分子团簇的量子化学研究

采用Hartree-Fock方法、密度泛函(DFT)方法(BLYP、B3LYP)和MP2方法对Se4分子团簇的各种可能构型进行了结构优化和频率分析, 结果表明有5种构型是势能面上的稳定驻点, 同时对上述4种量子化学方法计算结果的差异进行了分析。并对这5种构型的结构稳定性、几何构型、前线分子轨道、Mulliken布局分析和偶极矩进行了分析, 根据分析结果对Se4分子的某些物理和化学性质进行了预测。     

免疫分析法进展

本文首先从试剂分析的观点对免及分析的原理进行了论.述,对抗体作为分析试剂进行了评价并且总结了标记免投分析的三种方式和四个环节;其次,对免疫分析的现状作了综述,并评述了当代免反分析的五个热点:基因工程抗体,生物素一亲合素多重标记体系,时间分辨荧光免疫分析,多组分免疫分析和自动化免疫分析;最后,对免疫分析的发展趋势作了讨论。     

活性炭表面基团的定性和定量分析

利用过硫酸铵对石油焦基活性炭进行了氧化处理, 并使用元素分析、 傅里叶变换红外光谱(FTIR)、 带质谱检测的程序升温脱附(TPD-MS)、 X射线光电子能谱(XPS)和X射线吸收近边结构(XANES)等方法对样品进行了分析和表征, 并对不同表征方法所得结果进行了对比分析. 结果表明, 元素分析所得结果与TPD-MS分析结果较吻合, XPS和XANES分析所得含氧量结果偏小.     

超声提取-超声波辅助固相微萃取色谱法测定蔬菜中的有机氯、菊酯类农药残留量

建立了一种USE-SPME-GC联用测定蔬菜中有机氯和菊酯类农药残留量的新方法,并对分析条件进行优化和探讨,实验表明,萃取液中基体杂质和色素对分析结果干扰较大,我们提出稀释的方法较好的解决这个问题。对实际蔬菜样品进行了测定和分析。     

Fe(Ⅲ)、Co(Ⅱ)、Ni(Ⅱ)、Cu(Ⅱ)和Zn(Ⅱ)含硫Schiff碱配合物的合成

合成了5种含硫Schiff碱,8种相应的金属配合物。并对合成的配体和配合物进行了元素分析,红外光谱分析。对有代表性的化合物还进行了¹HNMR和质谱分析。确定了可能的分子结构式。     

食品中农药残留分析的样品前处理技术进展*

本文综述了近年来食品中农药残留分析的样品前处理技术,重点对超临界流体萃取法在食品农药残留分析中的应用及其联用技术进行了评述;同时对固相微萃取、微波辅助萃取和凝胶渗透色谱法进行了总结。对食物中农药残留分析技术的发展方向进行了讨论。     

近红外光谱快速测定混胺组分含量

研究了用近红外光谱分析混胺组分三乙胺和二甲苯胺含量的方法。对波长范围的选择和基线处理方法进行了研究,用偏最小二乘法线性回归分析建立三乙胺和二甲苯胺的校正模型。将近红外法测定结果与标准方法测定结果进行了比较,对光谱测量的重复性进行了考察,对温度的影响进行了分析。所有分析研究结果表明：在试样恒温的条件下,近红外光谱分析简单、快速、准确。     

毛细管电泳技术在氨基酸分析中的研究进展

对毛细管电泳技术在氨基酸分析中的研究进展进行了综述,分析了直接法和衍生法对氨基酸进行分析的优缺点,详细叙述了毛细管电泳中的紫外、激光诱导荧光、电化学及质谱等检测方法在氨基酸分析中的应用,并重点总结了毛细管电泳在手性氨基酸分离中的应用.     

介电电泳芯片及其在细胞分析中的应用

简要阐述了在交流和直流电压电场中,介电电泳(DEP)芯片进行细胞分离富集的机理.按照驱动电场的差异对DEP芯片进行了分类,分析和比较了DEP芯片微电极的叉指电极、抛物线电极、堡式电极、三维电极等典型结构.特别对近年来DEP芯片在单细胞分析、细胞分离与富集以及临床细胞分析中的应用进展进行了综述,并对其应用前景和发展方向进行了展望.     

过氧化苯甲酰的安全性研究

利用分子结构特性对过氧化苯甲酰的分解原理进行了分析,并通过热分析、撞击感度和爆发点试验对其安全性进行了评价,得到相关的安全数据。     

膨胀型环状类磷酸酯蜜胺盐阻燃剂的合成及阻燃聚丙烯的结构与性能

以双季戊四醇、三季戊四醇、多聚磷酸、五氧化二磷和三聚氰胺为原料,合成了膨胀型环状类磷酸酯蜜胺盐阻燃剂,并与聚丙烯共混制成阻燃聚丙烯.红外分析表明该阻燃剂具有环状结构.通过扫描电镜和X射线衍射对阻燃聚丙烯进行了结构分析和表面纹理的表征.实验结果表明：该阻燃剂阻燃性能良好,但在聚丙烯中的分散性较差;用甲基纤维素对该阻燃剂进行表面化学修饰以后,该阻燃剂在聚丙烯中的分散性及阻燃材料的机械性能得到了明显的改善.     

Synthesis of a novel hybrid synergistic flame retardant and its application in PP/IFR

A novel inorganic-organic hybrid synergistic flame retardant was prepared by sol-gel reaction and characterized by NMR and FT-IR. It showed that the fire resistance of polypropylene/intumescent flame retardant (PP/IFR) composites could be improved with the combination of hybrid synergistic flame retardant. The char morphology and structure of PP composites were characterized by SEM and Raman spectra. The influence of the hybrid flame retardant on the thermal degradation process of PP composites was analyzed by FT-IR and the rheological behavior of the PP composites was also evaluated. The thermal stability of PP composites was characterized by TGA, weight loss difference and integral procedural decomposition temperature (IPDT). It indicated that the hybrid synergistic flame retardant had good synergistic effect with IFR.     

协效阻燃聚丙烯的阻燃性能

本文研究了以聚磷酸铵(APP)为主阻燃剂,次磷酸铝(AHP)和三聚氰胺氰尿酸盐(MCA)为辅阻燃剂的协效阻燃体系对聚丙烯(PP)阻燃性能的影响。 采用垂直燃烧测试、极限氧指数(LOI)测试、热重分析、锥形量热仪测试、扫描电子显微镜分析等技术手段对所制备的阻燃样品进行了阻燃性能分析。 结果表明:单独添加任一质量分数30%阻燃剂,均不能使PP获得良好的阻燃性能;当阻燃剂总质量分数保持在30%,m(APP)：m(AHP)：m(MCA)=4：1：1时获得理想阻燃效果,此时阻燃PP的LOI为33%,垂直燃烧测试达到V-0级,热释放速率峰值(PHRR)从765.7 kW/m²降为122.7 kW/m²。     

聚乙烯用阻燃剂及其复配体系的研究进展

综述了国内外聚乙烯用阻燃剂及其复配体系的研究进展,对无卤阻燃剂作了较为详细的介绍,最后对聚乙烯用阻燃剂今后的发展趋势作了简单的分析。     

Combustion properties and thermal degradation behavior of polylactide with an effective intumescent flame retardant

An intumescent flame retardant spirocyclic pentaerythritol bisphosphorate disphosphoryl melamine (SPDPM) has been synthesized and its structure was characterized by Fourier transformed infrared spectrometry (FTIR), ¹H and ³¹P nuclear magnetic resonances (NMR). A series of polylactide (PLA)-based flame retardant composites containing SPDPM were prepared by melt blending method. The combustion properties of PLA/SPDPM composites were evaluated through UL-94, limiting oxygen index (LOI) tests and microscale combustion calorimetry (MCC) experiments. It is found that SPDPM integrating acid, char and gas sources significantly improved the flame retardancy and anti-dripping performance of PLA. When 25 wt% flame retardant was added, the composites achieved UL-94 V0, and the LOI value was increased to 38. Thermogravimetric analysis (TGA) showed that the weight loss rate of PLA was decreased by introduction of SPDPM. In addition, the thermal degradation process and possible flame retardant mechanism of PLA composites with SPDPM were analyzed by in situ FTIR.     

Effects of melamine polyphosphate and halloysite nanotubes on the flammability and thermal behavior of polyamide 6

Melamine polyphosphate (MPP) and halloysite nanotubes (HNT) were introduced to polyamide 6 (PA6) by melt blending in order to improve the fire resistance. PA6 composite containing 12% flame retardants with good spinnability was obtained. The flammability of PA6 composite was characterized by limiting oxygen index (LOI), UL‐94 vertical burning and cone calorimeter (CONE) tests. The results indicated that the LOI value could reach 24.0 vol.% and UL‐94 rating could achieve V2 level at the presence of 12% flame retardants. CONE data demonstrated that peak heat release rate was significantly reduced from 554 kW/m² of neat PA6 to 368 kW/m² of the sample containing flame retardants. Thermal analysis indicated that the thermal stability and char formation were improved by the presence of flame retardants. The morphology of residue char was characterized by scanning electron microscopy; and it suggested that a network‐structured protective char layer had been formed. The possible synergism between MPP/HNT and their flame retardant mechanism was also analyzed and discussed. Copyright © 2014 John Wiley & Sons, Ltd.     

软质聚氨酯泡沫塑料用无卤阻燃剂的研究

本文以羟基苯氧膦丙烯酸(CEPP)和三聚氰胺(MA)为原料合成了一种含磷、氮无卤阻燃剂(CMA),采用FT-IR表征了阻燃剂的化学结构,并将该阻燃剂用于软质聚氨酯泡沫(FPUF)的阻燃。用扫描电镜(SEM)研究了阻燃剂的加入对FPUF的形态的影响,通过LO I和垂直燃烧(Cal.117A)测试研究了该阻燃剂对FPUF的阻燃效果。结果表明,CMA可以有效提高FPUF的阻燃性:当CMA的添加量为10%时,FPUF即可通过Cal.117A测试,其LO I值也从17.3提高到23.0;随阻燃剂添加量的增加,FPUF的阻燃性能也逐渐提高。TG测试结果表明CMA的加入对FPUF的热稳定性没有多大影响。     

火焰原子吸收法测定储氢镁合金中高含量钠

建立火焰原子吸收分光光度计测定储氢镁合金中高含量钠的方法。样品经盐酸溶解后,采用火焰原子吸收光谱计测定储氢镁合金中的钠。通过调整燃烧器的角度,选择钠的次灵敏吸收谱线降低测量灵敏度,可消除高倍数稀释造成的误差,提高了测量准确度。方法线性范围为0.001 5%~0.60%,检出限为0.001 5%。4个标准镁合金样品钠含量测定结果均在允许范围内,相对标准偏差为2.04%~3.45%(n=8)。该法适用于镁合金中高含量钠的测定。     

火焰原子吸收光谱法测定煤矸石中铜的样品前处理技术改进

采用火焰原子吸收光谱法测定了煤矸石中Cu的含量.研究了实验预处理技术、消解体系的控制选择及仪器条件的优化,建立了相应的原子吸收光谱测定方法.方法的RSD在1%~3%之间,加标回收率达到96.5%~104%.     

Fabrication of diatomite‐based microencapsulated flame retardant and its improved fire safety of unsaturated polyester resin

To achive excellent fire resistance, new microcapsule flame retardants (DMCAD and DMPPD) were prepared using 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide combined with melamine cyanurate or melamine polyphosphate as the shell material and diatomite as the core material. The successful assembly of DMCAD and DMPPD was detailed characterized by Fourier transform infrared (FT‐IR) spectra, X‐ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Meanwhile, the flame retardancy and thermal stability of the unsaturated polyester resin (UPR)/DMCAD and UPR/DMPPD composites were also studied. The addition of DMCAD and DMPPD effectively improves the flame retardance properties of UPR, and the effect of DMPPD was better. The limiting oxygen index (LOI) of UPR/DMPPD‐3 increased by 11.6% when compared with that of UPR, and the sample achieved V‐0 rating. Moreover, the peak heat release rate (pHRR) and the total heat release (THR) rate of UPR/DMPPD‐3 were reduced by 67% and 26%, respectively. Under nitrogen condition and air condition, UPR/DMPPD showed better thermal stability and char‐forming ability from the thermogravimetric (TG) results. Residual char of the UPR composites was systematically analyzed with SEM and XPS. Finally, the flame retardant mechanism of DMPPD was proposed.