催化动力学光度法测定痕量锆

研究了在弱酸性介质中，锆（Ⅳ）催化过氧化氢氧化铬蓝黑Ｒ这一新的指示反应及其动力学条件，建立了一种高灵敏、高选择性测定痕量锆的新方法，方法检出限为３．７４×１０－１１ｇ／ｍＬ，线性范围０～１．１μｇ／２５ｍＬＺｒ（Ⅳ）．用于合金钢中痕量锆的测定，结果满意．     

Meso-四(对-磺基苯基)卟啉光度法测定螺旋藻中的痕量锌

在pH=4．5的乙酸-乙酸钠缓冲介质中，锌和meso-四-（对磺基苯基）卟啉生成1：l的黄色配合物，λmax=421nm，ε=4.34×105L·mol-1·cm-1。该法可不经分离直接测定螺旋藻中的锌,结果满意。     

Spectrophotometric determination of boron in complex matrices by isothermal distillation of borate ester into curcumin

In situ distillation of borate ester into the curcumin solution has been developed for the spectrophotometric determination of boron in a variety of complex matrixes. A polypropylene vessel containing the sample solution was placed inside a vessel (PP) containing 10 ml of curcumin solution and the distillation was carried out at room temperature/on a water bath. The borate ester collected in to the curcumin solution was evaporated to dryness on the water bath, taken in acetone and the absorbance was measured at 550 nm. In situ distillation of borate ester directly into the chromogenic reagent eliminates tedious sample treatment (before and/or after borate separation), use of methanol, complicated quartz set up, possible loss of boron and reduces the analysis time significantly. In situ dehydration of sample solution by ethanolic vapour in the absence of dehydrating acid prevents the formation of fluoborate and co-distillation of potential anionic interferents (nitrate and fluoride). This developed method has been applied for the determination of traces of boric acid in boron powder by the distillation of methyl borate at room temperature. For other matrixes (water, uranium oxide, uranyl nitrate, fluoride salt, etc.) distillation of ethyl borate was carried out on the water bath. LOD (3σ) was 5 ng g⁻¹ for water and 30 ng g⁻¹ for solid samples.     

多组分体系同时定性定量测定的逐步回归分析法

阐述了逐步回归分析法用于多组分体系同时定性定量分析的原理、实验及数据处理方法。分析了硝基酚类人工样、未知样及合成样。该法可用于仅知可能含有的组分范围的样品分析。     

Sensitive spectrophotometric kinetic determination of osmium by catalysis of the pyrogallol red-bromate reaction

Osmium(VIII) is determined by means of its catalytic effect on the oxidation of pyrogallol red (PGR) by potassium bromate at pH 6.0, 30°C and 545 nm. The decrease in absorbance of PGR (2.5 × 10^?5 M) in the presence of KBrO₃ (0.20 M) over a period of 0–150 s is proportional to the concentration of osmium(VIII) over the range 0–1400 ng ml^?1. The limit of detection of osmium was 0.65 ng ml^?1. The precision and accuracy of the method are described. The effects of the presence of 45 cations and anions on osmium determination were studied. The effects of probable interferences were completely removed by a single extraction of osmium as osmium tetraoxide into isobutyl methyl ketone and back-extraction into sodium hydroxide solution.     

新显色剂二溴硝基苯基重氮氨基偶氮苯的合成及与镉的显色反应的研究

作者合成了新显色剂2,6-二溴-4-硝基苯基重氮氨基偶氮苯(DBNDAA)。在pH8.5的硼砂-盐酸缓冲介质中,在Tween 80-SDBS存在下,该试剂与镉(Ⅱ)生成络合比为3:1的红色络合物,λ_(max)=500nm,ε_(500)=1.52×10~5L·mol~(-1)·cm~(-1)。镉量在0～28μg/25ml范围内遵守比耳定律。并测定了试剂的表观离解常数和络合物的表观不稳定常数。方法有良好的选择性。用该试剂测定了铝合金标样、环境水样及废水中的痕量镉,结果满意。     

钪—镧—对氟偶氮氯膦体系共显色效应的研究及应用

本文研究了钪－镧－对氟偶氮氯膦体系共显色效应的光度特性及测定钪的最佳条件，建立了光度法测定痕量钪的新方法。该法的表观摩尔吸光系数为８．５７×１０＾４Ｌ·ｍｏｌ＾－１·ｃｍ＾－１，Ｓｃ（Ⅲ）浓度在０．０－５．０μｇ／２５ｍｌ范围符合比尔定律。将本法用于镁基，铁基合成试样中痕量钪的测定，结果满意。     

耐尔蓝-铌钼杂多酸-聚乙烯醇-124体系测定铌

在聚乙烯醇-124存在下,耐尔蓝与铌钼杂多酸形成离子缔合物的适宜条件为:在0.025～0.10mol/L硫酸溶液中形成铌钼杂多酸;在1.1～1.8mol/L硫酸溶液中耐尔蓝与铌钼杂多酸形成离子缔合物。缔合物的组成比为NB:NbMo=3:1,λ_(maX)在615nm处,摩尔吸光系数ε为2.46×10~6L.mol~(-1).cm~(-1),符合比耳定律范围0～1.2μg Nb/25ml,至少稳定5h。考察了43种共存离子的影响,绝大多数元素不干扰测定。方法选择性好,灵敏度高,已用于合金钢和岩矿中铌的测定,结果满意。     

Kinetic Spectrophotometric Determination of Ritodrine Hydrochloride in Dosage Forms

A simple and sensitive kinetic method was developed for the determination of ritodrine hydrochloride in pharmaceutical preparations. The method is based upon a kinetic investigation of the oxidation reaction of the drug with alkaline potassium permenganate at room temperature for a fixed 12.5 min; the absorbance of the colored permenganate ion was measured at 609 nm. The absorbance concentration plots were rectilinear over the range of 1.6–11.2 μg mL^?1 (r = 0.9992) with a minimum detectability of 0.096 μgmL^?1 (2.88 × 10^?7 M). The different experimental parameters affecting the development and stability of color were carefully studied and optimized. The determination of ritodrine hydrochloride by the fixed concentration and rate constant methods is also feasible with the calibration equations obtained, but the fixed time method has been found to be more applicable. The proposed method was applied successfully to the determination of ritodrine hydrochloride in tablets and ampoules with average recoveries of 100.37 ± 0.93% and 100.42 ± 0.87%, respectively. The results obtained were in good agreement with those obtained using a reference method for comparison. A proposal of the reaction pathway is also presented.