氢化物发生原子荧光法测定饮用水中的微量硒

氢化物发生原子荧光法测定饮用水中的微量硒时。仪器条件和试剂的浓度选择很重要。本文对条件的最佳化进行了实验。并对方法的精密度、准确度和检出限进行了讨论。     

HPLC-UV测定水中微量溴酸根的方法

针对水中微量溴酸盐的测定问题,建立了一种用苯酚为衍生试剂、用HPLC-UV检测的柱外衍生测定方法.本方法的检出限为0.82μg·L-1,在溴酸根浓度为5～50μg·L-1范围内具有良好的线性关系(R2=0.9986).测定系列溴酸根浓度的相对偏差(RSD)均小于5%,样品加标平均回收率为99.8%～110.9%.     

Hydrogen storage and distribution systems

Hydrogen storage and transportation or distribution is closely linked together. Hydrogen can be distributed continuously in pipelines or batch wise by ships, trucks, railway or airplanes. All batch transportation requires a storage system but also pipelines can be used as pressure storage system. Hydrogen exhibits the highest heating value per weight of all chemical fuels. Furthermore, hydrogen is regenerative and environment friendly. There are two reasons why hydrogen is not the major fuel of toady’s energy consumption: First of all, hydrogen is just an energy carrier. And, although it is the most abundant element in the universe, it has to be produced, since on earth it only occurs in the form of water. This implies that we have to pay for this energy, which results in a difficult economic task, because since the industrialization we are used to consuming energy for free. The second difficulty with hydrogen as an energy carrier is the low critical temperature of 33 K, i.e. hydrogen is a gas at room temperature. For mobile and in many cases also for stationary applications the volumetric and gravimetric density of hydrogen in a storage system is crucial. Hydrogen can be stored by six different methods and phenomena: high pressure gas cylinders (up to 800 bar), liquid hydrogen in cryogenic tanks (at 21 K), adsorbed hydrogen on materials with a large specific surface area (at T < 100 K), absorbed on interstitial sites in a host metal (at ambient pressure and temperature), chemically bond in covalent and ionic compounds (at ambient pressure), oxidation of reactive metals e.g. Li, Na, Mg, Al, Zn with water. These metals easily react with water to the corresponding hydroxide and liberate the hydrogen from the water. Finally, the metal hydroxides can be thermally reduced to the metals in a solar furnace.     

电化学氢化物发生法处理含锑废水及对锑的回收

采用电化学氢化物发生法对模拟含锑废水进行处理,锑与水电解产生的氢形成氢化物从溶液中脱除,而后收集并加热分解锑化氢得到金属锑.实验表明,在酸性条件下对Sb(Ⅲ)去除效果较好,p H=4时去除率为76.1%.Sb(Ⅲ)与电解水产生的氢结合形成锑化氢从溶液中逸出是溶液中锑去除的最主要途径(回收率为66.2%),电沉积和吸附也对锑的去除做出少量贡献.Sb(Ⅴ)须预还原为Sb(Ⅲ)再氢化进行去除.试用了铅、石墨、钨这3种电解阴极材料,铅电极处理效果最佳.     

Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

Pharmaceutical residues have become tightly controlled environmental contaminants in recent years, due to their increasing concentration in environmental components. This is mainly caused by their high level of production and everyday consumption. Therefore there is a need to apply new and sufficiently sensitive analytical methods, which can detect the presence of these contaminants even in very low concentrations. This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues, mainly from the group of non-steroidal anti-inflammatory drugs (salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen, and dicofenac), in wastewaters and surface waters. This analytical method is based on solid phase extraction, derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GC×GC- TOF MS). Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix. The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice, Czech Republic. The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.     

Determination of 4-tert-octylphenol in surface water samples of Jinan in China by solid phase extraction coupled with GC-MS

Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with solid phase extraction (SPE). Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio (S/N = 3) was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations (RSD) was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows: 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.     

连续流动氢化物发生原子荧光法测定水中硒

文章介绍连续流动一氢化物发生一原子荧光测定水中硒的方法,研究了盐酸浓度、硼氢化钾浓度、灯电流、光电倍增管负高压、泵速、载气和屏蔽气流量等对测定硒的影响,找出测定水中硒最佳条件,在最佳条件下,校准曲线相关系数为0.9999.方法检出限为0.0095μg/L,方法的测量范围为0.038-300μg/L,回收率在91.8%-...     

CaH2对Cu-Ce-La-ZSM-5催化分解NO性能的影响

实验采用一步离子交换法制备Cu-Ce-La-ZSM-5催化剂,然后采用共混法制得Cu-Ce-La-ZSM-5/CaH2催化剂。采用扫描电镜（SEM）,电感耦合等离子体发射光谱（ICP-AES）,X射线衍射（XRD）,红外（FTIR）以及NO吸脱附（NO-TPD）对催化剂进行表征。结果显示CaH2的加入使得催化剂中铜离子存在形式发生变化,催化剂表面变光滑洁净,并且吸附NO能力增强。NO催化分解实验的结果表明CaH2提高了催化剂活性和抗氧性。CaH2助催性是由于其受热分解过程中产生的H2能将Cu^2＋还原为具有催化活性的Cu^＋,同时使催化剂表面洁净光滑更容易吸附NO。     

Microwave-Assisted Solvent-Free or Aqueous-Based Synthesis of Biodegradable Polymers

Microwave radiation was used as the energy source for various types of chemical derivatizations of polysaccharides and for the synthesis of biodegradable polyesters in solvent-free or aqueous-based reaction systems. A medium to high degree of substitution was obtained for starch acetates, starch succinates, carboxymethyl konjac, aminated starch, and aminated chitosan. Ring-opening polymerization of lactide and -caprolactone proceeded rapidly even at low power output in the presence of tin octanoate catalyst. Complete monomer conversion and high molecular weight were achieved in less than 6 minutes under nonisothermal conditions. The yield rapidly increased with increasing power output and showed no significant change in a wide range of batch sizes. Polycaprolactone was successfully grafted from starch and konjac acetate in 3 minutes, yielding as high as 24% grafting efficiency and 25% grafting degree.     

CaH_2对Cu-Ce-La-ZSM-5催化分解NO性能的影响

实验采用一步离子交换法制备Cu-Ce-La-ZSM-5催化剂,然后采用共混法制得Cu-Ce-La-ZSM-5/CaH2催化剂。采用扫描电镜(SEM),电感耦合等离子体发射光谱(ICP-AES),X射线衍射(XRD),红外(FTIR)以及NO吸脱附(NO-TPD)对催化剂进行表征。结果显示CaH2的加入使得催化剂中铜离子存在形式发生变化,催化剂表面变光滑洁净,并且吸附NO能力增强。NO催化分解实验的结果表明CaH2提高了催化剂活性和抗氧性。CaH2助催性是由于其受热分解过程中产生的H2能将Cu2+还原为具有催化活性的Cu+,同时使催化剂表面洁净光滑更容易吸附NO。