Extension of the range of resonator scanning spectrometer into submillimeter band and some perspectives of its further developments

Extension of the working frequency of modern resonator spectrometers into submillimeter wave range is described. Experimental record of atmospheric absorption spectrum covering 45-370 GHz range is demonstrated for the first time, and measured water vapor J′_{ka′, kc′}-J_{ka, kc} = 5_1,5-4_2,2 at 325 GHz line parameters are presented. For the first time pressure lineshift for the 325-GHz water vapor line is measured. Further extension of working range is discussed. New estimations of physical limits of time needed for measurements of absorption in the whole Backward Wave Oscillator (BWO) range are given for phase continuous synthesizer regime. Basic schemes of fast broadband continuous phase synthesized sources are discussed. Verification of the previous measurements of water vapor 3_1,3-2_2,0 at 183 GHz line parameters is presented. Comparisons with ringdown resonator spectrometers are given.     

Q value related mass determinations using a Penning trap

We report here about measurements of reaction and decay Q values by precise determination of pairs of atomic masses. These were performed with the Penning trap mass spectrometer SMILETRAP. Measurements with Penning traps give reliable and accurate masses, in particular Q values, due to the fact that certain systematic errors to a great deal cancel in the mass difference between the two atoms defining the Q value. Some Q values that are of fundamental interest will be discussed here, for example, a new Q value for the ⁶Li (n,γ) ⁷Li reaction, for the β-decay of tritium, related to properties of the electron neutrino mass, and for the neutrino-less double β-decay of ⁷⁶Ge, related to the question of whether the neutrino is a Majorana particle or not. In case of the latter two we report the most accurate Q values, namely 18,589.8(12) eV for the tritium decay and 2,038.997(46) keV for the neutrino-less double β-decay of ⁷⁶Ge.     

Quantitation in capillary electrophoresis-mass spectrometry

CE-MS has evolved into a strong alternative to LC-MS. Most of CE-MS applications deal with characterization and identification. However, quantitative aspects have gained importance in, e.g., pharmaceutical and biotechnological applications. Here we summarize and evaluate various methodological aspects in order to achieve sensitive and reproducible results. Similar to LC-MS, aspects of matrix influence on the electrospray process need to be carefully addressed when quantitative results are intended by CE-MS. Due to a more complicated coupling special emphasis needs to be put on the CE-MS interface. Generally linearity over more than three orders of magnitude can be achieved by CE-ESI-MS. Furthermore, a literature survey has been performed in order to give an overview over quantitative measurements performed by CE-MS. The precision can be doubled when changing from a structural related to an isotopically labeled internal standard. Thus a level of precision better than 5% RSD can be achieved.     

Phosphorus-containing podands

A number of monopodands havingo-diphenylphosphinyl terminal groups were synthesized by alkylating sodium derivatives of oligoethylene glycols witho-(bromomethyl)phenyldiphenylphosphine. The stability constants of the complexes of these ligands with alkali metal cations at 25 °C were determined conductometrically in a THF—chloroform solution (41, v/v). The complexing ability of monopodands with respect to the cations studied increases monotonically as the number of electron-donating sites increases (from 3 to 8) for all of the cations except Li⁺ and, to some extent, Na⁺. In the case of Li⁺ a smooth decrease in the stability of the complexes is observed. The monopodands obtained in this work differ drastically in this regard from their structural isomers, bis[o-(diphenylphosphinylmethyl)phenyl] ethers of oligoethylene glycols, which had been studied previously.For part 10, see ref. 1.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 952–956, May, 1993.     

Robust estimates of the theoretical standard deviation to be used in interlaboratory precision experiments

Interlaboratory experiments often contain results that strongly deviate from other results obtained in the same laboratory under repeatability conditions, or laboratory means that strongly deviate from other laboratory means. In ISO 5725-2 [1] and IUPAC [2], the basic standards for the organisation and analysis of interlaboratory experiments for the determination of precision of a measurement method, outlier tests are performed in order to detect such situations and to finally decide whether these values are retained in the analysis or discarded as outliers. This outlier treatment, which always has a subjective aspect, becomes unnecessary by using robust estimates of the repeatability and reproducibility standard deviation. This paper proposes to use Rousseeuw’s Q _n as an extremely robust and efficient estimate of the standard deviation. Two examples show the performance of the new method.     

Patterns in the precision of quantitative data from multicomponent gas chromatographic or gas chromatographic-mass spectrometric analysis

The dispersion of the quantitative results in the analysis of volatile compounds from multicomponent mixtures by different fractionation techniques (solid-phase microextraction and direct thermal desorption) followed by GC or GC-MS presents nonrandom patterns related to the existence of different factors in the fractionation process or in the chromatographic separation which affect, to a different extent, the recovery of the sample components. Statistical techniques have been used to show the relative importance of these factors. The improvement in data precision achieved by using volatile compound concentration ratios is discussed.     

Precise and accurate quantitative C NMR with reduced experimental time

In order to detect small variations in ¹³C isotopomers concentrations, high sensitivity, accuracy and precision have to be achieved. To assess such criteria, when using ¹³C NMR, ¹³C bi-labelled ethanol has been proposed as a molecular probe. Advantage has been taken of the pre-established structural relationship between the peak areas of the ¹³C NMR spectrum of this molecule, i.e. the ratio of signal areas is set to a fixed value. It is shown that the quality performance, required by quantitative ¹³C NMR spectroscopy, is not affected by a large reduction of the repetition delay using relaxation reagents.     

蒸发器支撑板板孔精密测量系统

建立了蒸发器支撑板板孔精密测量系统,并提出了基于边缘约束条件的轮廓参量测量方法.首先采用图像处理技术将待测目标转化为二维离散坐标点,计算其最小外接矩形并对轮廓进行预定位;然后将轮廓分割成相互重合的"扩展邻域轮廓",建立以曲率角为原则的边缘约束算法对各轮廓段精确定界,实现对轮廓参量的精密测量.实验和误差分析表明,该系统测量准确度优于0.02mm,对具有复杂轮廓的零件参量测量有参考价值.     

某机载瞄准系统精度评估测试方法

为了评估某型机载瞄准系统的精度,根据飞行试验参数测试需要,提出了通过图像测量与DGPS融合处理方法进行瞄准精度评估的试验方案。该方案利用飞行试验获取的图像数据与其他测量数据相结合,建立精度评估的方法,该评估方法在该机载武器瞄准系统精度评估得到应用,并且可在同类试验课题中推广应用。     

基于精确时间协议的HL-2M装置定时同步网络研究

基于HL-2M装置对时序精度的要求,参考ITER的设计方案,设计了基于精确时间协议(PTP)的HL-2M分布式时间通讯网络,使HL-2M装置的时钟同步和事件触发的精度从微秒级提高到亚微秒级,最终优于100ns.