SiO2粒子对PMMA/SAN共混体系相分离行为的影响

采用小角激光光散射(SALLS)并结合动态流变学方法,考察了气相法二氧化硅(SiO2)粒子的加入对聚甲基丙烯酸甲酯/苯乙烯-丙烯腈无规共聚物(PMMA/SAN)共混体系相行为的影响,得到了添加SiO2粒子前后的相图,发现SiO2粒子对基体相行为的影响与基体的组成有关.对PMMA/SAN(60/40)体系,加入SiO2粒子后相分离温度上升,但并未改变相分离机理,仍为亚稳单相分解过程(spinodal decomposition,SD);而对于PMMA/SAN(30/70)体系,加入SiO2粒子后却降低了体系的相分离温度.该现象可能是SiO2粒子和基体组分界面间组成与PMMA/SAN共混物基体组成的差异造成的.     

高效耗能黏弹性阻尼框架结构减震性能研究

提出了高效耗能黏弹性阻尼器,研究了该阻尼器对框架结构的减震机理。首先给出了高效耗能黏弹性阻尼器的结构构造,推导了小震、大震与巨震作用下的阻尼放大系数计算公式,由此分析了该放大系数的变化规律。此外,还推导了设置高效耗能黏弹性阻尼框架结构的等效阻尼比。分析表明,框架结构设置高效耗能黏弹性阻尼器在阻尼等效前后顶部位移反应时程曲线相差不超过10%。     

ICP-AES测定饮用水中微量钼

应用ICP-AES直接测定生活饮用水中微量钼,检出限:0.01μg/mL;精密度:RSD 0.76%-2%;加标回收率:97.6%-105%.     

微波消解-石墨炉原子吸收光谱法测定菜籽及饼粕中铅和镉

目前菜籽及饼粕的综合利用越来越受到人们的重视,同时重金属的污染问题也日益引起人们广泛的关注,因此测定菜籽及饼粕中铅和镉的含量具有十分重要的意义。文章研究了微波消解溶剂、微波时间和压力对样品消解效果的影响,优化了石墨炉原子吸收光谱法测定条件,建立了一种快速检测菜籽及饼粕中铅、镉含量的有效方法。研究表明,铅、镉的检出限分别为2.172 μg·L-1(54.30 ng·g-1)、0.243 μg·L-1(6.075 ng·g-1),其线性范围分别为0～100 μg·L-1,0～8 μg·L-1;样品测定回收率在80.8%～110.7%之间,RSD小于5.3%。该法具有检出限低、灵敏度高、快速、准确的特点,用于实际样品测定的结果令人满意。     

Synthesis of 2′-Borono-benzaldehyde-7- (8-hydroxy-5-sulfoacid)Qninoline Hydrazone and Recognition of Pb2 +

合成了2 ′,3′和4′-硼酸基苯甲醛-7-(8-羟基-5-磺酸基)喹啉腙衍生物(化合物1～3),研究了硼酸基团取代位置对主体分子识别金属离子客体性能的影响,比较了不同主体分子与Pb2+结合能力的差异.研究结果表明,在pH=7.0的KH2 PO4 -NaOH缓冲溶液中,3种腙衍生物对Pb2+均具有选择性识别作用,主客体分子间形成1∶1型的发光配合物.其中邻位取代的化合物1与Pb2+的结合能力比化合物2和3强,配合物1-P2+的最大发射波长为477 nm,稳定常数为1.1 ×103 L/mol.其它金属离子如Cu2+,Mn2+,Mg2+,Fe2+,Ca2+,C02+,Ni2+,Hg2+,Cd2+和Ag+等对主体分子荧光光谱的影响较小.同时,荧光强度的变化值与p2+浓度在0.36～ 10 μmol/L范围内呈现良好的线性关系,相关系数R=0.9976(n=16),检出限为0.23 μmol/L.将此方法用于环境水样中Pb2+的测定,回收率为92％～108％.     

Chlorination reaction behavior of Zircaloy-4 hulls: experimental and theoretical approaches

Chlorination reaction behavior of Zircaloy-4 (Zry-4) cladding hulls was demonstrated by using a quartz reactor system. By reacting at 380 °C for 3 h, mass of the Zry-4 hulls decreased by 65.8 wt% with Cl₂ utilization of 87.1 mol%. Composition of collected product was analyzed and it was revealed that concentration of Zr was higher than 99.97 wt%. The purity of Zr in the experimental result was higher than expectation when considering Sn (1.31 wt%) and Fe (0.25 wt%) contents which can produce gaseous SnCl₄ and FeCl₃ at the experimental condition. Theoretical calculations were performed to clarify the high purity of Zr by using the HSC code. The simulation results revealed that formation of ZrCl₄ is more preferred than SnCl₄, FeCl₃, and CrCl₃. The preference of chloride formation was confirmed by the theoretical calculation, and it was suggested that the major constituents of Zry-4 might react with Cl₂ to produce chlorides in an order of ZrCl₄ > CrCl₃ > SnCl₄ > FeCl₃. It was also suggested that continuous removal of ZrCl₄ and sufficient supply of Zr source during the chlorination reaction might have contributed to the high purity of Zr.     

In situ deposition behavior of silica-based layers and its effect on thermal degradation of IN713 turbine blades during operation of a micro-gas turbine

This study examined the in situ deposition behavior of silica-based layers on IN713 turbine blades during the operation of a 13 kgf-class gas turbine at a rotation speed of 20,000/min as well as its effect on the degradation of the metallic substrate. Tetraethylorthosilicate (TEOS) was mixed with the fuel (liquid petroleum gas, LPG) and burned to generate silica-based coating precursors for deposition from the flame. Two deposition conditions were adopted. For condition 1 (C1), the silicon-to-carbon ratio in the mixed fuel was set at 0.1 mol% for the first 5 min and at zero mol% for the final 95 min in a 100-min operation. For condition 2 (C2), the ratio was set at 0.005 mol% during the entire 100 min operation. The total TEOS feed was the same under both conditions. C1 resulted in a rather uniform and thicker (5-10 μm on the pressure side) porous silica-based coating on the blade than C2. The in situ deposited layer of C1 was well preserved on the blade and protected the underlying metallic substrate from oxidation during the entire 100 min operation. The layer on the C2 blades was ∼5 μm thick at the region near to root, but was too thin in the other areas on the blade to be protective. The early build-up of a porous layer to an effective thickness on the blades produced a thermal barrier toward the substrate as well as a diffusion barrier toward the oxidizing elements during operation.     

Spectroscopic Properties and Electronic Structure of Bis(L—Histidine)Copper(II) Dinitrate Dihydrate

Electronic absorption spectrum, photoacoustic absorption spectrum and ESR spectrum of bis(L-histidine)copper(II) dinitrate dihydrate crystal were recorded. The experimental results are discussed quantitatively with ligand field theory (LFT) and the radial wave function of non-free copper(II). Our calculations coincides well with the experimental results, and in particular, provides significant correlations between the spectra and coordination structures. The ESR spectrum gives some information about the restudy of classification for the ESR spectra of bis(amino acidato)copper(II) complexs. Additionally, the differences between crystal and frozen solution spectra due to the variance of PH are also reported for the title compound.