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Dr. Biswas received his Ph.D. from POSTECH, South Korea.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"194151",title:"Dr.",name:"Abhijit",middleName:null,surname:"Biswas",slug:"abhijit-biswas",fullName:"Abhijit Biswas",profilePictureURL:"https://mts.intechopen.com/storage/users/194151/images/system/194151.png",biography:"Dr. Abhijit Biswas is a research associate at the Indian Institute of Science Education and Research (IISER) Pune, in India. His research goal is to design and synthesize highest quality epitaxial heterostructures and superlattices, to play with their internal degrees of freedom to exploit the structure–property relationships, in order to find the next-generation multi-functional materials, in view of applications and of fundamental interest. His current research interest ranges from growth of novel perovskite oxides to non-oxides epitaxial films, down to its ultra-thin limit, to observe unforeseeable phenomena. He is also engaged in the growth of high quality epitaxial layered carbides and two-dimensional non-oxide thin films, to exploit the strain, dimension, and quantum confinement effect. His recent work also includes the metal-insulator transitions and magneto-transport phenomena in strong spin-orbit coupled epitaxial perovskite oxide thin films by reducing dimensionality as well as strain engineering. He is also extremely interested in the various energy related environment friendly future technological applications of thin films. In his early research career, he had also extensively worked on the tailoring of metal oxide crystal surfaces to obtain the atomic flatness with single terminating layer. Currently, he is also serving as a reviewer of several reputed peer-review journals.\nDr. Biswas received his B.Sc. in Physics from Kalyani University, followed by M.Sc in Physics (specialization in experimental condensed matter physics) from Indian Institute of Technology (IIT), Bombay. His Ph.D., also in experimental condensed matter physics, was awarded by POSTECH, South Korea for his work on the transport phenomena in perovskite oxide thin films. 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\n
1. Introduction
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The correlation between the volcanic activity and the earthquakes is a well-known subject of investigation. It commonly refers to two distinct aspects: first, the seismicity in volcanic areas related to magmatic and hydrothermal movements, which is of interest for predicting the possible volcano unrest [1] and second, discussed in this chapter, the possible triggering of eruptions caused by stress transfer due to strong earthquakes, even located far from the volcano edifice [2]. A recent study carried out to a global scale [3] has shown that this mechanism of triggering is effective for very strong earthquakes (Mw ≥ 7.5) located within 200 km from the volcano. In Italy, the availability of reliable catalogs covering several centuries of earthquake and eruptive observations gives the possibility to explore the long-distance volcanic/seismic relationship with more detail. According to previous studies [4, 5, 6], such link is particularly evident for the eruptions of Mt Vesuvius, near Naples, in southern Italy (triangle in Figure 1).
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Figure 1.
Epicenters of Mw ≥ 6.0 earthquakes occurred in Italy between 1600 and 2016 (declustered catalog).
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The Vesuvius volcano is one of the most studied in the world. Through the centuries, eruptions were described by Neapolitan and foreign scholars. A significant step was performed on 1841, with the institution of the “Osservatorio Vesuviano”, the first volcanology observatory in the world. Nowadays, Mt Vesuvius is monitored by a dense network of seismic, geochemical, and GPS stations (http://www.ov.ingv.it/ov/it/vesuvio). Its eruptive history for the last 2000 years is well known through the historical sources and the archaeomagnetic dating of volcanic deposits [7]. In particular, in the last millennium, after a few centuries of weak activity, the Vesuvius awakened on 1631 and entered in a long period of sustained and almost continuous activity concluded with its last eruption of 1944 [8], followed by the current phase of quiescence.
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In the last few decades, geological and geophysical investigations have improved the knowledge about the tectonic setting of Mt Vesuvius as well as its internal structure and magmatic system [4, 9, 10]. Concerning the relationships with far seismicity, [4] has furnished statistical evidence for the time correlation between the eruptions of Mt Vesuvius and moderate-strong earthquakes (Mw ≥ 5.4) in the Southern Apennines. In [5], such correlation is modeled as the effect of mutual stress transfer working at distances up to 150 km. In [6], it has been observed that the synchronization of eruptions with Mw ≥ 6 earthquakes occurring throughout the national territory, even hundreds of kilometers far from the volcano and in different tectonic domains. This finding has suggested the occurrence of a common cause at the basis of the two phenomena rather than a direct interaction or mutual triggering.
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The investigation of the seismic/volcanic relationship requires two components: statistical methods to assess the existence of the correlation and to estimate its strength and geophysical methods able to furnish realistic models for its occurrence. This chapter is focused on the first aspect and presents an application of the modified Ripley’s K-function to countrywide strong seismicity and to the eruptions of Mt Vesuvius since the seventeenth century.
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Statistics alone is not able to distinguish between a causal relationship (earthquake triggering eruptions) and the co-causal hypothesis (an external mechanism controlling both earthquakes and eruptions). Elements on this topic can be obtained looking at the bradyseism of the Campi Flegrei caldera (white diamond in Figure 1). The caldera and Mt Vesuvius are very near (25 km apart), share a similar regional tectonic environment, and, according to [11], have a common magma chamber. Furthermore, they alternate over time: the caldera was at rest during the intense eruptive period of Mt Vesuvius (1631–1944) and reactivated with an uplift process just after its conclusion (around 1950). Similarly to the eruptions of Mt Vesuvius, the phases of major uplift coincide with accelerated seismic activity in Italy. In a way, the two volcanoes look like twin systems with related behavior. The hypothesis here assumed is that what observed for the sismic/volcanic connection at Campi Flegrei in the last few decades can be reasonably extended to the past activity of Mt Vesuvius. In respect to analyzing rare eruptions, the bradyseism offers more details, thanks to the density of uplift measures in the last 70 years (almost continuous since 2000).
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Recent works [6, 12, 13] have pointed out the correspondence between variations in the rate of seismicity throughout Italy and the climatic changes of the last millennium. In particular, the seismic activity accelerated during the most severe period of the Little Ice Age (between 1600 and 1900), while it seems to decrease in the current phase of global warming.
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At the end of this chapter, it will be shown that this correspondence can be extended to the eruptive history of Mt Vesuvius. The finding leads to the hypothesis that the climate-related surface processes like glaciation/deglaciation and sea level changes could play a significant role in regulating both the eruptions and the earthquakes.
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2. Volcanological and seismological data
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The eruptive history of Mt Vesuvius is drawn from the Smithsonian’s Global Volcanism Program (GVP) database ([14]; http://www.volcano.si.edu), where each eruption is described by its start date, by its end date, and by the Volcanic Explosivity Index (VEI [15]). An eruption can last from days to decades, and the VEI is attributed based on the strongest, often final, episode. The current analysis has been performed for the eruptions with VEI ≥ 2, assuming that for Mt Vesuvius, the catalog is complete at this level since the year 1600. This is a work hypothesis that seems to be acceptable given the proximity of the volcano to Naples, one of the largest cities in Europe since the Middle Ages. The selected dataset includes 25 eruptions since 1631. The last eruptive cycle started on 1913 and concluded on 1944 (VEI = 3).
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The earthquake catalog herein adopted is the same of [13]. Its main characteristics and the processing steps are summarized as it follows. For the years between 1600 and 2014, the seismic events are drawn from the latest revision of the “Catalogo Parametrico dei Terremoti Italiani” (CPTI15, release 1.5 [16]). The dataset extends up to the end of 2016 with the earthquakes reported in the European-Mediterranean Regional Centroid Moment Tensor (RCMT) Catalog [17]. The resulting catalog includes the earthquakes located in Italy and in a narrow surrounding area. Among these events, only the mainshocks have been considered: the clusters of aftershocks have been removed using the algorithm described in [18]. It is important to guarantee that the catalog is complete at the same magnitude level in different time periods to avoid a biased analysis. To this purpose, after considering the completeness analysis carried out in [19], the catalog is assumed to be complete for a moment magnitude Mw larger or equal to 6. The selected dataset contains 60 earthquakes, including the recent destructive earthquake of Central Italy, occurred on August 24, 2016 (Mw 6.2 [17]).
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A correlation analysis has been performed for the vertical ground movements at Campi Flegrei. A time history for the period 1905–2017 has been obtained merging the geodetic measurements available from 1905 to 2009 for the benchmark 25A in a leveling line established by the Istituto Geografico Militare (IGM) on 1905 [20], the measurements collected between January 2000 and July 2013 at the GPS station RITE located about 200 m from the benchmark 25A [21], and more recent GPS measurements from the same station (August 2014–April 2017) published in the online monthly bulletins published by the Osservatorio Vesuviano (http://www.ov.ingv.it/ov/campi-flegrei).
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3. Time correlation between the eruptions of Mt Vesuvius and strong earthquakes throughout Italy
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In this section, the times of occurrence of Vesuvius’ eruptions, V = {V1, …, VnV}, and those of strong earthquakes in Italy, E = {E1, …, EnE} are compared to assess their time correlation. There are different techniques to perform the task. One possibility, if the number of events sufficiently large, is to compare the histograms representing the time distribution of the events: the period of observation (tstart, tend) is subdivided in nb bins of equal width Δt and the analysis is performed for the two time series X = {X1, …, Xnb} and Y = {Y1, …, Ynb}, where Xi and Yi are the number of eruptions and earthquakes in the ith time bin, respectively. The degree of correlation can be assessed parametrically, using Pearson correlation, which assumes a bivariate normal distribution of data, or non-parametrically, using either Kendall or Spearman rank correlation, which are independent on the type of data distribution. A more flexible way to represent and compare two time distributions of events (useful even in the case they are rare) looks at their smoothed time density obtained by Gaussian kernel estimation [22]. The correlation coefficient (Pearson, Kendall or Spearman) is computed for the two functions
where ϕ(z;h) is the kernel function (zero-mean normal density function in z with standard deviation h), and h is the smoothing parameter (the larger h, the larger the degree of smoothing). Both approaches suffer a common limitation: their results depend on the time resolution adopted for the analysis (i.e., the width of the bin for the histogram, the smoothing parameter for kernel density estimation). In general, a large time window could lead to similar flat distributions and then to a spurious high correlation. A partial solution is to perform a sensitivity analysis, checking how the value of the correlation coefficient varies for different time resolutions. A totally different approach is that based on the bivariate, Ripley’s K-function [23] simplified for one dimension [24, 25]. It works directly on the two sets of event times, avoiding any transformation and arbitrary choice of parameters and consequent loss of information. The K-function is a function of time with equation.
where I() is the identity function (it returns 1 if its argument is true, 0 otherwise) and T is the total period of observation in years. The K-function is transformed to obtain the L-function
The L-function is associated with a 95% confidence envelope computed using N randomizations of V and E (N = 1000 in the present analysis). If, for given t, LVE(t) is larger than the confidence envelope, then the number of couples for which |Vi − Ej| < t is significantly larger than those awaited in a random distribution: it is an indication of synchrony within a time lag t between the two sets of events. Similarly, values of LVE(t) within the confidence envelope indicate independence, while values falling under the confidence envelope indicate asynchrony or repulsion. In the following, the synchronization of events is explored graphically by means of their smoothed time densities, while it is assessed formally examining the L-function. The analysis updates that performed in [12] for an older version of the earthquake catalog.
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The eruptive history of Mt Vesuvius between the seventeenth century and the beginning of the twentieth century is illustrated in Figure 2a. After a long period of weak activity (6 eruptions since 1100, including a VEI 2 eruption on 1500 and a VEI 1 eruption on 1570), the volcano reactivated with the strong eruption of 1631 (VEI 5), followed by 24 eruptions (4 with VEI = 2, 19 with VEI = 3, and 1 with VEI = 4). Their smoothed time densities computed for h = 10 years (continuous line in Figure 2a) indicate two peaks around 1700 and 1850, as well as an overall oscillatory behavior with a time period of about 50 years. Such trend is very similar to that of the earthquakes (dashed line in Figure 2a). Eruptions and earthquakes appear almost synchronous on six regular oscillations. The characteristics of such oscillations were explored graphically in [6]. A more formal test based on Schuster spectrum analysis [26] has been adopted in [13] for the oscillations of seismicity. It demonstrates the statistical significance of the oscillations and refines the estimation of their time period to 46 years. Applied to the set of Vesuvius’ eruptions the same test fails, indicating that the oscillations are too weak to gain a statistical significance. Nonetheless, the similarity between the two smoothed time densities is such to suggest a formal test for synchronization. The L-function and the corresponding 95% envelope computed for the two sets of events are traced in Figure 3a. The time correlation is significant for the time lags of 3 and 9 years, where the L-function exceed the 95% envelope. Figures 2b and 3b show the same comparison performed for 9 earthquakes located above the 44th parallel north (evidenced with dashed line in Figure 1), at more than 400 km from the Vesuvius. Even in this case, the two time densities are similar, with a good correspondence on the two peaks near 1700 and 1850 and less precision on the other local maxima, especially before 1700. The L-function (Figure 3b) reflects such deteriorated time correlation: the 95% envelope (dashed line) is just touched for a time lag of 3 years, while there is a widespread time synchronization significant at the 90% confidence level (dotted line) for various time lags up to 25 years, the semi-period of oscillation. Such result indicates that there is some degree of overlapping among the positive part of the oscillations, near the local maxima.
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Figure 2.
Time distribution of strong earthquakes in Italy compared to Vesuvius’ eruptions in the time period 1600–1920: (a) seismicity of the entire territory; (b) earthquakes located north of 44° lat.
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Figure 3.
L-function in the modified Ripley’s test for synchronization [23, 24, 25] applied to the series of strong earthquakes in Italy and Vesuvius’ eruptions occurred in the time period 1600–1920: (a) seismicity of the entire territory; (b) earthquakes located north of 44° lat.
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4. Further check on the possible volcanic triggering by earthquakes: the case of the Campi Flegrei caldera
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After more than three centuries of quiescence, with almost continuous deflating, the Campi Flegrei caldera reactivated around 1950 and, since then, has been subjected to uplift steps of various amplitudes. The vertical movements are documented since 1905 by irregular geodetic levelings and indirect measurements [20], as well as, since 2000, by continuous GPS data [21]. Such a time series, its correlation with strong seismicity and the complementarity with the eruptions of Mt Vesuvius are shown in Figure 4. The last eruptive phase of Vesuvius (1913–1944) coincides with the largest seismic oscillation of the last century (peak around 1920), with the Campi Flegrei slowly deflating. Around 1950, the situation is inverted, with the Vesuvius at rest and the caldera that reactivated with two major episodes on 1970 and 1983 almost synchronous with the second (both in amplitude and chronologically) oscillation of seismicity. Around 2004, the caldera started a slower and more reduced uplift phase, currently still active, that coincides with the last, less energetic cycle of seismicity (three earthquakes: 2009, L’Aquila, Mw 6.3; 2012, Emilia, Mw 6.1; and 2016, Central Italy, Mw 6.2).
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Figure 4.
Smoothed time density of Mw ≥ 6.0 earthquakes in Italy since 1900 (top) compared to the smoothed time density of Vesuvius’ eruptions (middle) and the elevation of the Campi Flegrei caldera (bottom).
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For the last century, the seismic catalog is complete at a much lower magnitude threshold (Mw 4.8 according to [19]) and the magnitude estimation itself is more reliable. This allows performing a direct comparison between the uplift and the energy radiated by the earthquakes, a quantity which is sampled at a larger number of points than in previous analysis (127 mainshocks with Mw ≥ 4.8 since 1950 compared to 8 with Mw ≥ 6). The relationship is illustrated in Figure 5 for the cumulative uplift (the deflating phases were removed) and the cumulative radiated energy ES expressed in erg computed from Mw according to the equation
Comparison between the uplift time series of the Campi Flegrei caldera (deflating episodes removed) and the cumulative energy released by earthquakes with Mw ≥ 4.8 occurred in Italy in the time period 1950–2016.
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drawn from [27]. Since 1950, the vertical movements and the cumulative earthquake energy chase each other, according to an irregular pattern (uplift steps either precede or follow periods of major energy release). Concerning the possible triggering of the uplift by earthquakes, just one step is clearly preceded by a strong earthquake located near the seismo/volcanic coupling zone (SVCZ in the following) delineated in [5]: step S3 in Figure 5 (1983), preceded by the 1980 Irpinia earthquake (Mw 6.8, located about 95 km east of the caldera). Of the other steps, that of 1952 (S1 in Figure 5) has no significant seismicity preceding it; that of 1970 (S2) is preceded by the 1968 Belice earthquake (Mw 6.4), located in Sicily, at more than 300 km from the caldera, while the previous significant earthquake in the SVCZ occurred 8 years before the uplift (1962 Irpinia earthquake, Mw 6.2, located 80 km north-east of the caldera). The more gradual uplift that started on 2004 (S4, shown in detail in Figure 6) was preceded on 2002 by two moderate earthquakes, one (Mw 5.9) located externally to the SVCZ in the Tyrrhenian sea (270 km south-east of the caldera) and the other one, with Mw 5.7, located within the SVCZ, 120 km north-east of the caldera (2002 Molise earthquake). After 2004, the uplift goes strictly in parallel with the energy release, with the three strong earthquakes of 2009, 2012, and 2016 located externally to the SVCZ, in central and northern Italy (172, 509, and 221 km north-west of the caldera, respectively). As a consequence, if a triggering effect exists, it is rather fuzzy. In particular, it should involve earthquakes that are external to the SVCZ (e.g., those post-2004) with response times that are not proportional to the distance (e.g., the 1962 earthquake, the nearest to the caldera, which could have triggered an uplift with a delay of 8 years).
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Figure 6.
Comparison between the uplift time series of the Campi Flegrei caldera (deflating movements removed) and the cumulative energy radiated by earthquakes with Mw ≥ 4.8 occurred in Italy in the time period 2000–2016.
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5. Eruptions, earthquakes, and the climate
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The facts described so far suggest that point-to-point elastic stress transfer alone is not sufficient to explain the large-scale seismic/volcanic correlation involving the Neapolitan volcanic district. Perhaps, more general mechanisms should act. Previous works [6, 12, 13] noted the correspondence between the seismic transient that took place between 1600 and 1900 (three time the annual rate of destructive earthquakes in respect to the previous period) and the occurrence of the Little Ice Age (LIA). Furthermore, the current phase of global warming is synchronous with the gradual reduction of seismic activity through the last century (Figure 4). Previous works have suggested a possible role of the climate, which could affect both the seismicity and the volcanism through variations of the surface loads (sea level, ice at the poles and glaciers) and consequent changes of the stress field at depth. A similar mechanism is supported by a number of geophysical models and statistical studies available in the literature [28], although most of them (e.g., [29]) refer to the deglaciation and the sea level increase (about 120 m) that followed the last glacial maximum of 21,000 years ago.
\n
What outlined is a promising field of investigation, although very problematic. Just to say, there are a number of climate indexes, most of which are not direct measures but reconstructions obtained by correlation with biological, chemical, and geophysical data. There is no consensus on the beginning of the LIA as well as on its spatial extension (global or restricted to a more limited area, for example, the Euro-Asiatic region) and its temporal evolution. All such complicates the assessment of the time correlation, which is just the first step of the task. The work [6] reports some graphical comparisons between Italian seismicity, the global sea level, and the global sea level rate, since 1700. More robust statistical methods are adopted in [12] to assess the degree of correlation between Italian seismicity of the last millennium and a reconstruction of the global surface temperature [30]. In that case, a point process (the sequence of Mw ≥ 6.1 earthquakes in Italy occurred since 1100) was compared with a continuous time function (the time series of temperature) using binomial logistic regression [31]. The analysis found a significant negative correlation for a time lag of 174 years: the probability to have an earthquake during the year y has a negative dependence on the temperature recorded 174 years before (the higher the temperature, the lower the probability of an earthquake). The relationship is illustrated in Figure 7 (modified from [12]), where the smoothed time density of earthquakes (continuous line) is plotted together to the time series of the global surface temperature anomaly ΔT (difference with the mean temperature in the reference period 1961–1990, dashed line), with the y-axis reversed (increasing values downward) and the x-axis translated by 174 years. In addition (in respect to the original figure), Figure 7 reports the smoothed time density of the Vesuvius’ eruptions (dotted line): even such curve matches the negative temperature anomaly, although the eruptive activity stops in the first half of the twentieth century.
\n
Figure 7.
Comparison among the smoothed time density of Mw ≥ 6.1 earthquakes occurred in Italy since 1100, the smoothed time density of VEI ≥ 2 eruptions of Mt Vesuvius, and a reconstruction of the global surface temperature anomaly ΔT [30]. The plot of temperature is reversed (increasing values downward) and shifted by 174 years to evidence the estimated anticorrelation with the earthquakes.
\n
The transformation from global surface temperature to water/ice surface load is not so immediate. Also, the physical justification of a delay of 174 years could be problematic. It is possible that other, even more local climate indexes are more appropriate. The paper [32] describes the common behavior of glaciers and lakes in west-central Europe over the last 3500 years. Representative of this, the authors report the advance/retreat time history of the Great Aletsch glacier (Alps of Valais, Switzerland), the largest glacier in the European Alps. In Figure 8, such data are compared with the time densities of Mw ≥ 6 earthquakes in Italy and VEI ≥ 2 Vesuvius’ eruptions since the year 1100 (as the glacier data are given with low detail, the densities are smoothed for a large smoothing parameter, h = 40 years). The resemblance among the three curves is remarkable. In the post-1600 period, they share the bimodality with time lags extremely reduced in respect to the comparison with the temperature (about 50 years for the peaks near 1700). In the pre-1600 period, they have three common oscillations, although with different amplitude. The figure offers also an example of the lack of direct correspondence between temperature and ice extension. In fact, the Great Aletsch glacier was at a local minimum around 1450, a period characterized by low global temperature (Figure 7). Such finding indicates that other factors must be taken into consideration (e.g., the precipitation regime).
\n
Figure 8.
Comparison among the smoothed time density of Mw ≥ 6.0 earthquakes occurred in Italy since 1100, the smoothed time density of VEI ≥ 2 eruptions of Mt Vesuvius, and the fluctuation (increasing values indicate advance) of the Great Aletsch glacier according to [32].
\n
\n
\n
6. Conclusions
\n
The analysis of updated and new data confirms the existence of a close relationship between the Italian seismicity and the volcanic activity in the Neapolitan area. Such a correlation involves not only the Mt Vesuvius but also the Campi Flegrei caldera, which was reactivated with a significant rate of uplift during the last 70 years. This type of seismic/volcanic correlation was previously explained as the effect of the elastic stress transfer from earthquakes sharing the same tectonic environment of the volcano (southern Apennines). This view implies a rather specific, event-to-event correspondence between earthquakes and eruptions. The evidences furnished in the present chapter indicate a looser, less specific correspondence, where the volcanic activity reflects the time density of a population of earthquakes, including also events located in northern Italy, an area dominated by a rather different stress regime (compressive instead of distensive). Continuous data from the geodetic monitoring of the Campi Flegrei also suggest that the time correlation is less episodic (i.e., related to events) and involves also a smooth evolution (e.g., the rather regular expansion of the caldera since 2004 illustrated in Figure 6). The picture here outlined suggests an alternative, common mechanism at the basis of both types of activity. The load/unload of the earth surface by climate processes is a possible candidate. The graphical comparison of Figure 8 suggests that regional (e.g., European) instead of global effects should be considered. The last point of interest emerging from the seismic/volcanic comparative analysis is the observed complementary behavior between the Vesuvius and the Campi Flegrei caldera. Although it could be a purely accidental effect, it encourages a holistic approach that looks at the Neapolitan volcanic district as a single integrated system rather than a set of distinct volcanoes.
\n
\n
Acknowledgments
\n
This research was supported by Regione Autonoma Friuli Venezia Giulia and Regione Veneto. All the figures were produced using the Generic Mapping Tool, version 5.1.1 [33].
\n
\n',keywords:"Mt Vesuvius, Campi Flegrei caldera, Italian seismicity, event synchronization, Ripley’s K-function",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/57785.pdf",chapterXML:"https://mts.intechopen.com/source/xml/57785.xml",downloadPdfUrl:"/chapter/pdf-download/57785",previewPdfUrl:"/chapter/pdf-preview/57785",totalDownloads:470,totalViews:201,totalCrossrefCites:1,totalDimensionsCites:1,hasAltmetrics:0,dateSubmitted:"March 14th 2017",dateReviewed:"October 26th 2017",datePrePublished:"December 21st 2017",datePublished:"July 18th 2018",dateFinished:null,readingETA:"0",abstract:"The time correlation between the eruptions of Mt Vesuvius and the occurrence of strong earthquakes in Italy has been revised using new and improved catalogs and data made available in the last decade. It has been shown that this correlation is statistically significant and involves also the earthquakes located very far from the volcanic edifice (hundreds of kilometers). In particular, the earthquakes and the Vesuvius’ eruptions agree on a transient of accelerated activity between 1600 and 1900. A similar correlation has been found between the seismicity and the uplift episodes at the nearby Campi Flegrei caldera occurred in the last 70 years: there is strict similarity between the two cycles, the first one centered around 1970–1980 and the second one started on 2004 and still continuing and involving recent strong earthquakes (2009 L’Aquila earthquake, 2012 Emilia earthquake and 2016 Central Italy earthquake). The synchronization to such a long distance has suggested the occurrence of large-scale climatic processes controlling both the earthquakes and the volcanism. The comparison with climatic indexes like the global surface temperature and the extension of glaciers in western-central Europe has indicated a possible role of climatic parameters in controlling volcanism and seismicity.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/57785",risUrl:"/chapter/ris/57785",book:{slug:"volcanoes-geological-and-geophysical-setting-theoretical-aspects-and-numerical-modeling-applications-to-industry-and-their-impact-on-the-human-health"},signatures:"Pier Luigi Bragato",authors:[{id:"206830",title:"Dr.",name:"Pier Luigi",middleName:null,surname:"Bragato",fullName:"Pier Luigi Bragato",slug:"pier-luigi-bragato",email:"pbragato@inogs.it",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Volcanological and seismological data",level:"1"},{id:"sec_3",title:"3. Time correlation between the eruptions of Mt Vesuvius and strong earthquakes throughout Italy",level:"1"},{id:"sec_4",title:"4. Further check on the possible volcanic triggering by earthquakes: the case of the Campi Flegrei caldera",level:"1"},{id:"sec_5",title:"5. Eruptions, earthquakes, and the climate",level:"1"},{id:"sec_6",title:"6. Conclusions",level:"1"},{id:"sec_7",title:"Acknowledgments",level:"1"}],chapterReferences:[{id:"B1",body:'Sparks RSJ, Biggs J, Neuberg JW. Monitoring volcanoes. Science. 2012;335:1310-1311. DOI: 10.1126/science.1219485\n'},{id:"B2",body:'Marzocchi W, Zaccarelli L, Boschi E. Phenomenological evidence in favor of a remote seismic coupling for large volcanic eruptions. Geophysical Research Letters. 2004;31:L04601. DOI: 10.1029/2003GL018709\n'},{id:"B3",body:'Nishimura T. Triggering of volcanic eruptions by large earthquakes. Geophysical Research Letters. 2017. DOI: 10.1002/2017GL074579\n'},{id:"B4",body:'Marzocchi W, Scandone R, Mulargia F. The tectonic setting of Mount Vesuvius and the correlation between its eruptions and the earthquakes of the Southern Apennines. 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DOI: 10.4401/ag-6431\n'},{id:"B22",body:'Bowman AW, Azzalini A. Applied Smoothing Techniques for Data Analysis. Oxford: Oxford University Press; 1997\n'},{id:"B23",body:'Ripley BD. Modeling spatial patterns. Journal of the Royal Statistical Society. 1977;B39:172-212\n'},{id:"B24",body:'Doss H. On estimating the dependence between two point processes. Annals of Statistics. 1989;17:749-763\n'},{id:"B25",body:'Gavin DG, Hu FS, Lertzman K, Corbett P. Weak climatic control of stand-scale fire history during the late holocene in southeastern British Columbia. Ecology. 2006;87:1722-1732\n'},{id:"B26",body:'Ader TJ, Avouac JP. Detecting periodicities and declustering in earthquake catalogs using the Schuster spectrum, application to Himalayan seismicity. Earth and Planetary Science Letters. 2013;377-378:97-105. DOI: 10.1016/j.epsl.2013.06.032\n'},{id:"B27",body:'Gutenberg B, Richter CF. Magnitude and energy of earthquakes. Annali di Geofisica. 1956;9:1-15\n'},{id:"B28",body:'McGuire B. Waking the Giant: How a Changing Climate Triggers Earthquakes, Tsunamis, and Volcanoes. Oxford: Oxford University Press; 2013\n'},{id:"B29",body:'Luttrell K, Sandwell D. Ocean loading effects on stress at near shore plate boundary fault systems. Journal of Geophysical Research. 2010;115:B08411. DOI: 10.1029/2009JB006541\n'},{id:"B30",body:'Mann ME, Zhang Z, Hughes MK, Bradley RS, Miller SK, Rutherford S, Ni F. Proxy-based reconstructions of hemispheric and global surface temperature variations over the past two millennia. Proceedings of the National Academy of Sciences of the United States of America. 2008;105:13252-13257. DOI: 10.1073/pnas.0805721105\n'},{id:"B31",body:'Venables WN, Ripley BD (2002) Modern Applied Statistics with S, fourth ed. New York: Springer, ISBN: 0-387-95457-0\n'},{id:"B32",body:'Holzhauser H, Magny M, Zumbühl HJ. Glacier and lake-level variations in west-central Europe over the last 3500 years. The Holocene. 2005;15:789-801. DOI: 10.1191/0959683605hl853ra\n'},{id:"B33",body:'Wessel P, Smith WHF, Scharroo R, Luis JF, Wobbe F. Generic mapping tools: Improved version released. EOS Transactions of the American Geophysical Union. 2013;94:409-410. DOI: 10.1002/2013EO45000\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Pier Luigi Bragato",address:"pbragato@inogs.it",affiliation:'
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Namık Çağatay",authors:[{id:"138405",title:"Prof.",name:"M. Namik",middleName:null,surname:"Çagatay",fullName:"M. Namik Çagatay",slug:"m.-namik-cagatay"},{id:"290307",title:"Dr.",name:"Özlem",middleName:null,surname:"Bulkan",fullName:"Özlem Bulkan",slug:"ozlem-bulkan"},{id:"290457",title:"MSc.",name:"Bilgehan",middleName:null,surname:"Toksoy",fullName:"Bilgehan Toksoy",slug:"bilgehan-toksoy"}]},{id:"66126",title:"Fingerprinting Sources of the Sediments Deposited in the Riparian Zone of the Ruxi Tributary Channel of the Three Gorges Reservoir (China)",slug:"fingerprinting-sources-of-the-sediments-deposited-in-the-riparian-zone-of-the-ruxi-tributary-channel",signatures:"Zhonglin Shi, Dongchun Yan, Anbang Wen and Yongyan Wang",authors:[{id:"290401",title:"Dr.",name:"Zhonglin",middleName:null,surname:"Shi",fullName:"Zhonglin Shi",slug:"zhonglin-shi"},{id:"292470",title:"Dr.",name:"Dongchun",middleName:null,surname:"Yan",fullName:"Dongchun Yan",slug:"dongchun-yan"},{id:"292825",title:"Prof.",name:"Anbang",middleName:null,surname:"Wen",fullName:"Anbang Wen",slug:"anbang-wen"},{id:"292827",title:"Dr.",name:"Yongyan",middleName:null,surname:"Wang",fullName:"Yongyan Wang",slug:"yongyan-wang"}]},{id:"66184",title:"A Long-Term Prediction of Beach Changes around River Delta using Contour-Line-Change Model",slug:"a-long-term-prediction-of-beach-changes-around-river-delta-using-contour-line-change-model",signatures:"Takaaki Uda, Shiho Miyahara, Toshiro San-nami and Masumi Serizawa",authors:[{id:"13491",title:"Dr.",name:"Takaaki",middleName:null,surname:"Uda",fullName:"Takaaki Uda",slug:"takaaki-uda"},{id:"122917",title:"Dr.",name:"Masumi",middleName:null,surname:"Serizawa",fullName:"Masumi Serizawa",slug:"masumi-serizawa"},{id:"287386",title:"Ms.",name:"Shiho",middleName:null,surname:"Miyahara",fullName:"Shiho Miyahara",slug:"shiho-miyahara"},{id:"288256",title:"Mr.",name:"Toshiro",middleName:null,surname:"San-Nami",fullName:"Toshiro San-Nami",slug:"toshiro-san-nami"}]},{id:"67292",title:"The Role of Mangroves in Coastal and Estuarine Sedimentary Accretion in Southeast Asia",slug:"the-role-of-mangroves-in-coastal-and-estuarine-sedimentary-accretion-in-southeast-asia",signatures:"Punarbasu Chaudhuri, Subhamita Chaudhuri and Raktima Ghosh",authors:[{id:"216896",title:"Dr.",name:"Punarbasu",middleName:null,surname:"Chaudhuri",fullName:"Punarbasu Chaudhuri",slug:"punarbasu-chaudhuri"},{id:"290438",title:"Ms.",name:"Raktima",middleName:null,surname:"Ghosh",fullName:"Raktima Ghosh",slug:"raktima-ghosh"},{id:"290966",title:"Dr.",name:"Subhamita",middleName:null,surname:"Chaudhuri",fullName:"Subhamita Chaudhuri",slug:"subhamita-chaudhuri"}]}]}]},onlineFirst:{chapter:{type:"chapter",id:"62594",title:"Surface Modification of Fe3O4 as Magnetic Adsorbents for Recovery of Precious Metals",doi:"10.5772/intechopen.79586",slug:"surface-modification-of-fe3o4-as-magnetic-adsorbents-for-recovery-of-precious-metals",body:'\n
\n
1. Introduction
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Magnetic materials that are paramagnetic, ferrimagnetic, and ferromagnetic have received much attention because of their unique properties especially ready to modify and nontoxic [1, 2]. Magnetite (Fe3O4), one of many magnetic materials, is widely investigated for possible magnetic resonance imaging, sensor, and adsorbent. Magnetic nanoparticles typically consist of a magnetic core, a coating, and, in some cases, surface active modifiers.
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The magnetite nanoparticles have a high surface area that yields numerous active sites. However, preparation of Fe3O4 nanoparticles is problematic since it can agglomerate, which leads to the decrease in the active sites. Coating with organic or inorganic surfactants is one way to avoid the particle agglomeration. The organic surfactants act as capping agents, but at times, they can give bigger particle size. Inorganic capping agent such as silica (SiO2) has exceptional physical and chemical properties. SiO2 is chemically stable in acidic solution and tuneable for modification. Coating of Fe3O4 nanoparticles with SiO2 will also avoid the agglomeration and protect them from dissolution in acidic solution. SiO2 will cover the surface of each Fe3O4 nanoparticle to form Fe3O4/SiO2 nanoparticle core-shell system [3].
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Morel et al. have coated Fe3O4 particles with SiO2 to form core-shell having nanometer scale with an average diameter of 49 nm [4]. The success of Fe3O4/SiO2 core-shell nanoparticle formation depends on the size of magnetite. However, stirring with the magnetic bar during the preparation causes condensation and agglomeration of the particles. The nonmagnetic mechanical stirring method was chosen for the preparation of Fe3O4 nanoparticle [5].
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Many researchers used thiol group as an adsorbent for [AuCl4]− ion with a better performance [2, 3, 6, 7, 8, 9]. We have reported on the synthesis of the Fe3O4/SiO2 nanoparticle core-shell modified with a thiol group. The Fe3O4/SiO2 nanoparticle core-shell preparation was performed by applying nonmagnetic stirring method. For improving adsorption capacity, modification with thiol group has been conducted. The thiol groups are of the soft bases.
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On the other hand, the [AuCl4]− ions are classified as weak acid species, thus provided specific interaction with each other based on Pearson’s hard-soft acid-based concepts [10]. The adsorption kinetics, adsorption capacity, and interaction model for the adsorption of [AuCl4]− ion in solution by Fe3O4/SiO2 nanoparticle core-shell adsorbent are reported. A recent review of the matter can be found elsewhere [11].
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Figure 1 shows the schematic architecture of the magnetite-silica-functional groups. The core is magnetite to function as the important part for separation. The shell is silica, which can protect the magnetite from dissolution especially when it contacts with an acidic environment. Modification of the silica surface can be realized by silanization to give functional groups having an important function to react with the metal cations. The functional group must have a strong bond with the surface via complex formation.
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Figure 1.
Step-by-step of Fe3O4@SiO2 core-shell preparation and functionalization [3].
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Recovery of the magnetic material is key in the process following the adsorption. The spent adsorbent can be separated using a magnetic field. Figure 2 shows how the used magnetic is separated by the external magnetic field. The magnetic adsorbent that has a high content of rare metals can be subject to dissolution and further separation. It is important to state that in the industrial purpose the powerful electromagnet system can be applied to do the job. In the purification, there are many possible green purification processes of metallurgy, starting from electrochemical separation to blast furnace.
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Figure 2.
Image of simplified recovery technique of spent magnetic material after adsorption of precious metals [3].
\n
\n
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2. Preparation of Fe3O4
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Magnetite is commonly prepared by co-precipitation of Fe(II) and Fe(III) salts with suitable bases. Sodium hydroxide and ammonia are both commonly used in the preparation of magnetite. There are many bases that can be used to help control the size and the shape of the particles. Magnetite nanoparticles can be prepared in the presence of carboxylate such as laurate, palmitate, linoleate, and so on. The addition of surfactant helps reduce the particle size and control the shape. The required shape is usually spherical with a diameter of the nanoscale.
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For co-precipitation methods, the size, shape, and composition of the resulting nanoparticles very much depend upon the following [12]:
The type of precursors’ salts used, for example, chloride, sulfate, perchlorate, or nitrate
The Fe2+/Fe3+ ratio
The mixing orders
The mixing rates
The reaction temperature
The pH value
The ionic strength of the media
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The remaining issue is that magnetite nanoparticles are easily oxidized to maghemite, so this method is often used to obtain nanoparticles of magnetite and maghemite with the small size of 4–20 nm. Grüttner et al. have listed the size, coating, heating behavior, and magnetic properties of some iron oxide nanoparticles produced by this method [13]. Nanoparticles are produced by this method range in size from 4 to 45 nm. For fixed-synthesis conditions, the quality of the magnetite nanoparticles is very reproducible. Although co-precipitation is unquestionably the easiest process and highly scalable, it is not without issues. Controlling the shape is not easy, and the nanoparticles can be more varied in size than that produced in some other methods [12].
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Precursors for the Fe(II) include ferrous sulfate, ferrous nitrate, and ferrous chloride. Some use ferrous acetate and ferrous oxalate. The most used precursor is ferrous sulfate. For the Fe(III), we can use ferric chloride, ferric nitrate, and so on. Ferric nitrate is used a lot. Ferric acetate and ferric oxalate are also commonly used as Fe(III) precursors.
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The Fe(II) to Fe(III) molar ratio must be controlled strictly at 1:2. Therefore, the concentration of the starting material must be fixed. The oxidation of the Fe(II) ion must be contained by controlling the atmosphere by the use of inert atmosphere. During the co-precipitation, the nitrogen gas must be kept flowing to reduce possible oxidation process. Other noble gases could be used, which give a better magnetite product.
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There are various ways to prepare Fe3O4 nanoparticles, such as hydrothermal synthesis [14], co-precipitation [15], microwave irradiation [16], oxidation of Fe(OH)2 by H2O2 [17], and microemulsion [18]. The Fe3O4 nanoparticles synthesized by a hydrothermal method in the presence of sodium sulfate have a particle size of 160 nm [14]. Among various ways to prepare Fe3O4, hydrothermal is one of the simple methods because it gives unique characters. The shape and size of nanoparticles have a good homogeneity and high degree of crystallinity [19].
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The widespread method to produce Fe3O4 is by co-precipitation of Fe2+/Fe3+ solution mixture with a molar ratio of 1:2 in alkaline solution [15, 20]. The reaction for Fe3O4 formation by co-precipitation method is shown in chemical Eq. (1). Although this method is well known for synthesis Fe3O4, the molar ratio of reactant, pH, and temperature still need attention to get the proper size and morphology [15]:
Microwave irradiation might be a promising method in processing materials due to its thermal and nonthermal effects. Microwave synthesis has the advantages of short reaction time, small particle size, and narrow size distribution. Aging under microwave irradiation in short period yields Fe3O4 nanoparticles with complete crystalline structure than those aged for 7 days at room temperature [16]. Yu et al. used H2O2 as an oxidizing agent to construct nano-sized superparamagnetic Fe3O4 powders with the size of 8–10 nm. The Fe(OH)2 precipitates were partially oxidized to generate ultrafine Fe3O4 nanoparticles in the presence of surfactants [17]. Work on the control of the size of magnetite-silica via sol–gel method has also been reported [21].
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Some researchers use capping agent to control crystal growth during Fe3O4 nanoparticle formation. Co-precipitation technique was used to prepare magnetite nanoparticles with diameter around 35 nm using 0.90 M NaOH solution as the precipitating agent and trisodium citrate as a capping agent. The precursors are ferric and ferrous chloride salts with predetermined Fe3+/Fe2+ molar ratio. The diameter of silica-coated magnetite nanoparticles synthesized by Stöber method was about 50 nm. Due to an electrostatic interaction between the Fe3+/Fe2+ ions of the Fe3O4 NPs and trisodium citrate surfactant, a stable magnetic fluid containing dispersed Fe3O4 NPs was produced [22]. A green and facile method for synthesis of magnetite nanoparticles was proposed [23]. Nano-sized polyhedral particles were synthesized by heating an aqueous solution of Fe2+, Fe3+, and urea at 85°C. The use of PVA in the synthesis system gives spherical magnetite nanoparticles with loose structure, unaggregated. The size of the microspheres can be tuned by changing the concentration of PVA. Upon addition of acetic acid to the system with PVA, microspheres with looser structure were produced. The size of the microspheres can further be tuned by changing the concentration of acetic acid. The co-precipitation of Fe2+ and Fe3+ in aqueous solutions under ultrasound irradiation results in smaller Fe3O4 NPs with a narrow size distribution (4–8 nm) than that produced without ultrasound irradiation [4]. Diethylene glycol (DEG) is also possibly used to control the particle size as reported earlier. This surfactant takes an important role in the preparation of magnetite/zinc oxide hybrid material [24].
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3. Coating of Fe3O4 with SiO2
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The next step is coating magnetite with silica (SiO2). It is usually performed via silanization reaction. The functional group that is ready to bond to iron oxide is methoxy silane (CH3-O-Si-) or ethoxy silane (CH3-CH2-O-Si-). After the reaction, it forms a covalent bond of Fe-O-Si leaving the end group remains free. The leaving group is methane and ethane. The reaction is better to be done in an organic solvent. The silane group may have a spacer of long ethylene chain (-CH2−). The ending of the silane may be carboxylic, an amine group, hydroxyl, and so on. The surface of the silica has different accesses to the organic functional groups [25].
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For example, modification by the use of 3-mercaptopropyltrimethoxysilane (3-MPTS) [3] reaction is depicted as a chemical reaction (2). For further surface modification, we can use other silanization compounds [3]:
Iron oxide is not stable in acidic condition. After coating with silica, the magnetite core is usually stable in the acidic solution. It will come readily with a proton to give its corresponding ion either Fe2+ or Fe3+. Dissolution of the magnetite will make the core-shell system unstable and break the bond between Fe-O-Si. To make sure that the magnetite is not dissolved in the acidic solution, we can test it by the use of an acid such as hydrochloric acid or nitric acid. The concentration of total iron as Fe2+ or Fe3+ can be an indicator if the magnetite is still strong. If high concentration of Fe3+ is found in the solution, we can say that the magnetite structure is collapsed and even broken down.
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The visual indication can be seen from the color of the dispersion of Fe3O4@SiO2 core-shell. The solution of Fe3+ in the solution is pale yellow. If the dispersion color is pale yellow, it can be concluded that magnetite does dissolve. The color is getting dark when the more magnetite dissolved in the dispersion. A combination of atomic absorption spectrometry and visual observation helps us make sure the magnetite core is still strongly intact.
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Fe3O4/SiO2 core-shell nanoparticles were obtained by dispersing Fe3O4 into the mixture solution of 80 mL of ethanol, 20 mL of deionized water, and 1.0 mL of concentrated aqueous ammonia solution (28 wt.%). After this, the mixture solution was homogenized by ultrasonication for 30 min to form a uniform dispersion. Subsequently, a certain amount of tetraethoxysilane (TEOS) was added dropwise into the solution with vigorous stirring. After stirring at room temperature for 6 h, the product was separated with a magnet bar, washed with deionized water for three times, and dried in vacuum at 50°C for 12 h. A series of SiO2@Fe3O4 particles were prepared with 1–9% SiO2 content [26].
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The silica coating used on a core particle has several advantages. The essential advantages of the silica coating compared with another inorganic (metal or metal oxide) or organic coating are as follows: It reduces the bulk conductivity and increases the suspension stability of the core particles. Also, silica is the most chemically inert material available; it can block the core surface without interfering in the redox reaction at the core surface [27]. There are two methods for coating Fe3O4 with silica, by acidic hydrolysis of silicate in aqueous solutions and the modified Stöber process [4, 28].
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The Stöber method consists of the alkaline hydrolysis of tetraethyl orthosilicate (TEOS) in ethanol/water mixture in the presence of Fe3O4 NPs [28]. The Stöber process is applied to the classic sol–gel process [29]. The Stöber synthesis has the advantage of being easy to scale up for commercial applications and the possibility to effortlessly transfer the nanoparticles into aqueous solutions [30]. Some methods that lead to the synthesis of Fe3O4/SiO2 are shown in Table 1.
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Core
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Shell
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Method
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Precursors
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Method
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Basic reagent
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Wet chemical reaction
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FeCl3, N2H4
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Sol–gel
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TEOS
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Wet chemical reaction
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FeCl3, FeSO4
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Hydrolysis
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Na2SiO3
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Wet chemical reaction
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FeCl3, FeSO4
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Hydrolysis
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Commercial SiO2
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A chemical reaction in microemulsion
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FeCl3, FeSO4
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Sol–gel reaction in microemulsion
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TEOS
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Table 1.
Methods for synthesis of Fe3O4 coated with SiO2.
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About the modification and application of magnetic materials, a coating of Fe3O4 by the use of various materials has been reported elsewhere. TiO2@Fe3O4, TiO2@Fe3O4@chitosan, and methyl pyrazolone-functionalized TiO2@Fe3O4@chitosan were prepared for photocatalytic degradation of dyes [32]. They found that the core is important for separation and the shell is an active catalyst. The degradation of dye using these catalysts can reach up to 98–99%.
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Thioctic acid-modified silica-coated magnetite nanoparticles, RS-SR-NH-SiO2@Fe3O4, have been prepared, and its ability for the recovery of Au(III) in aqueous solutions was evaluated [31]. The Au(III) adsorption capacity of the produced adsorbent is about 25 mg/g. The possible interaction is shown in Figure 3. Another study shows the success of recovery of gold from copper anode slime by means of magnetite nanoparticles [33]. The surface of magnetite was also modified with oleic acid, methyl methacrylate, and ethylenediamine (EDA-MMA-OA@ Fe3O4) giving the adsorption of indium of about 54 mg/g [34].
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Figure 3.
Possible interaction between RS-SR-NH-SiO2@Fe3O4 and au(III) ions [31].
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An interesting example of functionalization of Fe3O4 is by the use of dithiocarbamate, and it is applied as a magnetic nano-adsorbent for recovery of precious metal nanoparticles by contacting the nano-adsorbent with Au, Ag, Pd, or Pt hydrosols [35]. The magnetic particles are very efficient for Au due to strong affinity of sulfur-containing groups at the magnetite surfaces with this metal. Since Au colloids are used in laboratory and industrial contexts, the material could have an impact on the development of nanotechnology to recover precious metals like Au [35] and Ag. Another trial is modification using chitosan and EDTA. It shows more selective for the quasi-precious metal of Cu than Cd and Pb [36].
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4. Surface functionalization of Fe3O4@SiO2−X
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In reaction (1), we can see the steps of surface modification of Fe3O4@SiO2 core-shell to form Fe3O4@SiO2−X, where X is a functional group. The layer of SiO2 was usually coated on the surface of Fe3O4 using the Stöber method. The prepared Fe3O4 nanoparticles were used as cores and dispersed in ethanol, and it was added to a three-neck round-bottom flask in ethanol and deionized water. The solution of the concentrated ammonia solution was added. After 15 min, TEOS was added dropwise in 10 min. The mixture was allowed for mechanical stirring for 8 h to perform the silica coating. The produced Fe3O4@SiO2 was separated and washed with deionized water and ethanol [37].
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Direct modification by the use of organic compound is also studied, without first modification by silica. Magnetic nanoparticles modified with third-generation dendrimers followed by ethylenediaminetetraacetic acid (EDTA) were prepared and tested for their performance for recovery of precious metals that are Pd(IV), Au(III), Pd(II), and Ag(I) in the aqueous system [38]. It is interesting that high valence Pd(IV) and Au(III) exhibit relatively better adsorption efficiency than that of Pd(II) and Ag(I) with lower valence. It suggests that the adsorption of precious metals by this type of materials modified with EDTA is a function of valence. When the competing ion such as Zn(II) presents, the adsorption efficiency of the adsorbent for all four precious metals, which are Pd(IV), Au(III), Pd(II), and Ag(I), reduces much.
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Magnetite nanoparticles could be directly modified with an organic compound of oleic acid. Iron oxide surface possibly bonds to carboxylic end of lauric acid [21]. However, this method of functionalization might not produce an acid-resistive magnetic adsorbent. The bond between lauric acid and magnetite could be easily damaged when the acidic solution is used. Therefore, the magnetite modified with lauric acid may find application in biological systems since both lauric acid and magnetite are biocompatible.
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Silane compound such as (3-aminopropyl)trimethoxysilane (APTMS) could be used to coat magnetite nanoparticles. The product can be described as Fe3O4@SiO2-CH3-NH2. Further surface modification by alginate gives Fe3O4@SiO2-CH3-NH2-AA. The alginate forms the outer shell of the magnetite by electrostatic interaction with amine [39]. Figure 1 shows a step-by-step extension of magnetite coating and functionalization. Silica coating will allow further functionalization via silanization, extension (additional of the spacer), and functional group attachment. The functional groups should be free to bond the metal ion either by an ionic or covalent coordination bond. Directed functional groups allow selective reaction with certain cation.
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5. Characterization
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Characterization of the magnetite can be done by at least five methods, which are vibrating sample magnetometer, powder X-ray diffraction, electron microscopy, elemental analysis, and infrared (IR) spectroscopy. The vibrating sample magnetometer (VSM) can reveal the magnetic properties of the magnetic materials. The microscopic images can be obtained commonly by the use of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic force microscopy (AFM). Nanomaterials are best to characterize by TEM and AFM. The IR spectroscopy is useful to detect the functional groups present on the magnetite surface. The IR spectroscopy is one of the methods to make sure that functionalization of the surface is successful.
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For elemental analysis, a nondestructive energy dispersive X-ray spectrometry (EDS) can be used to estimate the chemical composition. The SEM is usually equipped with EDS system. The EDS results may lack precision and accuracy; however, it can detect the chemical composition in situ. The destructive methods such as atomic absorption spectrometry, UV–Vis spectrometry, and so forth may be used in place of EDS method. The destructive methods are usually not of choices for this type of materials.
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One major analytical method in the magnetite characterization is powder X‐ray diffraction. Figure 4 shows the XRD patterns of Fe3O4 and Fe3O4/SiO2 solid nanoparticle core-shell. The Fe3O4 diffraction patterns have five main peaks at 2θ values of 30.1°, 35.5°, 43.3°, 57.1°, and 62.5°. The Fe3O4 has a cubic system as confirmed by JCPDS Card No. 88–0315. The magnetite phase can be detected with certainty by XRD. However, when it is coated with silica, the intensity of the XRD peaks will be much diminished since silica is an amorphous solid. Further decrease in the XRD is expected after organic modification on top of the silica layer.
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Figure 4.
XRD patterns of Fe3O4 (top) and Fe3O4/SiO2 nanoparticle core-shell modified with a thiol group (bottom) [3].
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The FT-IR could also be useful for more characterization of magnetic materials. It can offer details of the bond between the core, the shells, and the surface modifiers. Here is the example, the FT-IR spectra of Fe3O4 and Fe3O4/SiO2 nanoparticle core-shell are presented in Figure 5. Both spectra have a broad peak at 586 cm−1. The peak is attributed to the Fe-O stretching mode of magnetite. The peak at 3400 cm−1 is due to the O-H stretching mode. The sharp peak at 1100 cm−1 can be attributed to the Si-O-Si stretching mode. The Si-O bending vibration mode of the silanol group is seen at 964 cm−1. It indicates that the silica has coated well the outer surface of Fe3O4 particles [3]. The surface modification of Fe3O4/SiO2 nanoparticles by thiol groups can give a better interaction with [AuCl4]− ions in the solution. The FT-IR spectra of the Fe3O4/SiO2 nanoparticle core-shell after modification with thiol group are shown in Figure 5. The peak at 686 cm−1 is attributed to the C-S bending vibration mode. The peak at near 2570–2590 cm−1 is attributed to the stretching vibration mode of S-H. The S-H stretching vibration mode is not usually detected [2]. The band at around 2850–2900 cm−1 is due to the stretching vibration of C-H of methylene. This result suggests that the surface modification of Fe3O4/SiO2 nanoparticle core-shell is successful.
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Figure 5.
FT-IR spectra of resulted Fe3O4 (a), Fe3O4/SiO2 nanoparticle core-shell (b), and Fe3O4/SiO2 nanoparticle core-shell modified with a thiol group (c) [3].
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The covering of Fe3O4 nanoparticle core-shell by using silica does not only protect the magnetite core from dissolution in acid but also control the agglomeration of Fe3O4 particles. Silica acts as a capping agent for each Fe3O4 nanoparticle to form Fe3O4/SiO2 core-shell. Figure 6 shows the TEM images of Fe3O4/SiO2 nanoparticle core-shell. The Fe3O4/SiO2 nanoparticle core-shell has a size of approximately 10–20 nm. The size of Fe3O4/SiO2 core-shell can be observed. These results prove that the synthesis of Fe3O4/SiO2 nanoparticle core-shell is successful.
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Figure 6.
TEM image of Fe3O4/SiO2 nanoparticle core-shell [3].
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In situ analysis of adsorbent is preferable to understand the chemical composition of the product without a change in its nature. Figure 7 shows the EDX spectra of modified Fe3O4/SiO2 solid nanoparticle core-shell. The sulfur content is 1.32% (w/w). It suggests that thiol group is present on the surface of Fe3O4/SiO2 nanoparticle core-shell material. It confirms the FT-IR spectra. The modification of Fe3O4/SiO2 solid nanoparticle core-shell by 3-MPTS will give free thiol groups on the nanoparticles’ surface. The thiols are expected to form covalent coordination bond with the target ion.
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Figure 7.
EDX spectra of Fe3O4/SiO2 nanoparticles modified with thiol group [3].
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The EDX may also give details of atomic mapping across the sample, especially that of the functional group. For example, sulfur atom in the thiol group is mapped by the EDX method nicely. Functional groups such as amine, thiol, sulfonate, and phosphate may be better detected by EDX rather than destructive methods such as UV–Vis spectrophotometry.
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6. Adsorbent performance
\n
Table 2 shows a comparison of adsorbent performance for adsorption of precious metals especially gold and palladium [3, 38]. The first two rows show the adsorption performance of magnetic material modified with thiol and dendrimers. It shows that functionalization of the magnetite is very important to increase the adsorption capacity. Thiol group on the surface of magnetite produces high affinity toward Au(III). As we know, thiol can strongly react with gold to form a covalent bond. However, the adsorption capacity of magnetite is still far below that of adsorbent produced by the use of lignin as a precursor.
Comparison of adsorption capacities (qmax) of some adsorbents for selected precious metals from aqueous solution. Data presented here are based on the Langmuir isotherm.
\n
An adsorbent of magnetic nanoparticles modified by thiourea for effective and selective adsorption of precious metals like gold(III), palladium(II), and platinum(IV) in aqueous acid solution has also been reported. It needs contact time of less than 30 min to reach maximum capacity. Its maximum adsorption capacity of precious metals as determined by Langmuir model was 43.34, 118.46, and 111.58 mg/g for Pt(IV), Au(III), and Pd(II), respectively, at pH 2 and 25°C [40]. The adsorption is selective for Au(III) even in the presence of high concentrations of interfering ion Cu(II). The recycling was achieved by the use of a solution containing 0.7 M thiourea and 2% HCl. The result of the adsorption–desorption test shows that the adsorbent is reusable for the recovery of precious metals.
\n
In general, the adsorption capacity of the magnetite-based adsorbent can reach up to 118.46 mg/g, which is very promising. It may still be less than that of lignin derivatives. For chitosan-modified magnetite, it even can reach the capacity for gold(III) of 707 mg/g [41]. The core‐shell‐modifier based adsorbent may not have such a high adsorption capacity. The modification step was done through the reaction between chitosan and polymeric Schiff’s base of thiourea/glutaraldehyde in the presence of magnetite.
\n
After adsorption test, desorption of the adsorbed cation must also be examined. Complete desorption of the adsorbed cation indicates a better adsorbent performance. In most cases, the acids can desorb adsorbed ion from the surface. The desorption process may use strong acids such as HCl, H2SO4, and HNO3. The cation is believed to form complex coordination bonds with the surface, and leaching them is difficult.
\n
On the other hand, application of concentrated acid solution may damage the structure of adsorbent. Therefore, mildly acidic solutions are usually employed to release the cation from the adsorbent’s surface. People use a complexing agent to release the adsorbed metal cations. Thiourea and EDTA are of important environmentally friendly complexing agents.
\n
Thiourea solution in 1 M HCl was employed to liberate [AuCl4]− ions that had been adsorbed by the material [3]. Thiourea has a better affinity than that of thiol and amine groups. It can form a complex ion with [AuCl4]− ion to dissolve back into the solution. According to the HSAB theory, both thiol and [AuCl4]− ion are among the weak bases. A strong coordination bond forms between thiourea and [AuCl4]− ion.
\n
Figure 8 depicts the curve of desorption of [AuCl4]− ion by thiourea in 1 M HCl solution at various concentrations following adsorption by the magnetite modified with a thiol group. Dilute thiourea solution can only desorb 43 mg/g [AuCl4]− ion of initially adsorbed 68 mg/g or 60% of the total [AuCl4]− ions bond to the surface. Figure 9 displays schematic adsorption of [AuCl4]− ion by magnetite modified with a thiol group and desorption. The desorption is done by applying thiourea in HCl solution. The concentration of the thiourea is low. The thiol group may form a covalent coordination bond with [AuCl4]− ion on the adsorbent surface.
\n
Figure 8.
Profile of [AuCl4]− ion desorption by HCl/thiourea at various concentration [3].
\n
Figure 9.
Adsorption and desorption of AuCl4− ions by magnetite nanoparticles modified with a thiol group [3].
\n
\n
\n
7. Summary
\n
Modified magnetic adsorbents have been synthesized and used in the recovery of precious metals from aqueous solutions. Among the magnetic materials, magnetite is studied widely. Surface modification of nanoscale magnetite core is crucial to have a better adsorption capacity, stability, and turnover. The key issues of the magnetic adsorbent include size and shape of the core, choice of surface modification, adsorption capacity, stability, and recyclability. The size of the magnetite core is also better if it is in the nanoscale rather than in micron scale. It will improve the contact between pursued ions and adsorbent surface. The surface modification must have a good affinity toward certain precious metal cations. Many researchers attempt to combine adsorption capability and magnetic properties of the magnetite-based adsorbent for certain metal recovery from the solution. Selective adsorbents are also of interest for separation of precious metals from a complex system such as industrial waste. Adsorption selectivity is highly considered for complex matrices. Magnetite core has low stability in strongly acidic aqueous media. Coating with silica has two advantages, for protection against the acidic environment and a binding site for further functionalization. A suitable modification of the magnetic particles by coating or functionalization using inorganic components or organic molecules is usually needed.
\n
The synthesis of magnetite as the core material has been established. The use of salts of Fe(II) and Fe(III) with careful stoichiometric calculation is a must. The pH of the magnetic formation should also be controlled, either by the use of sodium hydroxide or ammonia solution. In many cases, ammonia can give better homogeneous particles. It may be better to add a stabilizing agent for reducing aggregation of the magnetite nanoparticle and improve the stability of the colloid. Coating of magnetite with silica has also been well understood. TEOS and TMOS are the main choices for the outer shell of the magnetite, although sodium silicate may work. Silica is a preferable coating since it is resistant to acid and base, which will protect the magnetite core.
\n
The final surface modification is functionalization of the silica with ligands that will strongly bind the cations. The end of the modification chain must have a special interaction with the cations, especially through coordination bonds. The functional groups could be an amine, carboxylate, thiol, sulfonate, amide, hydroxyl, and so on. Based on reagent availability, the functional groups determine the selectivity toward certain precious metal cations.
\n
The release of the adsorbed metal cations after being concentrated in the adsorbent can be realized using acids and strong complexing agents. The acids are usually not desirable since they can cause the magnetite core to dissolve. Dissolution will damage the structure of the magnetite, which may not be possible to reuse. Complexing agents such as thiourea and EDTA can give a better option to minimize the damage to the magnetite-based adsorbents.
\n
Purification of the recovered metals may be done through well-known processes. Electrochemical process is the best choice of metallurgy. Other methods by the use of chemical reduction could also be selected. In the large scale, we can consider blast furnace combined with a redox reaction. One important point to consider, the use of environmentally friendly reprocessing of the metals must always be prioritized.
\n
\n
\n
8. Future recommendation and direction
\n
The conventional metal reprocessing uses chemicals that are not environmentally friendly. The magnetite-based adsorbents offer technology that can reduce the application of toxic chemicals. The adsorbents give the possibility to reduce, reuse, and recycle for a few times. The magnetic core of the adsorbent is also readily synthesized with environmentally benign precursors. The coating with silica protects against acid and base media during application and recycle. The silica coating can also facilitate the attachment of the functional groups, which is critical in the modification step.
\n
The current advanced electronic devices utilize the precious metals in their important components. The waste of electronic devices grows rapidly along with an increase in smartphone and PC use. Computer parts like processors, memories, motherboards, hard drives, and CD/DVD drives contain gold and other precious metals such as silver, palladium, and so on. The conventional gold recovery process uses cyanide ions for complex ion formation and electrolysis. The current technology attempts to recover gold and other precious metals from computers’ and smartphones’ components by utilizing magnetite nanoparticles. The new magnetic materials are effective yet environmentally friendly to recover precious metals. The magnetic adsorbents could also be the future of reclaiming precious metals from the waste of the other industries.
\n
In the magnetic adsorbent development, the magnetite core could be possibly substituted with other oxides of transition metals such as manganese, cobalt, or nickel if they maintain strong magnetic characters. However, silica is the main choice for easy coating of the magnetic core, which also helps protect the magnetic core from dissolution in the acidic and basic media. The presence of the ligands on the surface of the magnetite-silica core-shell is critical for adsorption process. The environmentally safe polymers and simple molecules may be used to facilitate coordination bond with the target cations. The desorption process must be done using suitable solutions. The solution for desorption should leave the adsorbent in good shape for further reuse and turnover. The present technology available for purification of the recovered metals may apply electrochemical, chemical, and thermal processes.
\n
\n
Symbols and abbreviations
AFM
atomic force microscopy
APTMS
aminopropyl trimethoxysilane
DEG
diethylene glycol
EDTA
ethylenediamine tetraacetate
EDA-MMA-OA
ethylenediamine, methyl methacrylate, and oleic acid
EDX
energy dispersive X-ray spectroscopy
JCPDS
Joint Committee on Powder X-ray Diffraction Standards
MPTS
mercaptopropyltrimethoxysilane
NPs
nanoparticles
PVA
polyvinyl alcohol
qe
maximum capacity of adsorbent (mg/g)
SEM
scanning electron microscopy
TEOS
tetraethyl orthosilicate
TEM
transmission electron microscopy
VSM
vibrating sample magnetometer
\n',keywords:"magnetic nanoparticle, recovery, silica, precious metal, adsorption, desorption",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/62594.pdf",chapterXML:"https://mts.intechopen.com/source/xml/62594.xml",downloadPdfUrl:"/chapter/pdf-download/62594",previewPdfUrl:"/chapter/pdf-preview/62594",totalDownloads:1059,totalViews:413,totalCrossrefCites:2,dateSubmitted:"March 12th 2018",dateReviewed:"June 18th 2018",datePrePublished:"November 5th 2018",datePublished:"November 14th 2018",dateFinished:null,readingETA:"0",abstract:"Magnetic nanoparticles such as magnetite have been studied intensively for their unique properties that are susceptible to a magnetic field, ready to coat with silica and able to modify with a variety of functional groups. The magnetite-silica core-shell system offers flexibility for extensive modification. The magnetic core is also important in the separation by the use of a magnetic field. The shell, meanwhile, is needed for protection of the magnetic core and further modification. Functional groups at the surface shell are critical in the reaction with target precious metal ions during application. In this contribution, we will have a comprehensive look at the preparation, characterization, and use of the magnetite core-shell modified with functional groups as a magnetic adsorbent. After adsorption, the materials together with the ions can be recovered by the use of magnet before further separation and purification.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/62594",risUrl:"/chapter/ris/62594",signatures:"Roto Roto",book:{id:"7471",title:"Advanced Surface Engineering Research",subtitle:null,fullTitle:"Advanced Surface Engineering Research",slug:"advanced-surface-engineering-research",publishedDate:"November 14th 2018",bookSignature:"Mohammad Asaduzzaman Chowdhury",coverURL:"https://cdn.intechopen.com/books/images_new/7471.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"185329",title:"Prof.",name:"Mohammad Asaduzzaman",middleName:null,surname:"Chowdhury",slug:"mohammad-asaduzzaman-chowdhury",fullName:"Mohammad Asaduzzaman Chowdhury"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:null,sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Preparation of Fe3O4",level:"1"},{id:"sec_3",title:"3. Coating of Fe3O4 with SiO2",level:"1"},{id:"sec_4",title:"4. Surface functionalization of Fe3O4@SiO2−X",level:"1"},{id:"sec_5",title:"5. Characterization",level:"1"},{id:"sec_6",title:"6. Adsorbent performance",level:"1"},{id:"sec_7",title:"7. Summary",level:"1"},{id:"sec_8",title:"8. Future recommendation and direction",level:"1"},{id:"sec_11",title:"Symbols and abbreviations",level:"1"}],chapterReferences:[{id:"B1",body:'Haw CY et al. Hydrothermal synthesis of magnetite nanoparticles as MRI contrast agents. Ceramics International. May 2010;36(4):1417-1422\n'},{id:"B2",body:'Zhang S et al. Thiol modified Fe3O4@SiO2 as a robust, high effective, and recycling magnetic sorbent for mercury removal. Chemical Engineering Journal. Jun. 2013;226:30-38\n'},{id:"B3",body:'Roto R, Yusran Y, Kuncaka A. Magnetic adsorbent of Fe3O4@SiO2core-shell nanoparticles modified with thiol group for chloroauric ion adsorption. 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Catalysis Today. 2011;175(1):293-298\n'},{id:"B27",body:'Ghosh Chaudhuri R, Paria S. Core/shell nanoparticles: Classes, properties, synthesis mechanisms, characterization, and applications. Chemical Reviews. 2012;112(4):2373-2433\n'},{id:"B28",body:'Stober W, Fink A. Controlled growth of Monodispersed silica spheres in the Micron size range. Journal of Colloid and Interface Science. 1968;26:62-69\n'},{id:"B29",body:'Liu J et al. Extension of the stöber method to the preparation of monodisperse resorcinol-formaldehyde resin polymer and carbon spheres. Angewandte Chemie, International Edition. 2011;50(26):5947-5951\n'},{id:"B30",body:'Gholami T, Salavati-niasari M, Bazarganipour M. Superlattices and microstructures synthesis and characterization of spherical silica nanoparticles by modified Stöber process assisted by organic ligand. Superlattices and Microstructures. 2013;61:33-41\n'},{id:"B31",body:'Abd Razak NF, Shamsuddin M, Lee SL. Adsorption kinetics and thermodynamics studies of gold(III) ions using thioctic acid functionalized silica coated magnetite nanoparticles. Chemical Engineering Research and Design. 2018;130:18-28\n'},{id:"B32",body:'Abdelwahab NA, Morsy EMH. Synthesis and characterization of methyl pyrazolone functionalized magnetic chitosan composite for visible light photocatalytic degradation of methylene blue. International Journal of Biological Macromolecules. 2018;108:1035-1044\n'},{id:"B33",body:'Ranjbar R, Naderi M, Omidvar H, Amoabediny G. Gold recovery from copper anode slime by means of magnetite nanoparticles (MNPs). Hydrometallurgy. 2014;143:54-59\n'},{id:"B34",body:'Chiou CS, Chuang KJ, Chen HW, Chen YC. Magnetite modified with amine polymer to adsorb indium ions. Powder Technology. 2015;279:247-253\n'},{id:"B35",body:'Lopes JL, Marques KL, Girão AV, Pereira E, Trindade T. Functionalized magnetite particles for adsorption of colloidal noble metal nanoparticles. Journal of Colloid and Interface Science. 2016;475:96-103\n'},{id:"B36",body:'Ren Y, Abbood HA, He F, Peng H, Huang K. Magnetic EDTA-modified chitosan/SiO2/Fe3O4 adsorbent: Preparation, characterization, and application in heavy metal adsorption. Chemical Engineering Journal. 2013;226:300-311\n'},{id:"B37",body:'Habila MA, Alothman ZA, El-Toni AM, Labis JP, Soylak M. Synthesis and application of Fe3O4@SiO2@TiO2 for photocatalytic decomposition of organic matrix simultaneously with magnetic solid phase extraction of heavy metals prior to ICP-MS analysis. Talanta. 2016;154:539-547\n'},{id:"B38",body:'Yen CH, Lien HL, Chung JS, Der Yeh H. Adsorption of precious metals in water by dendrimer modified magnetic nanoparticles. Journal of Hazardous Materials. 2017;322:215-222\n'},{id:"B39",body:'Yang L et al. Modification and characterization of Fe3O4 nanoparticles for use in adsorption of alkaloids. Molecules. 2018;23:562\n'},{id:"B40",body:'Lin TL, Lien HL. Effective and selective recovery of precious metals by thiourea modified magnetic nanoparticles. International Journal of Molecular Sciences. 2013;14(5):9834-9847\n'},{id:"B41",body:'Donia AM, Atia AA, Elwakeel KZ. Recovery of gold(III) and silver(I) on a chemically modified chitosan with magnetic properties. Hydrometallurgy. 2007;87(3-4):197-206\n'},{id:"B42",body:'Chang YC, Chen DH. Recovery of gold(III) ions by a chitosan coated magnetic nano-adsorbent. Gold Bulletin. 2006;39(3):98-102\n'},{id:"B43",body:'Parajuli D, Kawakita H, Inoue K, Funaoka M. Recovery of gold(III), palladium(II), and platinum(IV) by aminated lignin derivatives. Industrial and Engineering Chemistry Research. 2006;45(19):6405-6412\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Roto Roto",address:"roto05@ugm.ac.id",affiliation:'
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada, Yogyakarta, Indonesia
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Open Access publishing helps remove barriers and allows everyone to access valuable information, but article and book processing charges also exclude talented authors and editors who can’t afford to pay. The goal of our Women in Science program is to charge zero APCs, so none of our authors or editors have to pay for publication.
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