Total Reflection X-Ray Fluorescence Analysis

In Total Reflection X-Ray Fluorescence Analysis (TXRF), the sutface of a solid specimen is exposed to an X-ray beam in grazing geometry. The angle of incidence is kept below the critical angle for total reflection, which is determined by the electron density in the specimen surface layer, and is on the order of mrad. With total reflection, only a few nm of the surface layer are penetrated by the X rays, and the surface is excited to emit characteristic X-ray fluorescence radiation. The energy spectrum recorded by the detector contains quantitative information about the elemental composition and, especially, the trace impurity content of the surface, e.g., semiconductor wafers. TXRF requires a specular surface of the specimen with regard to the primary X-ray light. 

Vol. 140. Total Reflection X-Ray Fluorescence Analysis. By Reinhold Klockenkamper... 

Similar to the analytical procedure for trace analysis in high purity GaAs wafers after matrix separation, discussed previously,52 the volatilization of Ga and As has been performed via their chlorides in a stream of aqua regia vapours (at 210 °C) using nitrogen as the carrier gas for trace/matrix separation.58 The recoveries of Cr, Mn, Fe, Ni, Co, Cu, Zn, Ag, Cd, Ba and Pb determined after a nearly quantitative volatilization of matrix elements (99.8 %) were found to be between 94 and 101 % (except for Ag and Cr with 80 %). The concentrations of impurities measured by ICP-DRC-MS (Elan 6100 DRC, PerkinElmer Sciex) after matrix separation were compared with ICP-SFMS (Element 2, Thermo Fisher Scientific) and total reflection X-ray fluorescence analysis (TXRF Phillips). The limits of detection obtained for trace elements in GaAs were in the low ngg-1 range and below.58... 

The loaded filters were digested with nitric acid under pressure at 160 °C. The quantitative determination of the concentrations of 23 trace elements (As, Ba, Ca, Cd, Cr, Cu, Fe, K, Mn, Mo, Ni, Pb, Rb, S, Sb, Se, Sn, Sr, Ti, V, Y, Zn, and Zr) was performed by total-reflection X-ray fluorescence analysis (TXRF) after addition of an internal Co standard [STOSSEL, 1987 MICHAELIS, 1988]. Further details of the sampling method and the trace analysis were given in [MICHAELIS and PRANGE, 1988]. 

Zimmermann, S., Messerschmidt, J., von Bohlen, A., Sures, B. Determination of platinum, palladium and rhodium in biological samples by electrothermal atomic absorption spectrometry as compared with adsorptive cathodic stripping voltammetry and total-reflection X-ray fluorescence analysis. Anal. Chim. Acta 498, 93-104 (2003)... 

Total reflection X-ray fluorescence analysis Electron microprobe analysis Particle induced X-ray emission Synchrotron radiation induced X-ray emission... 

Modern Techinques in Electroanalysis. Edited by Petr Vanysek Total Reflection X-Ray Fluorescence Analysis. By Reinhold Klockenkamper Spot Test Analysis Clinical, Enviromental, Forensic, and Geochemical Applications, Second Edition. By Ervin Jungreis... 

Figure 6.11 Geometric construction of a total reflection fluorescence spectrometer. The incident angle is less than 0.1° so that the primary X-ray beam is totally reflected from the flat substrate. (Reproduced with permission from R. Klockenkamper, Total-Reflection X-ray Fluorescence Analysis, John Wiley Sons Inc., New York. 1997 John Wiley Sons Inc.)...

Klockenk mper, R. (1997) Total-Reflection X-ray Fluorescence Analysis, John Wiley Sons, New York. 

Ebert M, Mair V, Tessadri R, Hoffmann P, Ortner HM (2000) Total-reflection X-ray fluorescence analysis of geological microsamples. Spectrochim Acta 55 205-212 Eisenberger P, Lengeler (1980) Extended X-ray absorption fine-structure determination of coordination numbers limitations. Phys Rev 22 3551-3562... 

Klockenkamper R (1997) Total-reflection X-ray fluorescence analysis. J. Wiley and Sons, New York Klockenkamper R, von Bohlen A (2001) Total-reflection X-ray fluorescence moving towards nanoanalysis a survey. Spectrochim. ActaB56 2005-2018. 

Streli C, Wobrauschek P, Bauer V, Kregsamer P, Goegl R, Pianetta P, Ryon R, Pahlke S, Fabry L (1997) Total reflection X-ray fluorescence analysis of light elements with synchrotron radiation and special X-ray tubes. Spectrochim Acta 52 861-872... 

Streli C (1997) Total reflection X-ray fluorescence analysis of light elements. Spectrochim Acta 52 281-293... 

Vazquez C, de Funes SF, Casa A, Adelfang P (2000) Application of total reflection X-ray fluorescence to studies of the geographical distribution of arsenic and other toxic trace elements in ground waters of Argentina Pampa plain. J Trace Microprobe Tech 18 73-81 von Czamowski, Denkhaus E, Lemke (1997) Determination of trace element distribution in cancerous and normal human tissues by total reflection X-ray fluorescence analysis. Spectrochim Acta 52 1047-1052... 

In catalytic Pd(0) reactions, this phosphonium salt was treated with a Pd(ll) source, base, and substrates to form an active catalyst for Sonogashira, Suzuki, and Heck coupling chemistry (Eq. 42, Eq. 43, Eq. 44). The reactions used 0.5 mol% of the Pd catalyst, >99.9% of which was recovered based on Pd analysis of the filtrate of a nanofiltration using UV-visible and total reflection X-ray fluorescence analysis. The spectroscopic analyses reportedly could detect as little as 0.05% of the 0.01 mmol of starting Pd catalyst in the leachate. The membrane used in this chemistry was a solvent-resistant nanofiltration membrane consisting of a porous poly(acrylonitrile) layer and a dense surface layer of poly(dimethylsiloxane). This membrane worked through nine cycles in the... 

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