On practical metrology and chemical analysis: etalons and traceability systems

 National measurement systems are infrastructures to ensure, for each nation, a consistent and internationally recognised basis for measurement. Such complex systems have historical, technical, legal, organisational and institutional aspects to connect scientific metrology with practical measurements. Underlying any valid measurement is a chain of comparisons linking the measurement to an accepted standard. The ways the links are forged and the etalons (measurement standards) to which they connect are defining characteristics of all measurement systems. This is often referred to as traceability which aims at basing measurements in common measurement units – a key issue for the integration of quantitative chemical analysis with the evolving physical and engineering measurement systems. Adequate traceability and metrological control make possible new technical capabilities and new levels of quality assurance and confidence by users in the accuracy and integrity of quantitative analytical results. Traceability for chemical measurements is difficult to achieve and harder to demonstrate. The supply of appropriate etalons is critical to the development of metrology systems for chemical analysis. An approach is suggested that involves the development of networks of specialised reference laboratories able to make matrix-independent reference measurements on submitted samples, which may then be used as reference materials by an originating laboratory using its practical measurement procedures. Received: 31 July 1995 Accepted: 19 August 1995     

ACT3: a high-speed, high-precision electrical impedance tomograph

Presents the design, implementation, and performance of Rensselaer's third-generation adaptive current tomograph, ACT3. This system uses 32 current sources and 32 phase-sensitive voltmeters to make a 32-electrode system that is capable of applying arbitrary spatial patterns of current. The instrumentation provides 16 b precision on both the current values and the real and reactive voltage readings and can collect the data for a single image in 133 ms. Additionally, the instrument is able to automatically calibrate its voltmeters and current sources and adjust the current source output impedance under computer control. The major system components are discussed in detail and performance results are given. Images obtained using stationary agar targets and a moving pendulum in a phantom as well as in vivo resistivity profiles showing human respiration are shown     

Excitation loss of open resonators

Reported here are the results on level and structure of the radiated field of an open resonator at and off resonance. On the basis of the modelling problem rigorous solution and the measurements at 4-millimeter wavelength we find there are no ways to compensate the radiated field from an open electromagnetic structure at resonance. Analysis of open resonator excitation efficiency shows that the mismatch loss of a slot-fed open resonator runs to 34% while at the aperture-feed excitation this is not more than 6% for the same-geometry resonator.     

Erratum: Synthesis and characterization of diorganotin(IV) complexes of Schiff bases with ONO‐type donors and crystal structure of [N‐(2‐hydroxy‐4‐nitrophenyl)‐3‐ethoxysalicylideneiminato]diphenyltin(IV)

The article referenced above was first published online on 30 August 2007 with incorrect pagination; the pagination has now been corrected online and in print. Copyright © 2007 John Wiley & Sons, Ltd.     

Microstructural evolution of decagonal quasicrystal in the undercooled Al72Ni12Co16 alloy melts

The microstructure evolution of decagonal quasicrystals in Al₇₂Ni₁₂Co₁₆ alloy was investigated by the electromagnetic melting and cyclic superheating method. Single-phase decagonal quasicrystals have been obtained when the undercoolings were larger than 60 K. The decagonal quasicrystals formed at various undercoolings show different microstructural morphologies. Furthermore, grain refinement was found near the undercooling of 120 K. Based on current thermodynamic and dendrite growth theories, a dimensionless superheating parameter was adopted to explain the effect of processing conditions on the microstructure of Al₇₂Ni₁₂Co₁₆ alloy. The result indicate that the fine equiaxied microstructure of decagonal quasicrystal (D-phase) formed near on undercooling of 120 K originates from the break-up of dendrites.     

Quantification of trace elements in human serum fractions by liquid chromatography and inductively coupled plasma mass spectrometry

On‐line coupling of LC and ICP‐MS has been used for fractionation and detection of species of Cu, Fe, I, Se and Zn in human serum. It has been shown that anion exchange chromatography provided better separation capability (both intra‐ and inter‐element) than size‐exclusion chromatography. The mobile phases for ion exchange chromatography consisted of Tris–HNO₃ buffer and ammonium salt (nitrate, acetate or formate). Formate was found to be the best mobile phase counter ion, enabling good chromatographic separation, and is acceptable for mass spectrometry too. The quantitative evaluation of element concentrations adhering to individual fractions was performed by the peak area normalization method. The repeatability of results ranged from 3 to 15% (depending on the element concentration level) and represented the main part of the result uncertainty. The accuracy of Cu and Zn fraction determinations was confirmed by comparison with the isotope dilution technique. Copyright © 2006 John Wiley & Sons, Ltd.     

Application of N,N‐bis(diphenylphosphino)aniline palladium(II) complexes as pre‐catalysts in Heck coupling reactions

Palladium(II) complexes with N,N‐bis(diphenylphosphino)aniline ligands catalyse the Heck reaction between styrene and aryl bromides, affording stilbenes in good yield. The structures of two of the complexes used as pre‐catalysts have been determined by single‐crystal X‐ray diffraction. Copyright © 2007 John Wiley & Sons, Ltd.     

Solution-Processed n-Type Organic Field-Effect Transistors With High on /off Current Ratios Based on Fullerene Derivatives

Solution-processed n-type organic field-effect transistors (OFETs) based on the fullerene derivative {6}-1-(3-(2- thienylethoxycarbonyl)-propyl)-{5}-l-phenyl-[5,6]-C61 (TEPP) and phenyl-C61-butyric acid methyl ester (PCBM) in a multiring source/drain structure are reported. Devices with TEPP show high electron mobility up to 7.8 x 10^-2 cm²/Vs in the saturation regime for bottom-contact OFETs with Au S/D electrodes with a solution-processed fullerene derivative. The ON/OFF ratios reported in this letter, which are in the range of 10⁵ -10⁶, are among the highest values reported for such devices. This mobility is always higher compared to PCBM devices prepared in identical conditions. The mobility of TEPP and PCBM increased with increasing temperatures in the range of 100-300 K with activation energy of 78 and 113 meV, respectively, which suggests that the thermally activated hopping of electrons is dominant in TEPP.     

Performance of space-time codes for a large number of antennas

We study the asymptotic behavior of space-time codes when the number of transmit and receive antennas grows to infinity. Specifically, we determine the behavior of pairwise error probabilities with maximum-likelihood (ML) decoding and with three types of receiver interfaces: the ML interface, the linear zero-forcing (ZF) interface, and the linear minimum-mean-square-error (MMSE) interface. Two situations are studied: when the number of receiving antennas grows to infinity while the number of transmitting antennas is finite, and when both numbers grow to infinity but their ratio remains constant. We show that with ML or linear interfaces the asymptotic performance of space-time codes is determined by the Euclidean distances between codewords. Moreover, with the two linear interfaces examined here the number r of receive antennas must be much larger than the number t of transmit antennas to avoid a sizeable loss of performance; on the other hand, when r ≫ t, the performance of these linear interfaces comes close to that of ML. The dependence of error probabilities on Euclidean distance is valid for intermediate signal-to-noise ratios (SNRs) even when the number of antennas is small. Simulations validate our theoretical findings, and show how asymptotic results may be substantially valid even in a nonasymptotic regime: thus, even for few antennas, off-the-shelf codes may outperform space-time codes designed ad hoc