Study on flow ratiometry for fully automated high-throughput titration

全自动高通量滴定的流量比率法研究

• 批准号: 17590033
• 负责人: TANAKA Hideji
• 金额: $ 1.34万
• 依托单位: The University of Tokushima
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 2005
• 资助国家: 日本
• 起止时间: 2005 至 2006
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-17590033/
• 关键词: flow titration; flow ratiometry; flow analysis; feedback-based control; titrimetry; high throughput titration

Flow ratiometry, which had been developed by the head investigator in 2000, was applied to titrimetry with high throughput rate. In the developed system, titrant flow rate is linearly increased/decreased in accordance with control signal from a computer, while total (titrant + titrand) flow rate was hold constant. A program was newly written in house for full automation of controlling the system, acquiring analytical signal and analyzing the data. The algorithm was constituted of two operation modes. Feedback-based variable triangular wave control mode was used for locating the equivalence point. Scan direction of the control signal was changed from upward to downward, and vice versa, at an instant of the detection of the equivalence point. Subsequent fixed triangular wave control mode was used for further limiting the scan range just around the equivalence point. Thus, the scan in needless range can be avoided and unprecedented high throughput rate (maximally 34 titrations per minute) was realized. The method was successfully applied to acid-based and chelatometric titrations with photometric or potentlometric detection. However, simultaneous titration of calcium and magnesium ions using both photometric and potentiometric sensors still has a problem to be solved : precision of the analytical results is not so high. The method was also applied to the automatic and rapid determination of the electrolytic dissociation constants of acids and bases at various conditions.

首席研究员于2000年开发的流量比率用于高吞吐量的滴定法。在开发的系统中，根据计算机的控制信号，滴滴流量线性增加/降低，而总（滴定 +滴定）流速保持恒定。一个程序是在内部新编写的，以完全自动控制系统，获取分析信号并分析数据。该算法由两种操作模式组成。基于反馈的可变三角波控制模式用于定位等效点。控制信号的扫描方向从向下更改为向下，反之亦然，在对等点的检测中。随后的固定三角波控制模式用于进一步限制等效点附近的扫描范围。因此，可以避免使用不必要的范围的扫描，并且实现了前所未有的高吞吐量（每分钟最大滴定34个滴定）。该方法成功地应用于具有光度或电量学检测的基于酸和螯合测量值。然而，使用光度法和电位测量传感器同时对钙和镁离子同时滴定仍有一个问题要解决：分析结果的精度不是很高。该方法还应用于在各种条件下的酸和碱基的电解离解常数的自动和快速测定。