5-芳亚甲基海因的微波合成和晶体结构

用芳醛、海因为原料在微波辐射下合成了一系列的5-芳亚甲基海因，产物的结构经红外、核磁共振、单晶X射线衍射分析表征．     

5-不饱和取代海因的紫外光谱及其应用

亚苄基海因、对羟基亚苄基海因、吲哚亚甲基海因的最大吸收波长分别在324、370、360nm处,而其相应的饱和取代海因则均无吸收。对羟基亚苄基海因由于酚羟基的存在,pH对其吸收光谱有较大影响。采用紫外分光光度法检测不饱和取代海因具有良好回收率,分别为99%～101%、95%～104%、98%～101%,更适合于加氢过程的在线检测。     

5,5-二苯基-2-硫代海因及其S-取代衍生物的绿色合成

以苯偶酰和硫脲为起始原料,在氢氧化钠水溶液中,合成了5,5-二苯基-2-硫代海因;再以5,5-二苯基-2-硫代海因为起始原料,与氯乙酸钠反应,在水相中合成了S-羧甲基-5,5-二苯基-2-硫代海因,考察了硫脲、氢氧化钠和水用量对合成5,5-二苯基-2-硫代海因产率的影响。考察了5,5-二苯基-2-硫代海因用量对合成S-羧甲基-5,5-二苯基-2-硫代海因产率的影响。确定了较佳工艺路线。产品结构经IR、1H NMR、13C NMR及质谱进行了表征。     

环境友好型消毒抗菌剂——二溴海因

二溴海因是一种高效、广谱、低残留的新型环境友好型消毒抗菌剂.介绍了二溴海因的结构、性质、抗菌机理、生产工艺与应用等.     

芦竹碱法合成DL-色氨酸

以芦竹碱和海因为原料,经缩合、水解合成DL-色氨酸,收率达41.6%。缩合反应的最佳工艺条件为:反应时间5 h、碘甲烷与芦竹碱的摩尔比为1.2∶1、乙醇钠与芦竹碱的摩尔比为0.8∶1、原料芦竹碱与海因的摩尔比为0.9∶1;水解反应的最佳工艺条件为:NaOH浓度为1.5 mol/L、水解时间10 h、吲哚甲基海因的浓度为0.2 mol/L、温度为100℃。     

杯芳烃衍生物和丙烯酰胺作为复合功能单体的分子印迹聚合物对海因类化合物的选择性识别研究

以杯[4]芳烃衍生物+丙烯酰胺作为复合功能单体,将其运用到分子印迹技术中,对海因类化合物R-苄基海因进行选择性识别.研究结果表明,由单一的杯[4]芳烃衍生物或丙烯酰胺作为功能单体的分子印迹聚合物对R-苄基海因的选择性均不高,而由杯[4]芳烃衍生物+丙烯酰胺作为复合功能单体的分子印迹聚合物对模板分子具有较高的特异选择性.     

制备苯甘氨酸和对羟苯甘氨酸反应过程中有关物质的毛细管电泳手性分析

在毛细管电泳仪上对苯海因、对羟苯海因等外消旋体进行了拆分条件的研究。建立制备苯甘氨酸和对羟苯甘氨酸过程中的反应物、中间体和产物的毛细管电泳手性分析方法。使用磷酸氢二钠 柠檬酸、磷酸 三乙醇胺电泳缓冲液 ,磺酰化β 环糊精作为手性识别试剂 ,6种化合物均获得满意的分离度     

(±)-N-叔丁氧羰基-3-乙基-戊氨酸的合成

在最优反应条件[海因2 mmol,n(3-戊酮)∶n(海因)=1.5,乙醇胺为碱,p H 4,于55℃反应6 h]下制得5-(1-乙基亚丙基)海因(4);4用5%Pd/C催化加氢制得5-(3-戊基)海因(5);5先在碱性条件下水解,再通过叔丁氧羰基保护氨基合成了(±)-N-叔丁氧羰基-3-乙基-戊氨酸,总收率43%,其结构经~1H NMR,~(13)C NMR和HR-ESI-MS确证。     

1-苄基-5-烷氧基海因的合成

以苄胺和氯乙酸为原料合成了N-苄基甘氨酸盐酸盐,然后与氰酸钾缩合环化合成了1-苄基海因,再经溴化、烷氧基化反应合成了3种海因衍生物,其中2种未见文献报道.产物经元素分析、IP和1H NMR确证.     

液相色谱-质谱法同时测定甜瓜样品中的噻菌灵、甲基托布津、扑海因

采用液相色谱-质谱法同时测定甜瓜样品中的噻菌灵、甲基托布津和扑海因含量。离子化技术采用大气压电喷雾( )方式,定量测定使用选择离子监测模式。检测离子m／x：202．25、343．28、331．07。检出限：噻菌灵为0．1pg,甲基托布津为10．2pg,扑海因为2．42ng;回收率为81．0％～110％;相对标准偏差为1．5％～16．8％。方法灵敏度高,选择性好,准确度高,用于甜瓜样品中噻菌灵、甲基托布津、扑海因的测定,获得了满意的结果。     

Water-Based Oil Spill Dispersants Based on Rosin Formaldehyde Resins

Water-soluble surfactants based on rosin acids were synthesized from condensed rosin acid-formaldehyde. This was completed by esterification of series of rosin acid formaldehyde resins with poly(ethylene glycol) having different molecular weights to produce series of rosin esters. The structure of the produced resins was determined by infrared and ¹HNMR analysis. The molecular weight of the produced surfactants was determined by gel permeation chromatography (GPC) technique. The surface properties of the prepared surfactants were determined by measuring the surface tension at different temperatures. The surface tension, critical micelle concentration (CMC), and surface activities were determined at different temperatures. Surface parameters such as surface excess concentration (Γmax), the area per molecule at interface (A_min), and the effectiveness of surface tension reduction (πCMC) were determined from the adsorption isotherms of the prepared surfactants. Some thermodynamic data for the adsorption process were calculated and are discussed. The dispersion efficiency of the prepared surfactants as petroleum oil spill dispersants was determined and correlated with the surface activity, concentrations of the prepared surfactants and type of petroleum crude oil.     

光度法快速测定不锈钢中的铬、镍、钼、钛、锰

试样用等体积硝酸和盐酸混合酸溶解,用高氯酸将Cr(Ⅲ)氧化为Cr(Ⅵ),用定量Fe(Ⅱ)将Cr(Ⅵ)定量还原为Cr(Ⅲ),用铬酸"剩余光度法"测定铬,丁二酮肟光度法测定镍,硫氰酸盐光度法测定钼,变色酸(1,8-二羟基萘-3,6-二磺酸)光度法测定钛,高锰酸光度法测定锰。测定结果与标准值基本一致,铬、镍、钼、钛、锰测定结果的相对标准偏差分别为0.2%、0.3%、1.5%、2.0%、2.0%。     

The sorption behavior of C<Emphasis Type="SmallCaps">s</Emphasis><Superscript>+</Superscript> ion on clay minerals and zeolite in radioactive waste management: sorption kinetics and thermodynamics

In this work, Cs⁺ ion sorption on some clays and zeolite were investigated. ¹³⁷Cs was used as a tracer. Activities were measured with a NaI crystal gamma counter. The particle size distribution was determined by a laser sizer. Surface area of the particles were determined by BET (Brunauer, Emmett and Teller method). Structure analysis was made by using X-ray diffraction. The chemical compositions of the solid samples were determined using a ICAP-OE spectrometer. Kinetic and thermodynamic parameters were determined. Due to very high uptake results; clay and zeolite can be proposed as a good sorbents in waste management considerations.     

PHOTOPOLYMERS: SYNTHESIS AND CHARACTERIZATION OF POLY(4-CINNA-MOYLPHENYL METHACRYLATE) WITH GLYCIDYL METHACRYLATE

Copolymers of 4-cinnmoylphenyl methacrylate (CPMA) with glycidyl methacrylate were synthesized in methyl ethyl ketone solution using benzoyl peroxide as initiator at 70 ± 1°C. They were characterized by UV, IR, ¹H-NMR, and ¹³C-NMR spectra. Their compositions were determined by ¹H-NMR technique. The monomer reactivity ratios were determined by the Fineman-Ross and Kelen-Tüdös methods. The molecular weights ([Mbar]_w and [Mbar]_n) of the polymers were determined by GPC technique. Thermogravimetric analysis of the copolymers were carried out in air. The T_g of the polymers were determined by differential scanning calorimetry. The photocrosslinking properties of the homo and copolymers were also discussed.     

碱土金属氧化物和过氧化物的O1s电子结合能测定

通过在谱仪真空中对碱土金属氧化物作原位加热, 使其表面碳酸盐分解, 然后记录其晶格氧的O_(1s)电子结合能. 结果表明测得的MgO, CaO, SrO和BaO 的O_(1s)结合能明显地低于大部分文献报导的数值. 本文测得的碱土金属氧化物的O_(1s)电子结合能与氧原子上的Sanderson电荷分数有合理的相关性. 本文测得的BaO_2的O_(1s)结合能是530.9 eV, 它比文献报导的数值要低.     

醋酸乙烯—二乙烯基苯共聚反应动力学

根据文献查得的Ｑ，ｅ值，计算了醋酸乙烯－二乙烯基二元共聚的竞聚率，预测其共聚的可能性。以甲苯为汽油为致孔剂，采用悬浮聚合方法合成该二元大孔共聚物。红外光谱分析跟踪共聚反应过程中乙酰氧基和苯环相对比例的变化，并测定共聚反应过程中比表面积，孔率和平均孔径的变化。     

OXIDATION OF POLYPROPYLENE HOMOPOLYMER IN THE MOLTEN STATE IN PRESENCE OF AIR

The oxidation of polypropylene (PP) homopolymer in air was performed using dodecanol-1 as an accelerator. The experiments were conducted under atmospheric pressure at 180-220°C. Spectroscopic data indicated the formation of polar groups such as ketones, esters, alcohols, anhydrides etc. as determined by FTIR and ESCA. The scanning electron microscopy (SEM) showed the variations of morphology of the oxidation products. The fusion temperatures were determined by differential scanning calorimetry (DSC). The variations of solubility of PPO as compared with the original PP were investigated in solvents such as MEK, THF, and toluene.

Surface tension and molecular weights were determined by tensiometry and gel premeation chromatography (GPC). The melt flow index (MFI) of different samples were determined.     

电感耦合等离子体原子发射光谱同时测定不锈钢食用器皿铬、镍、镉溶出量

用4％醋酸溶液浸泡取自不锈钢食用器皿钢片样品，在室温条件下浸泡24h，将浸泡液按6：1浓缩．通过优化试验确定实验条件，用电感耦合等离子体发射光谱仪准确测定浸泡液中Cr、Ni、Cd的浓度。实验过程操作简单，多种元素同时测定节约试验时间，精密度试验和回收率试验说明该方法检测结果准确可靠。     

Analytics of CVD Processes in the Deposition of SiC by Methyltrichlorosilane

 Gaseous species of the thermal methyltrichlorosilane decomposition were determined qualitatively and quantitatively by in situ infrared spectroscopy and gas chromatography. Surface species like SiCl _x were detected by reflexion in situ infrared spectroscopy. A CVD mechanism of this decomposition is introduced. The comparison between the layer composition determined by EPMA and determined by gas phase analysis is given.     

用IR和负离子FAB—MS测定EDTA,DTPA及其碱金属盐类结构

用ＩＲ和负离子ＦＡＢ－ＭＳ测定不同ｐＨ值下ＥＤＴＡ，ＤＴＰＡ，及其碱金属盐类，能直接给出它们的结构及其分子量，对于其碱金属盐类的混合物，不经分离，可以直接测定，能同时得到混合物中各组分的相对分子质量。