热耦合型二级高频脉冲管制冷机实验研究

降低制冷温度至4 K温区是高频脉冲管制冷机的最新发展要求。本文介绍了一套热耦合型二级高频脉冲管制冷机的性能特性,它可以达到低于15 K以下的最低温度,是目前报道的高频二级脉冲管制冷机能获得的最低温度．通过对制冷机一级预冷、二级输入功率、二级冷量、室温条件等影响的分析,从实验角度揭示了该二级制冷系统的复杂影响,为进一步的深入分析和改进提供了基础。     

Tests of quantum electrodynamics using ion traps

Experiments in ion traps on the g factors for the free and the bound electron in low-Z, hydrogen-like ions have provided the most accurate tests of quantum-electrodynamics calculations. Moreover they have been used to determine new and precise values for fundamental constants. Extensions to more stringent tests using ions of higher values of the nuclear charge Z are on the way. Also other QED tests such as Lamb shifts or hyperfine structures in H-like ions using traps will be feasible in the near future. The tests in bound systems, however, will be limited by nuclear structure effects which are difficult to calculate. Assuming the QED calculations as correct, the experimental results may be used to determine nuclear contributions and thus support nuclear models. Contribution presented at the TCP06, Vancouver Island, 2006.     

Optical biosensor for pharmaceuticals, antibiotics, hormones, endocrine disrupting chemicals and pesticides in water: Assay optimization process for estrone as example

Certain contaminants at trace concentrations in surface waters can have dramatic effects on the hormonal system of organisms in the aquatic environment. Therefore, immunoanalytical methods at a very low limit of detection (LOD) and a low limit of quantification (LOQ) are becoming more and more important for environmental analysis and especially for monitoring drinking water quality. Environmental monitoring of antibiotics, hormones, endocrine disrupting chemicals, and pesticides in real water samples (e.g. surface, ground or drinking water) with difficult matrices places high demands on chemical analysis. Biosensors have suitable characteristics such as efficiency in allowing very fast, sensitive, and cost-effective detection. Here we describe an assay optimization process with a fully automated immunoassay for estrone which resulted in a LOD below 0.20 ng L⁻¹ and a LOQ below 1.40 ng L⁻¹. In contrast to common analytical methods such as GC-MS or HPLC-MS, the biosensor used requires no sample pre-treatment and pre-concentration. The very low validation parameters for estrone are the result of the continuous optimization of the immunoassay. The basis of our sensitive assay is the antibody with a high affinity constant towards estrone. During the optimization process, we reduced the amount of antibody per sample and improved the chip surface modification. Finally, this proceeding led to a calibration routine with an amount of antibody of only 3.0 ng per sample (sample volume: 1.0 mL). The reduction of the amount of antibody per sample results in better validation parameters (LOD, LOQ, and IC₅₀), but this reduction leads to the current device-related limitation of the River Analyser (RIANA).For some endocrine disrupting compounds, no effect levels (NOELs) in the lower nanogram per liter range are reported. This defines the challenge, which analytical methods have to compete with and our RIANA instrument with its improved sensitivity for the detection of a single hormone in the lower nanogram per liter range is a powerful tool in aquatic analytics in addition to the common analytical methods.     

Cyclisierungen unter beteiligung von fluoridionen. 2. Mitteil. [1], [2]. 4.5-perfluor-1.3-dioxolane

4.5-Perfluoro-1.3-dioxolanes $\text{2}$ are available by reaction of 2(α-chloroalkoxy)perfluoro-carbonyl halides $\text{3}$ or -ketone $\text{9}$ with fluoride ions. A mechanism for the intramolecular ring- closure-reaction is proposed. Hydrogen atoms at C-2 in $\text{2}$ can be exchanged photochemically by chlorine. Starting from the 2-monochloro-derivatives $\text{16}$ the 2-monofluoro-4.5-perfluoro- 1.3-dioxolanes $\text{18}$ are formed by reaction with triethylamine- hydrofluoride.     

The electron impact fragmentation of 3- and 4-styrylpyridazine

The electron impact mass spectrometric fragmentation of trans-3- and trans-4-styrylpyridazine is reported in detail, including a comparison with other aza-stilbenes. With regard to a distinction between the two isomeric styrylpyridazines, the intensity ratio of the M⁺ and [M-1]⁺ ions, the general degree of fragmentation and the elimination pathways of nitrogen proved to be most characteristic.     

Double indication in catalytic-kinetic analysis: simultaneous photometric and thermometric indication of the iodine-azide reaction in closed and flow systems

The iodine—azide reaction catalyzed by sulphur-containing compounds is followed simultaneously by optical and thermometric measurements in closed and flowing systems. In the closed system, thiosulphate can be determined in the range 32.4–324 μg ml^-1, by observing the turbidity caused by the nitrogen formed during the reaction and the temperature changes. With the flow apparatus, thiosulphate can be determined in the range 112–1120 μg ml^-1 by continuously mixing the sample and reagent solutions. H₂S in nitrogen 5–100 ppm) is measured by sweeping the gas into the reaction Cuvette. In a third flow procedure, H₂S is liberated continuously from sodium sulphide solutions (0.1–10 μg S^2- ml^-1) by ascorbic acid, and swept to the measuring cuvette with nitrogen.     

Immunosensor for estrone with an equal limit of detection as common analytical methods

Immunoanalytical methods at a very low limit of detection (LOD) and a low limit of quantification (LOQ) are becoming more and more important for environmental analysis and especially for monitoring drinking water quality. Biosensors have suitable characteristics such as efficiency in allowing very fast, sensitive, and cost-effective detection. Here we describe a fully automated immunoassay for estrone with a LOD below 0.20 ng L^–1 and a LOQ below 1.40 ng L^–1. In contrast to common analytical methods such as GC-MS or HPLC-MS, the biosensor used requires no sample pre-treatment and pre-concentration. The basis of our sensitive assay is the antibody with a high affinity constant towards estrone. The very low amount of antibody per sample results in low validation parameters (LOD, LOQ, and IC50), but this assay for estrone represents the current device-related limitation of the River Analyser (RIANA).     

Singularity in the thermal boundary resistance between superfluid (4)He and a solid surface

We report new measurements in four cells of the thermal boundary resistance R between copper and (4)He below but near the superfluid-transition temperature T(lambda). For 10(-7)< or =t identical to 1-T/T(lambda))< or =10(-4) fits of R = R(0)t(-x(b))+R(B) to the data yielded x(b) approximately equal to 0.18, whereas a fit to theoretical values based on the renormalization-group theory yielded x(b) = 0.23. Alternatively, a good fit of the theory to the data could be obtained if the amplitude of the prediction was reduced by a factor close to 2. The results raise the question whether the boundary conditions used in the theory should be modified.