Recent Advances of Halloysite Nanotubes in Biomedical Applications.

Halloysite nanotubes (HNTs) have emerged as a highly regarded choice in biomedical research due to their exceptional attributes, including superior loading capacity, customizable surface characteristics, and excellent biocompatibility. HNTs feature tubular structures comprising alumina and silica layers, endowing them with a large surface area and versatile surface chemistries that facilitate selective modifications. Moreover, their substantial pore volume and wide range of pore sizes enable efficient entrapment of diverse functional molecules. This comprehensive review highlights the broad biomedical application spectrum of HNTs, shedding light on their potential as innovative and effective therapeutic agents across various diseases. It emphasizes the necessity of optimizing drug delivery techniques, developing targeted delivery systems, rigorously evaluating biocompatibility and safety through preclinical and clinical investigations, exploring combination therapies, and advancing scientific understanding. With further advancements, HNTs hold the promise to revolutionize the pharmaceutical industry, opening new avenues for the development of transformative treatments.

Fluorescence microscopic investigation of PCE superplasticiser adsorption in calcined clay blended cement.

Global efforts to minimise carbon dioxide emissions are also leading to attempts to use calcined clays (CC) as a partial substitute for cement in concrete. While the hydration mechanism of such CC blended cements is now well understood, the range of effective admixtures like polycarboxylate ethers (PCE) is limited. There are PCE types that promise relatively high effectiveness, but the mechanisms of action are not yet sufficiently understood. For a detailed understanding of the adsorption of such PCEs, spatially resolved studies of the binder were performed using a combination of fluorescence and scanning electron microscopy. In a comparison of two superplasticisers, the investigations have shown different sites of preferred adsorption in a CC blended system and the results can be correlated with flow tests and setting behaviour. The investigations have shown that a certain PCE type has a higher adsorption on CC and other components of a blended system in comparison to other types.

Mechanistic Implications of the Varying Susceptibility of PAHs to Pyro-Catalytic Treatment as a Function of Their Ionization Potential and Hydrophobicity.

Transition metal catalysts in soil constituents (e.g., clays) can significantly decrease the pyrolytic treatment temperature and energy requirements for efficient removal of polycyclic aromatic hydrocarbons (PAHs) and, thus, lead to more sustainable remediation of contaminated soils. However, the catalytic mechanism and its rate-limiting steps are not fully understood. Here, we show that PAHs with lower ionization potential (IP) are more easily removed by pyro-catalytic treatment when deposited onto Fe-enriched bentonite (1.8% wt. ion-exchanged content). We used four PAHs with decreasing IP: naphthalene > pyrene > benz(a)anthracene > benzo(g,h,i)perylene. Density functional theory (DFT) calculations showed that lower IP results in stronger PAH adsorption to Fe(III) sites and easier transfer of π-bond electrons from the aromatic ring to Fe(III) at the onset of pyrolysis. We postulate that the formation of aromatic radicals via this direct electron transfer (DET) mechanism is the initiation step of a cascade of aromatic polymerization reactions that eventually convert PAHs to a non-toxic and fertility-preserving char, as we demonstrated earlier. However, IP is inversely correlated with PAH hydrophobicity (log Kow), which may limit access to the Fe(III) catalytic sites (and thus DET) if it increases PAH sorption to soil OM. Thus, ensuring adequate contact between sorbed PAHs and the catalytic reaction centers represents an engineering challenge to achieve faster remediation with a lower carbon footprint via pyro-catalytic treatment.

Experimental data and modeling of sulfadiazine adsorption onto raw and modified clays from Tunisia.

In recent years, the increasing detection of emerging pollutants (particularly antibiotics, such as sulfonamides) in agricultural soils and water bodies has raised growing concern about related environmental and health problems. In the current research, sulfadiazine (SDZ) adsorption was studied for three raw and chemically modified clays. The experiments were carried out for increasing doses of the antibiotic (0, 1, 5, 10, 20, and 40 µmol L-1) at ambient temperature and natural pH with a contact time of 24 h. The eventual fitting to Freundlich, Langmuir and Linear adsorption models, as well as residual concentrations of antibiotics after adsorption, was assessed. The results obtained showed that one of the clays (HJ1) adsorbed more SDZ (reaching 99.9 % when 40 µmol L-1 of SDZ were added) than the other clay materials, followed by the acid-activated AM clay (which reached 99.4 % for the same SDZ concentration added). The adsorption of SDZ followed a linear adsorption isotherm, suggesting that hydrophobic interactions, rather than cation exchange, played a significant role in SDZ retention. Concerning the adsorption data, the best adjustment corresponded to the Freundlich model. The highest Freundlich KF scores were obtained for the AM acid-treated and raw HJ1 clays (606.051 and 312.969 Ln µmol1-n kg-1, respectively). The Freundlich n parameter ranged between 0.047 and 1.506. Regarding desorption, the highest value corresponded to the AM clay, being generally <10 % for raw clays, <8 % for base-activated clays, and <6 % for acid-activated clays. Chemical modifications contributed to improve the adsorption capacity of the AM clay, especially when the highest concentrations of the antibiotic were added. The results of this research can be considered relevant as regard environmental and public health assessment since they estimate the feasibility of three Tunisian clays in SDZ removal from aqueous solutions.

Characterization of percutaneous absorption of calcium, magnesium, and potentially toxic elements in two tailored sulfurous therapeutic peloids: a comprehensive in vitro pilot study.

Pelotherapy treatments in thermal spas, which utilize peloids composed of clay minerals mixed with saltwater or mineral-medicinal water, can have various effects on spa users, ranging from therapeutic to potential adverse reactions. Despite the widespread use of peloids, comprehensive information on the penetration and permeation of essential and potentially toxic elements into deeper layers of the skin during pelotherapy is limited. Understanding the concentrations of these elements is crucial for evaluating therapeutic benefits and ensuring safety. This study investigates the in vitro availability and absorption of calcium, magnesium, and potentially toxic elements in two peloids, considering their formulation matrix. To replicate the pelotherapy methodology, an in vitro permeation experiment was conducted using a vertical diffusion chamber (Franz cells) and a biological system with human skin membranes from five Caucasian women, age range between 25 and 51 years. The experiment involved heating the peloids to 45℃. The results emphasize the possible transport properties of chemical elements in peloids, providing valuable information related to potential therapeutic efficacy and safety considerations. Despite no apparent differences between peloids' chemical composition, the method identified permeation variations among chemical elements. The methodology employed in this study adheres to the guidelines outlined by OECD for analyzing skin absorption through an in vitro approach. Furthermore, it aligns with the associated OECD guidance document for conducting skin absorption studies. The replicability of this methodology not only facilitates the analysis of peloids pre-formulation but also provides a robust means to evaluate the effectiveness of therapeutic elements during topical administration, particularly those with potential toxicity concerns.

Dispersive Solid Phase Extraction of Melatonin with Graphene/Clay Mixtures and Fluorescence Analysis in Surfactant Aqueous Solutions.

In this work, the dispersive solid phase extraction (dSPE) of melatonin using graphene (G) mixtures with sepiolite (SEP) and bentonite (BEN) clays as sorbents combined with fluorescence detection has been investigated. The retention was found to be quantitative for both G/SEP and G/BEN 4/96 and 10/90 w/w mixtures. G/clay 4/96 w/w mixtures were selected to study the desorption process since the retention was weaker, thus leading to easier desorption. MeOH and aqueous solutions of the nonionic surfactant Brij L23 were tested as desorbents. For both clays and an initial sample volume of 25 mL, a percentage of melatonin recovery close to 100% was obtained using 10 or 25 mL of MeOH as desorbent. Further, using a G/SEP mixture, 25 mL as the initial sample volume and 5 mL of MeOH or 60 mM Brij L23 solution as the desorbent, recoveries of 98.3% and 90% were attained, respectively. The whole method was applied to herbal tea samples containing melatonin, and the percentage of agreement with the labeled value was 86.5%. It was also applied to herbal samples without melatonin by spiking them with two concentrations of this compound, leading to recoveries of 100 and 102%.

Analytical and Antimicrobial Characterization of Zn-Modified Clays Embedding Thymol or Carvacrol.

Carvacrol and thymol are broad-spectrum natural antimicrobial agents. To reduce their volatility and improve their antimicrobial performance, synergistic systems were prepared loading the active molecules in zinc-modified clays. Montmorillonite (MMT) and zeolite (ZEO) were modified with zinc ions (ZnMMT and ZnZEO), with well-known antimicrobial properties, and then with carvacrol or thymol, reaching the 26 ± 3% and 33 ± 2% w/w of loading, respectively. The resulting hybrid materials were characterized by FT-IR, XPS, XRD, TGA, and GC-MS to evaluate carvacrol/thymol release in simulating food matrices. Antimicrobial assays carried out using spoiler and pathogenic bacterial strains showed that the antimicrobial activity of both thymol and carvacrol was largely preserved once they were loaded into Zn-modified clays. However, MMT hybrids showed an antibacterial activity significantly higher than ZEO hybrids at 50 mg/mL of thymol and carvacrol. For this reason, deeper antimicrobial evaluations were carried out only for ZnMMT composites. ZnMMT loaded with thymol or carvacrol produced inhibition zones against most of the target strains, also at 3.12 mg/mL, while the positive controls represented by the single molecule thymol or carvacrol were not active. The hybrid materials can be useful for applications in which the antimicrobial activity of natural molecules need to be displayed over time as requested for the control of microbial pathogens and spoilage bacteria in different applications, such as active packaging, biomaterials, and medical devices.

Pyro-Catalytic Degradation of Pyrene by Bentonite-Supported Transition Metals: Mechanistic Insights and Trade-Offs with Low Pyrolysis Temperature.

Transition metal catalysts can significantly enhance the pyrolytic remediation of soils contaminated with polycyclic aromatic hydrocarbons (PAHs). Significantly higher pyrene removal efficiency was observed after the pyrolytic treatment of Fe-enriched bentonite (1.8% wt ion-exchanged content) relative to natural bentonite or soil (i.e., 93% vs 48% and 4%) at the unprecedentedly low temperature of 150 °C with only 15 min treatment time. DFT calculations showed that bentonite surfaces with Fe3+ or Cu2+ adsorb pyrene stronger than surfaces with Zn2+ or Na+. Enhanced pyrene adsorption results from increased charge transfer from its aromatic π-bonds to the cation site, which destabilizes pyrene allowing for faster degradation at lower temperatures. UV-Vis and GC-MS analyses revealed pyrene decomposition products in extracts of samples treated at 150 °C, including small aromatic compounds. As the pyrolysis temperature increased above 200 °C, product distribution shifted from extractable compounds to char coating the residue particles. No extractable byproducts were detected after treatment at 400 °C, indicating that char was the final product of pyrene decomposition. Tests with human lung cells showed that extracts of samples pyrolyzed at 150 °C were toxic; thus, high removal efficiency by pyrolytic treatment does not guarantee detoxification. No cytotoxicity was observed for extracts from Fe-bentonite samples treated at 300 °C, inferring that char is an appropriate treatment end point. Overall, we demonstrate that transition metals in clay can catalyze pyrolytic reactions at relatively low temperatures to decrease the energy and contact times required to meet cleanup standards. However, mitigating residual toxicity may require higher pyrolysis temperatures.

Electrochemical Kinetics and Detection of Paracetamol by Stevensite-Modified Carbon Paste Electrode in Biological Fluids and Pharmaceutical Formulations.

Paracetamol (PCT), or acetaminophen, is an important drug used worldwide for various clinical purposes. However, the excessive or indiscriminate use of PCT can provoke liver and kidney dysfunction; hence, it is essential to determine the amount of this target in biological samples. In this work, we develop a quick, simple, and sensitive voltammetric method using chemically modified electrodes to determine PCT in complex matrices, including human serum and commercial solid formulations. We modify the carbon paste electrode with stevensite monoclinic clay mineral (Stv-CPE), using cyclic voltammetry, differential pulse voltammetry, and electrochemical impedance spectroscopy to characterise and detect PCT. The kinetics study provides a better electrochemical characterisation of the electrode behaviour, finding the detection and quantitation limits of 0.2 µM and 0.5 µM under favourable conditions. Further, the best linear working concentration range is 0.6-100 µM for PCT, applying the proposed method to the quantitative determination of PCT content in reference tablet formulations and biological samples for validation.

Controversial Issues Related to Dye Adsorption on Clay Minerals: A Critical Review.

This critical review points out the most serious and problematic issues to be found in the literature on the adsorption of dyes on clay minerals. The introduction draws attention to the fundamental problems, namely the insufficient characterization of adsorbents, the influence of impurities on the adsorption of dyes, and the choice of inappropriate models for the description of the very complex systems that clay minerals and their systems represent. This paper discusses the main processes accompanying adsorption in colloidal systems of clay minerals. The relationship between the stability of the colloidal systems and the adsorption of dye molecules is analyzed. The usual methodological procedures for determining and evaluating the adsorption of dyes are critically reviewed. A brief overview and examples of modified clay minerals and complex systems for the adsorption of organic dyes are summarized. This review is a guide for avoiding some faults in characterizing the adsorption of organic dyes on clay minerals, to improve the procedure for determining adsorption, to evaluate results correctly, and to find an appropriate theoretical interpretation. The main message of this article is a critical analysis of the current state of the research in this field, but at the same time, it is a guide on how to avoid the most common problems and mistakes.

Ultrafine Kaolinite Removal in Recycled Water from the Overflow of Thickener Using Electroflotation: A Novel Application of Saline Water Splitting in Mineral Processing.

The presence of ultrafine clay particles that are difficult to remove by conventional filtration creates many operational problems in mining processing systems. In this work, the removal of clay suspensions has been investigated using an electroflotation (EF) process with titanium electrodes. The results show that EF is a viable and novel alternative for removing ultrafine particles of kaolinite-type clay present in sedimentation tank overflows with low salt concentrations (<0.1 mol/L) in copper mining facilities based on the saline water splitting concept. Maximum suspended solid removal values of 91.4 and 83.2% in NaCl and KCl solutions, respectively, were obtained under the experimental conditions of the constant applied potential of 20 V/SHE, salinity concentration of 0.1 mol/L, and electroflotation time of 10 and 20 min in NaCl and KCl solutions, respectively. Furthermore, the visual evidence of particle aggregation by flocculation during the experiments indicates a synergy between EF and electrocoagulation (EC) that enhances the removal of ultrafine particles of kaolinite.

Hotspots and Trends of Layered Double Hydroxide-based Adsorbents for Polluted Water Treatment: Insights from Bibliometric Analysis.

The use of layered double hydroxides (LDHs) as adsorbent for water treatment has been gaining relevance in recent years. In this context, this work aimed to map, through a bibliometric study, the extent of research that deals with the theme. The scientific database used was the Web of Science, and the chronology of the search consideredthe period from 1997 to 2022. The bibliometix R-package and VOSviewer software were used in this study. The searches retrieved a total of 663 documents, from 69 countries, distributed among all continents, which China (328), India (51) and Japan (40) were the most productive countries. Important journals in the environmental area and with high impact factor, such as Chemical Engineering Journal (44), Applied Clay Science (38), Journal of Hazardous Materials (35) and Chemosphere (27) most published in the area. The network of keywords used by the authors indicates that the publications retrieved deal mainly with aspects related to the efficiency of (LDHs) in the removal of different pollutants, the composition, the synthesis route and the association with other materials and/or techniques. The result of this study constitutes an important tool for directing future research on the subject.

Bioaccessibility by perspiration uptake of minerals from two different sulfurous peloids.

The risks associated with the use of peloids in thermal centers, spas, or at home, must be tested to develop appropriate safety guidelines for peloids formulations and the release of substances of high concern. Additionally, the beneficial effects of some elements on human health should be assessed to aid in interpreting the therapeutic action and effectiveness of pelotherapy on dermatological or osteomuscular disorders. Therefore, a methodology was developed to better understand the biogeochemical behavior of the elements in formulated peloids. Two peloids were formulated with the same clay and two different sulfurous mineral-medicinal waters for 90 days, with light stirring every 15 days. Bentonite clay, with a high content of smectite and Ca and Mg as the main exchangeable cations, and high heat capacity, was used. The selected mineral-medicinal waters were collected from two Portuguese thermal centers with recognized therapeutic efficacy for rheumatic, respiratory and dermatological pathologies. The peloids were used without drying and withdrawn directly from the maturation tank, and a mixture of bentonite and demineralized water was prepared as a reference sample. A stabilized, ready-to-use, artificial perspiration test was used to simulate the peloids' interaction with skin. Thirty-one elements extracted from the two prepared peloids were analyzed using ICP-MS. The data were analyzed and related to the mineralogical composition of the original clay and supernatant composition of the maturation tanks. The content of some potentially toxic elements and metals' bioaccessibility by perspiration showed very low solubility and undetectable amounts extracted from the studied samples. This analytical method provided reliable information on dermal exposure and the identification of some elements that may enter the systemic circulation, requiring implementation of surveillance and control measures.

A comprehensive review on sustainable clay-based geopolymers for wastewater treatment: circular economy and future outlook.

In the present era of significant industrial development, the presence and dispersal of countless water contaminants in water bodies worldwide have rendered them unsuitable for various forms of life. Recently, the awareness of environmental sustainability for wastewater treatment has increased rapidly in quest of meeting the global water demand. Despite numerous conventional adsorbents on deck, exploring low-cost and efficient adsorbents is interesting. Clays and clays-based geopolymers are intensively used as natural, alternative, and promising adsorbents to meet the goals for combating climate change and providing low carbon, heat, and power. In this narrative work, the present review highlights the persistence of some inorganic/organic water pollutants in aquatic bodies. Moreover, it comprehensively summarizes the advancement in the strategies associated with synthesizing clays and their based geopolymers, characterization techniques, and applications in water treatment. Furthermore, the critical challenges, opportunities, and future prospective regarding the circular economy are additionally outlined. This review expounded on the ongoing research studies for leveraging these eco-friendly materials to address water decontamination. The adsorption mechanisms of clays-based geopolymers are successfully presented. Therefore, the present review is believed to deepen insights into wastewater treatment using clays and clays-based geopolymers as a groundbreaking aspect in accord with the waste-to-wealth concept toward broader sustainable development goals.

Characterization of clay and nanoclay extracted from a semi-arid Vertisol and investigation of their carbon sequestration potential.

Mitigation of global climate change by means such as soil carbon (C) sequestration has become an important area of research. Soil organic matter (SOM) that is stabilized with clay minerals is the most persistent in soils. Currently, little is known regarding the C sequestration ability of nanoclay extracted from Vertisols in semi-arid regions. Therefore, the aim of this study was to extract and characterize nanoclay and bulk clay from a Vertisol from Iran, in terms of physicochemical surface properties and resistance of SOM to chemical oxidation. The clay fractions were studied before and after H2O2 treatment by total C analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM), dynamic light scattering (DLS), pyrolysis gas chromatography mass spectrometry (GC-MS), Fourier transform infrared (FTIR) spectroscopy, specific surface area analysis, and zeta potential. TEM and SEM images showed that the diameter of the extracted nanoclays was 16-46 nm and their morphology was more porous than bulk soil clay. The nanoclay had a much greater specific surface area (111.9 m2 g-1) than the bulk clay (67.9 m2 g-1). According to total C, FTIR, and zeta potential results, the nanoclay was enriched with 1.4 times more C than the bulk clay after peroxide treatment, indicating enhanced soil C stabilization in the nanoclay. About 45% of the peroxide-resistant SOM in the nanoclay was associated with N-containing compounds, indicating that these compounds contribute to SOM stability. The results demonstrate important role of nanoclay in soil C sequestration in Vertisols.

Environmental impacts of rare earth production.

Rare earth elements (REEs) are important raw materials for green technologies. However, REE mining and production uses techniques that are often not environmentally sustainable. Life cycle assessment (LCA) is a well-recognized method for evaluating the environmental impacts of products and technologies. This article provides an overview of the environmental impacts based on published LCA results of primary REE production. Existing major REE deposits (Bayan Obo in China, Mountain Pass in the United States, Mount Weld in Australia, ion-adsorption deposits in several Chinese southern provinces) and currently possible production routes are compared. Alternative minerals, such as eudialyte, are also discussed. The article shows which environmental effects can be minimized by technology optimization and environmental safety strategies. Additionally, some of the environmental impacts discussed, may be difficult to mitigate, as they depend on the mineral type. Activities along the complex process chain of REEs production that have particularly high environmental impacts are identified.

Properties and Mechanisms for PFAS Adsorption to Aqueous Clay and Humic Soil Components.

The proliferation of poly- and perfluorinated alkyl substances (PFASs) has resulted in global concerns over contamination and bioaccumulation. PFAS compounds tend to remain in the environment indefinitely, and research is needed to elucidate the ultimate fate of these molecules. We have investigated the model humic substance and model clay surfaces as a potential environmental sink for the adsorption and retention of three representative PFAS molecules with varying chain length and head groups. Utilizing molecular dynamics simulation, we quantify the ability of pyrophyllite and the humic substance to favorably adsorb these PFAS molecules from aqueous solution. We have observed that the hydrophobic nature of the pyrophyllite surface makes the material well suited for the sorption of medium- and long-tail PFAS moieties. Similarly, we find a preference for the formation of a monolayer on the surface for long-chain PFAS molecules at high concentration. Furthermore, we discussed trends in the adsorption mechanisms for the fate and transport of these compounds, as well as potential approaches for their environmental remediation.

Potential of montmorillonite modified by an organosulfur surfactant for reducing aflatoxin B1 toxicity and ruminal methanogenesis in vitro.

BACKGROUND: Montmorillonite clay modified by organosulfur surfactants possesses high cation exchange capacity (CEC) and adsorption capacity than their unmodified form (UM), therefore they may elevate the adverse impact of aflatoxin B1 (AFB1) on ruminal fermentation and methanogenesis. Chemical and mechanical modifications were used to innovate the organically modified nano montmorillonite (MNM). The UM was modified using sodium dodecyl sulfate (SDS) and grounded to obtain the nanoscale particle size form. The dose-response effects of the MNM supplementation to a basal diet contaminated or not with AFB1 (20 ppb) were evaluated in vitro using the gas production (GP) system. The following treatments were tested: control (basal diet without supplementations), UM diet [UM supplemented at 5000 mg /kg dry matter (DM)], and MNM diets at low (500 mg/ kg DM) and high doses (1000 mg/ kg DM). RESULTS: Results of the Fourier Transform Infra-Red Spectroscopy analysis showed shifts of bands of the OH-group occurred from lower frequencies to higher frequencies in MNM, also an extra band at the lower frequency range only appeared in MNM compared to UM. Increasing the dose of the MNM resulted in linear and quadratic decreasing effects (P < 0.05) on GP and pH values. Diets supplemented with the low dose of MNM either with or without AFB1 supplementation resulted in lower (P = 0.015) methane (CH4) production, ruminal pH (P = 0.002), and ammonia concentration (P = 0.002) compared to the control with AFB1. Neither the treatments nor the AFB1 addition affected the organic matter or natural detergent fiber degradability. Contamination of AFB1 reduced (P = 0.032) CH4 production, while increased (P < 0.05) the ruminal pH and ammonia concentrations. Quadratic increases (P = 0.012) in total short-chain fatty acids and propionate by MNM supplementations were observed. CONCLUSION: These results highlighted the positive effects of MNM on reducing the adverse effects of AFB1 contaminated diets with a recommended dose of 500 mg/ kg DM under the conditions of this study.

Longitudinal relaxation rate measurements for different signals unveiled by nutation spectroscopy: Application to the characterization of two arrangements experienced by water in a clay network.

Nutation consists in monitoring the motion of nuclear magnetization under the application of a radiofrequency (rf) field. With an appropriate amplitude of the rf field, the nutation frequency depends on the NMR relaxation times. This property offers the possibility of differentiating species having the same Larmor frequency but differing by their relaxation times. This may occur for the composite proton NMR signal of water in complex systems. Separate nutation signals are thus observed with the possibility of measuring their longitudinal relaxation times by simply applying a saturation hard pulse, followed by an evolution interval, prior to the nutation sequence. This novel experiment has been used for studying the two sites existing for water in two kaolinite samples (one hydrated after stabilization of several months and the other nonhydrated). It turns out that water in these two sites differs essentially by its transverse relaxation time. Moreover, recovery is surprisingly biexponential for these two signals. A proper analysis of results obtained by this saturation-recovery nutation experiment provides not only the specific longitudinal relaxation rates of water in these two sites but also information about the averaging which occurs at long evolution times. This is discussed with regard of the structure and organization of the clay network. In particular, from relaxation rates at short evolution times, it is shown that this network is mainly constituted of ordered platelets, with a relatively weak proportion of randomly distributed platelets.

Detection of Interlayered Illite/Smectite Clay Minerals with XRD, SEM Analyses and Reflectance Spectroscopy.

Accurate determination of clay minerals can be challenging due to the natural occurrence of interlayered phases, i.e., layers of different clay species such as illite and smectite. The overlap of peaks of the constituent minerals (e.g., illite and smectite), and the similarity of diffraction patterns when not treated with ethylene glycol, hampers identification, especially when the clay content is low. We investigated the occurrence of interlayered illite/smectite in a rock sample from Rodalquilar, Spain, using X-ray diffraction, scanning electron microscopy and reflectance spectroscopy in the short-wave infrared wavelength range. For the first time, a precise determination of interlayered I/S conducted on the extracted clay fraction treated with ethylene glycol using such different approaches was provided. X-ray diffraction results demonstrated the presence of an I/S peak at around 8.4° in the untreated fraction coupled with a peak splitting at 6.7° and 9.4° 2θ when solvated with ethylene glycol. While spectroscopy indicated the occurrence of interlayered structures as a mixture of the two constituent minerals, the results of X-ray analysis showed that the interlayered clay consisted of two discrete phases (illite and smectite). The two discrete phases were observed in both the whole rock analysis and in the extracted clay fraction. This study shows that X-ray diffraction and validation with a scanning electron microscope is a mandatory, integrating tool for detecting interlayered phases since reflectance spectroscopy alone cannot be used to differentiate between interlayered clay minerals and non-interlayered mixtures. This work highlights the limits and advantages of three sensors (X-ray diffraction, scanning electron microscopy and reflectance spectroscopy) to investigate clay mixtures and interlayering, representing a significant contribution to confidence in the interpretation of interlayered clays, this being essential in mineral exploration and prospecting.