容量法测定氧化钒中的各种价态钒

用NaOH溶液处理样品，分离V（V）然后以Fe(Ⅱ）滴定测定之。定量加入过量的V（V）到上述残渣中并用H2SO4溶解，用Fe(Ⅱ）滴定，计算出V（Ⅱ），V（Ⅲ）的含量。V（Ⅳ）的测定是通过从总钒量中扣除V（Ⅱ）、V（Ⅲ）、V（Ⅴ）的含量得到。V（Ⅱ）、V（Ⅲ）和V（Ⅴ）的回收率均大于96％，其8次测定结果的相对标准偏差分别为：9．8％、0．4％、1．2％；本法快速、简便，在实际应用中效果良好。     

Spectroscopic fingerprints of valence and spin states in manganese oxides and fluorides

We performed a systematic study of soft X-ray absorption spectroscopy in various manganese oxides and fluorides. Both Mn L-edges and ligand (O and F) K-edges are presented and compared with each other. Despite the distinct crystal structure and covalent/ionic nature in different systems, the Mn-L spectra fingerprint the Mn valence and spin states through spectral lineshape and energy position consistently and evidently. The clear O- and F-K pre-edge features in our high resolution spectra enable a quantitative definition of the molecular orbital diagram with different Mn valence. In addition, while the binding energy difference of the O-1s core electrons leads to a small shift of the O-K leading edges between trivalent and quadrivalent manganese oxides, a significant edge shift, with an order of magnitude larger in energy, was found between divalent and trivalent compounds, which is attributed to the spin exchange stabilization of half-filled 3d system. This shift is much enhanced in the ionic fluoride system. This work provides the spectroscopic foundation for further studies of complicated Mn compounds.     

Analysis of polyfluoroalkyl substances and bisphenol A in dried blood spots by liquid chromatography tandem mass spectrometry

Dried blood spots (DBS), collected as part of the newborn screening program (NSP) in the USA, is a valuable resource for studies on environmental chemical exposures and associated health outcomes in newborns. Nevertheless, determination of concentrations of environmental chemicals in DBS requires assays with great sensitivity, as the typical volume of blood available on a DBS with 16-mm diameter disc is approximately 50 μL. In this study, we developed a liquid–liquid extraction and high-performance liquid chromatography/tandem mass spectrometry method for the detection of perfluorooctanesulfonate (PFOS), perfluorooctanoate (PFOA), and bisphenol A (BPA) in DBS. The method was validated for accuracy, precision, and sensitivity, by spiking of target chemicals at different levels on Whatman 903 filter cards, which is used in the collection of DBS by the NSP. Contamination arising from collection, storage, and handling of DBS is an important issue to be considered in the analysis of trace levels of environmental chemicals in DBS. For the evaluation of the magnitude of background contamination, field blanks were prepared from unspotted portions of DBS filter cards collected by the NSP. The method was applied for the measurement of PFOS, PFOA, and BPA in 192 DBS specimens provided by NSP of New York State. PFOS and PFOA were detected in 100 % of the specimens analyzed. The concentrations of PFOS and PFOA measured in DBS were similar to those reported earlier in the whole blood samples of newborns. BPA was also found in 86 % of the specimens at concentrations ranging from 0.2 to 36 ng/mL (excluding two outliers). Further studies are needed to evaluate the sources of BPA exposures and health outcomes in newborns.     

Optoelectronic and Self‐assembly Properties of Porphyrin Derivatives with Click Chemistry Modification

A series of functionalized porphyrin molecules containing electron‐rich alkynes, synthesized by means of the Sonogashira coupling reaction were further modified by reacting the ethynyl groups with click reagent through a formal [2+2] click reaction. The photophysical and electrochemical properties of the porphyrin derivatives were studied by UV/Vis spectroscopy and cyclic voltammetry. We show that the optoelectronic properties are affected by the click reagent groups and central metal ions. The functionalized porphyrin molecules show strong charge‐transfer (CT) bands in the visible region (near‐IR region) and potent redox activities. Through a phase‐exchange self‐assembly method, the highly organized morphologies were observed by scanning electron microscopy (SEM). The functionalized porphyrin molecules represent an interesting set of candidates for optoelectronic device components. The effect of the metal ions or click reagent groups on the self‐assembly properties were also studied by the UV/Vis spectroscopic titration experiments.     

Effects of mechanical loadings on the performance of a piezoelectric hetero-junction

A fully-coupled model for a piezoelectric hetero-junction subjected to a pair of stresses is proposed by discarding the depletion layer approximation. The effect of mechanical loadings on PN junction performance is discussed in detail. Numerical examples are carried out for a p-Si/ZnO-n hetero-junction under a pair of stresses acting on the ntype ZnO portion near the PN interface, where ZnO has the piezoelectric property while Si is not. It is found that the bottom of conduction band is lowered/raised near the two loading points due to the decrease/increase in the electron potential energy there induced by a tensile-stress mode via sucking in majority-carriers from two outside regions, which implies appearance of a potential barrier and a potential well near two loading points. Furthermore, the barrier height and well depth gradually become large with increasing tensile stress such that more and more electrons/holes are inhaled in loading region from the n-/p-zone, respectively. Conversely, rising/dropping of conduction band bottom is brought out near the two loading points by a compressive-stress mode due to the increase/decrease in the potential energy of electrons by pumping out the majority-carriers from the loading region to the two outside regions. Therefore, a potential well and a potential barrier are induced near the two loading points, such that more and more electrons/holes are driven away from the loading region to the n-zone/p-zone, respectively, with the increasing compressive stress. These effects are important to tune the carrier recombination rate near the PN interface. Thus, the present study possesses great referential significance to piezotronic devices.     

紫外光引发环氧树脂的下行前线聚合行为

采用紫外光(UV)引发法研究了221型脂环族环氧树脂的下行前线聚合行为.探讨了光引发剂、热引发剂用量和预热温度等对聚合前线的推动速率Vf和前线引发时间ti的影响,并利用傅里叶变换红外光谱(FTIR)、热重(TG)和差示扫描量热(DSC)等对固化物结构和热性能进行了表征.研究结果表明,提高光引发剂浓度、热引发剂浓度或预热温度,均可提高聚合前线的推动速率Vf,缩短引发时间ti.采用该技术制备的环氧树脂固化物具有较好的均一性及热稳定性.     

CsI:Tl晶体对高能X光照射量的响应关系研究

在X光探伤系统中使用效率较高的CsI：Tl晶体作为X光转换体。CsI：Tl晶体对X光的响应关系是精密图像处理、定量测量所需的一项重要参量。理论上已经推导了CsI：Tl晶体对X光的响应呈现线性关系,并针对性地设计了在^60Co放射源上的定量测量实验,所获数据不仅充分证明了理论推导的正确性,还证明了相应系统的这种线性关系的线性度非常好。     

Scaling and universality of integer quantum Hall plateau-to-plateau transitions

We have investigated the integer quantum Hall plateau-to-plateau transition in two-dimensional electrons confined to AlxGa(1-x)As-Al0.33Ga0.67As heterostructures over a broad range of Al concentration x. For x between 0.65% and 1.6%, where the dominant contribution to disorder is from the short-range alloy potential fluctuations, we observe a perfect power-law scaling in the temperature range from 30 mK to 1 K with a critical exponent kappa = 0.42 +/- 0.01.     

Bipolar copolymers comprised mesogen‐jacketed polymer containing oxadiazole units and PVK as host materials for electroluminescent devices

Nonconjugated bipolar transport polymers have been developed as host materials for electroluminescent devices by incorporating both electron‐transporting and hole‐transporting functionalities into copolymers. The random copolymer PCt‐nvk3‐7 containing mesogen‐jacketed segment of P‐Ct have been synthesized and characterized. The effect of mesogen‐jacketed segment content of these bipolar copolymers on device performance has been investigated. The results of polymer light‐emitting diodes (PLEDs) show that the jacketed content of copolymers has a significant effect on device performance: lowering charge transport and facilitating the hole‐electron recombination leads to much higher current efficiency. Applying these high triplet random copolymers as host, the maximum current efficiency of 0.70 cd/A and the maximum brightness of 1872.8 cd/m² was achieved for PCt‐nvk3‐7 with an orange‐emitting complex dopant. The results suggest that the bipolar copolymers PCt‐nvks can be good host polymers for electrophosphorescent devices. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 7861–7867, 2008