分光光度法测定盐酸环丙沙星

研究了０．１ｍｏｌ·Ｌ－１的硫酸介质中,盐酸环丙沙星与三氯化铁的显色反应。盐酸环丙沙星浓度在３．３×１０－５～７．３×１０－４ｍｏｌ·Ｌ－１（０．０１２～０．２７ｍｇ·Ｌ－１）范围内符合比尔定律,ε＝１．８５×１０３Ｌ·（ｍｏｌ·ｃｍ）－１。测得络合物组成比为１∶１。本方法简便准确,可用于片剂和胶囊中盐酸环丙沙星的测定。     

新试剂BTPAPT的合成及其分析性能

报道新试剂１－（２－苯并噻唑）－３－（４－偶氮苯基）－三氮烯（简称ＢＴＰＡＰＴ）的合成、性能及与镉，汞、银、锌在表面活性剂存在下的显色反应。研究结果表明，该试剂与镉、汞、银、锌的显色反应灵敏，其摩尔吸光系数分别为：１．４０×１０￣５Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）、１．２３×１０￣５Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）、３．６０×１０￣４Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）和１．１０×１０￣４Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）。     

稀土—偶氮胂Ⅲ配合吸附波法测定稀土元素

在ｐＨ值为３的ＮＨ３．Ｈ２Ｏ－ＮＨ４Ｃｌ介质中,镧,铈,镨与偶氮胂Ⅲ（ＡＳＡⅢ）形成配合物,并于－０．７１Ｖ（ｖｓ．ＳＣＥ）处产生灵敏的配合物吸附波峰电流与镧,铈,镨浓度分别为３．６×１０＾－８～１．４×１０＾－６ｍｏｌ／Ｌ,１．８×１０＾－８～８．６×１０＾－７ｍｏｌ／Ｌ,３．５×１０＾－８～７．０×１０＾－７ｍｏｌ／Ｌ范围内呈线性关系,测得镧与偶氮胂Ⅲ的配合比为１：１。稳定常数为４．５×１０＾     

分光光度法测定盐酸环丙沙星

研究了０．１ｍｏｌ·Ｌ＾－１的硫酸介质中，盐酸环丙沙星与三氯化铁的显色反应。盐酸环丙沙星浓度在３．３×１０＾－５￣７．３×１０＾－４ｍｏｌ·Ｌ＾－１（０．０１２￣０．２７ｍｇ·Ｌ＾－１）范围内符合比尔定律，ε＝１．８５×１０＾３Ｌ·（ｍｏｌ·ｃｍ）＾－１。测得络合物组成比为１：１。本方法简便准确，可用于片剂和胶囊中盐酸环丙沙星的测定。     

测定亚硝胺的电位型霉变玉米胚组织传感器研究

利用霉变玉米胚组织研制了对二甲基亚硝胺（ＤＭＮＡ）、二乙基亚硝胺（ＤＥ－ＮＡ）和甲基苄基亚硝胺（ＭＢＮＡ）等选择性响应的新型组织传感器。该传感器灵敏度高,重现性好,选择性好,其线性范围２．０×１０－６～２．０×１０－３ｍｏｌ·Ｌ－１,检测下限１．３×１０－７ｍｏｌ·Ｌ－１,斜率为５９．２（３０°Ｃ,ｐＨ７．５）。     

磷锑钼三元杂多酸光度法测定药品中的抗坏血酸

研究了少量抗坏血酸与磷锑钼三元杂多酸体系的显色特性，建立了借磷锑钼三元杂多蓝测定抗坏血酸的分光光度法。最佳显色条件为［ＰＯ３－４］＝３０×１０－４ｍｏｌ·Ｌ－１，［ＳｂⅢ］＝４５×１０－５ｍｏｌ·Ｌ－１，［ＭｏＯ２－４］＝７５×１０－３ｍｏｌ·Ｌ－１，Ｐ∶Ｓｂ∶Ｍｏ＝１∶０１５∶２５，［Ｈ加入］／［Ｍｏ］＝５７。测定波长为λｍａｘ＝７１０ｎｍ，线性范围为１～５０μｇ·ｍＬ－１，回归方程为Ａ＝３６８０Ｃ－００１４，线性相关系数ｒ＝０９９９８，表现摩尔吸光系数ε７１０＝３６８×１０３Ｌ·ｍｏｌ－１·ｃｍ－１，检出限为０２μｇ·ｍＬ－１，标准回收率为９５％～１００％，变异系数ｃｖ≤０３４％（ｎ＝６）。与二元磷钼杂多酸方法相比，省去了水浴加热的繁琐操作，而且由于锑（Ⅲ）的引入，显色在室温下３５ｍｉｎ便可完成，并可稳定５ｈ。     

新显色剂甲氧基-苯并噻唑重氮氨基偶氮苯与汞的显色反应及应用研究

研究了新显色剂６－甲氧基－苯并噻唑重氮氨基偶氮苯与Ｈｇ（Ⅱ）的显色反应。在非离子表面活性剂存在下的ｐＨ１０．５Ｎａ２Ｂ４Ｏ７～ＮａＯＨ缓冲介质中,Ｈｇ（Ⅱ）与该试剂形成１∶２的稳定络合物,其λｍａｘ＝５２５ｎｍ,ε５２５＝１．６８×１０５Ｌ·ｍｏｌ－１·ｃｍ－１。汞含量在０～８μｇ／１０ｍＬ范围内遵守比尔定律。用于废水中汞的测定,得到满意的结果     

采用乙基紫萃取光度法测定碱中表面活性剂的含量

提出了一种测定重碱,纯碱中阴离子表面活性剂（简称ＡＯＴ）的萃取光度法,乙基紫与ＡＯＴ形成稳定的离子缔合物,可被甲苯萃取。甲苯萃取的最大吸收波长在６１０ｎｍ,其摩尔吸光系数为１．３６×１０＾４Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。     

5－Br－TAR的合成及其在反相HPLC分离测定Co（Ⅱ）、Cr（Ⅵ）、Rh（Ⅲ）中的应用

以合成的新试剂５－Ｂｒ－ＴＡＲ为往前衍生试剂，首次用阴离子表面活性剂Ｓ，Ｄ．Ｓ．为对离子试剂。以含１×１０（－２）ｍｏｌ·Ｌ（－１）的ｐＨ５．８的乙酸－乙酸钠缓冲溶液和３．５×１０（－４）ｍｏｌ·Ｌ（－１）的Ｓ．Ｄ．Ｓ．的甲醇－水（６８：３２，Ｖ／Ｖ）为流动相，在Ｃ（１８）柱上，１５ｍｉｎ内分离测定了Ｃｏ（Ⅱ）、Ｒｈ（Ⅲ）、Ｃｒ（Ⅵ）的５－Ｂｒ－ＴＡＲ配合物。当ＳＮＲ＝２时，检出限分别为０．４９、０．３２、０．４４ｐｐｂ。用于废水及电镀液中Ｃｏ（Ⅱ）、Ｃｒ（Ⅵ）的测定，效果较好。     

苯妥英钠化学传感器的研制

研制了苯妥英钠ＰＶＣ膜化学传感器，该传感器选择性好，稳定性好，其线性范围为１．０×１０＾－１－１．０×１０＾－５ｍｏｌ／Ｌ，检测下限为１．８×１０＾－６ｍｏｌ／Ｌ，为５９．１ｍｖ／ｐｃ（２９８Ｋ，ＰＨ＝４．０－１１．５）。     

Continuous Flow Methylene Blue Active Substances Method for the Determination of Anionic Surfactants in River Water and Biodegradation Test Samples

Anionic surfactants are commonly determined with the use of the methylene blue active substances (MBAS) standard method, which is time‐consuming and labor‐intensive. Therefore, new methods for determination of anionic surfactants are needed. In this study, the standard MBAS method for determination of anionic surfactants was modified and adjusted to work in a continuous flow system combined with spectrophotometric measurement. The developed method was found to be satisfactory in terms of sensitivity and precision, with a short time of analysis. The quantification limit for anionic surfactants was at 16 μg L^?1, with a relative standard deviation of 1.3 % for a model sample and 3.8 % for a river water sample. The results obtained for environmental samples were comparable to those obtained by using the standard MBAS method; however, the developed continuous flow method is faster, more sensitive and consumes smaller doses of chemical reagents.     

水中阴离子表面活性剂测定方法概述

简要介绍了表面活性剂的性质,阴离子表面活性剂的种类及其对水体环境的危害;重点对水中阴离子表面活性剂的测定方法即分光光度法、两相滴定法、高效液相色谱法、薄层层析法及离子选择性电极分析法等进行了综述;提出了水中阴离子表面活性剂测定方法向信息化、实时快速在线监测智能化和检测仪器向微型化的方向发展。     

Determination of sodium sulfate in anionic surfactants by nonaqueous titration

A convenient and easy method was developed for nonaqueous titrimetric determination of sodium sulfate in the presence of sulfonate and sulfate type anionic surfactants. Sodium sulfate and the anionic surfactants were converted to sulfuric acid and the corresponding organo-sulfonic or organo-sulfuric acids by the addition of an excess of perchloric acid. The resulting acid mixture was then titrated in methanol with cyclohexylamine. The sulfate content was calculated from the difference of the two end points of the differentiating titration curve. For the determination of sodium sulfate in typical anionic surfactants, the relative standard deviation varied from 0.7 to 2.0% at the 0.3-10% sodium sulfate levels. The method provides a rapid and precise determination of inorganic sulfates in sulfonated or sulfated materials.     

分光光度法测定水中微量阴离子表面活性剂

在用HCl溶液调节pH=12.0的NaOH溶液中,5-甲基-2-[3-(4-苯基-2-噻唑基)三氮烯基]苯磺酸(MPTTBSA)与氯化十六烷基吡啶(CPC)形成离子缔合物MPTTBSA-CPC。在该溶液中加入阴离子表面活性剂时,能定量置换出离子缔合物中的MPTTBSA,使缔合物在最大吸收波长556 nm处的吸光度下降,阴离子表面活性剂的浓度与溶液的褪色程度呈良好线性关系,从而建立了阴离子表面活性剂光度测定法。实验结果表明,十二烷基磺酸钠(SLS)和十二烷基苯磺酸钠(SDBS)的表观摩尔吸光系数分别为1.24×104 L·mol-1·cm-1和1.07×104 L·mol-1·cm-1,在0～2.5×10-5 mol·L-1范围内服从比尔定律。该方法应用于生活污水中微量阴离子表面活性剂(以SLS计)的测定,结果与亚甲基蓝法测定结果基本一致。     

亚甲蓝分光光度法测定阴离子表面活性剂的改进

亚甲蓝分光光度法（GB7494-87）的操作流程过于繁琐,样品分析耗时耗力,现进行简化改进,旨在建立一种简便、快速的测定水中阴离子表面活性剂的方法。     

EQCN based cholinesterase biosensors

The binding of acetylcholinesterase (AChE) to a propidium-modified piezoelectric quartz crystal and its surface enzymatic activity have been investigated.Propidium binds to a site remote to the active center of AChE - the peripheral anionic site (PAS) - which is located on the rim of the gorge to the active site.The gold electrodes of the quartz crystal were first modified with 11-mercaptoundecanoic acid to which propidium was coupled. AChE binding was monitored by a quartz crystal nanobalance (QCN), followed by amperometric activity evaluation of the AChE loaded on the sensor. Interestingly, the binding is strong but does not inhibit AChE. However, an excess of propidium in solution inhibits the immobilized enzyme. The surface enzymatic activities observed depend on the amount of enzyme and differ according to the type and species, i.e. number of enzyme subunits (Electrophorus electricus tetrameric, Drosophila melanogaster mono- and dimeric form - DmAChE).The operational stability and regeneration, effect of propidium in solution and detection limit for substrate for various AChEs were investigated amperometrically.     

Development of a biosensor for glycated hemoglobin

The development of an electrochemical piezoelectric sensor for the detection of glycated hemoglobin is presented. The total hemoglobin (Hb) content is monitored with a mass-sensitive quartz crystal modified with surfactants, and the glycated fraction of the immobilized Hb is determined by subsequent voltammetric measurement of the coupled ferroceneboronic acid.Different modifications of the sensor were tested for their hemoglobin binding ability. Deoxycholate (DOCA) was found to be the most suitable among the examined modifiers. Piezoelectric quartz crystals with gold electrodes were modified with DOCA by covalent binding to a pre-formatted 4-aminothiophenol monolayer. The properties of the Hb binding to DOCA and the pH effect on this interaction were studied.In the proposed assay for glycated hemoglobin at first an Hb sample is incubated with ferroceneboronic acid (FcBA), which binds to the fructosyl residue of the glycated Hb. Then this preincubated Hb sample is allowed to interact with the DOCA-modified piezoelectric quartz crystal. The binding is monitored by quartz crystal nanobalance (QCN). The amount of FcBA present on the sensor surface is determined by square wave voltammetry. The binding of FcBA results in well-defined peaks with an E⁰′ of +200 mV versus Ag/AgCl (1 M KCl). The peak height depends on the degree of glycated Hb in the sample ranging from 0% to 20% of total Hb. The regeneration of the sensing surface is achieved by pepsin digestion of the deposited Hb. Thus the sensor can be re-used more than 30 times.     

Statistical modeling of adsorption isotherm of potassium on aza[7]helicene-coated gold electrode attached to quartz crystal microbalance

ABSTRACT

A chemically coated piezoelectric sensor has been used for the determination in liquid phase of the adsorption isotherm of potassium. A thin film of aza[7]helicene was attached to the surface of a gold electrode of a quartz crystal microbalance using spin coating method.

Statistical physics formalism was applied to elucidate the adsorption mechanism of potassium onto coated electrode by aza[7]helicene. The simulation results showed that a monolayer adsorption occurs with the number of potassium per site about 1 and the adsorption energy is less than 30 kJ.mol^?1, characteristic of physical adsorption.

The statistical model was used to investigate three thermodynamic potentials such as the entropy, the free enthalpy, and the internal energy. It is found that the adsorption took place with releasing energy, such behavior confirms the exothermic character of the adsorption process.     

环境中阴离子表面活性剂检测方法研究进展

概述了阴离子表面活性剂给水环境带来的危害,深入分析了目前阴离子表面活性剂的主要测定方法以及各优缺点,并对今后检测方法的改进方向进行了介绍,指出联用技术将成为未来水环境中阴离子表面活性剂检测的主要技术。     

Compound surfactant-based emulsion method for the preparation of high-porosity alumina microspheres

Porous alumina microspheres have attracted significant attention owing to their high mechanical strength and excellent chemical and thermal stability. The emulsion method is considered as a simple and controllable method for the preparation of inorganic microspheres. However, preparing alumina microspheres with the emulsion method is challenging because the emulsification of the precursor is inhibited by the rapid hydrolysis of aluminum alkoxide. Herein, we report a new emulsion method for the preparation of high-porosity alumina microspheres using a combination of ionic and non-ionic surfactants; in this method, the compound surfactants act as a template agent to guide aluminum alkoxide to form a lamellar structure through self-assembly. The decomposition of the templating agent and transformation of the alumina crystal at a high temperature result in structural collapse and formation of lamellar pores. Compound surfactants increased the spheroidization rate of the emulsion from 47% to 63% after hydrolysis, whereas the particle size was decreased by almost half. Additionally, the morphology and porosity of the alumina microspheres were changed. With increasing anionic surfactant content, the porosity increased initially and then decreased. The porosity of the alumina microspheres reached a maximum value of 76% at the 1:1 mass ratio of the non-ionic to anionic surfactants. Heat treatment was found to change the size of lamellar pores, with the pore diameter reaching maximum value at 1300 °C. The compound surfactants also increased the compressive stress and specific surface area of the porous alumina microspheres.