Flow Injection Chemiluminescence Determination Of Tetracyclines

Abstract

A fast and simple flow injection chemiluminescence method for the determination of trace amounts of tetracyclines is proposed based on the chemiluminescence of the KMnO₄ - TCs redox reaction in acidic medium in the presence of a sensitizer, OP. The response to the concentration of tetracyclines is linear in the range of 1.00 to 1000 μg mL^?1 with a relative standard deviation < 2.3 % for determination of 50.0 μg mL^?1 of each antibiotic (n = 11). The detection limits for tetracycline, oxytetracycline and chlortetracycline are 0.40, 0.52 and 0.60 μg mL^?1, respectively. The recommended method is suitable for automatic and continuous analysis and has been successfully tested for determination of tetracyclines in commercial formulations. The chemiluminescence intensity was found to be remarkably enhanced when in the presence of OP micellar system; possible reasons for this observed micellar induced enhanced chemiluminescence is given.     

聚乙烯醇及磷酸酯气相润滑下氮化硅的磨损特性研究

采用球－三盘磨损试验机在３７０℃，聚乙烯醇及磷酸三甲苯基酯气相润滑下研究了Ｓｉ３Ｎ４与Ｍ５０工具钢对磨时的磨损特性．结果表明：在气相润滑下聚乙烯醇可以有效地降低Ｓｉ３Ｎ４的磨损；在聚乙烯醇中添加少量的三甲苯基磷酸酯可以进一步降低Ｓｉ３Ｎ４的磨损．Ｘ射线光电子能谱分析发现，Ｓｉ３Ｎ４的摩擦表面形成了主要由元素碳、氧和磷组成的固体润滑膜，Ｓｉ３Ｎ４发生了氧化并生成了ＳｉＯ２和—ＳｉＮＯ等化合物，而三甲苯基磷酸酯则在摩擦过程中发生了降解．     

Separation and determination of non-ionic surfactants of the nonylphenol polyglycol ether type by liquid chromatography

A normal-phase method for the separation and determination of non-ionic surfactants of the 4-nonylphenol polyglycol ether (NPEO) type by liquid chromatography is described, based on a LiChrosorb-Diol column and nonpolar linear gradient elution, with spectrophotometric detection at 275 nm. The method was applied to the determination of NPEO oligomers in the technical surfactants Arkopal N-20, N-40, N-60 and N-100 and in aqueous solutions from flotation processes. The relative standard deviations were 2.47–5.62%. The detection limits for nonylphenol polyglycol ether with 2, 4, 6, 8, 10, 13 and 15 ethoxy units were 51, 57, 64, 74, 85, 118 and 132 ng, respectively. The method can also be used for the determination of other alkylphenol polyglycol ethers. Reversed-phase LC with an octadecylsilica column was investigated and can be applied to the identification of the alkyl group present.     

Interactions of Polyglycol Ethers with Anionic Surfactants in Water

In order to determine the thermodynamic properties of the aggregation process between sodiun dodecyl sulfate (SDS) and polyglycol ethers (PEG) with average molar mass 35000, 20000, and 10000, the temperature dependence of polymer-surfactant ?nteraction is used. Surface tension, ionic conductivity, and solubilization methods have been used to quantify the interactions.It was found that the transfer of SDS micelles from aqueous media to aqueous polymer media is more feasible than the reverse. In addition, the hydropholic interaction seems to be important, as opposed to the charge-nonpolar type interaction.     

聚乙二醇-聚醋酸乙烯酯-盐复合膜导电性能的研究

采用PEG/PVAc复合物作为高分子固体电解质的基质材料,PEG/PVAc<1/1(mol)时两者有较好的混溶性并破坏了PEG的结晶。研究了高氯酸盐对PEG/PVAc复合膜导电率的影响,结果是随着盐浓度的增加,导电率增大,在同一盐浓度下电导率依次Y(ClO_4)_3>Nd(ClO_4)_3>LiClO_4>NaClO_4,首次将稀土盐用于高分子固体电解质,得到了较高的室温电导率(10~(-6)s·cm~(-1))。加入添加剂以及提高温度和湿度,均能提高复合膜的导电率。     

环氧树脂／PEG／OMMT杂化体的合成及性能研究

以三乙基苄基氯化铵为催化剂,制备了环氧树脂E-44和聚乙二醇（polyglycol,PEG）的杂化体A;将接枝了马来酸酐的PEG与E-44共混,制备了杂化体B。比较杂化体A和杂化体B的性能及其对E-44的增韧效果。结果表明,杂化体A具有水溶性和较好的表面活性,且对E-44具有优异的增韧效果,加入质量分数40％的杂化体A可使E-44的冲击强度提高203％,适量的有机蒙脱土（organic montmorillonite,OMMT）可有效弥补杂化体A增韧时所引起的剪切强度下降。杂化体B中的PEG与E-44几乎没反应,但PEG会参与其固化反应,从而显著提高E-44的韧性,只是效果不如杂化体A。     

Modeling of the three-phase equilibrium in systems of the type water + nonionic surfactant + alkane

Liquid–liquid equilibria of systems water (A) + C_iE_j surfactant (B) + n-alkane (C) have been modeled by a mass-action law model previously developed and so far successfully applied to a series of binary water + C_iE_j systems and to the ternary system water + C₄E₁ + n-dodecane. These calculations provide the basis for the presented modeling. The aqueous systems give information about the association constants and the χ_AB-parameter of the Flory–Huggins theory and the ternary C₄E₁-system provides universal temperature functions for the χ_AC- and the χ_BC-parameter. The three-phase equilibrium for seven ternary C_iE_j systems (i = 6–12, j = 3–6) has been calculated by fitting one additional parameter for each of both temperature functions to the characteristic “fish-tail” point. The agreement with the experimental data is reasonably well. For systems with very small three-phase areas the results can considerably be improved by individual temperature functions that incorporate the experimental temperature maximum of the “fish” into the parameter fit. Based on the parameters of the system water + C₈E₄ + n-C₈H₁₈ the “fish-shaped” phase diagram of the system water + C₈E₄ + n-C₁₄H₃₀ was predicted reasonably well.     

KMnO4-OP Chemiluminescence system for FIA determination of hydrogen peroxide

A fast and simple KMnO₄-OP chemiluminescence system for flow-injection analysis of hydrogen peroxide is described. When a mixture of sample and OP is injected into acidic KMnO₄, solution in a flow-cell, strong chemiluminescence occurs. The response is linear to the concentration of hydrogen peroxide in the range of 1.0 × 10^–8 to 6.0 × 10^–5 mol/l with 0.1 mol/l permanganate, and the upper limit of linear response could be extended to 6 × 10^–3 mol/l by increasing the permanganate concentration. The relative standard deviation of the method is between 1.6 and 2.3%. The detection limit is 6.0 × 10^–9 mol/l. This method is suitable for automatic and continuous analysis and has been successfully tested for determination of hydrogen peroxide in rain water. The chemiluminescence intensity was found to be remarkably enhanced in the presence of the OP micellar system.     

乳化剂OP对铜的电位溶出峰的增敏作用

本文研究了乳化剂OP对微分电位溶出法测定痕量铜的影响。发现在0.10mol/L HC1-0.10mol/L HNO_3介质中,乳化剂OP能使铜的溶出峰高度增大,增敏作用发生在溶出阶段。应用本法测定了酒中铜含量,铜离子在2.5～25ng/ml范围内,峰高与浓度呈线性关系,方法的相对标准偏差为1.27％～1.43％,标准加料回收率为92％～105％。     

聚乙二醇萃取-水杨基荧光酮光度法测定原油中的铝

采用聚乙二醇-硫酸铵-铝试剂体系萃取分离,以水杨基荧光酮-溴化十六烷基三甲铵为显色体系,建立了测定原油中铝的分光光度法。考察了显色体系的测定条件及萃取分离条件。络合物的最大吸收波长为554nm,表观摩尔吸光系数ε=6.446×10~4L/(mol·cm)。铝含量在0～5μg/(25 mL)范围内符合比尔定律。方法应用于原油中铝的测定,相对标准偏差为2.3％,加标回收率为98.3％～103.9％。