オンライン分離前濃縮を用いるタングステン中の微量鉄のフローインジェクション原子吸光分析

Flow injection analysis absorption spectrometry for determination of trace iron in tungsten with on-line separation and preconcentration

Tungsten has a high melting point, low resistance, and excellent chemical resistance, and is used as an industrial material for lamp electrodes (filaments) and electrodes for large-scale integrated circuits. Since trace components in the material have a significant effect on the performance and reliability of the device, it is extremely important to determine the concentration of the components in order to evaluate the material properties. In this study, a separation and preconcentration method using a flow injection (FI) system has been developed for the analysis of trace elements in tungsten by AAS. A cation exchange resin column was used for separation and preconcentration. The spike and recovery tests of trace amounts of iron in tungsten were performed by the proposed FI system, and good recoveries were obtained without interference from the tungsten matrix. The proposed system has a 7-fold higher enrichment factor with a sample volume of 3.7 mL and a detection limit of 9 ppb (equivalent to 3.7 µ g g―1 in a solid sample), which enables highly sensitive analysis. The amount of waste fluid per sample analysis is extremely small (27 mL), and the relative standard deviation of 50 ppb iron solution measured five times repeatedly is 2.7 %, which enables accurate analysis. The system is capable of rapid analysis, taking only 6 minutes per sample, and the amount of liquid waste is less than one-tenth that of conventional method, thus reducing the burden on the environment. In this report, iron was selected as the target analyte, but this system is also expected to be applied to highly sensitive analysis of components that can be adsorbed on cation exchange resin.

Creators ASANO Hitoshi

Creators SHIRAISHI Yukihide