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Article

Chemical and Thermal Changes in Mg3Si2O5 (OH)4 Polymorph Minerals and Importance as an Industrial Material

by
Ahmet Şaşmaz
,
Ayşe Didem Kılıç
* and
Nevin Konakçı
Department of Geological Engineering, Fırat University, Elazığ 23119, Türkiye
*
Author to whom correspondence should be addressed.
Appl. Sci. 2024, 14(22), 10298; https://doi.org/10.3390/app142210298
Submission received: 12 September 2024 / Revised: 13 October 2024 / Accepted: 6 November 2024 / Published: 8 November 2024
Browse Figures
Versions Notes

Abstract

:
Serpentine (Mg3Si2O5(OH)4), like quartz, dolomite and magnesite minerals, is a versatile mineral group characterized by silica and magnesium silicate contents with multiple polymorphic phases. Among the phases composed of antigorite, lizardite, and chrysotile, lizardite and chrysotile are the most prevalent phases in the serpentinites studied here. The formation process of serpentinites, which arise from the hydrothermal alteration of peridotites, influences the ratio of light rare earth elements (LREE) to heavy rare earth elements (HREE). In serpentinites, the ratio of light rare earth elements (LREE)/heavy rare earth elements (HREE) provides insights into formation conditions, geochemical evolution, and magmatic processes. The depletion of REE compositions in serpentinites indicates high melting extraction for fore-arc/mantle wedge serpentinites. The studied serpentinites show a depletion in REE concentrations compared to chondrite values, with HREE exhibiting a lesser degree of depletion compared to LREE. The high ΣLREE/ΣHREE ratios of the samples are between 0.16 and 4 ppm. While Ce shows a strong negative anomaly (0.1–12), Eu shows a weak positive anomaly (0.1–0.3). This indicates that fluid interacts significantly with rock during serpentinization, and highly incompatible elements (HIEs) gradually become involved in the serpentinization process. While high REE concentrations indicate mantle wedge serpentinites, REE levels are lower in mid-ocean ridge serpentinites. The enrichment of LREE in the analyzed samples reflects melt/rock interaction with depleted mantle and is consistent with rock–water interaction during serpentinization. The gradual increase in highly incompatible elements (HIEs) suggests that they result from fluid integration into the system and a subduction process. The large differential thermal analysis (DTA) peak at 810–830 °C is an important sign of dehydration, transformation reactions and thermal decomposition, and is compatible with H2O phyllosilicates in the mineral structure losing water at this temperature. In SEM images, chrysotile, which has a fibrous structure, and lizardite, which has a flat appearance, transform into talc as a result of dehydration with increasing temperature. Therefore, the sudden temperature drop observed in DTA graphs is an indicator of crystal form transformation and CO2 loss. In this study, the mineralogical and structural properties and the formation of serpentinites were examined for the first time using thermo-gravimetric analysis methods. In addition, the mineralogical and physical properties of serpentinites can be recommended for industrial use as additives in polymers or in the adsorption of organic pollutants. As a result, the high refractory nature of examined serpentine suggests that it is well-suited for applications involving high temperatures. This includes industries such as metallurgy and steel production, glass manufacturing, ceramic production, and the chemical industry.

1. Introduction

Anatolia, located in the Alpine orogenic belt on the southern branch of the Neotethys, consists of ultramafic rocks spread over wide areas (Figure 1). The study area (Alacakaya-Elazıg) on the Eastern Anatolian fault zone bears traces of serpentinization, carbonation, ophicalsite formations and lisvenitization, developed under the influence of tectonism. The ocean, which was formed in the Middle–Upper Triassic by the rifting of the Cimmerian Continent surrounding Turkey, was most extensive in the Jurassic–Lower Cretaceous. In the Upper Cretaceous, the southern branch of the Neotethys disappeared by diverting towards the north. The ophiolites, which were first settled towards the end of the Cretaceous, continued to settle towards the south with Eocene–Miocene compressional tectonics [1,2].
Serpentinite is a metamorphic rock composed mostly of serpentine group minerals such as lizardite, antigorite and chrysotile. This rock, which has fascinating shades of green, is usually banded or layered. These minerals are formed through the hydration of olivine-(Mg2+, Fe2+)2 SiO4 in silica-poor serpentinites at relatively low temperatures [3]. The formation of antigorite, lizardite and chrysotile minerals by the crystallization of structurally different serpentine B polymorphs constitutes the serpentinization process [4,5,6,7,8]. Low-grade serpentinites include lizardite and chrysotile [8]. Current studies [6,8] show that serpentinization occurs due to the hydration effect in the initial phase, with an approximately 20–40% volume increase. The serpentine minerals, especially fibrous B polyform (chrysotile), break as the serpentinite does not expand to cover the increase in volume [9,10,11,12].
Serpentinization is a process characterized by reduction–oxidation and dissolution–precipitation reactions when ultramafic rocks are exposed to water and fractured at the crustal level. When primary silicates transform into serpentines, the density varies between 3.3 and 2.7 g/cm3, and there is a significant increase in volume [13,14,15,16,17,18]. Evans et al. [4] indicated a direct connection between serpentinization and arc magmatism. Previous studies have stated that ocean floor spreading is the only pathway for the hydrothermal alteration of serpentinites in ultramafic rocks in the mantle. The combination of magnetite and antigorite is only possible in ocean floor serpentinization. This serpentinization produces serpentine minerals, Fe–Ni alloys, magnetite, alkaline solutions and gases (H2, CH4) [11,12,13]. Studies on Mg-rich olivine (forsterite) indicate that precipitations of magnetite (Fe3O4) form along the crystallite boundaries, similar to those observed in volcanic olivines at 600–900 °C HTA under an O2 environment [14]. Complex phase changes between silicates and Fe oxides, including the formation of magnetic FeO, are likely to occur [15]. During serpentinization, water is consumed, but no significant dissolved components other than H2 are released [16,17,19]. The hydration of mantle peridotite with seawater causes the oxidation of Fe in primary minerals (pyroxene and olivine) to Fe (III) in secondary phases, following the reaction 2FeO + H2O = Fe2O3 + H2 [18]. The main hosts of ferric Fe are magnetite, Fe3+2Fe2+O4 and Fe3+-serpentine minerals. This is due to the high-T regime, characterized by the rapid diffusion rates of Fe–Mg above 400 °C, and thermodynamic equilibrium can only be reached above 600 °C [19]. Ulmer and Trommsdorff [20] stated that serpentine minerals, with a total weight of ~13% H2O, are important in the water cycle in subduction zones and in the melting of heat flow in the mantle wedge.
Serpentinite can be used in different areas (construction, ceramics, agriculture, mining, steel, etc.) due to its physical properties, especially the presence of high Mg and Si concentrations, as well as its surface properties [21]. The serpentinite group is a potential source due to the high magnesium content of the protolith. Today, the use of serpentinites in agriculture is being investigated in countries with temperate climates. Some studies have been conducted to evaluate serpentinite minerals’ performance as agricultural and magnesium fertilizers. For example, a study conducted in New Zealand evaluated the performance of serpentinites and dunites as magnesium sources [22]. Another study examined the effects of serpentinite magnesium fertilizer on feed efficiency [23] and Błońska et al. [24] examined the effect of serpentinite soil on nutrients in Poland. Luz et al. [25] evaluated the agricultural potential of serpentinites in Brazil, and Carmignano et al. [26] the performance of serpentinites in soybean crops. Blaskowskı et al. [27] investigated the agricultural potential of mining wastes consisting of dunite and serpentinite. Serpentine lizardite is used as an additive in ceramic and glass production due to its resistance to high temperatures. It can be used in construction materials, especially stone blocks and paving materials [28]. Chrysotile has been widely used in thermal insulation and fire-protection applications. As regards mechanical and industrial applications, chrysotile has been used in a variety of industrial applications, especially where heat and wear resistance are required. Chrysotile is frequently used as a firefighting material [29]. It is used in the automotive industry, in brake pads and clutch systems [30], and as an insulation material in electrical devices to provide heat and wear resistance [31]. One of the countries that uses chrysotile the most to produce friction materials is Iran (2000 tons every year) [32]. Chrysotile is used as a filler for asphalt pavement and resin plastics on traffic roads. In industrial applications, chrysotile is used by combining it with phenolic polypropylene and plastics in heating systems and industrial furnaces, coatings, packaging materials, aircraft wing fuel tanks, rocket tail nozzle tubes, rocket ablation prevention materials. Chrysotile’s many industrial applications include the following: 80% is used for construction materials, asbestos sheet and cement products; 7% is used for friction materials; and a usage of <3% has been reported for chrysotile textiles [33]. In building materials, chrysotile can be used as ceiling flooring, roof tiles, sound insulation boards, house panels, pipe insulation and wall panels. Additionally, various chrysotile cement products are also used today [34]. Similarly, it is used to produce vitrified materials and for cathode ray tube (CRT) glass parts [35]. In terms of environmental benefits and safety, alternative asbestos materials are among the most researched topics today to avoid the use of chrysotile [36].
Serpentinites are distributed across various regions worldwide, with global reserves estimated to be in the hundreds of millions of tons. Serpentinite reserves can be found in Australia, Paraguay, Italy, New Zealand, Russia, Canada, the USA, Brazil and Türkiye [37,38]. There are serpentinite and serpantinize ultramaphites within the Guleman, Koçali and Kömürhan ophiolites on the Eastern Anatolian Fault zone (Figure 1).
This study aimed to determine microstructural characterization and the petrographic, geochemical properties, geotectonic environments of the Guleman ophiolite serpentinites used in contemporary fields such as agriculture, industry, automotives, etc.

2. Materials and Methods

Twenty-five representative samples were collected from the Guleman ophiolite for petrographic and geochemical studies. After petrographic investigations conducted in the Geology Engineering laboratories of Fırat University (Elazığ-Türkiye), samples showing a high degree of serpentinization were prepared for geochemical analysis. Serpentine mineral species were identified under a Leitz brand polarizing microscope (Leitz, Oberkochen, Germany).
Serpentinite, which has industrial importance, was examined as a novel material. The ICP-MS NexION 2000 (Perkin Elmer Inc., Shelton, CT, USA) device, which includes a quartz nebulizer gasifier, cyclonic spray circle and an integrated autosampler, was used for oxide and elemental analyses of the samples. After the rock sample was crushed into a powder using a mortar in the laboratory, it was placed in 18.3 MΩ ultrapure water. The precipitated particles were separated, and the sample was weighed in a solution containing 1% hydrochloric acid–ultrapure water. Approximately 0.5 g of the sample was mixed with each 1% hydrochloric acid–ultrapure water solution. Cem brand Mars 6 One Touch (CEM Corporation, Matthews, NC, USA) was transferred to Teflon microwave containers and pre-pared in the microwave by adding 10 mL of concentrated nitric acid to each sample. ICP-MS calibration solutions were prepared by diluting commercially available multi element standards with 1% (nitric acid–ultra pure water) at the concentrations specified in Table 1. Additionally, ICP-MS calibration was performed before each measurement. For the control of elemental analyses, 100 ppb 45Sc, 89Y, 209Bi was used as the internal standard. The results obtained are listed in Table 1.
DTA/TG, SEM and XRD analyses of the selected samples were performed in Erzincan Binali Yıldırım University Physics laboratory (Türkiye). Serpentine samples were ground in 75 micras mesh. The powdered sample was compressed into a container made of an inert material (platinum). DTA analyses used alumina powder as an inert reference material. A heating rate of 20 °C, maximum temperature of 900 °C and air/argon/N2 atmosphere was used in the tests.
High-resolution scanning electron microscopy was used to analyze the microstructural properties of the samples. Electron microscope images were taken directly from the external surfaces of the samples. Fresh samples were prepared for SEM analyses. The other 5 faces were turned into smooth surfaces so that the broken surface was protected. This process was carried out at Erzincan Binali Yıldırım University Faculty of Science Center. These samples were then coated with gold under vacuum in the SEM laboratory of EBYU Department of Physics (Türkiye). SEM analyses were performed using a QUANTA FEG 450 model electron microscope (Thermo Fisher Scientific, Eindhoven, The Netherlands). Granular structures could be clearly observed in the SEM photographs. SEM microphotographs of samples partially doped with Ag instead of Bi at different magnifications have been taken. Fibrous, plate or needle-like structures can be seen in the serpentinites [15,39].
X-Ray diffraction patterns were examined to determine the serpentine types. The abbreviation JCPDS stands for “Joint Committee on Powder Diffraction Standards”, which refers to a database containing X-Ray diffraction data for various materials. XRD (X-Ray diffraction) analysis enables the determination of the mineralogical structure of materials by comparing the results with the cards in this database. In summary, JCPDS cards serve as standard references for identifying specific crystal structures and compositions [16]. The JCPDS card numbers for serpentinite minerals are as follows: Lizardite is JCPDS 14-177, Chrysotile is JCPDS 14-116, and Antigorite is JCPDS 19-131 [17]. This was confirmed by XRD using an SC-70 detector operating at 15 mA and 40 kV at EBYU.

3. Findings

The serpentinites found in ultramaphites belonging to the Guleman ophiolite in the study area, comprising the Elazığ-Alacakaya district on the Alpine orogenic belt, were massive, and exhibited the mesh and bastite textures typical of hydrated oceanic peridotites [3,22], intersected by multiple generations of serpentine veins (Figure 2A,C). In the samples, they were revealed to be predominantly grayish to dark greenish, medium- to coarse-grained, and characterized by interlocking textures (Figure 2B,D). Many samples displayed crude foliation with shear planes, along with lineation marks (slickensides) and remnants of serpentine patches on their surfaces.
In the samples examined, serpentinization was almost complete, and primary mineral inclusions (pyroxene, olivine, spinel) were rarely observed. Olivine and/or pyroxene were accompanied by iron oxides distributed heterogeneously within the network fabric. Spinels were frequently oxidized (Figure 3). The partial preservation of the original mesh texture of the main minerals (olivine and orthopyroxene) shows that the temperature was not very high, and the serpentinized parent rock had a high mafic mineral content. The orthopyroxene was replaced with chrysotile, forming a network around the relic minerals [7,13,21,26] (Figure 3). The hydration of the orthopyroxe mineral was pseudo-morphic. The serpentine, which was determined to have a reticular texture, and lizardite were the products of the serpentinization of orthopyroxene, since the rock was chrysotile and predominantly lizardite (SiO2 < 44% at lizardite–chrysotile). The SiO2 content of the samples was <44%, and the SEM images show chrysotile+lyzarite. The combination of these two minerals indicates a temperature of approximately 400 °C. Also, morphologically speaking, serpentinites exhibit a platy or flaky habit, are often fibrous, have a soapy texture, and are predominantly composed of chrysotile and lizardite. Dehydration during formation at high temperatures can lead to talc formation. The typical pseudomorphs may change as the processes of metamorphism and shearing progress. Lizardite is occasionally found in elongated patches aligned parallel to the slip direction along the foliation (Figure 3), while chrysotile has a typical fibrous appearance.

3.1. Geochemistry

The bulk chemical composition of the investigated serpentinites featured low contents of SiO2 (39.52% on average) and TiO2 (0.1–0.2% by weight), high MgO (36.67% average) and Na2O (0.1% on average) contents, and Al2O3 contents that were moderate to high (0.3 to 16.9 wt.%) (Table 1). The CaO content was high, at 1.70% on average. The substitution of Mg with Fe in antigorite, in contrast with the exclusive presence of Mg in pure lizardite, underscores the findings that lizardite is more conducive to carbonation compared to antigorite [10,28]. The total Fe2O3 content was also high (5–10.6 wt.%) (Table 1). The Mg/Si ratio of serpentinite samples was between 1.18 and 1.38 (~1.33) and Mg# [Mg/(Mg + Fe)] 0.78 and 0.92, indicating that mantle peridotites in MOR (Mg# 0.89–0.92) feature a different formation environment, or that the environment has changed in subsequent processes. The total Ni content of the samples was 1001–2033 ppm.
The analysis results are listed in Table 1 and Table 2. The ΣREE values of serpentinites varied between 2.51 and 3.42 ppm. While the ΣLREE contents ranged from 1.58 to 2.67 ppm, the ΣHREE contents ranged from 0.87 to 0.96 (Figure 4a,b) (Table 2). The ΣLREE/ΣHREE ratios were between 1 and 3, with Ce showing a strong negative anomaly (0.1–12) and Eu shooing a weak positive anomaly (0.1–0.3) (Figure 4b). The presence of these elements indicates rock–water interaction during serpentinization, and the evidence of the gradual release of highly incompatible elements (HIEs) indicates functions resulting from fluid integration into the system and following a subduction process [23]. Furthermore, the positive Eu anomaly can also be attributed to the formation of lizardite during ocean serpentinization or the dissolution of plagioclase in hydrothermal fluid circulation [25,26]. This suggests that oceanic serpentinization fluid leaches Eu during fluid–rock interaction, rather than reacting with the plagioclase of the serpentinites [29,30,31]. The enrichment in LREE and HREE ratios occurs after melting or during melting due to the interactions with liquid [29]. The moderate siderophiles Ni and Co [30], highly siderophile elements Pd, Pt, Cs and Zr [31], and elements such as F, As, Cl and Sb are found in serpentinites, which shows fluid interaction between the subducted crust and sediments during the hydration of peridotites [32,33,34,40].
The analyzed samples were serpentines derived from harzburgite (olivin and orthopyroxene in thin sections). The REE compositions of these samples show a compatible distribution (Figure 4a). The REE values of the samples were above ~0.1. While Nd, Ce and Tb showed negative anomalies, the Pr, Eu, Tm and La contents showed positive anomalies in the chondrite diagram. Finally, the serpentinites were depleted or enriched in LREE (from ~0.1 to 100 CI-Chondrite) and had HREE contents varying from 0.1 to ~10 CI-Chondrite. The REE distributions of these serpentinites, which are rich in trace elements (U, K, Cs, Rb), are compatible with the characteristics of subduction zone serpentinites (~100 PM; Figure 4). In addition, serpentinites can be divided into abyssal, mantle wedge and subduction zone according to their formation environments. The amount of Ti is an important indicator for determining the protoliths of serpentinites. Another feature of subduction-zone serpentinites is high Ti (30–500 ppm), Yb (0.02–1 ppm) and Mg (>0.4 ppm) values [34,35]. These features are compatible with the analyzed Elazığ serpentinites (Ti 30–66 ppm, Yb 0.1–0.3 ppm, Mg 0.70–0.83 ppm) (Table 1).
LREE enrichment indicates that the serpentinites did not undergo partial melting but were formed by melt/rock interaction, and/or were enriched in the subduction zone by fluids during hydration [5,41,42,43,44,45,46,47,48]. At the same time, these serpentinites were rich in Pb. The fact that this feature, described by Niu [49] in mantle wedge serpentinites and Tonga fore-arc peridotites, is also observed in subduction serpentinites shows that it originates from depleted basaltic magma, as well as abyssal and mantle wedge peridotites. Rock interactions led to a strong enrichment in U. Most of our examples indicated similar behaviors. In geology, chromatographic processes generally concern the separation and analysis of minerals and elements. This process, which is a laboratory technique, is used in the analysis of geological samples. It is important for the separation and analysis of minerals and elements, and the detection of contamination. The percolation of silicate melts through mantle peridotite, whether by reactive porous flow or the chromatographic process (fractionation), results in the enrichment of light rare earth elements (LREE), as well as incompatible elements such as Th and U [38]. Considering the incompatible elements, it can be said that the melt/rock interaction occurring before serpentinization affects the geochemical composition of serpentinites. Trace element enrichments probably originate from the passive continental margin [34]. This is because, at both passive margins, there are high incompatible trace element concentrations due to fluid remixing and smaller partial melting via metasomatizing melts before serpentinization [39,50]. The MgO-SiO2, MgO-Fe2O3 and Ni-Ce diagrams show that the serpentinites examined are lizardite and chrysotile, and that these minerals are accompanied by talc (Figure 5). The serpentinites showed a mineral assemblage of olivine, chrysotil, lizardite, magnetite, brucite, chlorite, talc and carbonate. In the primitive mantle normalized trace element variation diagrams for forearc and MOR serpentinites, enrichments in U, Sb, Rb, Pb, Sr and Li, compared to elements with similar compatibility, characterize subduction zone serpentinites (Figure 4). Strong enrichments in large ion lithophile elements (LILE), especially Cs and Rb (Figure 4), are also similar to what is found in forearc serpentinites. At the same time, trace element patterns normalized to the flat primitive mantle with positive U, Rb, Sm and Ti anomalies indicate the interference of fluids in the subduction zone and forearc region (Figure 4b). Also, some MOR serpentinites show a positive Eu anomaly EuN/EuN* (0·655 × 9). However, most of the incompatible trace elements (Nb, Th and Ce) are present in extremely low amounts [36]. The compositional values of serpentinites depend on their characteristics, as shown in the literature [35,36,37,38,39,40,51] (Figure 5).

3.2. Microstructure Characteristics (SEM, TG, DTA)

The thermal decomposition of brucite, first with the release of physical water, causes a continuous mass loss until around 500–550 °C [37,38,39,40,52]; then, the dehydroxylation of layered silicates and the disruption of the crystal lattice occur [43,53]. Another significant thermogravimetric analysis (TGA) confirmed mass loss. The endothermic peak in the differential thermal analysis (DTA) curve and the major exothermic derivative (DTG) peak occurred between 610 and 700 °C (Figure 6). Sharp and highly exothermic DTA peaks at approximately 810–830 °C indicate the formation of new minerals such as olivine, pyroxene forsterite or enstatite [40,41,42,46]. In the case of sample 6, similar TGA steps are seen, except that the second step is divided into two steps, with an extra step forming between 610 °C and 650 °C. Also, in sample 6, the sharp and high exothermic DTA peak after 810 °C disappeared (did not form), so no new mineral formation occurred in this sample.
The SEM images of the samples are given in Figure 7. Sample 2 contained Fe, Si, Al, Mg, O and C. Sample 5 contained Fe, Ca, Si, Mg and O, and sample 6 contained Fe, Si, Al, Mg and O. When we compare the samples to each other, the atomic percentages of both Mg and O are high compared to other elements. All the samples contained Fe, Si, Mg and O elements in their structures. The SEM images of samples show chemical color contrasts between dark and very compatibly colored schist serpentine minerals and light gray serpentinite clasts. The SEM examinations show the morphology and changes of serpentine crystals with small crystal sizes (0.1–0.3 µm), depicted in Figure 7a–c. As shown in Figure 7a, chrysotile consists of thin and flexible fibrils with a length/diameter ratio of >3 [38], and lizardite has a plate-like morphology, as shown in Figure 7c. The X-Ray diffraction patterns are shown in Figure 8. When the analysis results are evaluated, the types of serpentine minerals can be identified as lizardite, a small amount of chrysotile, and forsterite. The X-Ray results support those of EDX analyses.

4. Discussion and Conclusions

Residual mantle peridotites or ultramafic cumulates protoliths serpentinites is located in orogenic zones. These serpentinites consist of abyssal peridotites and mantle wedge peridotites; the protolith of Guleman serpentinites contains traces of primary orthopyroxene and olivine [45]. These residual minerals (olivine and orthopyroxene in Figure 3) indicate that the protoliths of the serpentinites were mantle peridotite dunite or harzburgite. Serpentine group minerals are formed by the hydration of silica poor olivine/pyroxene minerals at relatively low temperatures.
In serpentinites, there is a linear relationship between alteration mineralogy and texture. One of the specific features demonstrating this relationship is the bastite texture (in harzburgite) formed by the serpentinization of orthopyroxene [46]. Another feature is the lizardite vein networks with relict olivine cores, which are also observed in the Guleman serpentinites (Figure 3).
When examining the results of whole-rock analyses presented in Table 1, the LOI (loss on ignition; wt.%) values of the serpentine samples range from 8% to 11% (Sp1–Sp9), indicating a high degree of serpentinization, which is consistent with the observed excessive serpentinization and the presence of mesh texture (Table 1, Figure 3). Guleman serpentinites are refractory serpentinites; high MgO (usually >35 wt.%; Table 1), high Mg# (78–82), low Al2O3/SiO2 (<0.01) and high MgO/SiO2 (0.6–0.95) show that it is high. Major element compositions show that the examined serpentinites are similar to the major element compositions of forearm/mantle wedge serpentinites and abyssal plate serpentinites, except for their refractory properties [54], because abyssal plate serpentinites exhibit higher FeO, lower SiO2, MgO and Al2O3 contents compared to forearc/mantle wedge serpentinites. According to studies [5,6,7,8,9,10,26], a high MgO value indicates lizardite, while chrysotile develops along the cracks. In a geological environment, Mg/Si varies between 1.18 and 1.38 (~1.33 ppm), the Mg# [Mg/(Mg + Fe)] values vary around 78–82, and the Ti value is >100 ppm, indicating the presence of subduction-zone serpentinites [30]. The ΣREE values in the analyzed serpentinites are 1–44 ppm, while the ΣLREE values are 0.8–6.22 ppm and ΣHREE values are 0.6–38 ppm. The ΣLREE/ΣHREE ratios are 0.16–4 ppm. Additionally, the negative Ce anomaly (0.1–12 ppm) and the weakly positive Eu anomaly (0.1–0.3 ppm) are caused by the interaction between fluids and rock. Highly incompatible elements are an indication of fluid integration into the system during subduction [23]. In particular, elements such as U, K, Cs, and Rb are highly present in these serpentinites (~100 PM). The ΣREE values of the samples are between 1–44, the ΣLREE value is between 0.8–6.22, and the ΣHREE contents are between 0.6–38. The ΣLREE/ΣHREE ratios are 0.16–4 and high Ce (0.1–12) shows a weakly positive Eu anomaly (0.1–0.3). These features indicate fluid intrusion into the rock structure during serpentinization, during which highly incompatible elements (HIEs) are gradually introduced into the serpentinization process. Additionally, as regards LREE enrichment, it was found that serpentinites do not undergo partial melting and structural changes with melt/rock interactions, and that the Pb content is high in serpentinites exhibiting this feature. All data show that the compositions of the examined samples are quite similar to the compositions of the mantle wedge/back rocks, but are contaminated by subduction components.
The samples presented characteristics favorable to industrial raw materials when they were evaluated in terms of MgO content (36.67% on average) and SiO2 content (high at 35–43). In the MgO–SiO2–H2O–CO2 equilibrium system, the equilibrium temperatures required for the serpentinization reaction and the presence of chrysotile minerals (record-ed by SEM, TG and XRD analyses) are approximately 350–425 °C, depending on the pressure (Pf-PH2O). Guleman serpentinite samples are industrially durable serpentinites with high MgO (32–42 wt.%, except for Sp 01) and low Al2O3 contents (0.4–6.9 wt.%; Table 1). As a result, in the experimental studies, serpentinization temperatures for chrysotile were found to be 350–425 °C, depending on the pressure, lizardite and chrysotile were stable at temperatures below <400–440 °C, and antigorite developed at higher temperatures. So, serpentine minerals may feature areas of gradual stability depending on their composition (Fe and Al amounts), oxygen fugacity (Fe2+, Fe3+) and H2O activity [18,55,56,57].
Figure 7 shows SEM images of the examined samples, showing that the serpentinite minerals are less chrysotile and predominantly lizardite. SEM images of the examined samples and MgO-SiO2, MgO-Fe2O3 and Ni-Ce diagrams also confirm the presence of chrysotile and lizardite minerals.
The large DTA peak in sample 2 at 810–830 °C is a sign of dehydration, transformation reactions and thermal decomposition. Serpentine minerals, which are phyllosilicates containing water in their crystal structure, begin to lose water around 800 °C. This occurs as an endothermic (heat sinking) peak in the DTA. Regarding the sample examined, the XRD data show that it is forsterite (Mg2SiO4). Additionally, at such high temperatures, olivine and pyroxene forsterite, enstatite and clinoenstatite may develop [40,41,42,43,44,45,46,56]. A sudden decrease in the mass of a sample around 800 °C under thermogravimetric analysis (TG or TGA) indicates the development of a significant mass loss in the TG curve as water molecules leave the structure during dehydration. Thermal decomposition at high temperatures can cause a sudden decrease in mass. The decomposition products can often be gaseous or present in different solid phases, leading to mass loss. The presence of carbonate minerals (e.g., magnesite, MgCO3) in the serpentinite sample also makes it possible that these carbonates will thermally decompose at around 800 °C, releasing carbon monoxide (CO) and carbon dioxide (CO2) gas (Figure 6). The sudden mass loss in the TG curve can be explained as forsterite transformation or CO2 release. Similarly, the same situations apply in sample 5 and sample 6. The absence or scarcity of carbonate minerals (calcite, dolomite) in the serpentinites examined generally indicates that the XCO2 values given during serpentinization are negligibly low [5,45].
The large DTA peak in sample 2 at 810–830 °C is a sign of dehydration, transformation reactions and thermal decomposition. Serpentine minerals, which are phyllosilicates containing water in their crystal structure, begin to lose water around 800 °C. This manifests as an endothermic (heat sinking) peak under DTA.
The samples’ XRD data show that this was forsterite (Mg2SiO4). A peak at 810–830 °C on the DTA graph indicates dehydration or mineral phase transformations. At this temperature, serpentine, a hydrous phyllosilicate, is endothermic. The fact that serpentinites contain magnesite causes the release of CO2 gas through thermal decomposition at approximately 800 °C, and the sudden mass loss in the TG curve indicates the release of forsterite and CO2.
The serpentinites exhibit highly intriguing physicochemical properties and possess significant potential for application in various industrial areas. However, despite this potential, the number of studies conducted on these minerals remains relatively limited. Given the substantial reserves in Elazıg (Turkey), exploring new applications for serpentinites could give rise to important opportunities. Besides CO2 capture, utility in catalysis can also be considered, given this mineral group’s strong adsorption capacity. Chrysotile is usually present in small and harmless amounts (<5%). It has seen use in industrial applications throughout the 20th century. It shows such physical properties as flame resistance, high tensile strength, thermal insulation, and chemical resistance. It has been observed that lizardite and chrysotile, minerals derived from the serpentine group under study, are suitable for industrial use due to their high MgO and SiO2 contents.
The refractory nature of the examined serpentine typically indicates that it is suitable for high-temperature applications, especially in industries requiring high temperatures such as metallurgy and steel production, the glass industry, ceramic manufacturing, and the chemical industry. Now, chrysotile is used in various industries such as sound, heat, and fire insulation, as well as in brake linings, clutch pedals, and gasket materials. Chrysotile’s remaining uses include in friction materials (7%), textiles, and other applications (10%) [58].

Author Contributions

Methodology, formal analysis, investigation, resources, writing—original draft preparation, writing—review and editing, project administration, funding acquisition, A.Ş., A.D.K. and N.K. All authors have read and agreed to the published version of the manuscript.

Funding

This study was supported by the Fırat University with FUBAP-MF.24.49.

Data Availability Statement

The original contributions presented in the study are included in the article, further inquiries can be directed to the corresponding author.

Conflicts of Interest

The authors declare no conflicts of interest.

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Applsci 14 10298 g001
Figure 1. (A) Distribution of ophiolites (green color) in the study area and its surroundings [2]. (B) Simplified geological map [1].
Figure 1. (A) Distribution of ophiolites (green color) in the study area and its surroundings [2]. (B) Simplified geological map [1].
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Applsci 14 10298 g002
Figure 2. Serpentinite samples with mesh (A,B) and bastite (C,D).
Figure 2. Serpentinite samples with mesh (A,B) and bastite (C,D).
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Applsci 14 10298 g003
Figure 3. Optical microscope (OM) view of thin sections taken from serpentinites. Olivine (Ol) and orthopyroxene (opx) minerals surrounded by lizardite (A) and chrysotile (B).
Figure 3. Optical microscope (OM) view of thin sections taken from serpentinites. Olivine (Ol) and orthopyroxene (opx) minerals surrounded by lizardite (A) and chrysotile (B).
Applsci 14 10298 g003
Applsci 14 10298 g004
Figure 4. Chondrite (a) and primitive mantle spider (b) diagrams of serpentinites [41].
Figure 4. Chondrite (a) and primitive mantle spider (b) diagrams of serpentinites [41].
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Figure 5. Discriminating diagrams of serpentine minerals.
Figure 5. Discriminating diagrams of serpentine minerals.
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Applsci 14 10298 g006
Figure 6. The DTA and TGA thermograms of the serpentinite samples: (a) Sample 2, (b) Sample 5, (c) Sample 6.
Figure 6. The DTA and TGA thermograms of the serpentinite samples: (a) Sample 2, (b) Sample 5, (c) Sample 6.
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Applsci 14 10298 g007
Figure 7. SEM images of the serpentinite samples. (a) Sample 2, (b) Sample 5, (c) Sample 6.
Figure 7. SEM images of the serpentinite samples. (a) Sample 2, (b) Sample 5, (c) Sample 6.
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Applsci 14 10298 g008
Figure 8. Whole-rock X-Ray diffraction (XRD) spectra of selected samples.
Figure 8. Whole-rock X-Ray diffraction (XRD) spectra of selected samples.
Applsci 14 10298 g008
Table 1. Results of major oxide (%) and some trace elemental (ppm) analyses of serpentinite by LA-ICPMS.
Table 1. Results of major oxide (%) and some trace elemental (ppm) analyses of serpentinite by LA-ICPMS.
Major OxidesNa2O
(%)		MgO
(%)		Al2O3
(%)		SiO2
(%)		P2O5
(%)		K2O
(%)		CaO
(%)		TiO2
(%)		MnO
(%)		Fe2O3
(%)		LOITOTALScVCoNiCuZnGaRbSrYZrNbMoCdBaTiCrSnMnCsTa
Sp-010.322.86.937.30.11.14.50.20.3511.399.620721810014359.9101027.3192.450.13322226108141.10.2
Sp-030.138.80.540.40.10.10.10.10.17.411.8100.4412879653260.910100.220.1524932233118030.10.1
Sp-040.134.90.635.10.10.14.90.10.17.211.4100.431291972194461.110320.42.90.252<1032432106190.1<0.1
Sp-060.138.20.341.90.10.10.20.20.16.611.6100.66167515453421.710100.11.60.150.6<1036625109341.2<0.1
Sp-080.137.70.841.50.10.10.10.10.16.611.3100.2827731819426210100.21.90.151.1<1032112117220.1<0.1
Sp-090.137.20.842.10.10.10.40.10.26.69.1100.15155411974322.2101014.42.6150.8<1030201<102740.1<0.1
Sp-100.137.32.638.30.10.10.10.10.398.099.9924817275351.110101.52.70.151.6<1066772<105650.1<0.1
Sp-110.133.51.937.80.10.14.230.10.18.31.699.87339611841534110291.23.40.151.1<1033381<104150.1<0.1
Sp-120.136.70.537.10.10.12.60.10.16.73.499.8204482175724440.8101400.42.50.150.8<1034206<103240.1<0.1
Sp-140.138.50.639.30.10.110.10.1741.399.963674150317331.110200.320.151.1<1055189<102170.10.1
Sp-150.138.40.841.80.10.10.20.10.1101.399.971996203319340.810100.42.30.151.1<1058204<102190.10.1
Sp-160.137.60.8400.10.10.10.10.17.91.999.953174151312311.510100.31.90.151.3<1037311<108120.1<0.1
Sp-170.137.90.640.10.10.10.80.10.110.61.499.9122875173913290.710100.11.90.150.7<1044197<106130.10.1
Sp-180.136.20.838.40.10.12.40.10.17.91.299.8843891019113470.910102.82.60.151.5<1031312<109130.1<0.1
Sp-210.138.10.437.70.10.10.50.10.210.01.799.99268017407410.710100.21.30.150.7<1052423<105770.1<0.1
Sp-230.141.10.743.10.10.10.80.10.19.671.799.901573168711360.910100.11.60.151.1<1035178<103110.1<0.1
Sp-240.142.10.641.70.10.13.420.10.17.11.499.802791186023410.910100.61.50.150.9<1037120102930.1<0.1
Sp-250.136.73.337.40.10.15.10.10.17.82.099.80377911754282.91075.42.74.50.350.8<1033344<104350.1<0.1
Sp-270.133.83.340.00.10.110.10.19.11.499.803468132320372.118102.84.60.350.7<1034221<102090.1<0.1
Table 2. Rare earth element (ppm) analysis results of serpentinites.
Table 2. Rare earth element (ppm) analysis results of serpentinites.
Trace Elements (ppm)LaCePrNdSmEuGdTbDyHoErTmYbLu∑REE∑LREE∑HREE
Sp-010.900.480.160.340.220.110.180.180.180.080.190.050.180.043.292.390.90
Sp-030.350.270.120.380.180.120.220.220.160.090.180.040.170.052.551.640.91
Sp-040.440.420.100.360.210.110.200.180.190.100.180.040.170.042.741.840.90
Sp-060.880.320.110.370.150.130.190.210.170.090.200.050.190.043.102.150.95
Sp-080.660.440.130.420.160.120.240.160.180.080.190.040.180.053.052.170.88
Sp-090.920.420.180.380.220.130.230.190.190.070.210.040.200.043.422.670.94
Sp-100.380.300.120.360.180.100.260.170.190.080.220.050.210.052.671.700.97
Sp-110.230.310.120.440.210.120.180.180.160.080.220.040.180.042.511.610.90
Sp-120.440.400.100.350.150.130.220.160.160.090.180.050.190.042.661.790.87
Sp-140.360.290.090.340.160.140.210.200.180.080.190.040.200.052.531.590.94
Sp-150.280.300.110.450.220.130.230.180.160.090.180.050.160.052.591.720.87
Sp-160.360.310.110.420.180.120.240.220.190.090.180.040.190.042.691.740.95
Sp-170.340.330.140.430.210.120.250.160.210.090.200.050.200.052.781.820.96
Sp-180.250.280.100.440.150.140.220.170.180.090.220.050.190.052.531.580.95
Sp-210.220.300.090.460.220.110.180.200.190.080.180.040.210.042.521.580.94
Sp-230.350.300.140.380.180.130.220.180.190.080.220.050.190.052.661.700.96
Sp-240.240.340.130.360.210.120.230.190.170.100.190.040.160.052.531.630.90
Sp-250.330.320.180.430.150.110.240.210.180.090.210.050.200.042.741.760.98
Sp-270.370.280.110.410.160.120.200.180.190.080.200.050.180.052.581.650.93
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Şaşmaz, A.; Kılıç, A.D.; Konakçı, N. Chemical and Thermal Changes in Mg3Si2O5 (OH)4 Polymorph Minerals and Importance as an Industrial Material. Appl. Sci. 2024, 14, 10298. https://doi.org/10.3390/app142210298

AMA Style

Şaşmaz A, Kılıç AD, Konakçı N. Chemical and Thermal Changes in Mg3Si2O5 (OH)4 Polymorph Minerals and Importance as an Industrial Material. Applied Sciences. 2024; 14(22):10298. https://doi.org/10.3390/app142210298

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Şaşmaz, Ahmet, Ayşe Didem Kılıç, and Nevin Konakçı. 2024. "Chemical and Thermal Changes in Mg3Si2O5 (OH)4 Polymorph Minerals and Importance as an Industrial Material" Applied Sciences 14, no. 22: 10298. https://doi.org/10.3390/app142210298

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Şaşmaz, A., Kılıç, A. D., & Konakçı, N. (2024). Chemical and Thermal Changes in Mg3Si2O5 (OH)4 Polymorph Minerals and Importance as an Industrial Material. Applied Sciences, 14(22), 10298. https://doi.org/10.3390/app142210298

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