by the meter is smaller than 0.40% (k = 2). It is planned to repeat these tests with LNG in order to compare the results with the LIN tests presented in this paper. This may reveal that testing with an explosion safe and environmentally friendly fluid such as LIN produces representative results for testing LNG flow meters.     

Multiple Measurement Models of Articulated Arm Coordinate Measuring Machines

The existing articulated arm coordinate measuring machines(AACMM) with one measurement model are easy to cause low measurement accuracy because the whole sampling space is much bigger than the result in the unstable calibration parameters. To compensate for the deficiency of one measurement model, the multiple measurement models are built by the Denavit-Hartenberg's notation, the homemade standard rod components are used as a calibration tool and the Levenberg-Marquardt calibration algorithm is applied to solve the structural parameters in the measurement models. During the tests of multiple measurement models, the sample areas are selected in two situations. It is found that the measurement errors' sigma value(0.083 4 mm) dealt with one measurement model is nearly two times larger than that of the multiple measurement models(0.043 1 mm) in the same sample area. While in the different sample area, the measurement errors' sigma value(0.054 0 mm) dealt with the multiple measurement models is about 40% of one measurement model(0.137 3 mm). The preliminary results suggest that the measurement accuracy of AACMM dealt with multiple measurement models is superior to the accuracy of the existing machine with one measurement model. This paper proposes the multiple measurement models to improve the measurement accuracy of AACMM without increasing any hardware cost.     

The variable sample size t control chart for monitoring short production runs

Starting the online monitoring of a quality characteristic by means of a control chart at the beginning of a short production run is often a challenging issue for quality practitioners: in fact, the frequent absence of preliminary information prevents from getting a precise estimate of the characteristic mean and standard deviation. Furthermore, for short runs having a finite rolling horizon, the number of inspections scheduled within the run can be too small to get sufficient samples allowing the phase I implementation of the chart to be completed. Recently, t control charts have been proposed as efficient means to overcome this problem because they do not need any phase I tentative control limits definition or preliminary process knowledge. In this paper, a variable sample size (VSS) version of the t chart is proposed. Adaptive control charts have been implemented with success in long runs: here, the performance of the variable sample size strategy is investigated for a chart used in a short run. The statistical performance of the VSS t chart is compared with the one of the fixed-parameter (FP) t chart for both scenarios of fixed and unknown shift size, with the latter situation being frequent in short-run manufacturing environments. An extensive numerical investigation reveals the potential benefits of the proposed chart. When the statistical design is optimized with respect to a fixed value of the shift size δ, the VSS t chart has a better statistical performance than the FP t chart for moderate to large values of δ. Conversely, for the unknown shift size condition, the VSS t chart always outperforms the FP t chart for in-control average sample sizes ASS₀?>?7. An illustrative example shows the implementation of the VSS during the production of a finite lot of mechanical parts.     

Memoryless disturbance-observer-based adaptive tracking of uncertain pure-feedback nonlinear time-delay systems with unmatched disturbances

This paper presents a delay-independent nonlinear disturbance observer (NDO) design methodology for adaptive tracking of uncertain pure-feedback nonlinear systems in the presence of unknown time delays and unmatched external disturbances. Compared with all existing NDO-based control results for uncertain lower-triangular nonlinear systems where unknown time delays have been not considered, the main contribution of this paper is to develop a delay-independent design strategy to construct an NDO-based adaptive tracking scheme in the presence of unknown time-delayed nonlinearities and non-affine nonlinearities unmatched in the control input. The proposed delay-independent scheme is constructed by employing the appropriate Lyapunov-Krasovskii functionals and the same function approximators for the NDO and the controller. It is shown that all the signals of the closed-loop system are semi-globally uniformly ultimately bounded and the tracking error converges to an adjustable neighborhood of the origin.     

采用间接测量法对平面3-RPR机构进行运动学标定的仿真

采用间接测量对平面机构进行标定时，需要引进标准测量参照物，但参照物本身仍可能存在一定的尺寸误差；另外间接测量时要不断变换标准测量参照物的位置，又会引进位置误差。为便于解决实际问题，使研究更具可操作性，将上述误差和待标定的机构结构误差一起考虑对机构进行了标定仿真，同时在仿真过程中采用矩阵重构的方法来解决测量误差扰动的问题，避免了大规模的空间寻优。仿真结果表明，可以通过让动平台走过不同的轨迹组合来实现对平面机构的标定。     

能量色散X射线荧光分析法测定石油焦硫含量的研究

通过二次标样法建立了测定石油焦硫含量的能量色散X射线荧光（EDXRF）分析法,与传统的管式炉法相比,该方法具有测定速度快,重复性好,准确度高的优点,为此建立了相应的企业标准,以便在生产中应用。同时考察了样品的粒度、装样深度及水分对测定结果的影响。     

自动测试系统计量策略及指标确立准则研究

为解决自动测试系统缺乏有效的计量保障工程,提出了ATE计量策略和计量保障系统指标确定准则。采用通用系统的设计思想,将系统结构划分为计量校准模块和计量资源输出模块。充分考虑测试资源实际应用情况和UUT技术指标,根据装备计量保障通用要求,以及测量不确定度评定与表示评定要求,保证系统内部形成阶梯溯源链的前提下,提出了整体计量指标的确定方法。实践证明,这种方法在工程实践中取得了较好的效果。     

An apparatus for simultaneous measurement of electrical conductivity and thermopower of thin films in the temperature range of 300-750 K

An automated apparatus capable of measuring the electrical conductivity and thermopower of thin films over a temperature range of 300-750 K is reported. A standard dc resistance measurement in van der Pauw geometry was used to evaluate the electrical conductivity, and the thermopower was measured using the differential method. The design of the instrument, the methods used for calibration, and the measurement procedure are described in detail. Given the lack of a standard National Institute of Standards and Technology (Gaithersburg, Md.) sample for high temperature thermopower calibration, the disclosed calibration procedure shall be useful for calibration of new instruments.