Lead poisoning is a preventable condition caused by exposure to environmental sources such as lead-containing dust or lead-painted consumer products. The history of lead poisoning prevention has been defined to some extent by the quality of the analytical methods available for lead measurements whether in environmental samples or biological tissues and fluids. The quality of blood lead methods has improved so greatly over the last three decades that we now know far more about the adverse health effects from low-level exposures. Recent evidence suggests that effects such as deficit in IQ occur below the current (periodically revised) U.S. CDC threshold of 10 μg/dL, such that no safe threshold appears to exist for children. Improvements in analytical techniques have also had an impact on the environmental measurement quality, yet many environmental thresholds have remained unchanged for decades. In light of our current understanding of the adverse health effects at low levels of exposure, new thresholds for lead in children’s products have been introduced by the U.S. CPSC. The adequacy of current analytical techniques to detect lead accurately at the new, lower thresholds is questionable. XRF offers the advantage of being rapid and nondestructive compared to techniques such as AAS that require extensive sample preparation. However, the accuracy of handheld XRF determinations of lead in painted toys is generally limited. A brief comparative study on the performance of several analytical techniques for the determination of lead in toys is presented at the end of this paper.

Accurate minor and trace element analysis via micro-XRF can be more difficult to accomplish in single crystal and polycrystalline materials due to diffraction phenomena which obscure elemental peaks and distort the spectral background. A primary-beam filter is commonly used to eliminate diffractive artifacts as well as tube characteristic lines, but this dramatically reduces the sensitivity to lighter elements. One way around this is to collect a spectrum with unfiltered excitation to obtain the low-energy region, i.e., Na, Mg, Al, and Si, and then collect other portions of the spectrum under more optimized conditions. The fundamental parameter method is capable of using multiple spectra to quantify the complete element suite of the sample. By unifying the quantification for several spectra taken under different excitation conditions, the overall results can be improved. We have applied this method to selected cases for geological and metallurgical samples. The combined method gives better results for all elements than the single spectrum quantification as judged by agreement with the values from the supplier.

The National Institute of Standards and Technology (NIST) certifies a variety of standard reference materials (SRM) to address specific aspects of instrument performance for divergent beam diffractometers. This paper describes SRM 640d, the fifth generation of this powder diffraction SRM, which is certified with respect to the lattice parameter. It consists of approximately 7.5 g silicon powder specially prepared to produce strain-free particles in a size range between 1 and 10 μm to eliminate size-broadening effects. It is typically used for calibrating powder diffractometers for the line position and line shape. A NIST built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the silicon powder measured at 22.5 °C. Both type A, statistical, and type B, systematic, errors have been assigned to yield a certified value for the lattice parameter of a=0.543 159±0.000 020 nm.