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自动分析仪测钴方法研究
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摘要
钴冶炼过程中,对沉钴液中钴含量的测定是指导控制生产不可缺少的环节。为了实现快速、准确、简便地测定钴的目的,我们将分光光度法和流动注射法结合起来,从化学、机械、电路三大学科入手,研制开发了一台针对性很强的智能型钴分析仪。
     智能型钴分析仪工作的化学依据是亚硝基R盐法测钴。用流动注射分析法讨论了显色剂浓度、管道内径、管长、流速和分析频率、注样体积以及管道几何形状对吸光度测定的影响。从实验结果得到,仪器工作的参考条件是:亚硝基R盐溶液0.01%,管道内径为0.5mm,反应管长为100cm,注样体积为150ul,编织反应器。此时,仪器测定钴含量的线性范围可达到:0.05~0.15克/升。
     结合自制仪器的特点,就高含量钴的测定方法进行多方面研究探讨。研究的内容包括计时梯度稀释法,直接分光光度法,差示分光光度法,区带稀释法,在线稀释法。其中,直接分光光度法和在线稀释法可以在不改变仪器的硬件和软件结构的条件下进行高含量钴的测定。直接分光光度法可获得测定高含量钴较广的线性范围:0.5~4.0克/升。在线稀释法则通过减小采样体积至50ul和增设反应混合室,以及提高载流流速来实现高含量样品的自动稀释,得到高含量钴测定的线性范围:0.5~2.0克/升。
The determination of cobalt is very necessary in guiding and controlling the manufacture in the process of extraction. In order to determine the cobalt fast and accurately, an intelligent instrument was developed which needed the knowledge of chemistry, machine and electric circuit. The spectrophotomctric method and the flow injection analysis were combined to develop the instrument.
    The intelligent instrument for cobalt works on the base of the chemical method of nitroso-R-salt. Some experiments were carried out by the method of flow injection analysis and the influence of chromogenic agent's concentration, the inside diameter of pipe, the length of pipe, the flow rate of carrier, the analysis rate, the sampling volume and the shape of pipe on the absorption were discussed. It is found that the best work conditions for the instrument is as following: The chromogenic agent's concentration is 0.01%, the inside diameter of pipe is 0.5mm, the length of pipe is 100cm, the sampling volume is 150ul, the pipe is knotted. Under these optimal conditions, the linear range of 0.05 ~ 0.15 g/ L is obtained.
    The methods of the determination of highly concentrated sample were investigated. The highly concentrated sample can be determined on the instrument without changing the hard ware and the soft ware by the directly spectrophotometric method and the method of on-line dilution. The linear range of the directly spectrophotometric method is 0.5 -4.0g/L. The method of on-line dilution can be taken to determine the highly concentrated sample. It is found that when the sampling volume was reduced to 50ul , the mixer was added and the flow rate was increased, the linear range is between 0.5~2.0g/L.
引文
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