Attapulgite Clay Research Articles

Calcined Attapulgite Clay as Supplementary Cementing Material: Thermal Treatment, Hydration Activity and Mechanical Properties

The present paper studied the effects of calcination temperatures (200–800 °C) on the appearance, mineral composition, and active SiO2 content in attapulgite and investigated the effects of attapulgite before and after calcination on the chemically bonded water content, the degree of reaction of cement paste, and the mechanical properties such as the flexural strength, compressive strength, and splitting-tensile strength of cement mortar. The results indicate that the calcination temperature changes the mineral composition of attapulgite, thereby affecting the hydration activity of cement-based materials. The attapulgite calcined at 500 °C (AT500) has the best enhancement on the hydration activity of cement-based materials. The calcination at 500 °C is most beneficial to the dissolution of SiO2, and the content of SiO2 reaches 20.96%. The contents of chemically bonded water in the samples incorporated with calcined attapulgite reduced and that of the samples incorporated with AT500 at 28 d is the same as that of the control group. The reaction degree of AT500 is 78.61% at 28 days. Calcined attapulgite clay can reduce the energy consumption of the cement industry and promote the sustainable development of attapulgite clay.

Physiological and Biochemical Mechanisms of Improving Salt and Drought Tolerance in Okra Plants Based on Applied Attapulgite Clay

Attapulgite clay (AC), which is rich in good adsorption, catalysis, rheology and heat resistance, is an important mineral resource. However, the roles of AC in regulating stress tolerance of plants have not been investigated. In this study, culture pot experiment was used to analyze the effects of AC applied into the soil on growth and physiological metabolism of okra plants. The applied AC significantly enhanced salt and drought tolerance of okra plants. Component analyses showed that the significant increases of ABA, proline, soluble protein, soluble sugar and photosynthetic pigment content, as well as the significant decreases of hydrogen peroxide, superoxide anion radical and malondialdehyde content were observed in okra plants grown in the soil with applied 30 g/kg AC under salt and drought stresses. Enzymatic analyses indicated the activities of 9-cis-epoxycarotenoid dioxygenase, pyrroline-5-carboxylate synthase, superoxide dismutase and peroxidase were also significantly increased under salt and drought stresses. These results demonstrate that the applied AC can alleviate damage caused by salt and drought stresses, leading to the enhanced salt tolerance and drought tolerance of okra plants. The AC has the potential to be used to develop plant growth regulators to enhance the tolerance to abiotic stresses in plants.

Shape stabilized attapulgite/myristic-palmitic acid composite PCM for thermal energy storage implementations in buildings

Depletion of energy resources and increasingly serious environmental problems due to increasing population and technological developments has led researchers to develop advanced energy storage techniques. The latent heat thermal energy storage method, in which phase change materials (PCMs) are used, is one of the most promising methods to overcome such problems. Fatty acids have been preferred mostly as solid–liquid PCMs for different thermal energy storage (TES) applications. However, the leakage difficulty of these PCMs significantly limits their utilizations in TES systems. This study is focused on eliminating this disadvantage of myristic acid (M)-palmitic acid (P) eutectic mixture (MPEM) with proper phase transition temperatures for thermal management of buildings. The developed eutectic mixture was then incorporated with attapulgite clay (ATC) to achieve shape-stabilized composite which does not allow liquid PCM leakage. FT-IR and SEM findings indicated the existence of good physicochemical compatibility between the ATC and MPEM. DSC analysis revealed that the composite had phase change temperature of 44–45 °C and latent heat of fusion of about 74 J/g, respectively. TGA test results showed that the fabricated composite has good thermal durability and stability. It can be inferred from the results that the produced ATC/MPEM composite had noteworthy potential as new admixture material with TES ability which can be used for energy saving and indoor thermal comfort improvement in buildings.

Hybrids Development between Greek Salvia Species and Their Drought Resistance Evaluation along with Salvia fruticosa, under Attapulgite-Amended Substrate

Aiming to obtain Salvia hybrids with ornamental value and high drought resistance, for xeriscaping, crossbreeding was made with Greek Salvia species. S. fruticosa and S. officinalis when used as seed parent were successfully crossed with S. pomifera ssp. pomifera, S. ringens and S. tomentosa, while when used as pollen parent it only succeeded between S. fruticosa and S. tomentosa. The growth of S. fruticosa and the four hybrids, S. officinalis × S. pomifera, S. officinalis × S. tomentosa, S. officinalis × S. ringens and S. fruticosa × S. ringens, selected for their ornamental traits, was evaluated under limited irrigation and modification of the substrate with attapulgite clay. The hybrids S. officinalis × S. ringens and S. officinalis × S. tomentosa developed a compact plant shape and most lateral shoots, desirable characteristics for potted plants and xeriscaping. All hybrids, especially S. officinalis × S. pomifera and S. officinalis × S. tomentosa, survived water stress better than S. fruticosa. Modification of the substrate with attapulgite, under limited irrigation, caused a decrease in the above ground/root biomass ratio in some hybrids and in S. fruticosa increased the dry weight of the root indicating increased drought resistance.

Deactivation and regeneration of solid acid and base catalyst bodies used in cascade for bio-oil synthesis and upgrading

The modes of deactivation -and the extent to which their properties can be restored- of two catalyst bodies used in cascade for bio-oil synthesis have been studied. These catalysts include a solid acid granulate (namely ZrO2/desilicated zeolite ZSM-5/attapulgite clay) employed in ex-situ catalytic fast pyrolysis of biomass, and a base extrudate (K-exchanged zeolite USY/attapulgite clay) for the subsequent bio-oil upgrading. Post-mortem analyses of both catalyst bodies with Raman spectroscopy and confocal fluorescence microscopy revealed the presence of highly poly-aromatic coke distributed in an egg-shell manner. Deactivation due to coke adsorption onto acid sites affected the zeolite ZSM-5-based catalyst, while for the base catalyst it is structural integrity loss, resulting from KOH-mediated zeolite framework collapse, the main deactivating factor. A hydrothermal regeneration process reversed the detrimental effects of coke in the acid catalyst, largely recovering catalyst acidity (∼80%) and textural properties (∼90%), but worsened the structural damage suffered by the base catalyst.

Inhibition of organosilane/ATP@HQ self-healing passivator for pyrite oxidation

Organosilane, with functional organic groups attached to inorganic silicon atoms, exhibits excellent passivation performance for pyrite. However, a considerable number of micro-cracks will gradually appear on the surface of passivation film under long-term corrosion of oxidizing medium, resulting in a significant decrease of passivation effect. To improve the stability and long-term performance of organosilane coating, a novel passivator (PT-ATP@HQ) with self-healing function was prepared to inhibit the oxidation of pyrite. We chose 3-mercaptopropyltrimethoxysilane (Prop-SH) and tetraethoxysilane (TEOS) as the host coating (PT), and attapulgite clay (ATP) loaded with 8-hydroxyquinoline (8-HQ) was used to endow the coating with better passivation and self-healing performance. The electrochemical and chemical leaching results showed that the addition of ATP@HQ greatly improved the passivation performance of PT coating. The passivation efficiencies of total Fe and SO42− reached to 88.1% and 79.2%, respectively. We also found that the protective capability of the scratched PT-ATP@HQ coating can be recovered automatically through 8-HQ release from ATP. The passivation and self-healing mechanisms were investigated by FT-IR, XPS, 29Si NMR, and other characterization methods, which were as follows: firstly, the organosilanes hydrolyzed to form highly active silanol groups, then dehydration condensation reaction occurred between silanol molecules and ATP@HQ to obtain cross-linked network structure connected by Si–O–Si bonds. After that, Si–OH groups reacted with the hydroxyl groups of pyrite to form Fe–O–Si bonds, thereby an inert and dense passivation film attached to the surface of pyrite. Once the passivation film is locally damaged, 8-HQ will automatically release to repair the cracks.

Fabrication of attapulgite/magnetic aminated chitosan composite as efficient and reusable adsorbent for Cr (VI) ions.

An efficient composite was constructed based on aminated chitosan (NH2Cs), attapulgite (ATP) clay and magnetic Fe3O4 for adsorptive removal of Cr(VI) ions. The as-fabricated ATP@Fe3O4-NH2Cs composite was characterized by Fourier Transform Infrared Spectroscopy (FTIR), Thermal Gravimetric Analyzer (TGA), Scanning Electron Microscope (SEM), Zeta potential (ZP), Vibrating Sample Magnetometer (VSM), Brunauer–Emmett–Teller method (BET) and X-ray photoelectron spectroscope (XPS). A significant improve in the adsorption profile was established at pH 2 in the order of ATP@Fe3O4-NH2Cs(1:3) > ATP@Fe3O4-NH2Cs(1:1) > ATP@Fe3O4-NH2Cs(3:1) > Fe3O4-NH2Cs > ATP. The maximum removal (%) of Cr(VI) exceeded 94% within a short equilibrium time of 60 min. The adsorption process obeyed the pseudo 2nd order and followed the Langmuir isotherm model with a maximum monolayer adsorption capacity of 294.12 mg/g. In addition, thermodynamics studies elucidated that the adsorption process was spontaneous, randomness and endothermic process. Interestingly, the developed adsorbent retained respectable adsorption properties with acceptable removal efficiency exceeded 58% after ten sequential cycles of reuse. Besides, the results hypothesize that the adsorption process occurs via electrostatic interactions, reduction of Cr(VI) to Cr(III) and ion-exchanging. These findings substantiate that the ATP@Fe3O4-NH2Cs composite could be effectively applied as a reusable adsorbent for removing of Cr(VI) ions from aqueous solutions.

Iron oxide loaded biochar/attapulgite composites derived camellia oleifera shells as a novel bio-adsorbent for highly efficient removal of Cr(VI)

Agricultural processing by-product have been used as the feed stock for effluent treatment to promote the utilization of agricultural waste, the development of green sustainable and construct a green ecological circle nowadays. Based on camellia oleifera shells, attapulgite, and ferric chloride, a novel iron oxide loaded biochar/attapulgite composite (Fe-BC/A) was synthesized via a one-step pyrolysis process and as a low-priced and efficient adsorbent for Cr(VI) removal from aqueous solution. The structure and composition of Fe-BC/A were characterized by SEM-EDS, FT-IR, XRD, and XPS, which confirmed iron oxide (analogous to α-Fe2O3 and β-FeOOH) and attapulgite clay were successfully incorporated with biochar. The maximum adsorption capacity of Cr(VI) by Fe-BC/A was 107 mg/g at pH 2.0, which was much higher than the original biochars (BC: 54.38 mg/g) and biochar/attapulgite composites (BC/A: 81.75 mg/g). The adsorption behavior of Fe-BC/A fitted better with pseudo second-order model and Freundlich model, which indicated that multilayer chemisorption might dominate Cr(VI) adsorption. The thermodynamic analysis of Fe-BC/A represented that removal of Cr(VI) was a spontaneous and endothermic process. Batch experiments results demonstrated that Fe-BC/A had great adsorption capability of Cr(VI) in a broad pH extent of 2.0–10.0, whose most favorable elimination for Cr(VI) at pH of 2.0 and the removal efficiency of Cr(VI) was about 80% at pH = 10 (C0 = 100 mg/L, 30 °C). Fe-BC/A exhibited a prominent tolerance to the coexisting ions during Cr(VI) removal and only a slight decrease (8.27%) in elimination efficiency after five adsorption-desorption cycles. Mechanism study revealed that electrostatic attraction, reduction, anion exchange, and complexation were involved in the removal of Cr(VI). This study implied the potential practical application of Fe-BC/A in the future Cr(VI) remediation from wastewater.

Preparation and Diagnostics of Schiff Base Complexes and Thermodynamic Study for Adsorption of Cobalt Complex on Iraqi Attapulgite Clay Surface

Three new complexes of Co(II), Ni(II), and Zn(II), containing ligand of Schiff base (DHMA) derived from methyldopa (mdop) with 3-hydroxybenzaldehyde have been prepared. The synthesized ligand and its complexes were diagnostics by using different physical techniques, The results showed that the complexes have an octahedral shape. In addition it has been studied the adsorption behavior, Uv-Vis technique that applied to survery the isotherm of adsorption. The results showed the possibility of applying the langmair equation. The effect of temperature on the adsorption of Co-complex on the surface of Iraqi Attapulgite clay was studied. The thermodynamic functions ΔGο, ΔHο and ΔSο of Co- complex have been studied and she was ΔGο =(-10.7766, -11.5205, -12.3537)KJ/ mol, this is evidence that the adsorption process is a spontaneous while ΔSο=( 63.6461)J/ mole.K which means an increase in the randomness. The value of ΔHο was (8544.29)J/mole indicate the endothermic natural of the process.

Synthesis, characterization, and adsorption properties of collagen and attapulgite‐filled copolymer biocomposites: Batch and column studies

AbstractSeveral biocomposites were synthesized by copolymerizing hydroxyethyl methacrylate (HEMA) and itaconic acid (IA) at varied molar ratios in the presence of different wt% of collagen (CLG) and attapulgite (APG) clay. The structure and properties of the biocomposite adsorbents were characterized by Fourier transform infrared apectroscopy, nuclear magnetic resonance, X‐ray photo electron spectroscopy, X‐ray diffraction, scanning electron microscope, transfer electron microscopy, energy‐dispersive X‐ray analysis, differential thermal analysis–thermogravimetric analysis, point zero charge analysis, mechanical properties, and pH reversibility tests. The synthesis variables were optimized with a central composite design of response surface methodology (RSM). The biocomposite prepared with an optimized composition of 1.5 wt% CLG, 1.7 wt% APG, and 5:1 molar ratio of HEMA:IA showed an adsorption capacity (Qe, mg/g) of 674.4/602.4 for methylene blue (MB)/Rose Bengal (RB) dye from a feed containing 200 mg/L of MB + RB dye mixture in batch mode. In a fixed bed in column mode, the optimized biocomposite showed a removal% of 82.8/71.3 for 100 mg/L inlet concentration, 20 ml/min flow rate, and 20 mm bed height with a breakthrough time of 23/31 min and a mass transfer coefficient (kmtc × 105 cm/s) of 8.36/7.67 for MB/RB as single dye solution.

Prediction of copper ions adsorption by attapulgite adsorbent using tuned-artificial intelligence model

Copper (Cu) ion in wastewater is considered as one of the crucial hazardous elements to be quantified. This research is established to predict copper ions adsorption (Ad) by Attapulgite clay from aqueous solutions using computer-aided models. Three artificial intelligent (AI) models are developed for this purpose including Grid optimization-based random forest (Grid-RF), artificial neural network (ANN) and support vector machine (SVM). Principal component analysis (PCA) is used to select model inputs from different variables including the initial concentration of Cu (IC), the dosage of Attapulgite clay (Dose), contact time (CT), pH, and addition of NaNO3 (SN). The ANN model is found to predict Ad with minimum root mean square error (RMSE = 0.9283) and maximum coefficient of determination (R2 = 0.9974) when all the variables (i.e., IC, Dose, CT, pH, SN) were considered as input. The prediction accuracy of Grid-RF model is found similar to ANN model when a few numbers of predictors are used. According to prediction accuracy, the models can be arranged as ANN-M5> Grid-RF-M5> Grid-RF-M4> ANN-M4> SVM-M4> SVM-M5. Overall, the applied statistical analysis of the results indicates that ANN and Grid-RF models can be employed as a computer-aided model for monitoring and simulating the adsorption from aqueous solutions by Attapulgite clay.

Prediction of lead (Pb) adsorption on attapulgite clay using the feasibility of data intelligence models.

This study investigates the performance of support vector machine (SVM), multivariate adaptive regression spline (MARS), and random forest (RF) models for predicting the lead (Pb) adsorption by attapulgite clay. Models are constructed using batch stochastic data of heavy metal (HM) concentrations under different physicochemical conditions. Implementation of auto-hyper-parameter tuning using grid-search approach and comparative analysis is performed against the benchmark artificial intelligence (AI) models. Models are constructed based on Pb concentration (IC), the dosage of attapulgite clay (dose), contact time (CT), pH, and NaNO3 (SN). Principle component analysis (PCA) and correlation analysis (CA) methods are integrated to assess the importance of the applied predictors and their relationship with the target. Research findings approved the potential of the grid-RF model as a marginal superior predictive model against the grid-SVM in terms of MAE, i.e., 3.29 and 3.34, respectively; moreover, the md scored the same, i.e., 0.93, which reveals the potential predictability for both. Nonetheless, grid-MARS and standalone MARS models remained likewise in their predictability. IC parameter demonstrated the highest influential among all the predictors with the highest value of importance in the case of all three evaluators. The solution pH and dose stands together with marginal differences in case of PCA method; however, solution pH and CT appeared with similarity impact using the PCA method.

Study of Efficacy Adsorption of Methyl Green by Attapulgite and Modified Attapulgite Clay from Aqueous Solution

This paper includes the modification of the attapulgite by precipitation of iron and aluminum compounds . Attapulgite (Atta) and modified attapulgite (Atta-m) clays are characterized by many techniques ( FTIR , XRD ,SEM with EDX ) .The attapulgite clay before and after modification were used as the adsorbents for adsorption of methyl green (MG) . The results Indicate ,that the percentage of removal (MG) at equilibrium by using (Atta) and (Atta-m) clay were reached to 94% and 97% respectively. Indicating that the clay modification process was in addition to a relative improvement in the adsorption potential of the clay after modification.

Processing of Iraqi Attapulgite For Using as Drilling Muds: A Comparison Study

Clay mineral processing is in charge on quality, quantity and functional properties of final produced clay. In this work, Iraqi attapulgite (Palygorskite) clay was processed with dry sieving, dispersing agent and wet sieving processes to make it suitable in oil and gas wells drilling fluids preparation. Yield of clay (quality) and yield of process (quantity) were taken as preferring criteria in choosing the proper process of Iraqi attapulgite clay preparation. XRD and FESEM tests were used for mineralogical and morphological identification respectively. OFITE viscometer was used to measure the rheological properties of the drilling fluids prepared with the produced attapulgite from the investigated processes. The results of this work showed that dry sieving process was failed in attapulgite separation. Moreover, dry grinding was a destructive process of the attapulgite crystalline structure which reduced the rheological properties up to 80%. The results showed that the dispersing agents process produces attapulgite clay with higher quality (101.94 and 89.87 barrle/ton) with fresh and salt water respectively and at low quantity of about 7%. While wet sieving process produces attapulgite clay with quality equals to (94.21 and 79.93barrel/ton) with fresh and salt water respectively and quantity reaching 40%. It follows that wet sieving was the recommended process in preparing Iraqi attapulgite to be suitable for oil and gas wells drilling fluid

Processing of Iraqi Attapulgite For Using as Drilling Muds: A Comparison Study

Clay mineral processing is in charge on quality, quantity and functional properties of final produced clay. In this work, Iraqi attapulgite (Palygorskite) clay was processed with dry sieving, dispersing agent and wet sieving processes to make it suitable in oil and gas wells drilling fluids preparation. Yield of clay (quality) and yield of process (quantity) were taken as preferring criteria in choosing the proper process of Iraqi attapulgite clay preparation. XRD and FESEM tests were used for mineralogical and morphological identification respectively. OFITE viscometer was used to measure the rheological properties of the drilling fluids prepared with the produced attapulgite from the investigated processes. The results of this work showed that dry sieving process was failed in attapulgite separation. Moreover, dry grinding was a destructive process of the attapulgite crystalline structure which reduced the rheological properties up to 80%. The results showed that the dispersing agents process produces attapulgite clay with higher quality (101.94 and 89.87 barrle/ton) with fresh and salt water respectively and at low quantity of about 7%. While wet sieving process produces attapulgite clay with quality equals to (94.21 and 79.93barrel/ton) with fresh and salt water respectively and quantity reaching 40%. It follows that wet sieving was the recommended process in preparing Iraqi attapulgite to be suitable for oil and gas wells drilling fluid

Investigation of attapulgite clay crushing by bionic tooth plates inspired from convex structures on body surface of dung beetles

A bioinspired tooth plate structures imitating convex structures on the head and body surfaces of dung beetles was presented and analysed using the discrete element method. Simulation results showed that compared with the regular tooth plates without bionic structures, the bionic crushing tooth plate offers a better performance and higher efficiency in crushing wet attapulgite clay. Based on the simulation results, a two-stage crushing machine was designed, produced, and validated through experiments. Experimental results confirmed that the developed crushing equipment with the bioinspired convex structures can effectively crush the attapulgite clay with high moisture content, which cannot be crushed by existing crushers due to the adhesion of the wet clay particles to the tooth plate surfaces. The produced crushing equipment has been applied for processing the attapulgite clay in China, and the design idea can be applied to develop other equipment for crushing rare earth minerals with high moisture content.

Preparation, characterization and application of activated clay biochar composite for removal of Cr(VI) in water: Isotherms, kinetics and thermodynamics

This study explored the feasibility of employing a new activated clay mineral biochar composite produced from simultaneous pyrolysis of Macadamia nutshells/groundnut shells biomaterials and calcination of attapulgite clay in the adsorptive removal of Cr(VI) from contaminated water. Fourier transform infrared spectroscopic analysis revealed the presence of absorption peaks at 1139 and 1027 cm−1 attributed to the biochar C–O and fingerprints of attapulgite. The parameters influencing the adsorption of chromium on the adsorbent surface were investigated, and it was shown that pH 3, contact time of 40 min, adsorbent mass of 100 mg and concentration of 2.5 mg L−1 were the optimal parameters. The removal mechanism involved adsorption of Cr(VI) through electrostatic attraction and/or subsequent reduction of Cr(VI) to Cr(III). At low Cr(VI) initial concentrations, the removal mechanism was dominated by chemisorption while at higher concentrations physisorption was more pronounced. The adsorption isotherm was best fitted with the Freundlich model. Thermodynamic data indicated the endothermic nature of adsorption process which was feasible and spontaneous. The achieved equilibrium adsorption capacity of 6.1 mg g−1 is comparable with the values reported for other adsorbents in literature.

Elemental mercury removal from coal-fired flue gas using recyclable magnetic Mn-Fe based attapulgite sorbent

Magnetic manganese-iron modified attapulgite sorbents (xMnFAy) were synthesized and employed for Hg0 removal from coal-fired flue gas. The effects of calcination temperature, MnO2 loading amount, reaction temperature, as well as the individual flue gas components on Hg0 removal were investigated. The 0.1MnFA loaded with 10 wt% MnO2 and calcined at 450 °C exhibited the optimal Hg0 removal activity, above 80% Hg0 removal at a high GHSV of 4 × 105 h−1. O2 promoted Hg0 removal via recovering surface oxygen and high valence metal ions (Fe3+ and Mn4+). NO improved Hg0 capture due to the formation of adsorbed NO2 and nitrate species, which functioned as active sites for mercury oxidation. SO2 prohibited Hg0 retention because of its competitive adsorption against Hg0 for the active sites and the sulfation of the sorbent. Besides, SO2 could reduce the high valence metal ions to a lower valence, which hampers Hg0 oxidation. The presence of NO could overcome the inhibitive effect of SO2 on Hg0 removal because the adsorbed NO2 and nitrate species were still retained on the sorbent surface in the case of SO2 existence·H2O inhibited Hg0 removal because of the competitive adsorption. 0.1MnFA could maintain its good Hg0 retention ability after five regeneration cycles. This work contributes to developing the cost-effective sorbents for Hg0 removal from coal-fired flue gas, as well as maximizing the utilization of attapulgite clay.

Construction of upconversion fluoride/attapulgite nanocomposite for visible-light-driven photocatalytic nitrogen fixation

Developing photocatalysts with wide spectrum absorption and strong nitrogen activation is critical for nitrogen fixation under mild conditions. Herein, one-dimensional natural clay attapulgite (ATP) supported YF3:Sm3+ were successfully synthesized via microwave hydrothermal method, and the composites were employed as the catalyst for photocatalytic nitrogen fixation under visible-light irradiation. Results indicated that the production of ammonia reached as high as 41.2 mg·L−1 within 3 h when the molar ratio of Sm3+ and the mass fraction of YF3:Sm3+ were optimized. The enhanced fixation performance is mainly due to that the modified ATP fibber with abundant active sites and the doped fluoride with defective vacancy facilitate the adsorption and activation of N2. Furthermore, the upconversion property of YF3:Sm3+ increases the harvesting of visible-light energy, meanwhile the Z-scheme heterostructure built between YF3:Sm3+ and modified ATP inhibits the recombination of charge carriers and retains high redox potentials for N2 reduction.

Influence of different wet milling on the properties of an attapulgite clay, contribution of inverse gas chromatography

An experimental study, using size measurements, X-ray diffraction (XRD), scanning electron microscopy (SEM) and inverse gas chromatography at infinite dilution (IGC-ID) and finite concentration (IGC-FC) conditions, has been carried out to evaluate, respectively, the changes of particles size, crystalline phases, morphology and surface properties evolution of attapulgite powder after grinding in wet media.The particles size decreases significantly after grinding in ball mill in different liquid media. The SEM analysis shows that the fibers are preserved during grinding in aqueous media. With IGC-ID, after grinding using wet ball milling in hydrochloric acid, the values of γsd determined by injection of alkane probes decrease significantly because of the disappearance of the insertion sites able to retain the probes. In the same grinding conditions, with IGC-FC, the specific surface area obtained with octane probe increases significantly from 114 m2/g to 156 m2/g.