Controlling water temperature for efficient coal/gangue recognition

Coal and gangue (black-gray solid wastes in coal) recognition is vital to avoid waste of resources and pollution of the environment during the coal production. Considering their color/temperature is very close to each other, the traditional visible image and infrared image analyzing method is hard to obtain satisfied recognition efficiency. Therefore, a new idea of the ‘liquid intervention + infrared monitoring’ method was proposed to improve the recognition efficiency. In this article, the coal/gangue recognition experiments with different water temperatures were conducted, and the infrared thermal imager was used to record temperature variation after water intervention. The results show that when the water temperature is lower than the ambient temperature, the temperature difference between coal and gangue reaches the maximum value within 10 s, which is five times that without water intervention. The mean value of temperature difference between coal and gangue shows an approximate linear downward trend with the increasing of water temperature. The results indicate that under the condition of water intervention, it is recommended to choose water with a temperature below the ambient air, which may be a new approach to improve the coal/gangue recognition efficiency under different complex environments in underground coal mines.     

溴代甲烷在TiO2上的光催化降解研究

系统地研究了CH₃Br在溶胶-凝胶法制备的TiO₂催化剂上的气相光催化氧化行为,考察了催化剂煅烧温度、催化剂中残留NO-3、反应物料中的水份、反应温度等催化剂制备及反应条件对催化剂反应性能的影响,并结合XRD、BET比表面积和FTIR等表征结果对TiO₂催化剂的反应行为进行了解释.实验结果表明,CH₃Br在TiO₂上的气相光催化氧化是典型的一级反应,表观活化能为13.7kJ/mol.反应初始阶段存在显著的催化剂失活现象,催化剂高温煅烧,NO-3及水等对该反应活性都有明显的抑制作用,提高反应温度有利于改善催化剂的反应性能.     

气提吸附／热脱附／气相色谱－质谱法分析污水中的痕量有机物

采用气提吸附／热脱附／气相色谱－质谱法对齐鲁公司所处地区工业污水进行分析。方法采用Ｔｅｎａｘ－ＧＣ吸附剂对样品进行气提吸附，脱附时样品直接进入色谱仪汽化室，一次进样即可完成全组分分析，共检测出含四氯丙醚在内的４０种有机组分，测定了各组分的程序升温保留指数。气相色谱－质谱法测定出四氯丙醚三个异构体的结构。     

Formation of Water Complexes with Organic Compounds in Solid Matter. IR Manifestation and DFT Study

In terms of FTIR study it was estimated that water forms the complexes with furan, thiophene, dichloromethane, tribromomethane in low temperature films at 90–150 K interval and with benzene in KBr matrix at ambient temperature. The mechanism of intermolecular interaction was simulated by ab initio calculation using DFT method. It was shown that complex formation occurs due to arising of hydrogen bond between hydronium ion of water cluster or single water molecule with organic components.     

Application of 1H NMR spectroscopy method for determination of characteristics of thin layers of water adsorbed on the surface of dispersed and porous adsorbents

The paper presents 1H NMR spectroscopy as a perspective method of the studies of the characteristics of water boundary layers in the hydrated powders and aqueous dispergated suspensions of the adsorbents. The method involves measurements of temperature dependence proton signals intensity in the adsorbed water at temperatures lower than 273 K. Free energy of water molecules at the adsorbent/water interface is diminished due to the adsorption interactions causing the water dosed to the adsorbent surface freezes at T < 273 K. Thickness of a non-freezing layer of water can be determined from the intensity of the water signal of 1H NMR during the freezing-thawing process. Due to a disturbing action of the adsorbent surface, water occurs in the quasi-liquid state. As a result, it is observed in the 1H NMR spectra as a relatively narrow signal. The signal of ice is not registered due to great differences in the transverse relaxation times of the adsorbed water and ice. The method of measuring the free surface energy of the adsorbents from the temperature dependence of the signal intensity of non-freezing water is based on the fact that the temperature of water freezing decreases by the quantity which depends on the surface energy and the distance of the adsorbed molecules from the solid surface. The water at the interface freezes when the free energies of the adsorbed water and ice are equal. To illustrate the applicability of the method under consideration the series of adsorption systems in which the absorbents used differed in the surface chemistry and porous structure. In particular, the behaviour of water on the surface of the following adsorbents is discussed: non-porous and porous silica (aerosils, silica gels); chemically and physically modified non-porous and porous silica (silanization, carbonization, biopolymer deposition); and pyrogeneous Al2O3 and aluminasilicas. The effect of preliminary treatment of the adsorbent (thermal, high pressure, wetting with polar and non-polar solvents) on the characteristics of the structurized water layers was discussed. The influence of the adsorbent porous structure on the free energy of the adsorbed water was also studied. The discussion of the obtained results was made.     

Evaluation of emulsion stability by thermogravimetric analysis (tg)

A rapid and simplified method for the determination of phase inversion temperature (PIT) and the stability of oil in water emulsions, stabilized by nonionic emulsifiers, is described. The method is based on the use of any thermogravimetric apparatus from which the rate of loss of water can be measured as a function of linear increase in the emulsion temperature. A DTG peak is obtained at the PIT: the emulsion in which the lowest PIT is observed is also the less stable one.     

Determination of pyrethroid,organophosphate and organochlorine pesticides in water by headspace solid-phase microextraction

Simultaneous determination of pyrethroid, organophosphate (OP) and organochlorine (OC) pesticides in water was achieved with headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-electron-capture detection (GC-ECD). The parameters affecting HS-SPME of pesticides from water were optimized, including extraction temperature, sample and headspace volumes, and sodium chloride amounts. The effects of desorption temperature, desorption time, and position of the fibre in the GC inlet were also investigated. Extraction temperature was the most important factor affecting the recoveries of analytes, and the optimized temperature was 96°C. The addition of salt did not increase extraction efficiencies of the pesticides from the water. The optimized desorption conditions in the GC were as follows: desorption time of 10?min; desorption temperature of 260°C; and a 2?cm position of the fibre in the inlet. The method detection limits were in the low-ng/L level with a linearity range of 50–1000?ng/L for the OCs, 50–5000?ng/L for the OP, and 50–20?000?ng/L for the pyrethroids. These data demonstrated that HS-SPME is a sensitive method for the determination of pyrethroid, OC, and OP pesticides in water.     

Analysis of herbicides in water using temperature-responsive chromatography and an aqueous mobile phase

A simple and rapid method has been developed for herbicides in water using temperature-responsive liquid chromatography (LC) and a column packed with poly(N-isopropylacrylamide) (PNIPAAm), a polymer anchored on the stationary-phase surface of modified silica. PNIPAAm reversibly changes its hydrophilic/hydrophobic properties in water in response to temperature. The method was used to determine five sulfonylurea and three urea herbicides. Separation was achieved with a 10 mM ammonium acetate (pH 3.0) isocratic aqueous mobile phase, and by changing the column temperature. The analytes were extracted from water by off-line solid-phase extraction (SPE) with an N-vinyl-pyrrolidone polymer cartridge. The average recoveries of the eight herbicides from spiked pure water, tap water and river water were 70-130% with relative standard deviations (RSDs) of <10%. The limits of quantitation (LOQ) of the eight herbicides were between 1 and 4 microg l(-1).     

The mean lifetimes of H-bonds in water supercritical states

The dynamics of H-bonds in supercritical water in the region close to the saturation curve was studied at constant pressures of 30 and 50 MPa and temperature 673 K. The mean lifetime of H-bonds and changes in the topological and dynamic characteristics of H-bonding in supercritical water caused by temperature, density, and pressure variations were determined by the molecular dynamics method with the use of the TIP4P-HB model potential.     

环境水样中总磷分析方法及仪器的研究进展

磷是生物不可或缺的营养元素之一,但由于人类活动影响,在地表水和近岸海水中总磷一直是主要污染指标。总磷测定通常分两步进行：一是将水样中各种不同形态的磷消解转化为可被检测的磷酸盐;二是测定消解后样品中的磷酸盐浓度。消解方法有硫酸-硝酸消解法、干法灰化法、微波辅助消解法、过硫酸钾-高温高压消解法、UV光氧化法等。测定方法包括电化学法、化学发光法、磷钼蓝分光光度法、磷钒钼黄分光光度法等。目前应用最为广泛的是过硫酸钾-高温高压消解法和磷钼蓝分光光度法。总磷测定仪器通常基于该消解法和测定法而开发,可分为用于实验室的水样离线分析仪和用于水体现场的在线分析仪两类。该综述总结了近20年来环境水样中上述总磷分析方法及仪器的研究进展,比较了各方法和仪器的特点,并分析了总磷分析方法和分析仪器的发展趋势。     

淀粉基高吸水性树脂吸水性能的测定条件评价

研究了测定条件对淀粉基高吸水性树脂吸水性能的影响,分别考察了测定方法、树脂粒径、初始加水量、水介质pH、温度及溶液中盐的质量分数对树脂吸水倍率和吸水速率的影响.结果表明,采用100目网筛过滤法测定树脂的吸水性能结果较准确;当吸水介质与干树脂的质量比为2 400∶1,pH为7时,可以使树脂达到最大饱和吸水倍率;在树脂粒径96～180μm范围内,随着树脂粒径的减小、水介质温度的升高及盐浓度的降低,树脂的吸水倍率和吸水速率增大.     

Method for analysis of the composition of acid soaps by electrolytic conductivity measurements

Here, we propose a method for determining the stoichiometry of acid-soap crystallites. The method is based on dissolving the crystallites in water at an appropriate working temperature, followed by measurement of the electrolytic conductivity of the obtained solutions. The working temperature is chosen in such a way that the only precipitate in the solutions is that of carboxylic acid, whereas the carboxylate salt is dissociated, and its content in the dissolved crystals determines the solution's conductivity. In the theoretical model for data interpretation, we took into account the dependence of the molar conductance on the ionic strength. The method was applied for determining the stoichiometry of acid-soap crystals collected from solutions of potassium myristate (tetradecanoate) at 25 degrees C. The crystals were dissolved in water at working temperature of 40 degrees C, at which the conductivity was measured. The stoichiometry of all samples determined in the present study coincides with that independently obtained by another method that is based on in situ pH measurements.     

Superheated water chromatography of phenols using poly(styrene-divinylbenzene) packings as a stationary phase.

A method for the superheated water chromatography of phenols was developed using a poly(styrene-divinylbenzene) (PSDVB) stationary phase. The stationary phase of superheated water chromatography must be stable against the attack of water. A durability test for PSDVB packings and octadecylsilyl (ODS)-silica gels indicated that PSDVB packings were stable in superheated water in the temperature range of 100-150 degrees C, whereas octadecylsilyl groups of ODS-silica gels cleaved even at 100 degrees C. The retention of phenols on the PSDVB stationary phase decreased with an elevation of the column temperature. The retention mechanism was characterized using a thermodynamic theory that has been used for describing retention in conventional RP-HPLC. The application of the present method to an environmental analysis was also demonstrated, in which a suitable separation with good peak shape was obtained for p-chlorophenol in river-water samples.     

Temperature effect on the selective hydration of sodium ion in nitrobenzene.

The effect of the temperature on the co-extraction of water molecules with Na+ from water to nitrobenzene (NB) in the presence of dipicrylaminate ion has been studied. The number (n) of water molecules co-extracted with a Na+ ion, as measured by the Karl Fischer method, increased from 3.1 to 5.2 with increasing temperature (6-65 degrees C). This observation is in apparent contradiction to the expectation from simple thermodynamics because hydration is generally an entropically unfavorable process. Additional 1H NMR experiments for the selective hydration of Na+ in deuterated NB have confirmed that the association constants of water with Na+ indeed decrease with increasing temperature. On the other hand, however, it has been shown that water solubility into NB substantially increases with temperature. We conclude that the latter effect overwhelms the former unfavorable entropy effect, which results in a net increase of the n-value, as observed.     

Predicting the melting temperature of ice-Ih with only electronic structure information as input

The melting temperature of ice-Ih was calculated with only electronic structure information as input by creating a problem-specific force field. The force field, Water model by AFM for Ice and Liquid (WAIL), was developed with the adaptive force matching (AFM) method by fitting to post-Hartree-Fock quality forces obtained in quantum mechanics∕molecular mechanics calculations. WAIL predicts the ice-Ih melting temperature to be 270 K. The model also predicts the densities of ice and water, the temperature of maximum density of water, the heat of vaporizations, and the radial distribution functions for both ice and water in good agreement with experimental measurements. The non-dissociative WAIL model is very similar to a flexible version of the popular TIP4P potential and has comparable computational cost. By customizing to problem-specific configurations with the AFM approach, the resulting model is remarkably more accurate than any variants of TIP4P for simulating ice-Ih and water in the temperature range from 253 K and 293 K under ambient pressure.     

低温下溶胶凝胶法制备TiO2纳米晶

从含过量水的溶胶出发,在室温下得到了TiO₂纳米晶。通过红外光谱,透射电子显微镜法和X射线粉末衍射法对含有过量水的溶胶体系中TiO₂纳米晶的室温形成机理进行了研究。与传统的溶胶凝胶法相比,在改良的溶胶凝胶体系中,在缩聚反应之前由于水过量使得钛的先驱体快速且充分的水解,从而生成[TiO₆]基团,随之形成TiO₂纳米晶。晶粒的尺寸为约3.5 nm,该法得到的TiO₂纳米晶比传统溶胶凝胶法得到的TiO₂纳米晶和商用光催化剂德固赛P25具有更好的光催化活性。     

Determination of polynuclear aromatic hydrocarbons in water by flotation enrichment and HPLC

A method of concentration and determination of several polynuclear aromatic hydrocarbons (PAHs) in water by flotation enrichment and HPLC is described. Triton X-100 was used as the foaming agent to extract the PAHs from water by passage of nitrogen. Reversed-phase liquid chromatography with coupled fluorescence detection was applied to separate and determine these PAHs. Various factors which may affect the recovery of PAHs from water, including pH, temperature and the concentration of Triton X-100 added, are discussed. This simplified method of concentrating PAHs from water has been applied to determine PAHs in water from Lake Erie. The method has practical value for the determination of PAHs in large volumes of water.     

Estimation of dry rubber content in natural rubber latex by differential scanning calorimetry

Differential Scanning Calorimetry (DSC) is employed to study the changes in enthalpy of natural rubber latex samples when heated under a controlled temperature program. It is found that the mass normalized areas of the DSC curves between room temperature and 170 °C for different latex samples are inversely proportional to the dry rubber content (DRC) of the samples, measured following the weighing and drying method. The changes in total enthalpy of the samples in this temperature range are interpreted as due to the variations in the quantity of water present in the samples. The measurements have been repeated by diluting selected samples with known quantities of water, and it is found that the normalized areas of the DSC curves are directly proportional to the amount of water added to the latex. The method can be used to estimate the DRC of natural rubber latex accurately. Its advantages and limitations are discussed.     

Determination of trace amounts of off-flavor compounds in drinking water by stir bar sorptive extraction and thermal desorption GC-MS.

A method for the determination of trace amounts of off-flavor compounds including 2-methylisoborneol, geosmin and 2,4,6-trichloroanisole in drinking water was developed using the stir bar sorptive extraction technique followed by thermal desorption-GC-MS analysis. The extraction conditions such as extraction mode, salt addition, extraction temperature, sample volume and extraction time were examined. Water samples (20, 40 and 60 ml) were extracted for 60-240 min at room temperature (25 degrees C) using stir bars with a length of 10 mm and coated with a 500 microm layer of polydimethylsiloxane. The extract was analyzed by thermal desorption-GC-MS in the selected ion monitoring mode. The method showed good linearity over the concentration range from 0.1 or 0.2 or 0.5 to 100 ng l(-1) for all the target analytes, and the correlation coefficients were greater than 0.9987. The detection limits ranged from 0.022 to 0.16 ng l(-1). The recoveries (89-109%) and precision (RSD: 0.80-3.7%) of the method were examined by analyzing raw water and tap water samples fortified at the 1 ng l(-1) level. The method was successfully applied to low-level samples (raw water and tap water).     

固相微萃取-高效液相联用分析环境水样中的痕量■

 应用固相微萃取与高效液相联用技术 (SPME HPLC)分析了环境水样中的痕量 艹屈 。对SPME的条件如萃取时间、萃取温度、离子强度、解吸方式、解吸溶剂、解吸时间和HPLC条件进行了优化 ,建立了SPME HPLC分析环境水样中痕量 艹屈 的方法 ,并将其用于分析自来水、雨水、矿泉水和江水等实际水样。方法的线性范围为 0 0 13μg/L～ 3 0 μg/L ,检出限为 2 7ng/L ,相对标准偏差 (RSD ,n =6 )为 5 6 % ,回收率为 10 3 2 %～ 119 3%。该方法适合于环境水样中痕量 艹屈 的分析 ,体现了SPME在样品前处理中快速、灵敏、简单、无溶剂的特点。