D2EHPA萃取稀土的有机相红外光谱及添加DMHPA的影响

本文研究了部分皂化的二（２－乙基己基）磷酸（Ｄ２ＥＨＰＡ）－正庚烷体系萃取稀土离子Ｙ＾３＋，Ｐｒ＾３＋，Ｎｄ＾３＋，Ｅｕ＾３＋后有机的傅里叶变换红外光谱（ＦＴ－ＩＲ）。发现不同稀土离子与萃取剂的配位能力有差异，并且皂化度对萃取有机相中的Ｐ＝Ｏ谱带的频率和吸收强度皆有影响，在Ｄ２ＥＨＰＡ中加入二（１－甲基庚基）磷酸（ＤＭＨＰＡ）导致Ｐ＝Ｏ谱带形状和吸收强度发生变化。     

DMHPA—RE（Ⅲ）凝胶态萃取有机相的性质及微观结构的研究

本文应用ＩＣＰ／ＡＥＳ，ＦＴＩＲ等手段研究了含稀土（ＲＥ）的ＤＭＨＰＡ（二（１－甲基庚基）磷酸）－Ｃ７Ｈ１６（正庚烷）凝胶态的萃取有机相中的Ｎａ＾＋和ＲＥ＾３＋的含量及凝胶干燥后的溶胀性质。     

TBP对部分皂化的DMHPA—正庚烷体系及萃取稀土有机相的影响

研究了部分皂化的二（１甲基庚基）磷酸（ＤＭＨＰＡ）磷酸三丁酯（ＴＢＰ）—正庚烷（Ｃ７Ｈ１６）体系及萃取稀土有机相的聚集状态。结果表明，ＴＢＰ可以扩大ＤＭＨＰＡＣ７Ｈ１６Ｈ２Ｏ微乳状液形成的区间，并且对萃取有机相的存在状态及水的行为有明显的影响，在一定的条件下有凝胶形成。ＦＴＩＲ光谱分析表明，该类凝胶中ＤＭＨＰＡ和ＴＢＰ与稀土离子以多种形式配位，ＴＢＰ与ＤＭＨＰＡ及水的氢键结合对凝胶网状结构的形成也起了一定的作用。     

二（2-乙基己基）磷酸络合萃取邻氨基苯酚的机理

在二（2-乙基己基）磷酸（D2EHPA）络合萃取邻氨基苯酚（OAP）实验中,研究了稀释剂种类、溶液的初始pH值等因素对OAP稀溶液分配比（D）的影响。溶液的初始pH值对萃取结果影响较大,当初始pH值在pKa1和pKa2之间时,分配比出现峰值;二（2-乙基己基）磷酸主要是通过离子缔合和质子交换来实现萃取的,而稀释剂则主要是物理萃取,在同一浓度下,二（2-乙基己基）磷酸的萃取能力随稀释剂的极性增大而提高,极性环境优于惰性稀释剂环境。红外光谱分析证明萃取过程存在离子交换和离子缔合反应。     

北京同步辐射装置3B1B生物光谱实验站

本文介绍北京同步辐射装置（ＢＳＲＦ）３Ｂ１Ｂ光束线、生物光谱实验站和圆二色谱仪的基本情况。报道北京正负电子对撞机（ＢＥＰＣ）同步辐射专用光期间，我们在站测量了１１种手征性生物和药物样品的圆二色（ＣＤ）谱，首次在国内利用同步辐射光获取了Ｄ－苯丙氨酸等样品的ＣＤ谱和Ｄ－及Ｌ－亮氨酸对称的ＣＤ曲线。     

流动注射在线液-液萃取FAAS法测定地表水中痕量铜

研讨了流动注射在线液－液萃取火焰原子吸收光谱法测定地表水中痕量铜的分析方法。采用ＡＰＤＣ为螯合剂,ＭＩＢＫ在线萃取后注入原子吸收光谱仪测定,其相对标准偏差（ＲＳＤ）为３．５％;检出限（３σ）为９．１１＊１０＾－２μｇ．Ｌ＾－１,加标回收率为９５％－１０３％。     

meso-四(4-磺基苯基)卟啉(TPPS)在微乳液中的行为研究

本文首次研究了ｍｅｓｏ－四（４－磺基苯基）卟啉（ＴＰＰＳ）在Ｏ／Ｗ型微乳液（Ｔｒｉｔｏｎ Ｘ－１００－壬烷－正戊醇－水）体系中的电子吸收光谱变化，计算了ＴＰＰＳ的电离常数Ｋａ及二聚常数ＫＤ。     

硅（磷）中心自由基与2─丁烯二酸二乙酯的加合反应机理

用ＥＳＲ方法研究了硅（磷）中心自由基与２－丁烯二酸二乙酯的加合反应机理．具有顺式构型的马来酸二乙酯（ＤＥＭ）与硅（磷）中心自由基反应，生成自由基加合物。ＤＥＭ的聚合反应受到抑制。具有反式构型的富马酸二乙酯（ＤＥＦ）易发生聚合反应，ＤＥＦ与硅（磷）中心自由基的加合反应受到抑制．ＤＥＦ与ＤＥＭ在反应性能上的差异，主要来自ＤＥＦ有较大的空间位阻效应．     

流动注射—溶剂萃取—原子吸收光谱法测定微量锰（Ⅱ）

本文研究了一种新的在线流动注射－溶剂萃取预富集－原子吸收光谱分析方法。它具有原理简单，萃取装置，萃取效率高，易操作等特点，经对地表水，人发和中草药中Ｍｎ（Ⅱ）进行在线ＦＩＡ－ＥＸＴ－ＡＡＳ分析得到比较好的结果。方法检出限为０．０７６μｇ．ｍｌ＾－１，ＲＳＤ１．０２％线性范围０．５－５．０μｇｍ．ｍｌ＾－１回收率９４－１０２％。     

萃取光度法测定高纯氧化钐中的铬

本文研究了正戊醇－高氯酸－Cr(Ⅵ）－二苯碳酰二肼体系的各种萃取条件,建立了萃取光度法测定微量铬的新方法。在高氯酸介质中,正戊醇能定量的萃取富集Cr(Ⅵ）－二苯碳酰二肼络合物。萃取前和萃取后络合物的最大吸收波长不变（543nm）,而试剂空白在此处均无吸收。校准曲线在0－5μg/mL范围内符合比耳定律。利用EDTA掩蔽稀土基体的干扰,用本法制定了高纯稀土氧经物中的铬含量,并作了加标回收实验结果令人满意。     

FTIR法研究络合萃取邻氨基苯酚萃合物的结构

利用红外光谱研究二（2-乙基己基）磷酸和磷酸三丁酯络合萃取邻氨基苯酚在不同情况下的反应机理。结果表明：二（2-乙基己基）磷酸主要与邻氨基苯酚的—NH2发生反应,与邻氨基苯酚的阳离子和中性分子络合。萃取过程存在离子交换和离子缔合两种机制,生成相同结构的萃合物;而磷酸三丁酯主要与邻氨基苯酚的—OH发生反应,与邻氨基苯酚的中性分子发生氢键缔合,生成相同结构的萃合物;两种情况下生成萃合物的结构都与pH无关。     

Study on Dispersion of TiO2 Particles During Polymerization of PET

An important factor influencing the stability of colloidal suspension is zeta potential (ζ-potential) on the surface of particles. In this work, ζ-potential of TiO₂ particles in ethylene glycol (EG) with various additives for poly(ethyleneterephthalate) (PET) polymerization, such as metallic salts, phosphoric acid and alkyl phosphates, were investigated by electrophoretic mobility method. The dispersion stability of TiO₂/EG suspension was influenced by decrease in the absolute value of the ζ-potential by the addition of metal acetates as well as phosphates. The addition of triethylamine (TEA) in the TiO₂/EG suspension restrained the change of ζ-potential from negative to positive, which resulted from phosphoric acid. The molar ratio of phosphoric acid to an acetate was found to have an influence on the dispersion ability of TEA in TiO₂/EG suspension. Effect of metallic salts, phosphoric acid and TEA on the stability of TiO₂/EG suspension was studied in the actual polymerization of PET. It was proved that the addition of TEA is highly effective for the dispersion of TiO₂ particles in PET, even in the presence of metallic salts, phosphoric acid and its alkyl phosphates.     

New Fillers for PBI-Based Composite Electrolytes in Polymer Fuel Cells

Nafion and derived perfluorinated polymers seem to be the most reliable materials in PEMFCs, despite a number of disadvantages, such as low operation conditions (T < 100°C) and high cost. In recent years, new classes of proton conducting membranes have been investigated. PBI membranes showed some advantages: high working temperatures; good chemical resistance; promising durability. Proton carriers are supplied by the presence of phosphoric acid in the membranes. Despite the good conductivity (about 0.1 S/cm at 80°C and RH = 80%) one of the main drawbacks is the leaching of the phosphoric acid under working conditions. In this work two different silica-based fillers, derivatised with phosphoric acid and imidazole-containing units, respectively, were prepared via sol–gel route and characterised from a thermal analyses (TGA-DTA), structural (XRD, IR and solid state NMR) and microstructural (BET) point of view. Impedance spectroscopy scans were carried out on PBI-based membranes filled with derivatised silica up to a content of 30 wt% in order to evaluate the role of the filler in the free phosphoric acid retention capability. The best scores in terms of permanent proton conductivity and acid doping level after leaching were obtained in case of imidazole-functionalised silica, which improves the basicity of the doped polymer system.     

Study on the effect of different acids on the structure and photocatalytic activity of mesoporous titania

Nanocrystalline mesoporous titania was synthesized via a combined sol–gel process with surfactant-assisted templating method using cetyltrimethyl ammonium bromide (CTAB) as the structure-directing agent. The process was catalyzed by different acid (hydrochloric acid, nitric acid, sulfuric acid, or phosphoric acid). The prepared samples were characterized by XRD, TEM, BET and FT-IR. The photocatalytic activity of the samples was determined by degradation of phenol in aqueous solution. Results showed that different acid had different effect on the structure and crystal phase of the samples. The sample adjusted by phosphoric acid showed highest surface area and photocatalytic activity. The formation mechanism of the samples catalyzed by different acid was also discussed.     

Shear Stress and Dielectric Analysis of H3PO4 Doped Polyaniline Based Electrorheological Fluid

We synthesized phosphoric acid (PA) doped polyaniline (PANI) particles (PANI‐PA) and investigated their electrorheological (ER) and dielectric characteristics when they were dispersed in silicone oil. Flow curves of the PANI‐PA based ER fluid under several applied electric field strengths were analyzed using a shear stress model. We also examined ER characteristics based on the relaxation time obtained from the dielectric spectrum.     

Synergistic effect between 4-(2-pyridylazo) resorcin and chloride ion on the corrosion of cold rolled steel in 1.0 M phosphoric acid

The synergistic inhibition between 4-(2-pyridylazo) resorcin (PAR) and chloride ion on the corrosion of cold rolled steel in 1.0 M phosphoric acid was studied using weight loss and potentiodynamic polarization method. Results obtained revealed that single PAR is not an effective inhibitor for steel corrosion in phosphoric acid, but in the presence of chloride ion, PAR may act as a good inhibitor due to the synergism. It is found that the adsorption of PAR accords with the Langmuir adsorption isotherm in the absence and presence of chloride ion. Potentiodynamic polarization studies show that PAR is an anodic inhibitor for steel in 1.0 M phosphoric acid, and with addition of chloride ion PAR acts as a mixed type inhibitor. The experimental temperature ranges from 30 to 45 °C. The kinetic data such as apparent activation energies and pre-exponential factors at different concentrations of the inhibitor were calculated, and the effect of the apparent activation energies and pre-exponential factors on the corrosion rates of cold rolled steel was discussed. The inhibitive action was satisfactorily explained by using kinetic models.     

Nucleating Efficiency of Organic Phosphates in Polypropylene

Organic phosphates used as nucleating agents can remarkably promote the stiffness and crystallization rate of polypropylene homopolymer and ethylene–propylene copolymer. In this article, the nucleating activity of 2,2′-methylene-bis(4,6-di-tert-butylphenyl) phosphoric acid and its derivatives for isotactic polypropylene (iPP) were investigated with a differential scanning calorimeter (DSC) and polarized light microscope (PLM), and their influence on mechanical properties of polypropylene was also studied. The results showed that the sodium salt (NA7) and the glyceride ester (NA8) of the organic phosphoric acid were of high nucleating efficiency. If 0.4 wt% of NA7 or NA8 was added to PP, the crystallization peak temperature of PP was raised 15°C or 11°C, respectively, the amount of crystallinity was increased by 3 to 6%, and the crystallization rate was enhanced significantly. The nucleating activity is thermally stable when the mixture of iPP and a nucleating agent was melted and crystallized repeatedly in the DSC. The nucleating agents mentioned above could increase the modulus of the polymer by 20 to about 30% and could increase the flexural strength by 10 to about 20%. However, a number of other organic phosphates tested have little nucleating effect.     

(18)O/(16)O and (13)c/(12)c fractionation during the reaction of carbonates with phosphoric Acid: effects of cationic substitution and reaction temperature

Abstract The factors for (18)O/(16)O fractionation between carbonates and CO(2) gas produced by the dissolution of the carbonates in phosphoric acid (sealed vessel method) have been investigated as a function of reaction temperature (20-90°C) and cationic substitution in the solid. Synthetic CaCO(3), Ca(0.75) Mn(0.25) CO(3), MnCO(3), BaCO(3) and SrCO(3) powders, and a natural kutnahorite sample were used as solids. The δ(18)O values of the gaseous CO(2) liberated by the reaction with phosphoric acid decrease with increasing temperature and seem to be a linear function of T(°K)(-2). The slopes are specific for different carbonates. No temperature-depended (13)C/(12)C fractionation seems to exist.