Development of Absolute Analysis System by Atomic Emission Spectrometry

本研究的目的是建立一种新的不使用分析标准溶液的多元素分析方法，其中电感耦合等离子体原子发射光谱法（ICP-AES）已被用作分析工具。近年来发展了许多仪器分析方法，ICP-AES是其中的一种方法，具有高灵敏度，同时或快速分析多元素的能力。然而，当用仪器方法测定元素或化合物时，为了使响应信号与分析物浓度相对应，需要标准溶液。也就是说，仪器方法是相对的分析技术。在电化学分析中，有些方法已被确立为“绝对分析技术”，不需要标准溶液。即便如此，它们对实际分析的适用性并不广泛。因此，在本课题中，为了实现ICP-AES的绝对分析，需要进行更多的基础研究。首先，观察元素的发射光谱，并在计算机中存储各元素在特定波长的发射强度作为参考发射强度。然后测量样品溶液中被分析元素的发射强度，然后计算参比物和被分析物发射强度的强度比来估计被分析物的浓度。如果测量系统没有变化，则可以根据上述原理成功地进行绝对分析。然而，在实际应用中，等离子体源、探测器、放大器等都会发生变化，因此需要对测量系统进行一些修正。使用标准光源进行校正是有效的，但是没有这样的标准光源。因此，采用单元素标准溶液（如铁）的单元素标准化方法被开发出来，该方法允许在计算机中对记忆的参考发射强度进行标准化。少

The aim of the present study is to develop a new analytical method for multi-element determination without use of analytical standard solutions, where induct-tively coupled plasma atomic emission spectrometry (ICP-AES) has been used for an analytical tool. Recently many instrumental analytical methods have been developed, and ICP-AES is one of such methods, which has capabilities of high sensitivity, and simultaneous or rapid multielement analysis. However, when the determination of elements or compounds is performed by instrumental methods, the standard solutions are required in order to standardize the responce signals corresponding to the analyte concentrations. That is, the instrumental methods are the relative analysis technique. In electrochemical analysis, some of the methods have been established as "absolute analysis technique", where the standard solutions are not necessary. Even so, their applicability to practical analysis is not wide. Therefore, some fundamental studies ha … More ve been carried out in the present research project to realize the absolute analysis by ICP-AES.First, the emission spectra of the elements were observed, and the emission intensity of each element at specific wavelength was memorized in a computor as the reference emission intensity. Next, the emission intensities of the analyte elements in the sample solution were measured, and then the intensity ratios of the reference and analyte emission intensities were calculated to estimate the analyte concentrations. If there are no variations of the measurement system, the absolute analysis can be successfully performed based on the principle mentioned above. Practically, however, the variations of the plasma source, detectors, amplifiers and so forth occur, and so some correction of the measurement system should be made. The correction with a standard optical source is effective, but such a standard light source is not available. Thus one-element standardization method using the one-element standard solution (e.g., iron) has been developed, which allows to normalize the reference emission intensities memorized in the computor. Less