In the total reflection X-ray fluorescence (TXRF) analysis, a primary X-ray beam with a small glancing angle is totally reflected on the surface of an analytical sample. Such a configuration of the radiation makes it possible to reduce significantly the amount of the scattered X-rays entering the detector. Consequently, the signal/noise ratio was significantly improved and the ultra-trace analysis was realized. 1 Since the total reflection requires an optically flat surface, the analytical targets have been mainly the silicon wafers important as semiconductor materials and the various solid thin films produced in laboratories. On the other hand, TXRF analysis of a liquid sample has been studied using a sample-carrier on which the liquid is dropped and dried. In the earlier studies, quartz plate samplecarriers were utilized, but cleaning before every use was indispensable. Moreover, a quantitative analysis of phosphor and aluminum was difficult. In order to avoid the interference due to the characteristic X-ray from the sample carrier, the alternatives such as germanium and boron nitride have been also studied. [2][3][4][5] However, these materials are too expensive to use in routine analysis. Recently, Wobrauschek and Aiginger 6 used thin foils of Mylar (polyethylene terephthalate) and Kapton (polyimide). Schmitt et al. 7 proposed a Perspex sheet (polymethylmethacrylate) sample-carrier, which is weak in acid corrosion but usable without precleaning. Hoffmann et al. 8 tested the drying methods of a water droplet using a 2 µm thick Mylar foil.The present study was carried out on the assumption that a silicon wafer is used as the sample-carrier, because the commercially available pieces of TXRF apparatus are currently designed for the inspection of silicon wafers. In order to use repeatedly an expensive silicon wafer sample-carrier, a disposable cover of hydrophobic film was examined. The disposable cover is also useful to reduce the influence of the characteristic X-ray of silicon. In the present study, optimum measuring conditions of TXRF have been studied using polyester (polyethylene terephthalate) film. The relative sensitivity factors of analytes to the internal standard element (scandium) yielded a satisfactory result for the analysis of iron and steel samples.
Experimental
EquipmentThe TXRF apparatus used is a TREX610 spectrometer (Technos, Japan). The X-ray source was a rotating tungsten counter-cathode, which was operated at 30 kV-150 mA. The emitted W L β1 rays were monochromatized in an analytical crystal (LiF 200 ). The fluorescent X-rays were detected with a Si(Li) solid-state detector cooled with liquid nitrogen. The effective measuring area of the detector was about 80 mm 2 (φ10 mm). The energy resolution was about 150 eV for the Mn K α spectrum (5.895 keV).
Cover film and fixingPolyester film was selected as the cover of samplecarrier, because it is hydrophobic and the fluorescence of its components does not disturb the TXRF analysis of metallic impurities. Moreover, polyester film has a sufficient...