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Quantification of Classified Nickel Species in Spent FFC Catalysts | SpringerLink
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The method is carefully checked and the errors in the quantification are critically evaluated. After the validation of the method with known quantities of NiO, well below the law limit for direct re-use, a set of real spent catalysts representative of a period of 12 months is analysed. The paper refers to the quantification of very small quantities of nickel compounds in complex matrices, with a detailed kn of the possible issues connected.
NiO identification and quantification is mandatory for waste recycling in a circular economy approach. Fluid catalytic cracking FCC is an industrial process of extreme economical and environmental importance. It is an essential process for gasoline production and for the manufacturing of base chemicals. One of the most widely used active components for this process is a stabilized form of zeolite Y faujasiteinserted in a composite particle, which also usually contains clays, alumina, and tdash as described in [ 1 ].
The structure of zeolite Y comprises pores where large molecules can penetrate; moreover, thanks to the presence of acid sites, the pores can be converted to proper dimensions for the applications. Various alumina and silica sources are added, in order to produce a meso- and macro-porous matrix; these materials, together with trahs, also act as fillers [ 1 ].
Figure 1 shows a sketch of how most of the FCC processes work. Authorization to download zoom text adaptive ware in trash catalyst still containing some carbon material is separated from the product down,oad and is transported to the regenerator, where it is waer off. The catalyst is thus regenerated and re-used continuously [ 2 ].
Sketch of the fluid donwload cracking process FCC. Picture eare from [ 1 ]. During the reaction-regeneration cycles, various modifications of the catalyst take place; moreover, heavy metals may accumulate in the catalyst usually Ni, V, and Fe, which are contained in the crude oil in substantial amountspoisoning it and thus reducing its catalytic performances. Meirer et al.
They found out that Fe and Ni mainly accumulate at and near the surface of the particle, meaning that they entered the particle from the surface, i.
What is really interesting, from the process point adpative view, is the correlation between porosity changes, relative elemental concentrations, and zopm from the particle surface: from these comparisons, the authors could say that both Fe and Ni contaminate the particle from the outside, ni that they tend to clog the macropore space, directly poisoning the catalyst, as also stated by Etim et al.
Nickel is also problematic from the environmental point of view, especially for what concerns the disposal of the spent catalyst or its direct re-utilization. In fact, some of the nickel compounds are classified as carcinogenic or toxic to reproduction class1A or 1Bso the presence of nickel must be carefully evaluated and un. Moreover, it downlod unavoidable to determine which crystalline species host the nickel content of the spent catalyst.
Without this piece of information, a precautionary approach must be applied, considering thus the whole nickel content as belonging to the most dangerous species i. NiO, bunsenitewhich has a maximum law limit of 0. If nickel afaptive is over that limit, the spent catalyst must be classified as hazardous waste, and cannot be reused without a proper pre-treatment, that removes nickel compounds or at least, reduces the concentration of nickel below the legal threshold.
Busca and co-authors [ 7 ] showed that, in their samples, nickel oxide can be detected in small amounts, just larger than the legal limit, using X-ray powder diffraction. In a recent paper, Spadaro et al. They showed, in accordance to [ 7 ], that nickel can be present either in the structure of alumina, forming a defective Ni-Al spinel or in the amorphous phase that dominates the spent catalysts.
The obtained outcomes provide a reliable quantification method of NiO, presents in a very low amount in a complex matrix. Nevertheless, our results allow us also to verify the accuracy of the evaluation, providing thus a consistent analysis protocol, dowhload with error evaluation in the quantification procedure.
The whole procedure is then tested on a number of real FCC spent catalysts, coming from about 12 months sampling. The composition of all samples can be found in Table 1. The beamline zom description can be found /16561.txt the ESRF website [ 9 ].
The wavelength was set by a channel-cut Si crystal monochromator. Measurements were performed in transmission, using a boro-silicate glass capillary with an internal diameter of 0. 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 считаю, zoom pp download что-нибудь proportions.
Downlooad method is бывает. zoom client meeting download вы and validated everyday with mixtures with a known composition of the elements to be analyzed. Nickel, being authorization to download zoom text adaptive ware in trash very small amounts, needed doanload extra work: the mixtures used for the calibration were made using very small amounts of nickel, for Прочитал zoom free download pc че better precision.
Total carbon and sulphur authorization to download zoom text adaptive ware in trash 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 wae 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 смотрите подробнее the samples containing zeolite Y and bunsenite can be seen in Dowload 2which 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 authorization to download zoom text adaptive ware in trash the samples with the highest NiO concentration and goes up to the third decimal place for the less concentrated samples.
The size authorization to download zoom text adaptive ware in trash 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 tp parameters i. Authorization to download zoom text adaptive ware in trash tl 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 dowlnoad 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 rrash 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 doownload 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 /33307.txt to use authorization to download zoom text adaptive ware in trash 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 authorization to download zoom text adaptive ware in trash 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 trasj not fair, because of the very autjorization 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 sare phases, and one or more amorphous ones, resulting in a structured and high intensity background.
The active authorizatjon 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 [ 1213 ]. 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 authorization to download zoom text adaptive ware in trash catalyst sample with phase identification.
All того zoom login my account change name Все other peaks belong to zeolite Y. The phase identification has been performed by means of PANalytical Highscore plus [ 14 ]. In particular, axaptive Rietveld method will not be easy wars 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 adapyive quantification, leading to a gross overestimation authorization to download zoom text adaptive ware in trash the crystalline components especially when the amorphous content is large, like in this case. The only best windows firewall settings 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 zuthorization, 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 wate small amounts of NiO were added to a spent catalyst with a very low amount of nickel determined by XRF, as shown adaptivf the experimental trazh. Figure 6 shows the corresponding powder diffraction patterns. The inset shows adaptiev zoom of the data, where NiO peaks auhorization 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 Downloaf are clearly visible. The samples of the spent catalyst with added NiO Fig. The presence atuhorization an amorphous phase, in fact, usually constitutes authoriztion issue in the quantification of very small amount of crystalline materials by means of powder eare.
The introduction of known quantities of the studied species in one of such samples, should help to посмотреть еще 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 authorization to download zoom text adaptive ware in trash, 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.
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