共查询到20条相似文献,搜索用时 15 毫秒
1.
微波等离子体增强辉光放电光源激发温度的研究 总被引:2,自引:0,他引:2
研究了一种改进型的微波等离子体增强辉光放电光源在光谱分析中的应用,对其重要的参数指标-激发温度进行了较为较细的考察。结果表明引入微波等离子体后辉光放电的激发温度明显高于单纯辉光放电时的激发温度。 相似文献
2.
The thermal decomposition of Zn-MPA complex was investigated under microwave irradiation. ZnO and ZnS nanocrystals could be obtained by decomposing Zn-MPA(3-mercaptopropionic acid) complex under different reaction conditions. It was found that both the pH value of the solution and the molar ratio of Zn2+ and MPA can play an important role in the formation of ZnO and ZnS nanocrystals. MPA mainly acts as an S source or as a complexing agent. This study provides a new route for the controllable preparation of semiconductor nanocrystals. 相似文献
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We report the first gas-phase observation of the electronic spectrum of a simple halocarbocation, CH2I+. The ion was generated rotationally cold (Trot approximately 20 K) using pulsed discharge methods and was detected via laser spectroscopy. The identity of the spectral carrier was confirmed by modeling the rotational contour observed in the excitation spectra and by comparison of ground state vibrational frequencies determined by single vibronic level emission spectroscopy with Density Functional Theory (DFT) predictions. The transition was assigned as 3A1 <-- X1A1. This initial detection of the electronic spectrum of a halocarbocation in the gas phase should open new avenues for study of the structure and reactivity of these important ions. 相似文献
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The use of neon as the operating gas for the analysis of aluminium samples with the microwave boosted glow discharge source has been studied. A new type of anode tube allowed the gas to enter the source near the sample surface so that more material was transported into the discharge. Erosion rates have been measured under conditions optimised for high line-to-background ratios and found to be lower than with argon (9 and 21 n/s, respectively). Despite the lower erosion rate the detection limits measured for a number of elements in aluminium are in the range 0.02-1 microg/g and comparable to those obtained with argon as the operating gas. 相似文献
5.
Rajeev Sakhuja S. M. Abdul Shakoor Santosh Kumari Anil Kumar 《Journal of heterocyclic chemistry》2015,52(3):773-779
An efficient methodology has been developed for the synthesis of quinoxalin‐2(1H)‐one derivatives of 2‐phenylimidazo[1,2‐a]pyridines by microwave‐irradiated Hinsberg heterocyclization between 2‐phenylimidazo[1,2‐a]pyridine‐3‐glyoxalates and o‐phenylenediamine using either montmorillonite K‐10 or Yb(OTf)3 as catalysts. Montmorillonite K‐10 was proven to be an efficient catalyst for the heterocyclization reaction between sterically hindered glyoxalate and o‐phenylenediamine only under microwave conditions. The use of Yb(OTf)3/tetrahydrofuran was also found to be an effective catalyst for the above chemical transformation among a series of Lewis acids screened under microwave conditions; however, comparatively lesser yields were obtained as compared with the use of montmorillonite K‐10. 相似文献
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Zhong-Hai Ji Yu Guo Jin Chen Li-Na Guo Bo Yang Xue-Fang Zhang Ling-Jia Meng Li Qin 《Chemical Papers》2016,70(10):1399-1407
Decomposition of flue gas desulfurization (FGD) gypsum in the presence of (10 mass %) magnetite and different mass fractions of anthracite, as a reducer, has been investigated under microwave irradiation in air atmosphere. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the decomposition residues. Both experiment results and theoretical analysis indicated that the optimum amount of anthracite added to the FGD gypsum (10 mass %) magnetite mixture was 8 mass %. Under optimum conditions, the maximum desulfurization degree after microwave treatment for 60 min at 1000?C was 93.86 %. Due to microwave heating and calcium ferrite formation, the decomposition temperature of FGD gypsum decreased to around 800°C in air atmosphere. Based on the XRD patterns and SEM images, the reaction of CaSO4 with the additives occurred from the centre to the surface where the liquid phase was generated under microwave heating. SEM images also showed a lower amount of the liquid phase in the outermost layer samples, which prevented the formation of a kiln ring under microwave heating. 相似文献
8.
Markus Damm Gerald Rechberger Manfred Kollroser C. Oliver Kappe 《Journal of chromatography. A》2010,1217(1):167-170
Parallel microwave-assisted gas chromatography (GC) derivatization protocols utilizing a silicon carbide (SiC)-based microtiter plate platform fitted with screw-capped GC vials were developed. For three selected standard derivatization protocols such as acetylation (exemplified for morphine), pentafluoropropionylation (for 6-monoacetylmorphine) and trimethylsilylation (for Δ9-tetrahydrocannabinol) complete derivatization was achieved within 5 min at 100 °C in a dedicated multimode microwave instrument using online temperature monitoring. Microwave irradiation leads to rapid and homogeneous heating of the strongly microwave-absorbing SiC plate, with minimal deviations in the temperature recorded at different positions of the plate. The current platform allows the simultaneous derivatization of 80 reaction mixtures under strictly controlled temperature conditions. Similar results can also be obtained using a standard hotplate as heating source, although heating to the target temperature of 100 °C is slightly slower. The results demonstrate that parallel microwave derivatization procedures can significantly reduce the overall analysis time and increase sample throughput for GC–MS-based analytical methods. 相似文献
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离子液体作用下微波辐照生物质快速热解制备生物质油(英文) 总被引:2,自引:0,他引:2
以离子液体1-丁基-3-甲基咪唑氯([Bmim]Cl)和1-丁基-3甲基咪唑四氟化硼([Bmim]BF4)为催化剂,在微波加热作用下,研究了稻草和锯屑的热解。微波加热20 min,稻草和锯屑的生物油产率分别为38%和34%。考察了微波加热时间、微波功率和离子液体用量对生物质油产率的影响。当以相同的离子液体为催化剂时,稻草微波热解得到的生物质油产率大于锯屑的。生物油成分主要有糠醛、醋酸和1-羟基-2-丁酮等,其含量主要取决于生物质原料和加入的离子液体的类型。 相似文献
11.
A novel magnetically excited microwave plasma emission source was developed and tested. Unlike previous microwave plasma sources which couple energy from the microwave electric field, this source couples energy from the magnetic field. The resultant plasma shape allows easy entrainment of wet sample aerosol, such as is produced by a conventional inductively coupled plasma (ICP) nebulizer and spray chamber, into the core of the plasma. Plasma support gas can be either nitrogen or air although better sensitivity is achieved using nitrogen. Good stability of operation was observed for both aqueous and organic solvents over a wide range of sample flows. The measured performance when used as a spectroscopic source in conjunction with an echelle polychromator showed detection limits approaching those of commercial ICP sources. 相似文献
12.
The use of neon as the operating gas for the analysis of aluminium samples with the microwave boosted glow discharge source has been studied. A new type of anode tube allowed the gas to enter the source near the sample surface so that more material was transported into the discharge. Erosion rates have been measured under conditions optimised for high line-to-background ratios and found to be lower than with argon (9 and 21 n/s, respectively). Despite the lower erosion rate the detection limits measured for a number of elements in aluminium are in the range 0.02–1 g/g and comparable to those obtained with argon as the operating gas. 相似文献
13.
Liliana B. Pierella Linsheng Wang Oscar A. Anunziata 《Reaction Kinetics and Catalysis Letters》1997,60(1):101-106
Conversion of pure methane and natural gas with different methane purity to aromatic hydrocarbons at. 773 and 873 K have been
investigated. Conversion of methane to aromatics under non-oxidizing conditions can be initiated by higher hydrocarbon mixtures
in the feed and, some special coke deposited on Mo/HZSM-5 catalyst at lower reaction temperature. Methane conversion of about
10–20% is obtained at 773 K. The possible reaction mechanism and product phase transformation process for conversion of pure
methane and natural gas at lower temperature are proposed. The thermodynamic limitation for methane conversion under non-oxidizing
conditions may be circumvented. 相似文献
14.
Volker Derdau Dr. Jens Atzrodt Dr. Jochen Zimmermann Dr. Carsten Kroll Francois Brückner 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(40):10397-10404
Conventional thermal and microwave conditions were compared for hydrogen–deuterium (H/D) exchange reactions of aminobenzoic acids catalysed by NaBD4‐activated Pd/C or RhCl3 with D2O as the deuterium source. We also investigated different NaBD4‐activated metal catalysts (including Pd/C, RhCl3 and Pt/C) under microwave conditions for an efficient H/D exchange of aromatic and heterocyclic compounds. Even higher deuterium incorporations were obtained for Pd/C and Pt/C catalyst mixtures due to the previously observed synergistic effect. Finally, we have applied these optimised conditions for one‐step syntheses of the MS standards of several pharmaceutically active compounds. 相似文献
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F. Pavese P.P.M. Steur Jin Seog Kim D. Giraudi 《The Journal of chemical thermodynamics》2011,43(12):1977-1983
The paper reports further results following the 2010 determinations at INRIM of the triple point temperature of the neon isotopes 20Ne and 22Ne, obtained on nearly-pure samples sealed in cryogenic cells, carrying an uncertainty much lower than the previous determinations. The further results, performed in the same experimental apparatus with an expanded uncertainty (k ≈ 2) of ≈30 μK for a single cell and ≈50 μK for the comparison of sample pairs, were obtained using the same model of cryogenic metal sealed cell for each sample, and by measuring different samples from the same gas batch of each isotope and from different gas batches showing a different content of isotopic and chemical impurities. The new determinations were intended to check the effect of measuring different samples and the gas batches, and of performing corrections based on different analytical assays for the isotopic and chemical impurities. The new results are in agreement with the previous determinations, confirming, with greater confidence, the value of the temperature difference for the two pure isotopes, 0.14658 K with an expanded uncertainty of 0.00007 K, and the temperature values on ITS-90 24.5422 K for 20Ne and 24.6888 K for 22Ne, within the larger expanded uncertainty, 0.00032 K, due to the present ambiguity of the ITS-90 definition. These values are also consistent with new determinations published by other laboratories. In addition, the ITS-90 values of INRIM 2010 determinations of Ttp of samples of neon (INRIM Ec2Ne, INRIM E4Ne, PTB Ne12, NPL Ne2) of natural isotopic composition with different 22Ne amount concentrations are reported, consistent with the values obtained for pure isotopes. 相似文献
17.
建立了微波消解-微波等离子体炬原子发射光谱(MPT-AES)法测定啤酒中微量元素。考察了微波前向功率、工作气流量、载气流量等参数,确定了MPT-AES法测定各元素的最佳实验条件。在该条件下铜、锌、铁、锰、硒、锶的检出限分别为7ng.mL-1、46ng.mL-1、13ng.mL-1、8ng.mL-1、1.2ng.mL-1、5.6ng.mL-1。相对标准偏差(RSD)均在0.9%~4.8%之间,线性范围分别为0.1~100μg.mL-1、0.5~100μg.mL-1、0.5~100μg.mL-1、0.1~100μg.mL-1、0.01~10μg.mL-1、0.05~100μg.mL-1,加标回收率均在96%~110%之间。 相似文献
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A system using a microwave induced plasma, as an emission source was optimized for total mercury determinations. The system contains a flow injection section in which mercury is reduced and deposited on a gold/platinum collector, and carried to the emission source. The microwave was generated in a Surfatron cavity. An experimental design was applied to optimize parameters concerning plasma conditions, amalgamation, desorption and mercury vapor generation. The limit of detection of the method was 14 pg ml(-1) of mercury, using peak area mode while LDs was 1.3 pg ml(-1) using peak height mode, with a 2% RSD and a linear dynamic range of almost three orders of magnitude. The accuracy was assessed using a certified reference material of atmospheric particulate National Institute of Standards and Technology (NIST) 2704. No significant difference at 95% confidence level was observed between the certified value and our result. 相似文献
20.
Isomorphic substitution of boron into ZSM‐5 zeolite under microwave‐assisted hydrothermal conditions was systematically studied. When microwave treatment and conventional heating were used, BZSM‐5 zeolite could be obtained within one day, whereas the synthesis of BZSM‐5 under conventional hydrothermal conditions took five days at 180 °C. Various parameters that affect the crystallization of BZSM‐5, such as templates, crystallization time, the silicon source and the Si/B ratio were investigated. Systematic variations of these parameters revealed that this zeolite can be obtained from the reaction mixture with optimized ratios of Si/B > 0.6. Among various tested sources, tetraethylorthosilicate (TEOS) turned out to be the best source for synthesis of borosilicate zeolite and further investigations were done with TEOS as silicon source. The obtained products were characterized by XRD, SEM, and IR spectroscopic techniques. 相似文献