三苯基锡（IV）哌啶氨荒酸酯的合成及结构研究

利用三苯基氯化锡和哌啶氨荒酸钠反应，合成了三苯基锡(IV)哌啶氨荒酸酯。通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征。用X-射线单晶衍射测定了该化合物的晶体结构。结果表明，化合物中锡原子呈五配位畸变三角双锥构型。     

三苯基锡(Ⅳ)哌啶氨荒酸酯的合成及结构研究

利用三苯基氯化锡和哌啶氨荒酸钠反应,合成了三苯基锡(Ⅳ)哌啶氨荒酸酯.通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征.用X-射线单晶衍射测定了该化合物的晶体结构.结果表明,化合物中锡原子呈五配位畸变三角双锥构型.     

氯·氨荒酸基·二苯基锗配合物的合成

以二苯基二氯化锡和氨荒酸盐为原料,合成了13种氯．氨荒酸基．二苯基锗配合物,利用元素分析,IR和1HNMR表征了这些配合物的结构,生物活性测试结果表明,该类化合物对KB和Bel癌细胞具有较好的抑制活性。     

氯代二苯基锗氨荒酸酯的合成及表征

以二苯基二氯化锗和氨荒酸钠为原料,合成了十三种氯代二苯基锗氨荒酸酯Ph2GeCl(S2CNRR'),利用元素分析、IR、1^HNMR、UV和MS表征了这些化合物的结构,确定了氨荒酸基是非均性的双齿形式与锗原子配位。生物活性测试表明,该类化合物对KB和BeL癌细胞具有较好的抑制活性。     

三苯基锗不饱和烃基酸衍生物的合成和性质

随着倍半锗氧类化合物的合成及应用研究的日益广泛 ,含 Ge_ O键的烃基锗衍生物的合成及应用也逐渐引起了人们的关注 .1 984年 ,L ukevics等 [1]合成了具有抗癌活性的介吗川类化合物 ,1 990年Kakimoto等 [2 ] 报道了具有杀菌活性的环状烃基羧酸的合成与应用 .但是三烃基锗的膦酸类衍生物的合成及生物活性研究均未见文献报道 .为了研究该类化合物的生理活性 [3～ 5] ,本文以三苯基氯化锗和炔基 (烯基 )膦酸钠为原料 ,在苯中反应 ,合成了一系列双 - O- (三苯基锗 )炔基 (烯基 )膦酸酯和单 - O-三苯基锗炔基 (烯基 )膦酸 ,部分化合物初步生理…     

二烷基氨荒酸二苯基锗盐的合成及性质研究

The diphenylgermanium bis-dithiocarbamates Ph₂Ge(S₂CR)₂ (I～VIII) have been synthesized by the reaction of Ph₂GeCl₂ with RCS₂Na in CH₂Cl₂ solvent. Their structures were characterized with IR, ¹H NMR, UV spectra and the in vitro antitumour activity are tested. In mentioned germanium complexes (I～VIII) the dithiocarbamatyl groups are monodentate ligands.     

二苄基锡双氨荒酸酯的合成

由二苄基二氯化锡与氨荒酸盐反应，合成了１０个新的二苄基锡双氨荒酯化合物，利用元素分析，ＩＲ和＾１ＮＮＭＲ表征了这些化合物的结构。     

三苯基锗烯或炔基膦酸衍生物的合成

由三苯基氯化猪与烯或炔基膦酸盐反应,合成了８种新的三苯基锗烯基或炔基膦酸衍生物,利用元素分析,ＩＲ和ＨＮＭＲ表征了这些化合物的结构     

苯基锗糠基羧酸衍生物的合成、性质及三苯基呋喃甲酸锗的晶体结构

利用二或三苯基氯化锗与糠基羧酸钠反应,合成了9种苯基锗糠基羧酸衍生物.通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行表征.用x-射线单晶衍射测定了三苯基呋喃甲酸锗的晶体结构.晶体属于单斜晶系,空间群PD21/c,α=].1945(4),b=O.9934(3),c=1.6284(5)nm,β=91.59(5)°,Z=4.在该化合物中,四配位的锗原子呈畸变的四面体构型.     

双(三苯基锗)不饱和烃基膦酸酯的合成

随着倍半氧锗类化合物的合成及应用研究的日益广泛,含Ge-O键的烃基锗衍生物的合成及应用研究也逐渐引起了人们的关注,相继合成了各种类型具有抗癌活性的含Ge-O键的烃基锗类化合物[1～3].但烃基锗膦酸衍生物的合成及应用研究尚未见文献报道.为了探讨该类化合物的结构及生物活性,本文以三苯基氯化锗和烯(炔)基膦酸钠为原料,合成了8种双(三苯基锗)不饱和烃基膦酸酯.……     

Preparation and properties of polyurethane networks based on α,ω-difunctional poly(hexafluoropropylene oxide)

Poly(hexafluoropropylene oxide), poly(HFPO), networks were prepared from functional polymers by end linking via urethane groups. The prepolymers were characterized by NMR spectroscopy and GPC. The networks were characterized by determination of the number of network chains from the shear modulus, and were snown to contain both trifunctional crosslinks and difunctional links. The properties of the networks were investigated by a range of techniques. Compared with fully-fluorinated networks formed via triazine cross-links, investigated previously, the urethane-linked networks were more readily prepared but were poorer elastomers, were less thermally stable, and were less resistant to swelling by common polar solvents. © 1995 John Wiley & Sons, Inc.     

Method extension study to validate applicability of AOAC Official Method 996.14 Assurance polyclonal enzyme immunoassay for detection of Listeria monocytogenes and related Listeria spp. from environmental surfaces: collaborative study

Test portions from 3 environmental surface types, representative of typical surfaces found in a food production facility, were analyzed by the Assurance Listeria Polyclonal Enzyme Immunoassay (EIA) and the U.S. Department of Agriculture/Food Safety and Inspection Service (USDA/FSIS) culture method for Listeria monocytogenes and related Listeria species. In all cases, naturally contaminated environmental test samples were collected from an actual food production facility by sponge or swab. Test samples from concrete surfaces were collected by both swab and sponge; sponge test samples were collected from rubber surfaces, and swabs were used to sample steel surfaces. Test portions from each surface type were simultaneously analyzed by both methods. A total of 23 collaborators, representing government agencies, as well as private industry in both the United States and Canada, participated in the study. During this study, a total of 550 test portions and controls was analyzed and confirmed, of which 207 were positive and 336 were negative by both methods. Six test portions were positive by culture, but negative by the EIA. Three test portions were negative by culture, but positive by the EIA. Two test portions were negative by EIA and by culture, but confirmed positive when EIA enrichment broths were subcultured to selective agars. The data reported here indicate that the Assurance Listeria EIA method and the USDA/FSIS culture method are statistically equivalent for detection of L. monocytogenes and related Listeria species from environmental surfaces taken by sponges or swabs.     

Method extension study to validate applicability of AOAC Official Method 997.03 visual immunoprecipitate assay (VIP) for Listeria monocytogenes and related Listeria spp. from environmental surfaces: collaborative study

Test portions from 3 environmental surface types, representative of typical surfaces found in a food production facility, were analyzed by the Visual Immunoprecipitate assay (VIP) and the U.S. Department of Agriculture/Food Safety and Inspection Service (USDA/FSIS) culture method for Listeria monocytogenes and related Listeria species. In all cases, naturally contaminated environmental test samples were collected from an actual food production facility by sponge or swab. Test samples from concrete surfaces were collected by both swab and sponge; sponge test samples were collected from rubber surfaces, and swabs were used to sample steel surfaces. Test portions from each surface type were simultaneously analyzed by both methods. A total of 27 laboratories, representing government agencies as well as private industry in both the United States and Canada, participated in the study. During this study, a total of 615 test portions and controls was analyzed and confirmed, of which 227 were positive and 378 were negative by both methods. Nine test portions were positive by culture, but negative by the VIP. Five test portions were negative by culture, but positive by the VIP. Four test portions were negative by VIP and by culture, but confirmed positive when VIP enrichment broths were subcultured to selective agars. The data reported here indicate that the VIP method and the USDA/FSIS culture method are statistically equivalent for detection of L. monocytogenes and related Listeria species from environmental surfaces taken by sponges or swabs.     

Synthesis, properties, and applications of urethane-modified acrylated poly(ester-amide)s

Epoxy resin-based unsaturated poly(ester-amide) resins (UPEAs) were treated with acryloyl chloride to afford acrylated UPEAs resins (AUPEAs). Urethane-based acrylated poly(ester-amide)s prepared by reaction with diisocyanate were characterized by elemental analysis, by molecular weight determination (by vapour pressure osmometry), by IR spectral study, and by thermogravimetry. The curing of interacting blends was monitored by differential scanning calorimetry (DSC). On the basis of DSC data in-situ glass-reinforced composites were prepared from the resulting materials and their mechanical, electrical, and chemical properties were characterized. Unreinforced blends were characterized by thermogravimetry.     

系列甘露糖醛酸寡糖的制备与鉴定

用酸降解法制备了系列甘露糖醛酸寡糖(聚合度2～8),并分析测定了寡糖的结构. 褐藻胶经部分酸水解,于pH=2.85处分级获得聚甘露糖醛酸. 继续用酸降解法降解聚甘露糖醛酸,经凝胶柱层析分离纯化,获得系列甘露糖醛酸寡糖. 用荧光标记糖电泳(FACE)对寡糖进行了分析,并用电喷雾离子化质谱(ESI-MS)、 核磁共振波谱(NMR)及红外光谱(FTIR)进行了结构表征. 本研究用酸降解法制备饱和甘露糖醛酸寡糖,用凝胶柱层析法分离获得系列聚合度的寡糖,为褐藻胶大分子构效关系研究和药物的筛选与发现提供了重要的基础资料.     

Kinetics and thermodynamics of the adsorption of some dyestuffs and p-nitrophenol by chitosan and MCM-chitosan from aqueous solution

The effect of initial concentration, temperature, and shaking rate on the adsorption of three dyestuffs [orange II (O-II), crystal violet (CV), and reactive blue 5 (RB5)] and an ideal adsorbate, p-nitrophenol (PNP), by chitosan (Sigma C-3646) and the effect of temperature on the adsorption of O-II and CV by monocarboxymethylated chitosan (MCM-chitosan) were investigated. Kinetic data obtained for the adsorption of each dyestuff and PNP by chitosan and of O-II and CV by MCM-chitosan at different temperatures were applied to the Lagergren equation, and adsorption rate constants (k(ads)) at these temperatures were determined. These rate constants related to the adsorption of O-II and RB5 by chitosan and of O-II by MCM-chitosan were applied to the Arrhenius equation, and activation energies (E(a)) were determined. In addition, the isotherms for adsorption, at different temperatures, of each dyestuff and PNP by chitosan and of O-II and CV by MCM-chitosan were also determined. These isothermal data were applied to linear forms of isotherm equations that they fit, and isotherm constants were calculated. Because the isotherm curves obtained for the adsorption of O-II and CV by chitosan and of CV by MCM-chitosan fit the Langmuir adsorption isotherm, b constants were applied to thermodynamic equations, and thermodynamic parameters (delta G, delta H, and delta S) were calculated. Lastly, chitosan and MCM-chitosan were compared with respect to the ability to take up the dyestuffs and PNP.     

电感耦合等离子体原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷的含量

通过样品处理、干扰实验、方法检出限、准确度和精密度实验,确定了最佳实验条件,建立了电感耦合等离子体-原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷含量的方法。试料经盐酸、硝酸、氢氟酸、高氯酸分解,用盐酸溶解盐类,过滤,采用电感耦合等离子体原子发射光谱法同时测定滤液中铜、锰、铝、钙、镁、钛和磷的含量。方法检出限为锰、钛和磷小于0.00085%,其它元素小于0.0054%,分析结果与分光光度法、X射线荧光光谱法(XRF)和原子吸收光谱法(AAS)分析结果一致,8个实验室对5个水平样品进行协同实验给出了方法的精密度。     

CO2加氢合成二甲醚的催化剂的制备

先采用均匀沉淀法制备出CuO—ZnO催化剂,然后以CuO—ZnO催化剂作为晶核采用水热合成法制备出CuO—ZnO／HZSM-5（氢型ZSM-5分子筛）复合催化剂．利用X射线衍射和氨程序升温脱附手段对复合催化剂进行表征,并应用于CO2催化加氢合成二甲醚的反应．研究结果表明,在相同的反应条件下,这种CuO—ZnO／HZSM-5复合催化剂与采用物理混合法制备出的复合催化剂相比具有更好的催化效果,不但提高了CO2的转化率、二甲醚的选择性以及二甲醚和甲醇的总选择性,同时还改善了催化剂的稳定性．     

Photophysical,Electrochemical, Thermal and Morphological Properties of Polyurethanes Containing Azomethine Bonding

In this paper, three new low band gap Schiff bases were prepared by using 3-etoxy-4-hydroxybenzaldehyde and different o-phylene diamines. Then, these Schiff bases were converted to low band gap polyurethane derivatives, and their photophysical, electrochemical, thermal, mechanical and morphological properties were investigated. Photophysical properties of the compounds were investigated by using UV-Vis and photoluminescence (PL) spectroscopy. Electrochemical properties of Schiff bases and polyurethanes containing azomethine were investigated by using cyclic voltammetry (CV). Thermal decomposition and transitions were determined by using TG-DTA, DMA and DSC techniques, respectively. Morphological properties of the compounds were also determined by using scanning electron microscopy (SEM). SEM images showed that polyurethanes containing azomethine consist of semi-crystalline particles.     

污泥中常规生物指标的检测

介绍了污泥中三种常规生物检测指标,即细菌总数、粪大肠菌群和蛔虫卵的检测方法。污泥中细菌总数的检测采用平皿计数法,先将污泥样品稀释后选取2~3个适宜的稀释度进行培养;污泥中粪大肠菌群的检测采用多管发酵法,分别将稀释后的污泥混悬液接种于乳糖蛋白胨培养基和EC培养液中进行初发酵和复发酵实验;污泥中蛔虫卵的检测采用漂浮法,利用饱和硝酸钠溶液的比重大于蛔虫卵的原理,通过分离、离心、洗涤等步骤将样品中的蛔虫卵集中于载物玻片上镜检计数。文章对污水处理厂检测及排放污泥有一定的指导意义。