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1.
Electrochemical preconcentration on a platinum filament, followed by atomization in an argon—hydrogen flame with simultaneous electrothermal heating of the filament, is used for the determination of selenium in technical sulphuric acid. The effect of experimental parameters such as acid concentration, deposition potential and temperature are described, and the speciation of selenium in sulphuric acid is discussed. The technical acids were found to contain selenium in the range 30–60 μg l-1.  相似文献   

2.
针对酒精灯火焰呈黄色的解释争议进行研究,以降低环境温度和减少氧气浓度为方向,设计了可观察环境温度变化对含氢燃料火焰颜色影响的仪器。对乙醇、丁烷、蜡烛等燃烧火焰进行降温测试,发现含氢燃料正常燃烧火焰颜色一般为黄色、降低环境温度后变为极淡的蓝色(光亮条件下)的规律,证明了燃烧过程中水分子处于激发态是导致火焰颜色由蓝色变为黄色的重要原因,钠元素的焰色反应不是酒精灯火焰呈黄色的唯一原因。对丁烷喷枪火焰颜色的降温测试,意外观察到4种疑似氢原子光谱的可见光谱线,为今后寻找该谱线提供了可借鉴的方向。研究过程可作为基于真实情境的研究素材,通过问题的发现、仪器的改进和规律的总结,提高学生运用化学知识解决真实问题的能力,培养学生的核心素养。  相似文献   

3.
Procedures are developed for determining volatile sulfur-containing impurities, hydrogen sulfide, simple mercaptans, sulfides, and disulfides in air and aqueous solutions. The procedures are based on the principle’s headspace gas chromatography and equilibrium preconcentration. The procedures differ from the officially approved ones in that the operations of sampling and sample preparation to gas-chromatographic analysis considerably reduce the loss of hydrogen sulfide and mercaptans unstable in humid air. The procedures provide the determination of sulfur-containing substances at the level of their maximum permissible concentrations (MPC) in industrial emissions and natural waters and the analytical range of four orders of magnitude; they can be implemented on gas chromatographs with flame ionization and flame photometric detectors, a quartz capillary column, and a thermostated gas-sampling valve.  相似文献   

4.

The combustible features of wheat dust easily induce a potential hazard in its processing and application. To clearly reveal the effects of porous mesh parameters on the flame propagation of wheat dust, a vertical combustion pipeline together with the data collecting by the high-speed photography and fine thermocouple was built. Results indicate that with the increase in the mesh scale, the dust combustion and peak temperature are intensified first and then decreased with a darker luminescence. The increasing mesh number shows an inhibition effect on both peak temperature and combustion pressure, but an accelerating first and then weakening effect on flame velocity. A smaller particle size contributes to a more complete combustion, causing a higher peak temperature and flame velocity. At the particle mass of 2.5 g, the maximum value of peak temperature, flame velocity and combustion pressure were obtained during the flame propagation.

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5.
Organophosphate esters have been extensively used as flame retardants and plasticizers. The analysis of organophosphate esters in the environment is a hot topic because many of them are toxic and persistent. We developed a novel procedure for determining organophosphate esters in sediment. In this work, pressurized liquid extraction and solid‐phase microextraction are used for sample preparation to extract and concentrate the analytes, which are then analyzed by gas chromatography with flame photometric detection. The extraction parameters of pressurized liquid extraction were investigated and optimized by orthogonal design and then evaluated by range analysis and analysis of variance. Under the optimal conditions, the proposed procedure showed wide linear ranges (0.90–100 ng/g) with correlation coefficients ranging from 0.9921 to 0.9990. The detection limits of the method were in the range of 0.009–0.280 ng/g with standard deviations ranging from 2.2 to 9.5%. Recoveries of the proposed method ranged from 82.3 to 108.9% with relative standard deviations <8.4%. The obtained method was applied successfully to the determination of organophosphate esters in real sediments with recoveries varying from 79.8 to 107.3%. The proposed method was proved to be simple, easy, and sensitive for analyzing organophosphate esters in sediment samples.  相似文献   

6.
A combined method of dynamic headspace-needle trap sample preparation and gas chromatography for the determination of formic and acetic acids in aqueous solution was developed in this study. A needle extraction device coupled with a gas aspirating pump was intended to perform sampling and preconcentration of target compounds from aqueous sample before gas chromatographic analysis. The needle trap extraction (NTE) technique allows for the successful sampling of short chain fatty acids under dynamic conditions while keeping the headspace (HS) volume constant. Two important parameters, including extraction temperature and effect of acidification, have been optimized and evaluated using the needle trap device. The method detection limits for the compounds estimated were 87.2microg/L for acetic acid and 234.8microg/L for formic acid in spite of the low flame ionization detection response for formic acid and its low Henry's law constant in aqueous solution. Precision was determined based on the two real samples and ranged between 4.7 and 10.7%. The validated headspace-needle trap extraction method was also successfully applied to several environmental samples.  相似文献   

7.
Transport properties of chemical species are required for many combustion models. A sensitivity analysis is conducted to assess the significance of transport properties and their underlying molecular parameterizations for atmospheric pressure premixed laminar flames for three different fuels and two different approaches to transport property calculations. The analysis is performed at both the macroscopic level of Arrhenius A-factors and transport coefficients as well as at the molecular scale. First- and second-order sensitivities of reactant, intermediate, and product species concentrations, temperature, and flame velocity were calculated with respect to various parameters, all within the mixture approximation using ADIFOR 2.0, a software package that supports exact differentiation. Parameters considered were the binary diffusion coefficients, pure species thermal conductivity coefficients, and thermal diffusion ratios. The more fundamental molecular parameters: collision diameters, well depths, dipole moments, polarizabilities, and the rotational relaxation collision numbers were also considered. Influential transport properties are found to be as important in flame modeling as influential reaction rates, and both should be taken into account when building chemical mechanisms. Transport parameter importance was found to vary according to the independent variable being considered and the flame type. Magnitudes of sensitivities appear to be more influenced by the underlying molecular parameters than the approach used to compute the transport properties. The number of significant sensitivities to transport parameters increases for the progression: flame temperature, flame velocity, reactant species, product species, and intermediate radical species. Many dependent variables have significant sensitivities to the pure species thermal conductivities of N2, O2, and the fuel. At the molecular level, large sensitivities to the collision diameters of several species are also observed, but significant sensitivity to well depths, although observed is less and more rare. Large sensitivities are not observed to the rotational relaxation collision number, the dipole moment, or to the molecular polarizability. Second-order sensitivities are significant for a number of dependent variables. © 2005 Wiley Periodicals, Inc. Int J Chem Kinet 37: 538–553, 2005  相似文献   

8.
A novel graphene oxide decorated with silver nanoparticles coating on a stainless‐steel fiber for solid‐phase microextraction was prepared. Scanning electron microscopy and X‐ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid‐phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single‐fiber repeatability and fiber‐to‐fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4–116.3% with relative standard deviations less than 16.2%.  相似文献   

9.
For the first time, the low‐density solvent‐based vortex‐assisted surfactant‐enhanced emulsification liquid–liquid microextraction, followed by GC‐flame photometric detection has been developed for the determination of eight organophosphorus pesticides in aqueous samples. A small volume of organic extraction solvent (toluene) was dispersed into the aqueous samples by the assistance of surfactant and vortex agitator. The extraction was performed in a special disposable polyethylene pipette, allowing using the reagents with lower density than water as extraction solvents. The influence parameters were systemically investigated and optimized: toluene (30 μL) and Triton X‐100 (0.2 mmol/L) were used as the extraction solvent and the surfactant, respectively, and the extraction was performed for 1 min under room temperature without adding sodium chloride. Under the optimum conditions, the validation parameters such as the RSD (n = 6; 2.1–11.3%), LOD (0.005 and 0.05 μg/L), and linear range (0.1–50.0 μg/L with correlation coefficients (0.9958–0.9992) showed the method was satisfying. The proposed method has been successfully applied to the determination of the organophosphorus pesticides in real samples with recoveries between 82.8 and 100.2%.  相似文献   

10.
Organophosphate esters, widely used as flame retardants and plasticizers, are regarded as a class of emerging pollutants. In this work, a novel approach was developed for the fabrication of a solid‐phase microextraction fiber by using hybrid silica‐based materials with immobilized ionic liquids with sol–gel technology, and the prepared solid‐phase microextraction fiber was then coupled with gas chromatography and flame photometric detection for the analysis of six organophosphate esters. The high loading of 1‐hexadecyl‐3‐methylimidazolium bis(trifluoromethylsulfonyl)imide was confined within the hybrid network. The developed solid‐phase microextraction fiber possesses a coating thickness of ~35 μm with good thermal stability and long lifetime. The parameters affecting the extraction efficiency such as extraction time, temperature, pH, and ionic strength of the sample solution were optimized. Under the optimized conditions, the limits of detection were in the range of 0.04?0.95 μg L?1, and the precision of the method assessed with repeatability and reproducibility of (RSD%) ?13 and ?29%, respectively. The proposed method was successfully applied to determine the six organophosphate esters in three real water samples, with recoveries in the range of 64.8?125.4% at two different spiking concentration levels. As a result, the proposed method demonstrated its potential for application in trace determination of organophosphate esters in actual water samples.  相似文献   

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