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在单段流动分析中同时进行多次进样以进行滴定和标准加入法。

Simultaneous multiple injection to perform titration and standard addition in mono-segmented flow analysis.

作者信息

Assali M, Raimundo I M, Facchin I

机构信息

Instituto de Química, UNICAMP, CP 6154, Campinas, São Paulo, CEP 13083-970, Brazil.

出版信息

J Autom Methods Manag Chem. 2001;23(3):83-9. doi: 10.1155/S1463924601000104.

Abstract

An automated system to perform titration and standard addition in monosegemented flow analysis by employing the simultaneous multiple injection is described. The system was controlled by aPC-AT-386 microcomputer through a home-made parallel interface, employing a diode array spectrophotometer as detector. Software was written in QuickBasic 4.5 to control the system and for data acquisition. A three-way solenoid valve was used in conjunction with a proportional injector to add the titrant solution or the standard solution to the sample, to carry out titration or standard addition, respectively. Only one standard solution was used in each procedure and different quantities of titrant or standard were added to the sample by controlling the time interval in which the solenoid valve was switched on. Titration and standard addition curves similar to those of the manual methods were obtained in both cases, since the sample dispersion was very low due to the air bubbles of the monosegment. The titration system was evaluated through the determination of Fe(II) with a KMnO4 standard solution in pharmaceutical preparations. The standard addition process was assessed by determining Cr(VI) in natural waters and domestic wastewater using the diphenylcarbazide method. The results obtained in both methodologies did not differ significantly from the reference methods at a 95% confidence level.

摘要

本文描述了一种在单段流动分析中通过同时多次进样进行滴定和标准加入的自动化系统。该系统由一台PC-AT-386微型计算机通过自制的并行接口控制,采用二极管阵列分光光度计作为检测器。软件用QuickBasic 4.5编写,用于控制系统和数据采集。使用一个三通电磁阀与一个比例进样器配合,将滴定剂溶液或标准溶液加入样品中,分别进行滴定或标准加入。每个程序仅使用一种标准溶液,通过控制电磁阀开启的时间间隔,向样品中加入不同量的滴定剂或标准物质。由于单段中的气泡使样品分散非常低,两种情况下均获得了与手动方法相似的滴定曲线和标准加入曲线。通过用高锰酸钾标准溶液测定药物制剂中的Fe(II)对滴定系统进行了评估。采用二苯卡巴肼法测定天然水和生活污水中的Cr(VI)对标准加入过程进行了评估。在95%置信水平下,两种方法获得的结果与参考方法相比无显著差异。

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