室温下合成纺锤形貌六方相NaLnF_4(Ln=Nd,Sm,Eu,Gd,Tb)纳米颗粒

室温下合成长250nm,宽100nm的纺锤形貌六方相的NaNdF4。NaEuF4,NaSmF4,NaGdF4和NaTbF4也用同样的方法获得。产物用XRD,TEM,HRTEM,FESEM和PL进行表征。PL光谱显示合成的NaEuF4的激发波长是394nm。NaEuF4有4个特征发射谱带,分别是591,615,650和681nm。     

基于超支化温敏聚合物制备温敏金纳米粒子

通过对不同分子量的超支化聚乙烯亚胺(hyperbranched polyethyleni mine,HPEI)的端基进行部分或完全异丁酰胺(isobutyric amide,IBAm)化,可以制备一系列具有不同低临界溶解温度(Lower Critical SolutionTemperature,LCST)的超支化温敏聚合物HPEI-IBAm。通过离子键或氢键之间的相互作用,所得超支化温敏聚合物可以吸附于柠檬酸钠还原并稳定的14nm的金纳米粒子(AuNP)的表面,从而得到具有温敏性质的金纳米粒子。所得温敏金的LCST都低于其相应的温敏聚合物,其差值在0.8至6℃之间。在pH值为9.18的缓冲溶液中,通过改变所用聚合物的分子量以及异丁酰胺基团的取代度,所得温敏金的LCST可控制在21.7~48.2℃之间。此外,所得温敏金的LCST也是pH值敏感的,通过溶液pH值的改变,所得温敏金的LCST值可以在更宽的范围内调节。增加溶液的碱性,LCST可能变化不大或降低,减小溶液的碱性会使LCST升高,直到消失。在偏酸的条件下,所得金复合物通常发生聚集,变得不稳定。此外,溶液中的盐度对所得温敏金的LCST也有影响,氯化钠和硫酸钠会降低其LCST,尤其是硫酸钠的效果更显著。     

A thermodynamic consistency test for the binary constant-temperature VLE data using numerically optimized binary parameters

A thermodynamic consistency (TC) test for the constant-temperature VLE data was investigated by numerically optimizing the binary parameters of the activity coefficient equations to satisfy the Gibbs–Duhem (GD) equation. It was shown that the one parameter Margules equation can best satisfy the GD equation, even if significant experimental errors are involved. A thermodynamic consistency (TC) criterion was defined using the one parameter Margules equation. The TC criterion showed that, of the 37 alkane–alkane, 18 methanol–water and 44 ethanol–water binaries, 36, 16 and 1 binaries are reliable, respectively. Simple liquid mixtures meet the TC criterion.     

Influence of the anode material on the characteristics of an analytical glow discharge cell

The energy transfer to the discharge gas due to various collision processes in the plasma and the heating of the sample are widely known effects in glow discharge (GD) spectroscopy. Despite of the considerable thermal effects and their serious influence on the performance of GD devices, measurements of the discharge gas and sample temperatures are not common at all. The gas temperature depends on the power absorption of the discharge as well as on the temperature of boundaries (sample and anode). In this work the influence of different anode materials in a Grimm-type source on the voltage–current characteristics, crater shapes and GD spectra is investigated. Anodes made of titanium and copper alloys, graphite, and steel with thermal conductivities covering a wide range of values are used. For a fixed voltage and pressure a decrease of the measured current is observed for bad thermal conductive anodes. Cooling of the sample results in an increase of the measured current. Both observations can be explained by changes of the discharge gas temperature. The temperature of the sample is measured from the back side and compared for different anodes. Further, it is found that the choice of the anode material (i) has no significant influence on the crater shape, (ii) results in slightly different sputtering rates and (iii) strong differences of the GD spectra.     

New simple method of measuring the surface glass transition temperature of polymers

A lap‐shear joint mechanical testing method has been probed to measure the surface glass transition temperature (T) of the thick bulk films of high‐molecular‐weight polymers. As T, the temperature transition “occurrence of autoadhesion–nonoccurrence of autoadhesion” has been proposed. The influence of chain flexibility, of molecular architecture, of polymer morphology, and of chain ends concentration on the T has been investigated. The correlation between the reduction in T with respect to the glass transition temperature of the bulk (T) and the intensity of the intermolecular interaction in the polymer bulk in amorphous polymers has been found. The effect of surface roughness on T has been discussed. © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 2012–2021, 2010     

Sample cleanup-free determination of mycophenolic acid and its glucuronide in serum and plasma using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry

Mycophenolic acid (MPA) is an immunosuppressant drug which powerfully inhibits lymphocyte proliferation. Since the early 1990s it has been used to prevent rejection in organ transplantation. The requirement of therapeutic drug monitoring shown in previous studies raises the necessity of acquiring accurate and sensitive methods to measure MPA and its major metabolite mycophenolic acid glucuronide (MPAG).The authors developed a sample cleanup-free, rapid, and highly specific method for simultaneous measurement of MPA and MPAG in human plasma and serum using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry. MPA- and MPAG-determinations were performed during a 2.0-min run time. Multiple calibration curves for the analysis of MPA and MPAG exhibited consistent linearity and reproducibility in the range of 0.05-100 (r > 0.999) mg L⁻¹ and 4-4000 mg L⁻¹ (r > 0.999), respectively. Limits of Detection were 0.014 mg L⁻¹ for MPA and 1.85 mg L⁻¹ for MPAG. Lower Limits of Quantification were 0.05 mg L⁻¹ for MPA and 2.30 mg L⁻¹ for MPAG. Interassay imprecision was <10% for both substances. Mean recovery was 103.6% (range 78.1-129.7%) for MPA and 111.1% (range 73.0-139.6%) for MPAG. Agreement was good for MPA and MPAG between the presented method and a validated HPLC-MS/MS method. The Passing-Bablok regression line for MPA and MPAG was HPLC-MS/MS = 1.14 UPLC-MS/MS—0.14 [mg L⁻¹], r = 0.96, and HPLC-MS/MS = 0.77 UPLC-MS/MS + 0.50 [mg L⁻¹], r = 0.97, respectively. This sample cleanup-free and robust LC-MS/MS assay facilitates the rapid, accurate and simultaneous determination of MPA and MPAG in human body fluids.     

High Tg nematic thermosets: Synthesis, characterization and thermo-mechanical properties

In this paper the synthesis and characterization of a new family reactive nematic oligomers based on 4-hydroxybenzoic acid (4-HBA) will be presented. We modified the backbone using para- and meta-substituted aromatic monomers such as terephthalic acid (TA), isophthalic acid (IA), hydroquinone (HQ), resorcinol (RS), 4,4′-bisphenol (BP) and 3-hydroxybenzoic acid (3-HBA). All oligomers, with a target M_n of 5000 and 9000 g mol⁻¹, were end-capped with reactive phenylethynyl functionalities and synthesized using standard melt condensation techniques. Curing of the phenylethynyl reactive functionalities proceeds through chain extension and crosslinking, depending upon the temperature and time and can be carried out between 310 and 400 °C. Fully cured nematic thermosets could be obtained with glass-transition temperatures previously not accessible (T_g > 400 °C). The cured polymers exhibit excellent tensile properties, i.e. tensile strength (83 MPa) and elongation at break (9%). This approach allows us to prepare all-aromatic polymers with a combination of useful properties such as ease of processing, high T_g’s, and excellent mechanical properties.     

Random low vinyl styrene-isoprene copolymers

The present work is to the syntheses and characterization of random, low vinyl copolymers containing styrene and isoprene (SIR’s). The content of these SIR’s ranged from 10% styrene/90% isoprene to 60% styrene/40% isoprene, and all were soluble in hexane solvent. The anionic polymerization of these SIR’s was initiated by a catalyst system of various sodium dodecylbenzene sulfonate (SDBS) to n-butyllithium (n-BuLi) ratios. The SDBS allowed for styrene to become randomly incorporated onto the polyisoprene chain without any increase in the 3,4-unit of the isoprene. The glass transition temperature of the resulting polymers could be controlled by the styrene content and microstructure (blocky versus random) in the polymer chain. Kinetic data confirmed that styrene and isoprene have similar reaction kinetics. NMR and ozonolysis confirmed that random, low vinyl SIR’s were indeed being synthesized. The unique features of this system are that it does not metallate the polymers as was seen in the previous publication using the sodium and potassium alkoxides. Molecular weight differences due to SDBS are discussed. Finally, rubber process analyzer (RPA) results were presented for various styrenes content SIR’s.     

色谱法测定催化剂中碳含量操作条件研究

根据燃烧-色谱法的原理建立了催化剂碳含量的测定方法并开发了催化剂高温定碳仪,通过考察燃烧温度、载气流速、桥流等对催化剂碳含量测定的影响,确定了测定催化剂碳含量的最佳操作条件。实验结果表明,在确定的最佳操作条件下,测定的催化剂碳含量与化学法基本相同。     

船用pH计检定装置的研究

研制了船用pH计检定装置。以基准电压集成电路作为电压标准,以单片机为控制中心,组成船用pH计检定核心部分,控制船用pH计检定装置输出标准电位。检定装置的pH值输出范围:0～14.0000 pH;pH示值误差:0.0003 pH;电压输出范围:-1999.99～+1999.99 mV;电压分辨率:0.01 mV;温度补偿范围:0～99.9℃。