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41.
M. N. Kotov V. F. Masterov V. V. Potapov A. V. Prichodko O. V. Smertin N. M. Shybanova 《International Journal of Infrared and Millimeter Waves》1993,14(8):1679-1687
Experimental investigations of superconductivity effects in single-phase and multiphase Bi2Sr2CaCu2O8 single-crystals have been carried out at 142 GHz frequency by means of the standing wave profile method [1]. Josephson harmonic generation has been observed to be responsible for the appearence of additional peaks on the standing wave profile of the open dielectric resonator loaded with a properly orientated multiphase high-Tc superconductor specimen. This leads to the conclusion that most of the Josephson junctions in multiphase crystals are located in certain crystallographic planes. The investigations of temperature dependencies showed that sharp resonant peaks of conductivity observed earlier [2] at 60 GHz could also be observed at 142 GHz. 相似文献
42.
本文研究了2,4-二氧代-1,3,2-苯并二氮磷杂环己烷的磷氢键对β-硝基苯乙烯、丙烯酸酯、丙烯腈及二硫化碳的加成反应,共合成了18个新的加成产物.发现通过选用不同的碱或控制碱的用量.可选择性的进行加成或开环反应.由X衍射证实:在加成产物的结构中,环外P-C键构象因受磷杂环船式构象影响,以邻位交叉式(A)为主. 相似文献
43.
Daixin Tong Keith D. Bartle Anthony A. Clifford Robert E. Robinson 《Journal of separation science》1992,15(8):505-509
A unified approach to sequential gas and supercritical fluid Chromatography using 50 μm i.d. open tubular columns is described. Sample introduction is performed by means of a rotary injection valve. In order that linear velocities can be optimized independently, a second rotary valve in the chromatographic oven is used to direct the flow of column eluate to the flame ionization detector through either fused silica tubing in GC, or a frit restrictor in SFC. Applications of sequential GC-SFC on a 50 μm i.d. open tubular column are demonstrated, and comparisons made between sequential GC-SFC on 50 and 100 μm i.d. columns. 相似文献
44.
Sameena Ashraf Keith D. Bartle Anthony A. Clifford Robert Moulder 《Journal of separation science》1992,15(8):535-538
Lubricating oil additives have been analyzed by supercritical fluid chromatography on open tubular and packed capillary columns. Carbon dioxide and modified carbon dioxide were used as mobile phases and detection was accomplished by flame ionization and micro UV. Rapid and efficient analysis of the lubricating oil additives was demonstrated. 相似文献
45.
H. A. Claessens M. J. J. Hetem P. A. Leclercq C. A. Cramers 《Journal of separation science》1988,11(2):176-180
In comparison with conventionally packed HPLC columns, from a theoretical point of view, open capillary liquid chromatography (OTLC) systems offer a number of advantages like high plate numbers and short analysis times. On the other hand, drastic changes have to be made to the instrumentation. In particular, the contribution to band broadening by the chromatographic equipment must be considerably reduced. In the present study an OTLC system was developed and evaluated, which yields satisfactory results for 26 μm i. d. columns. The determination of the contribution of the chromatographic equipment to the total band broadening is discussed. 相似文献
46.
The High Pressure Asher (HPA-S) was adapted with a Teflon liner for pressurized wet digestion in open vessels. The autoclave was partly filled with water containing 5% (vol/vol) hydrogen peroxide. The digestion vessels dipped partly into the water or were arranged on top of the water by means of a special rack made of titanium or PTFE-coated stainless steel. The HPA-S was closed and pressurized with nitrogen up to 100 bars. The maximum digestion temperature was 250 °C for PFA vessels and 270 °C for quartz vessels. Digestion vessels made of quartz or PFA-Teflon with volumes between 1.5 mL (auto sampler cups) and 50 mL were tested. The maximum sample amount for quartz vessels was 0.5–1.5 g and for PFA vessels 0.2–0.5 g, depending on the material. Higher sample intake may lead to fast reactions with losses of digestion solution. The samples were digested with 5 mL HNO3 or with 2 mL HNO3+6 mL H2O+2 mL H2O2. The total digestion time was 90–120 min and 30 min for cooling down to room temperature. Auto sampler cups made of PFA were used as digestion vessels for GFAAS. Sample material (50 mg) was digested with 0.2 mL HNO3+0.5 mL H2O+0.2 mL H2O2. The analytical data of nine certified reference materials are also within the confidential intervals for volatile elements like mercury, selenium and arsenic. No cross contamination between the digestion vessels could be observed. Due to the high gas pressure, the diffusion rate of volatile species is low and losses of elements by volatilisation could be observed only with diluted nitric acid and vessels with large cross section. In addition, cocoa, walnuts, nicotinic acid, pumpkin seeds, lubrication oil, straw, polyethylene and coal were digested and the TOC values measured. The residual carbon content came to 0.2–10% depending on the sample matrix and amount. 相似文献
47.
The paper presents the results of testing
the thermal stability and flammability of butadiene-acrylonitrile rubber vulcanizates
with different contents of combined acrylonitrile: Perbunan NT 1845 and Perbunan
NT 3945 from Bayer, containing unmodified and bromine- or iodine-modified
silica. The test results were obtained with the use of a derivatograph, measurements
of flammability by the method of oxygen index, in air and also with the use
of a cone calorimeter. The effect of the modification on the zeta potential
was also examined.
A considerable reduction in the flammability
of nitrile rubber vulcanizates filled with silica can be obtained by the modification
of filler with bromine or iodine. All the vulcanizates containing modified
silica are self-extinguishing. An appropriate filling of NBR 39 vulcanizates
with bromine-modified silica makes it possible to obtain non-flammable polymeric
materials. They neither ignite nor glow under the action of a flame source
for 30 s.
The findings can be a rational basis for the synthesis
of modified silica that can act as active filler and effective flame-retardant
agent at the same time. 相似文献
48.
Norbert V. Fehringer Dalia M. Gilvydis Stephen M. Walters Colin F. Poole 《Journal of separation science》1992,15(2):124-127
The combination of open tubular column gas chromatography with electrolytic conductivity detection has been evaluated for the determination of nitrogen-containing pesticide residues in food extracts. Optimization of the column position at the column-detector interface was crucial to the successful operation of the detector. The signal-to-noise ratio and response stability of the detector are greatly influenced by the composition of the electrolyte solvent. Large volume splitless injections using retention gaps and optimized detector operating conditions enabled pesticide residues in food extracts to be determined at sub parts-per-million levels. Although the electrolytic conductivity detector is less sensitive than the thermionic ionization detector, its greater nitrogen selectivity can he crucial to the determination of nitrogen-containing contaminants in food extracts, particularly in complex mixtures where phosphorus-containing contaminants or matrix compounds are also present. 相似文献
49.
Summary The successful application of the formerly presented concept of diffusion-averaged molecular weight, Md, to vacuum residues of crude oils, or their fractions, is described. The samples for establishing the calibration curve, logDvs. logM, were crude oil fractions with polydispersities smaller than 1.1. In a surprisingly good approximation the calibration curve is independent of the origin of these fractions if 500<M<10000. The validity of our calibration curve was demonstrated with more than 10 crude oil residues and with some of their hydrogenation residues [2]. 相似文献
50.