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Quantification of Classified Nickel Species in Spent FFC Catalysts | SpringerLink - Helping people is our priority.
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These, too, can become part of a zero trust architecture based around adaptive authentication. However, in practice, employees still need a secure way to log in to mission-critical applications.
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Authorization to download zoom text adaptive ware in trash
The recipe for the glass pellets was as follows: 1 g of sample powder and 8 g of a fluxer made by XRF services srl. The glass pellets were then analyzed in the spectrometer, using a calibration line for each element obtained with standards mixed in various proportions.
The method is checked and validated everyday with mixtures with a known composition of the elements to be analyzed. Nickel, being in very small amounts, needed some extra work: the mixtures used for the calibration were made using very small amounts of nickel, for a better precision.
Total carbon and sulphur were measured with an elemental analyser Icarus G4, Bruker. The red curve in the top graph corresponds to pure zeolite Y, to better appreciate the presence of NiO. In this section, three different methods i. The peaks for bunsenite are clearly marked and still visible even at the lowest concentration. The red pattern in the top graph of Fig. In the bottom graph of Fig.
Rietveld refinements of all the samples containing zeolite Y and NiO were performed using an accurately refined structure for zeolite Y on single phase diffraction data, specifically collected. Structure reported in Polisi et al. Si—O distances were soft-constrained, gradually decreasing the weight of the constrain up to 10 after the initial stages.
Extra-framework species were located into the zeolite porosities inspecting carefully the Fourier difference map of the electronic density and using the starting model, their location and species were determined considering the bond distances and the mutual exclusion rules. Species and their locations were similar to those reported in Polisi et al. The results of the Rietveld refinements of the samples containing zeolite Y and bunsenite can be seen in Table 2 , which shows the main parameters that were refined, with the standard errors provided by the minimization procedure on the last decimal place in brackets.
The magnitude of the standard error on NiO refined parameters obviously increases with the decrease of the amount of NiO in the sample: for instance, the standard error on the cell parameters is on the fifth decimal place for the samples with the highest NiO concentration and goes up to the third decimal place for the less concentrated samples.
The size and strain parameters of NiO were refined only for the sample with the largest concentration, and then used and kept fixed for all the others, because refining the microstructural parameters i.
An example of the actual fit, for an amount of NiO corresponding to 0. Table 3 provides the results of NiO quantification. The results of the quantification are shown in Table 3. Rietveld refinement results for zeolite Y spiked with 0. In the inset, a zoom with two of the NiO peaks clearly visible. For this purpose, a calibration using the peak areas of NiO could be fast and reliable enough. Peak areas have been evaluated using a pseudo-Voigt function.
The area of the main peak on NiO in zeolite Y same samples as in Sect. However, the area in peaks with such a small intensity is quite difficult to evaluate in a reliable way: the limits of the peaks are ill-defined, and it is always an issue to reliably evaluate how wide are the peaks vs background.
Small errors in the fit can result in large errors on the area itself. Even though the peak area is generally considered far more reliable than the peak height, when used for quantification purposes, the situation is different when the peak intensity is very small. The peak height may be, in such ill-conditioned cases, a safer choice.
Peak heights have been evaluated using a pseudo-Voigt function. The first check to be done is to understand how accurate we can be with these regression lines: in order to quantify the error made just because of the limited number of decimals in the calibration, we decided to use the regression lines to quantify the standard samples, i. Table 4 provides the details of this quantification. Figure 4 shows such a comparison.
The blue histogram and the grey line refer to NiO, with the height and the area regression method, respectively. Comparison of the accuracy for the quantification with the regression line method, with peak areas and peak heights.
Rietveld results are shown for comparison. Data are taken from Table 3. The comparison is not fair, because of the very different issues in the quantification for the two methods, but it is still edifying to make.
The data, relative to the Rietveld results, are taken from Table 3. However, the presence of these phases must be detected, in real life, in a complex matrix, such as the one of spent catalysts, containing various crystalline phases, and one or more amorphous ones, resulting in a structured and high intensity background.
The active catalytic phase zeolite Y is still present, even though with broader peaks; it clearly underwent some temperature driven decomposition reaction, as mullite is present in substantial amount. Anatase is usually present in FCC catalyst as an active matrix component and specifically as the active phase of vanadium traps [ 12 , 13 ]. Moreover, the structured background is a sign that the process of thermal decomposition of zeolite Y was almost complete, as an amorphous phase is definitely present.
Powder diffraction pattern of a typical spent catalyst sample with phase identification. All the other peaks belong to zeolite Y. The phase identification has been performed by means of PANalytical Highscore plus [ 14 ]. In particular, the Rietveld method will not be easy to apply, as it requires an internal standard for the quantification of the amorphous component, with some issues on the accuracy [ 15 ].
The Rietveld method, in fact, normalises the phase fractions, so that their sum is 1. In this way, only crystalline phases are taken into account in the quantification, leading to a gross overestimation of the crystalline components especially when the amorphous content is large, like in this case.
The only way to use the Rietveld method, when an amorphous component is present, is to couple it with RIR method, by means of addition of an internal standard; the procedure, however, is long and complex, subjected to quite large errors in the amorphous content evaluation, and to issues in the choice of the proper internal standard [ 15 ]. The idea was then to check whether NiO was still detectable in a complex matrix: small amounts of NiO were added to a spent catalyst with a very low amount of nickel determined by XRF, as shown in the experimental section.
Figure 6 shows the corresponding powder diffraction patterns. The inset shows a zoom of the data, where NiO peaks are well visibile above the background. Comparison of powder diffraction patterns of a spent catalyst with known quantities of NiO. In the inset, a zoom of the graph, where the peaks from NiO are clearly visible.
The samples of the spent catalyst with added NiO Fig. The presence of an amorphous phase, in fact, usually constitutes an issue in the quantification of very small amount of crystalline materials by means of powder diffraction. The introduction of known quantities of the studied species in one of such samples, should help to understand how and if the calibration lines are working in such ill-condition cases.
In the same way as previously done, the calibration for peak area and peak heights were used and compared. Table 5 shows the results. The peak areas and the peak height were determined using PANalytical Highscore plus [ 14 ].
The last column, i. Even though the accuracy is not optimal, the method is very quick and reliable. The relative differences are much larger than those estimated for the samples with fresh zeolite Y see for comparison Table 4. It is then clear that the complex nature of the matrix, its many diffraction peaks and the presence of an amorphous component play a key role in determining the accuracy of the method.
Regarding the results for NiO, it can be noted that the larger concentrations tend to be underestimated, but this is not true for the smallest one, which is largely overestimated. The results of this paragraph show that it is possible, quickly and easily, to evaluate a NiO concentration as low as ppm; even taking into account the large positive uncertainty of the determination, the result will still be below the law limit of ppm.
After the validation of the quantification method, the analysis of the issues connected to it, and the evaluation of the errors that can affect the measurement, the following step was to apply the method and the corresponding minimum detectable quantity to some real samples of spent catalysts. The samples are representative of quite a long period 12 months and have been characterised first from the chemical point of view by means of XRF.
X-ray powder patterns of all the samples were then checked for the presence and eventual quantification of nickel containing species. The graph in Fig. The inset shows the region of interest for the species studied. It can be seen that no peak is present in the regions of the two main peaks for both species. As we know that 0.
Powder diffraction patterns for the spent catalysts. Color figure online. The paper shows a very quick and relatively accurate way to determine whether a spent catalyst sample contains NiO with the corresponding concentrations, down to 0. A detailed study of known and very small concentrations of the two species in simple and more complex matrices provided the possibility to deeply understand their detection limit and the errors connected to their quantification.
Various methods have been applied for the quantification, and the following conclusions can be drawn: - the Rietveld method is quite accurate and reproducible, but it can be applied only when the matrix is crystalline and not particularly complex; using it in complex matrices, with an amorphous component, requires an internal standard, and it is not particularly accurate, in general, for very low concentrations of the two studied species; - the peak area and peak height methods showed to be very fast and quite reliable in the samples with fresh zeolite Y: in particular, for the smaller concentrations, the peak height method provides better results; in a complex matrix, similar to the one of real spent catalysts, the presence of NiO is well visible and quantifiable down to a concentration of 0.
The concentration limit of NiO for the direct re-use of waste materials is 0. The use of a very high resolution powder diffraction beamline, such as ID22 ESRF, provided very good results, because of its exceptional signal-to-noise ratio, and may be instrumental for the continuation of this work. Vogt, E. Article Google Scholar. Biswas, J. Meirer, F. Etim, U. UI layer. Architecture Components. UI layer libraries. View binding. Data binding library. Lifecycle-aware components. Paging Library.
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