A new setup for fast spatially resolved measurements of elemental trace amounts under total reflection conditions using a new colour X-ray camera is described. Samples prepared on conventional total reflection X-ray fluorescence (TXRF) reflectors were measured at BESSY II synchrotron. A spatial resolution of 50 × 50 µm² was obtained, while the required time for the investigation of a 10 × 10 mm² sample is 30 seconds. The set-up is up to 350 times faster than conventional X-ray fluorescence systems for elemental traces. The major components of the X-ray camera are polycapillary optics and a pn-CCD chip with an active area of 13 × 13 mm². This area is divided into 264 × 264 pixels of 48 × 48 µm². A full X-ray spectrum with a resolution of 152 eV @ 5.9 keV and a chip temperature of 246 K is recorded for each pixel. The chip has a read-out rate of 400 Hz.
A method for the determination of 22 trace impurities in solar grade silicon after dissolution in a mixture of HF and HNO3 and subsequent matrix evaporation is reported. The presented method involves a simple, inexpensive, one-vessel sample preparation apparatus design. The recoveries of B, Na, Mg, Al, P, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Mo, Sb, W, and Tl at 250 µg kg-1 level are in the range of 93 to 108%. After careful selection of monitored isotopes and their respective resolutions, a sector field mass spectrometer has been used to carry out the measurements. Limits of determination down to 120 ng kg-1 have been obtained using a calibration by three-point standard addition. The method was tested on diluted NIST SRM 57b silicon powder as well as on synthetic test samples and also applied successfully on raw solar grade silicon samples in an interlaboratory comparison including NAA.