SPECTROSCOUT is a portable energy-dispersive XRF analyzer with much of the analytical power of top-grade benchtop analyzers. In addition, energy dispersive X-ray (EDX) spectroscopy can be applied together with SEM to analyze the composition and crystallographic nature of the membrane sample 94. The principle of this. This article describes an investigation to verify the appropriateness of energy dispersive X-ray fluorescence (ED-XRF) spectrometry as an alternative to the methods mentioned above with reference to the United States Pharmacopeia (USP). The instrument used was an EDX-7000 with the Pharmaceuticals Impurities Analysis Method Package (Shimadzu).
Physical Underpinnings
In the quantum mechanical model of the atom, an electron’s energy state is defined by a set of quantum numbers. The primary quantum number, n, provides the coarsest description of the electron’s energy level, and all the sublevels that share the same primary quantum number are sometimes said to comprise an energy “shell.” Instead of describing the lowest-energy shell as the “n = 1 shell,” it is more common in spectroscopy to use alphabetical labels: The K shell has n = 1, the L shell has n = 2, the M shell has n = 3, and so on. Subsequent quantum numbers divide the shells into subshells: one for K, three for L, and five for M. Increasing primary quantum numbers correspond with increasing average distance from the nucleus and increasing energy (Figure (PageIndex{1})). An atom’s core shells are those with lower primary quantum numbers than the highest occupied shell, or valence shell.
Transitions between energy levels follow the law of conservation of energy. Excitation of an electron to a higher energy state requires an input of energy from the surroundings, and relaxation to a lower energy state releases energy to the surroundings. One of the most common and useful ways energy can be transferred into and out of an atom is by electromagnetic radiation. Core shell transitions correspond to radiation in the X-ray portion of the spectrum; however, because the core shells are normally full by definition, these transitions are not usually observed.
Wavelength Dispersive X Ray Spectroscopy
X-ray spectroscopy uses a beam of electrons or high-energy radiation (see instrument variations, below) to excite core electrons to high energy states, creating a low-energy vacancy in the atoms’ electronic structures. This leads to a cascade of electrons from higher energy levels until the atom regains a minimum-energy state. Due to conservation of energy, the electrons emit X-rays as they transition to lower energy states. It is these X-rays that are being measured in X-ray spectroscopy. The energy transitions are named using the letter of the shell where ionization first occurred, a Greek letter denoting the group of lines that transition belongs to, in order of decreasing importance, and a numeric subscript ranking the peak's the intensity within that group. Thus, the most intense peak resulting from ionization in the K shell would be Kα1 (Figure (PageIndex{2})). Since each element has a different nuclear charge, the energies of the core shells and, more importantly, the spacing between them vary from one element to the next. While not every peak in an element’s spectrum is exclusive to that element, there are enough characteristic peaks to be able to determine composition of the sample, given sufficient resolving power.