巧用注射器和Y型管改进铜与浓硫酸反应的实验

对现行教材及文献中铜与浓硫酸反应实验设计的优点和不足进行了分析,并在借鉴已有研究的基础上,秉承绿色化和微型化的实验设计理念,对该实验装置进行优化改进。通过利用一次性注射器和Y型管,使得整个实验过程在封闭系统中进行,实验现象明显的同时减少了药品用量,简化了操作步骤,尾气吸收彻底。     

Multisyringe Flow Injection Analysis for Determination of 1-Naphthylamine in Water Samples

1-Naphthylamine (NPA) is one of the main degradation products of pesticides derived from naphthalene, and a well-known bladder carcinogen in men. The Griess assay is used for NPA determination because of its high sensitivity and selectivity. The azo dye 4-(sulphophenylazo)-1-naphthylamine is formed, which shows a peak maximum at 540 nm. After optimizing multisyringe flow injection analysis (MSFIA) parameters, the analytical characteristics of the method were obtained, with a working linear range of 0.5 to 14 mg L⁻¹, according to the equation A = 0.0738±0.0019 [NPA] + 0.0028 ± 0.0042, r = 0.9997. Values for RSD (%) and E_rel (%) were calculated for the concentration levels of 0.5, 6 and 12 mg L⁻¹; values obtained were 1.1, 0.4 and 0.3% for RSD and 0.8, 0.3 and 0.2% for E_rel, respectively. LD was 0.01 mg L⁻¹ and LQ was 0.04 mg L⁻¹ NPA. The MSFIA procedure for the determination of NPA was applied to different water samples (well water, tap water, seawater, and wastewater from the EDAR-1, Palma de Mallorca water treatment plant), with satisfactory results and a throughput of 90 samples per hour.     

L-Malate Determination in Wines and Fruit Juices by Flow Injection Analysis Adaptation of a Coupled Dehydrogenase/Transferase System

Abstract

A flow injection system for the enzymatic determination of L-malate is described. It is adapted for the analysis of wines and fruit juices by in-line sample dilution. Malate dehydrogenase (MDH) and aspartate aminotransferase (AST) were coimmobilized on controlled pore glass. The NADH generated in the packed bed bienzyme reactor was detected fluorimetrically. Sufficient L-malate conversion could be achieved using the coupled transferase reaction to transform the reaction product oxaloacetate. The linear range of the unmodified flow injection system, 5 – 100 μ M of L-malate, could be increased up to 50 mM by means of zone sampling so that untreated samples could be analyzed directly. From 12 – 20 samples per hour could be analyzed with a standard deviation of less than 2 % depending on variation in the degree of dilution. The activity of the bienzyme reactor decreased less than 4% over an analysis period of 3 weeks with more than 1200 injections.     

光化学反应在流动注射分析中的应用研究 Ⅳ.亚甲基蓝光化学反应体系测定抗坏血酸

基于抗坏血酸光化学还原亚甲基蓝光化学反应,建立了流动注射光化学反应测定抗坏血酸的新方法。方法线性范围为0.12～5.60μg/ml,进样频率为55～60次/h。应用于医用维生素C片剂中抗坏血酸的测定,结果满意。     

气体扩散法测氨中几种流动注射扩展线性范围方式的比较及发酵液中氨态氮的测定

本文以气体扩散法测氨为例，比较了三种流动注射扩展线性范围方法的性能；讨论了影响分析精度的因素。把微升进样在线稀释技术同气体扩散光度法结合，测定了农药发酵液中氨态氮的含量。方法的回收率为９３—１０６％，每小时可分析６０—８０个样。     

Application of Boron as the Chromogenic Agent in Spectrophotometry I. A Novel Fading Spectrophotometric Method for the Determination of Aminomethylbenzoic Acid with Boric Acid

It is the first time that boron has been used as a chromogenic agent to determine aminomethylbenzoic acid (PAMBA) by the fading spectrophotometric method in this paper. The study indicates that at pH 10.00 the absorbance of PAMBA decreases when boric acid (BA) is added to the solution. A simple, rapid, sensitive and reliable novel method based on the product of PAMBA and BA is obtained. The stoichiometric ratio of the product is 1:2. Beer's law is obeyed in the range of PAMBA concentrations of 0.13 ? 38.40 μg/mL at a wavelength of 242 nm (ε₂₄₂ is 8.1 × 10⁴ L/mol/cm). The equation of linear regression is A = ‐0.06635 – 0.02914C (× 10^?5 M), with a linear correlation coefficient of 0.9974. The detection limit is 0.12 μg/mL and RSD 0.11%. The method is successfully applied to the determination of PAMBA in pharmaceutical samples, and average recoveries from pharmaceutical samples and urine samples were between 98.4 ? 102.5%. The other components in these samples do not interfere with the determination by the proposed method.     

Validation of a Rapid Multiresidue Method for the Determination of Pesticide Residues in Vine Leaves. Comparison of the Results According to the Different Conservation Methods

The QuEChERS method was applied to the determination of pesticide residues in vine (Vitis vinifera) leaves by LC-MSMS. The method was validated in-house for 33 pesticides representing 17 different chemical groups, that are most commonly used in grape production. Recoveries for the pesticides tested ranged from 75 to 104%, and repeatability and reproducibility relative standard deviations (RSD_r% and RSD_Rw%) were less than 20%. The method was applied to the analysis of pesticide residues in 17 market brands of vine leaves processed according to three different preservation methods and sampled from the Lebanese market. Dried vine leaves were more contaminated with pesticide residues than those preserved in brine or stuffed vine leaves. The systemic fungicides were the most frequently detected among all the phytosanitary compounds usually applied to grape production. Brine-preserved and stuffed vine leaves contained lower concentrations of the residues but still contained a cocktail of different pesticides.     

Automation of the Batch Method for Reaction Kinetic Studies Using Flow Injection Analysis. Kinetic Study of Hydrolysis Of N4-Acetylsulfanilamide,Acetylsalicylic Acid and Phenyl Phosphate

Abstract

The automation of the discontinuous (batch) method for kinetic stucfies using flow-injection analysis (FIA) is described. Aliquots of the reaction mixture are automatically injected in an appropriate manifold and the kinetic profile of the reaction is obtained as a series of absorbance peaks. Observed reaction rate constants are calculated using the Guggenheim and non-linear fitting approaches. The new method is evaluated in the kinetic study of the acid hydrolysis of N⁴-acetylsulfanilamide by colorimetric monitoring of sulfanilamide, the alkaline hydrolysis of acetylsalicylic acid (aspirin) by colorimetric monitoring of salicylate, and the enzymic hydrolysis of phenyl phosphate with alkaline phosphatase by colorimetric monitoring of phosphate. The automated flow-injection batch method can be used in kinetic studies of reactions with t_1/2 greater than 200 s.     

Critical Evaluation of Protonation Constants. Literature Analysis and Experimental Potentiometric and Calorimetric Data for the Thermodynamics of Phthalate Protonation in Different Ionic Media

The protonation constants of phthalate were determined in aqueous NaCl (0.1 ≤ I ≤ 5,mol⋅L⁻¹) and in aqueous Me₄NCl (0.1 mol⋅L⁻¹ ≤ I ≤ 3,mol⋅L⁻¹) at t = 25,^∘C. Experimental data were employed in conjunction with literature data from studies in different ionic media (Et₄NI: 0 ≤ I ≤ 1,mol⋅L⁻¹; NaClO₄: 0.05 mol⋅L⁻¹ ≤ I ≤ 2,mol⋅L⁻¹)to study the dependence on ionic strength using different models, such as the SIT and Pitzer equations, and an Extended Debye-Hückel type equation. Experimental calorimetric data in NaCl and protonation constants at different temperatures in Et₄NI (5 ≤ t ≤ 45^∘C) and in NaClO₄ (15 ≤ t ≤ 35 ^∘C) were also used to study their dependence on temperature. Recommended equilibrium data are reported together with a short discussion of a prospective protocol for drawing these data.