IONIC CONDUCTIVITY OF METHYLSILOXANE TERMINATED POLYETHYLENE OXIDE WITH LITHIUM PERCHLORATE NETWORK FILMS

Complex films of crosslinked poly(methylsiloxane-co-ethylene oxide) and lithium perchlorate were prepared. These solid state polymeric electrolytes show a markedly higher ionic conductivity, and excellent flexibility. The ionic conductivity of the network films closed to 10~(-5) Scm~(-1) at room temperature. The effects of Li~+ content, species and contents of crosslinking agents, molecular weight of poly(ethylene oxide) and temperature on the ionic conductivity of the network films were also investigated.     

Raman spectroscopic and structural studies of indigo and its four 6,6'-dihalogeno analogues

The Raman and electron impact mass spectra of synthetic indigo and its four 6,6'-dihalogeno analogues are reported and discussed. The influence of varying the halogen on these Raman spectra is considered. Particular emphasis is laid on distinguishing indigo from 6,6'-dibromoindigo and differentiating between the dihalogenocompounds, so as to develop protocols for determining whether artefacts are coloured with dyes of marine or terrestrial origin and whether such artefacts are dyed with genuine "Tyrian Purple" or with dihalogenoindigo substitutes that do not contain bromine. The value of even low resolution electron impact mass spectrometry in a forensic context as a means of identifying authentic 6,6'-dibromoindigo and distinguishing it from its dihalogenoanalogues is emphasised     

液相色谱-串联质谱法快速测定猪肝脏中恩拉霉素残留量

建立了快速测定猪肝脏中恩拉霉素残留量的液相色谱-串联质谱(LC-MS/MS)分析方法。猪肝脏样品用0.1 mol/L盐酸-乙腈(3∶7,体积比)提取2次,离心收集上清液后,加入乙酸乙酯和正己烷液液萃取净化提取液,离心分层后吸取下层提取液经0.1%甲酸稀释定容后进行LC-MS/MS分析。采用Acquity BEH C_(18)柱(100 mm×2.1 mm,1.7μm)进行色谱分离,以0.1%甲酸溶液-甲醇为流动相梯度洗脱;质谱采用电喷雾正离子(ESI~+)模式电离,多反应监测(MRM)模式采集数据,基质校准外标法定量。恩拉霉素A和恩拉霉素B基质标准溶液在2.0～500μg/L质量浓度范围内与定量离子对峰面积呈良好的线性关系,方法检出限分别为3.0、4.0μg/kg,定量下限分别为10、12μg/kg,空白猪肝脏的加标回收率为80.8%～90.3%,批内相对标准偏差(RSD)为0.90%～4.5%,批间RSD为3.0%～4.3%。与已建立的方法比较,该方法简单快速,准确度和精密度均较好,能满足动物组织中恩拉霉素残留量分析的需要。     

POLYMER-SUPPORTED LEWIS ACID CATALYSTS. Ⅵ. POLYSTYRENE-BONDED STANNIC CHLORIDE CATALYST

A polystyrene-bonded stannic chloride catalyst was synthesized by the method of lithium polystyryl combined with stannic chloride. This catalyst is a polymeric organometallic compound containing 0.25 mmol Sn (Ⅳ)/g catalyst. The catalyst showed sufficient stability and catalytic activity in organic reaction such as esterification, acetalation and ketal formation, and it could be reused many times without losing its catalytic activity.     

Preparation of a Star Network PEG-based Gel Polymer Electrolyte and Its Application to Electrochromic Devices

A star network polymer with a pentaerythritol core linking four PEG-block polymeric arms was synthesized, and its corresponding gel polymer electrolyte based on lithium perchlorate and plasticizers EC/PC with the character being colorless and highly transparent has been also prepared. The polymer host was characterized and confirmed to be of a star network and an amorphous structure by FTIR, ^1H NMR and XRD studies. The polymer host hold good mechanical properties for pentaerythritol cross-linking. Maximum ionic conductivity of the prepared polymer electrolyte has reached 8.83 × 10 ^-4 S·cm^-1 at room temperature. Thermogravimetry （TG） of the polymer electrolyte showed that the thermal stability was up to at least 150 ℃. The gel polymer electrolyte was further evaluated in electrochromic devices fabricated by transparent PET-ITO and electrochromically active viologen derivative films, and its excellent performance promised the usage of the gel polymer electrolyte as ionic conductor material in electrochrornic devices.     

Particle beam-mass spectrometric analysis of difluorophenyl triazole compounds using normal phase-HPLC

Normal phase liquid chromatography combined with particle beam mass spectrometry has been applied to the analysis of fluconazole, an anti-fungal agent, [2-(2,4-difluorophenyl)-1,3-bis(1H-1,2,4-triazol-1-yl)-propan-2-ol] and a related intermediate, UK-51060 [2-(2,4-difluorophenyl)-1-(1H-1,2,4-triazol-1-yl)-ethan-2-one]. Electron ionisation and chemical ionisation have been investigated in combination with quadrupole ion trap and magnetic sector mass spectrometers and the spectra obtained compared with those for direct probe analysis. A novel method for the introduction of the chemical ionisation reagent gas via the interface is described for particle beam-magnetic sector mass spectrometry. Multi-stage scan routines have been implemented on the ion trap for the selective storage of analyte species and removal of solvent ions. Detection limits for both spectrometers have been determined and are discussed in terms of interface geometry and analyte transport characteristics. Normal phase HPLC on silica provided a good separation of the intermediate from the later eluting fluconazole peak.     

Negative ion photoelectron spectroscopy of solvated electron cluster anions, (H2O) n − and (NH3) n −

The photodetachment spectra of (H₂O) _n ^=2?69/? and (NH₃) _n ^=41?1100/? have been recorded, and vertical detachment energies (VDEs) were obtained from the spectra. For both systems, the cluster anion VDEs increase smoothly with increasing sizes and most species plot linearly withn ^?1/3, extrapolating to a VDE (n=∞) value which is very close to the photoelectric threshold energy for the corresponding condensed phase solvated electron system. The linear extrapolation of this data to the analogous condensed phase property suggests that these cluster anions are gas phase counterparts to solvated electrons, i.e. they are embryonic forms of hydrated and ammoniated electrons which mature with increasing cluster size toward condensed phase solvated electrons.     

沥青热解残炭的燃烧特性

与轻质油品(汽油、柴油等)燃烧特性不同,重质燃料油在燃烧时,首先发生燃料的热分解,分解的产物扩散到气相空间发生着火、燃烧,最后剩下固体残炭,然后残炭再着火、燃烧,由于残炭的燃烧属于异相反应,比燃料气与空气的同相反应慢,导致其燃尽时间明显变长,文献[1]给出了沥青和十二烷单滴的燃烧过程温度变化曲线,从曲线可以看出,残炭的燃烧阶段明显比气体的燃尽时间长,而残炭的质量只为沥青质量的10%～20%[2,3]。虽然残炭含量低,但它在整个燃烧过程中占有十分重要的地位;文献[4]利用热重系统研究了渣油热加工的副产物石油焦的燃烧特性,主要从…     

利用LB技术以寡聚DNA为模板构建CdS纳米结构

利用Langmuir-Blodgett技术制备了十八胺（ODA）／十聚腺嘌呤（oligo-A10)单分子膜，并以其为模板制备了不同形状的Cds纳米结构，结果表明以在低膜压下转移的寡聚DNA单层为模板可诱导生成线形的Cds纳米结构，而以在主膜压下转换的寡聚DNA单层膜板得到的是Cds的球形结构聚集体。     

Synthesis of 4(3H)-Quinazolinone Derivatives and Their in vitro Antitumor Activity

Classical antifolates containing L-glutamic acid moiety in molecule have shortcomings such as drug resistance which is originated from the defective cell transport by mutation, and toxicity to the host which is due to unnecessarily long retention inside normal cells.[1] One strategy to overcome these shortcomings is to design nonclassical lipophilic inhibitors of folate requiring enzymes by deleting or modifying L-glutamic acid component from the folate analogues.