痕量苯酚的单扫描极谱法测定

研究了碱性介质中苯酚与对氨基苯磺酸重氮盐所形成偶氮化合物的极谱行为，并建立了痕量苯酚的极谱测定方法。方法用于污水中微量苯酚的测定，结果令人满意。     

导数脉冲极谱法测定高纯银中微量镉

普通极谱法测定高纯银中微量的镉,灵敏度不很高,往往达不到满意的结果。已有资料报导,导数脉冲极谱法测定镉的灵敏度可达1×10~(-8)M。我们使用国产JP-M1型脉冲极谱仪,用导数脉冲极谱法测定了高纯银中微量镉。本方法灵敏度高,准确,操作简单,快速;测定范围在2×10~(-7)     

矿石中痕量铀的脉冲极谱测定

脉冲极谱法是目前极谱分析中灵敏度最高的方法。用脉冲极谱测定微量铀的方法国外已有报道,Milner等在高氯酸-酒石酸体系中测定海水中微量铀,但需将四升海水预先浓缩;Fawceff等在硫酸-抗坏血酸体系中测定金属钚中微量铀,灵敏度为0.18ppm。肖铨盛曾介绍了在示波极谱仪上醋酸缓冲液中铀-铜铁试剂的吸附波,是目前国内测定微量铀的常用方法。我们使用国产JP-Ml型脉冲极谱仪,在抗坏血酸-草酸铵-醋酸铵体系中,可检出0.04ppm的铀。在寻找灵敏度更高的体系时,发现8-羟基喹啉、噻酚甲酰三氟丙酮(TTA)和铜铁试剂一样均能与铀产生灵敏的极谱波,但仍以     

硫氰酸钾—乙酸体系示波极谱法测定罐头食品中微量铜

食品卫生检验工作中微量铜的测定方法有二乙氨基二硫代甲酸钠比色法,原子吸收分光光度法,示波极谱法也有报道。根据极谱催化波的研究理论,CNS-离子可造就极谱催化波,提高测试的灵敏度。笔者在前人研究工作的基础上,结合自己的条件,进行了0.06mol·L~(-1)硫氰酸钾-0.15mol·~(-1)乙酸体系示波极谱法测定食品中微量铜,应用于罐头食品中微量铜的测定,只加一次试剂既可完成测定工作,方法具有简便、快速、准确、灵敏、样品用量少、成本低、稳定性好的优点,适合于大批、单个食品,水中微量铜的测定。     

锆钼蓝杂多酸的极谱行为及其应用

研究了锆钼蓝杂多酸在碱性溶液中的极谱行为 ,提出了测定微量锆的极谱法新体系。在0.04mol/L盐酸及抗坏血酸溶液中 ,锆 (Ⅳ)与钼酸铵反应形成锆钼蓝杂多酸 ,在pH8.5～10.5的NH3-NH4Cl缓冲溶液中 ,于-1.18V产生灵敏的极谱波,导数波高与锆(Ⅳ)的质量浓度在0.005～0.3mg/L范围内呈线性关系。研究了极谱波性质 ,证明其为吸附波 ,方法已用于岩石样品中微量锆的测定。     

极谱络合吸附催化波测定蔬菜中微量锗

用Ｇｅ（Ⅳ）－连苯三酚－０溴酸钠极谱络合吸附催化波测定蔬菜中微量锗，结果令人满意。同时比较了不同消化处理方法对测定结果的影响，并研究了该极谱波的形成机理。     

植酸中无机磷的极谱测定

本文研究了W-Sb-P三元杂多酸的极谱行为,并建立了微量磷的极谱测定方法。该方法有较高的灵敏度,可应用于植酸中无机磷的分析,可以不经分离直接测定。     

PMBP-金属络合物极谱行为研究 Ⅰ.PMBP及锆-PMBP络合物极谱行为研究与应用

本文研究了PMBP及PMBP与锆形成络合物的极谱行为,并建立了微量锆极谱测定方法。该方法灵敏度高,对铪的选择性较好。测定了18个地质标样获得满意的结果。     

催化极谱测定鼠肾中微量镉

生物材料中微量镉的测定方法有吸光光度法、原子吸收光谱法、微分电位溶出法和电感耦合等离子发射光谱法.鼠肾的重量大多数小于0.5g.上述方法测定鼠肾中微量镉,有的方法灵敏度低,重现性差,样品用量大,有些方法灵敏度高,样品用量少,但需价格昂贵的仪器及严格的安装使用条件.根据极谱催化波理论,笔者在前人研究示波极谱法测定人发、尿中微量镉的基础上,结合实验室条件,提出了鼠肾中微量镉的催化极谱测定,获得满意的结果.本法具有快速、灵敏、准确,样品用量少,仪器价格便宜的优点.     

微量铟的示波极谱测定

一、前言 Donoso等对铟-铜铁试剂的交流极谱波曾作过研究,但在其制定的磷酸盐缓冲体系中,铟的测定灵敏度不高,且在单扫描示波极谱仪上波形欠佳,因而不适于微量铟的测定。我们对铟-铜铁试剂络合物在弱酸性介质中的极谱行为进行了较仔细的研究,发现在pH3.8～6.3的醋酸盐缓冲介质中,于峰电位-0.80伏处,均能产生灵敏度很高的极谱波。通过实验,选定了最佳底液为pH5的醋酸-醋酸钠-铜铁试剂。波高与浓度的线性范围为0.005～1微克/毫升。本法测定铟的灵敏度较之目前采用的比色法、原子吸收和极谱法,要高出几倍到几十倍。方法操作简单,重现性好,适于岩石矿物中微量铟的测定。     

离子色谱法测定乙胺类物质中的氯离子

建立了离子色谱法快速测定乙胺类物质中氯离子的方法。通过简单的阀切换,去除大量的乙胺类物质,将氯离子富集在浓缩柱上,从而达到基体消除的目的,然后进行样品测定。在1.0～500.0μg/L浓度范围内,氯离子的线性相关系数为0.9999,相对标准偏差小于1.2%,加标回收率在92.7%～100.3%。方法已成功应用于乙胺类物质中氯离子的测定。     

NOTE: SYNTHESIS OF Cu(II) AND Zn(II) COMPLEXES WITH SCHIFF BASE DERIVATIVES OF 2-ACETYLPYRROLE

Abstract

Bis chelate complexes of Cu(II) and Zn(II) were synthesized with methylamine and ethylamine Schiff base derivatiies of 2-acetylpyrrole. Stable complexes were obtained, with the exception of the Cu(II) ethylamine adduct. which slowly hydrolyzed in air to yield a mixed ligand product containing one ethylamine Schiff base and one 2-acetylpyrrole per metal centre. The instability of the bis Cu(II) ethylamine Schiff base complex with respect to stable Cu(II) methylamine and Zn(1I) ethylamine complexes is discussed.     

二烯丙基乙胺的合成

以乙胺、烯丙基氯和碱为原料合成了二烯丙基乙胺,其结构经1H NMR,FT-IR和元素分析表征。考察了反应物摩尔比、反应温度、反应时间和相转移催化剂用量对收率的影响,采用正交实验设计法对工艺条件进行了优化。较佳的反应条件为:乙胺370 mmol,n(乙胺)∶n(烯丙基氯)∶n(NaOH)=1.0∶2.1∶2.1,PEG-6005 mol%,第一段于42℃反应6 h;第二段于60℃反应7 h,收率71.58%。回用分液所得水相和减压蒸馏所得低沸点馏分,能回收存在于水相和低沸点馏分中的中间产物和产物,收率由71.58%提高到83.66%。     

硅沸石完美骨架上的吸附1: 乙胺/FAU型沸石相互 作用

采用核磁、红外、XRD研究了FAU硅沸石与吸附的乙胺之间的相互作用,XRD谱显示乙胺的吸入导致沸石晶胞收缩、对称性改变,立方变四方。^2^9SiMASNMR上,FAU硅沸石的单峰分裂成四重峰,同时骨架的红外吸收峰移向低频。这些结果表明,FAU骨架与吸附的乙胺之间存在着强烈的相互作用。     

Kinetics of reduction of palladium(II) complexes with ethylamine on a dropping-mercury electrode

The reduction kinetics of palladium(II) complexes containing ethylamine is studied on a dropping-mercury electrode in solutions of pH 8–13.5 with different ethylamine concentrations in the presence of sodium perchlorate. An irreversible character of the reduction and a diffusion nature of limiting currents are established. Parameters of electrochemical kinetics and diffusion coefficient for the complexes are determined. At pH 11 and 12, the half-wave potential is independent of the ethylamine concentration in the concentration range 0.01 to 0.1 M. Tetraethylamine complexes of palladium(II) predominate in solution and presumably take part in the slow electrochemical step. Raising ethylamine concentration to 2 M makes E _1/2 more negative, due to specific ethylamine adsorption. Limiting currents of two waves, which occur at pH 8 and overall ethylamine concentration 0.01–0.02 M, are used to calculate two constants. One is the step stability constant for complex Pd(eta) ₄ ²⁺ . The other is the equilibrium constant for deprotonation of a ligand in Pd(eta) ₄ ²⁺ , which occurs at pH 13.1–13.5 and ethylamine concentrations 1 and 2 M.     

用循环拆分法制备手性萘乙胺

研究了1-(1-萘基)乙胺[(RS)-1]和1-(2-萘基)乙胺[(RS)-2]的循环拆分方法。以D-酒石酸为拆分剂,分别拆分(RS)-1和(RS)-2得到了(R)-1-(1-萘基)乙胺(收率31%,98%ee)和(R)-1-(2-萘基)乙胺(收率30%,98%ee),并对母液中的非目标对映异构体成功的进行了消旋化,实现了循环拆分。     

Fast ethylamine gas sensing based on intermolecular charge-transfer complexation

We have investigated the fast ethylamine gas sensing of 2-chloro-3,5-dinitrobenzotrifluoride(CDBF) loaded poly(acrylonitrile) nanofiber based on an intermolecular charge-transfer complexation.Reversible response and recovery were achieved using alternating gas exposure.This system shows a fast ethylamine gas sensing within 0.4 s.     

原位分子印迹法制备的连续棒型模板聚合物的手性识别

使用Ｒ－１－（１－萘基）乙胺为模板分子,α－甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,采用原位分子印迹分子制备了具有手性识别环境的连续棒型模板聚合物。色谱结果表明,这种连续棒型模板聚合物对模板分子Ｒ－１－（１－萘基）乙胺比对它的对映异构体Ｓ－１－（１－萘基）乙胺及其外消旋体具有更长的保留时间,更大的容量因子,展现了一定的手性识别能力。     

Gas chromatographic--mass spectrometric determination of phenylacetic acid in human blood

Phenyl acetic acid, a metabolite of 2-phenyl ethylamine, acts as a neuromodulator in the nigrostriatal dopaminergic pathway stimulating the release of dopamine. The evaluation of phenyl acetic acid concentration in the biological fluid reflects phenyl ethylamine levels thus allowing the assessment of the modulatory role of this endogenous substance. Changes in biological fluids levels of 2-phenylethylamine and/or in its metabolite have been reported in affective disorders, such as depression and schizophrenia. Recently, the occurrence of the "attention deficit hyperactivity syndrome" has been frequently reported in childhood population and involvement of dopaminergic dysfunction in this disease has been suspected. A fast, reliable and reproducible method for the determination of phenyl acetic acid in human blood, is therefore needed in order to have a screening tool for monitoring both healthy childhood population and suspected "attention deficit hyperactivity syndrome" patients. The gas chromatographic-mass spectrometric method here described makes use of a deuterated internal standard in order to overcome problems related to the lack of reproducibility often encountered when a derivatization step is performed.     

气液色谱法研究Ni[(C8H17)O)2PS2]2与脂肪胺加合反应的热力学性质

The equilibium constants of acid-base interaction between Mi(Octyl_dtp)_2 and alkylamine were determined by GLC method at several temperatures. Thermodynamic parameters △H and △S were evaluted as follows:ethylamine: △H=-11.5kJ mol~(-1) △S=-22.7J K~(-1) mol~(-1)diethylamine: △H=-18.1kJ mol~(-1) △S=-42.1J K~(-1) mol~(-1)The variations of logK versus temperature fit following equations:ethylamine: lgK=-1.19+598.9/Tdiethylamine: lgK=-2.20+945.6/T