Proton-induced x-ray emission analysis of tea leaves

Proton-induced X-ray emission (PIXE) spectroscopy has been used for the determination of the concentration of 12 elements in tea leaves of four different brands. The elements are: Cl, K, Ca, Ti, Mn, Fe, Ni, Cu, Zn, Br, Rb and Sr. The transference ratio of the elements into solution, when tea is leached by percolation is reported. It was found that some elements are totally transferred into solution and some are partially retained by the leaves. The significance of some of the elements found in the samples is discussed.     

Fourier analysis of polymer x-ray diffraction patterns

In analyzing the shapes of diffraction peaks from polymers, it has been mistakenly assumed that it is possible to distinguish between models based on “microstrains” and on paracrystallinity. It is shown that either paracrystallinity or distortions due to dislocations give rise to disorder of the second kind and cannot be distinguished by current diffraction methods. Fourier analysis of shapes of peaks from polymers gives quite satisfactory results, despite comments in the literature to the contrary. The analysis can now be carried out with single peaks; multiple orders are not required.     

Soil analysis by thin-film energy-dispersive x-ray fluorescence

Energy-dispersive x-ray fluorescence is advantageous for trace analysis of soils present as thin films. A target thickness of about 2 mg cm^-2 provides a compromise between optimal sensitivity and minimal absorption effect or optimal accuracy. Sample preparation involves only suspending the finely ground soil in water and drying this suspension on a thin mylar foil glued on a ring that fits into the x.r.f. spectrometer. The “effective sample weight” present in the exciting beam area is computed from the scatter peaks, a method that cancels out target heterogeneity problems. High accuracy is demonstrated for many elements in reference soil and rock materials; a precision around 5% and a detection limit around 10 ppm can be achieved. As an illustration, results for 16 trace elements and preliminary interpretation are given for a series of pedologically important soil samples from Brasil.     

Multivariate data analysis for x-ray fluorescence spectrometry

A multivariate data analysis procedure that uses singular value decomposition and the Ho-Kashyap algorithm is proposed to obtain calibration constants for x-ray fluorescence spectrometry. These calibration constants can be used to obtain results from experimental data by means of a simple dot product calculation. The method was tested on experimental data from the literature. Comparison of results showed that the method performs at least as well or better than the Rasberry-Heinrich method or its modifications. The method can be used to express calibration results obtained with a theoretically based program in such a way that they can be used conveniently in routine applications.     

Grazing incidence x-ray diffraction analysis of zeolite NaA membranes on porous alumina tubes.

Zeolite NaA-type membranes hydrothermally synthesized on porous alumina tubes, for dehydration process, were characterized by grazing incidence 2 theta scan X-ray diffraction analysis (GIXRD). The fine structure of the membrane was studied fractionally for surface layer and for materials embedded in the porous alumina tube. The thickness of the surface layer on the porous alumina tube in the membranes used in this study was approximately 2-3 microm as determined from transmission electron microscopy with focused ion beam thin-layer specimen preparation technique (FIB-TEM). To discuss the effects of the membrane surface morphology on the GIXRD measurements, CaA-type membrane prepared by ion exchange from the NaA-type membrane and surface-damaged NaA-type membrane prepared by water leaching were also studied. For the original NaA-type membrane, 2 theta scan GIXRD patterns could be clearly measured at X-ray incidence angles (alpha) ranging from 0.1 to 2.0 deg in increments of 0.1 deg. The surface layers of the 2 - 3 microm on the porous alumina tube correspond to the alpha values up to ca. 0.2 deg. For the CaA-type and the surface-damaged NaA-type membranes, however, diffraction patterns from the surface layer could not be successfully detected and the others were somewhat broad. For all the three samples, diffraction intensities of both zeolite and alumina increased with depth (X-ray incidence angle, alpha) in the porous alumina tube region. The depth profile analysis of the membranes based on the GIXRD first revealed that amount of zeolite crystal embedded in the porous alumina tube is much larger than that in the surface layer. Thus, the 2 theta scan GIXRD is a useful method to study zeolite crystal growth mechanism around (both inside and outside) the porous alumina support during hydrothermal synthesis and to study water permeation behavior in the dehydration process.     

Using x-ray analogs of elements to be determined in the x-ray fluorescence analysis of liquid samples

To construct calibration characteristics in x-ray fluorescence analysis, it is proposed to use calibration samples that contain compounds of chemical elements whose bright characteristic lines are close in wavelength to the analytical lines of the analytes. This approach is efficient in determining rare and expensive elements. The proposed approach is checked experimentally in the determination of W, Re, Er, and Yb in solutions.     

Multi-element analysis of urine by energy-dispersive x-ray fluorescence spectrometry

For multi-element analysis of human urine, 25-ml samples doped with yttrium as internal standard are evaporated gently and then ashed up to 460°C overnight. The residue is pelletized and analysed by energy-dispersive x-ray fluorescence. Acid addition to facilitate the digestion is not mandatory. Recoveries are nearly quantitative for traces of Fe, Ni, Cu, Zn and Sr, to a lesser extent for lead, but not for arsenic or selenium. The standard deviation per measurement is typically around 6%. The detection limits are such that some 10 elements can be determined simultaneously in normal urine, and possibly more in cases of importance to toxicology or industrial hygiene.     

High-precision energy-dispersive x-ray fluorescence analysis of manganese in ferromanganese

A high-precision x-ray fluorescence method for the determination of manganese in ferromanganese is described. The method involves excitation of the sample with a ¹⁰⁹Cd isotopic source and measurement with a high-resolution Si(Li) detector. To preserve the optimal energy resolution even at high count rates, the system incorporates a pulsed optical feedback preamplifier and a pulse pile-up rejector. The rejected pulses are corrected for by means of an adequate live-time correction circuit. Processing of the spectra is accomplished with the aid of a digital computer. The relative precision of the method is approximately 0.2%.     

Small-angle x-ray analysis of latex particles with core-shell morphology

A small-angle x-ray scattering (SAXS) study of latex particles consisting of a polystyrene (PS) core and a polymethylmethacrylate (PMMA) shell in theq-range 0.037 nm^–1q1.5 nm^–1 (q=(4/) sin (/2); : scattering angle) is reported. The particle size distributions of the latices have been determined by ultracentrifugation and allow a quantitative comparison of the experimental scattering intensities with theoretical models. The data obtained for the PS/PMMA latex are shown to be consistent with the proposed core-shell morphology. Separate studies of the PS-core-latex demonstrate that the amount of surfactant being adsorbed on the surface of the particles can be monitored directly. All results show that SAXS is well-suited to study the structure of latex particles in great detail.     

The application of x-ray diffraction analysis to uranium ceramics : Part II. Quantitatlve analysis of the uranium carbides

Different X-ray diffractometer methods are proposed for the determination of uranium carbides in binary and multicomponent mixtures (direct methods, internal standard and active dilution method). The relative standard deviation was found to be 2%. Limits of detection for UC₂ and UO₂ in UC were about 0.04%. Calculations showed that the UC₂ in the samples used contained 9.00 and 9.28±0.04 wt% of combined carbon, corresponding to UC_1.96±0.01 and UC_2.03±0.01.     

Determination of traces of fluorine or sulfur by x-ray analysis

New X-ray methods have been developed for the determination of as little as 1 μg of fluorine or as little as 0.1 μg of sulfur. Fluorine as fluoride is precipitated as lanthanum fluoride in 75% ethanol-water mixture and determined by measuring the amount of lanthanum present in the precipitate. Sulfur as sulfate is precipitated as barium sulfate from a barium sulfate saturated 50% ethanol-buffer mixture, using selenate as a coprecipitant, and determined by measuring the amount of sulfur present. Sulfur as sulfide is precipitated as cadmium sulfide and determined by measuring the amount of sulfur or cadmium in the precipitate.