Ferromagnetic xyloglucan–Fe3O4 green nanocomposites: sonochemical synthesis, characterization and application in removal of methylene blue from water

  • Shahzad Ahmad
  • Shiv Shankar
  • Anuradha MishraEmail author
Original Article


In present study, novel magnetic nanocomposites based on an agro-based material, non-toxic and biocompatible xyloglucan (XG) with magnetic iron oxide (Fe3O4) were synthesized by a simple, safe and ecofriendly sonication method. The synthesized nanocomposites (XG–Fe3O4) were characterized by various analytical techniques such as powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM)-energy dispersive X-ray (EDX), transmission electron microscopy (TEM)–EDX analysis and selected-area electron diffraction (SAED). The average crystallite size of the nanocomposites as estimated by the Scherrer analysis were in the range of 17–20 nm and thus exhibited no significant difference in mean particle size on changing the ratios of Fe3O4 and Xyloglucan. The high resoloution (HR) TEM analysis revealed nanorod like shape of synthesized Fe3O4 nanoparticles. Lattice fringes of the individual crystallites were seen in the HRTEM image, indicative of their good crystallinity. The distance of 0.29 nm was found in between the lattice fringes that confirmed the cubic structure of nanoparticles. The FTIR spectrum of nanocomposite indicated the interaction of functional groups in XG with the Fe3O4 nanoparticles at the surface. The SEM analysis revealed the average crystal size of pure Fe3O4 nanocrystals to be 22.4 nm. The SAED analysis revealed that the nanocomposites (20 nm) were very close to behaving as superparamagnets at room temperature. A preliminary study on removal of methylene blue (MB) dye from aqueous solution indicated that the nanocomposite has potential to be used for photocatalytic and adsorptive removal of MB from aqueous solutions.


Xyloglucan Nanocomposites Ferromagnetic TEM–EDX Polysaccharide Nanogels Hydrogels Dye removal 


The contamination of water streams by synthetic dyes has emerged as a serious environmental issue worldwide. During manufacturing and handling of synthetic dyes, 15–20% dyes are lost and released into waste water causing water pollution. Dyes are highly visible even at a very low concentration. Synthetic dyes present in waste water severely affect primary production in receiving water bodies and cause adverse biochemical effects on plants and aquatic animals. In humans, dyes may cause allergic dermatitis, skin problems, and cancer (Rong et al. 2014).

Different physico-chemical methods like electrolysis (Ruan et al. 2010), sorption (Lapwanit et al. 2018), photochemical destruction, membrane filtration (Karim et al. 2018), coagulation/flocculation, chemical precipitation and oxidation (Nidheesh et al. 2018; Mijinyawa et al. 2019) have been reported for the removal of dyes from the water. Sorption technique has drawn significant attention of the researchers due to its simplicity of operation, low cost and relatively high resistance to toxic substances (Lapwanit et al. 2018). The synthesis of novel and safe adsorbents with high sorption capacity following green chemistry principles to remove synthetic dyes is equally necessitated.

The sonochemical synthesis is considered as eco-friendly approach as compared to other methods (forced hydrolysis and precipitation, reactive sputtering, pulsed laser evaporation, sol–gel process and chemical vapor deposition) in the synthesis of materials based in metal oxides (Dolores et al. 2015; Hassanjani-Roshan et al. 2011; Sivasankaran and Kishor Kumar 2019). Sonochemical synthesis of metal oxide nanoparticles is considered safe as it does not produce toxic intermediates (Hassanjani-Roshan et al. 2011). Ultrasonic method for synthesis has been found to be particularly useful to prevent aggregation of the magnetic nanoparticles and ensures their intimate dispersion within the polymeric matrix.

Hydrogels, known for absorbing large amounts of water or biological fluids, are polymer networks. Hydrogels offer a wide variety of applications for various industries (Yuk et al. 2019). In the last few decades, polysaccharide-based hydrogels have been recognized as materials having exceptional properties (Dave and Gor 2018). Polysaccharide-based nanocomposites with different surface reactivity have drawn the significant attention of the researchers for the removal of dyes from water as they do not produce any toxic intermediates (Makarchuk et al. 2016) and may easily be separated from the wastewater under the influence of the magnetic field (Verma et al. 2017).

The major applications of polysaccharide-based nanocomposites include biomedical applications such as controlled drug releasing agents, in medicine, pharmacology and sensors, electronic devices, energy production and storage, food packaging films and water treatment (Ribeiro et al. 2009; Kirschning et al. 2017; Shankara et al. 2018; Mittal et al. 2018 Shankara et al. 2018; Mittal et al. 2018; Batista et al. 2019; Yuk et al. 2019). Additionally, these materials have their application in photocatalytic removal of synthetic dyes from their solutions. They are supposed to be the environmentally sustainable ideal materials for their potential utility in abatement of dye pollution in water for having unique properties like biodegradability, biocompatibility, and renewability (Yahya et al. 2018; Lassoued et al. 2018).

In the backdrop of aforesaid context, the synthesis of a new magnetic nanocomposite material based on tamarind seed xyloglucan (XG) using ultrasonic energy has been planned. XG from tamarind seeds is known to be a flocculant for water treatment (Mishra et al. 2006; Mishra and Bajpai 2006; Mishra 2013). The magnetic responsive behavior was introduced in XG hydrogel networks by Fe(II)/Fe(III) nanoparticles adsorption.

Materials and methods

The Tamarind seed powder (TSP) was obtained from Venus Starch Suppliers, Tamil Nadu, India and XG was extracted from TSP by the method described by Mishra and Malhotra (2012). Iron salts (FeCl2·4H2O and FeCl3·6H2O) used for the synthesis of nanoparticles and methylene blue (MB) dye (MB, Basic Blue 9 Color Index 52015) were purchased from Merck, India and CDH (P) Ltd. India, respectively.

Synthesis of Fe3O4 nanocrystals

Fe3O4 nanocrystals were synthesized using a mixture of FeCl2 and FeCl3 as per the method reported elsewhere (Raz et al. 2012). In a round bottomed flask (250 mL capacity), aqueous solution of FeCl2 and FeCl3 in the ratio of 1:2 was stirred at room temperature under N2 bubbling. Sodium hydroxide solution was added drop-wise until black coloured particles precipitated completely. The precipitate was washed multiple times with water and ethanol.

Preparation of magnetic nanocomposites of xyloglucan and Fe3O4 nanocrystals

The magnetic nanocomposites were obtained from the reaction of Fe3O4 nanocrystals and XG in four different weight ratios. The synthesized samples were assigned with codes, XF10, XF25, XF33 and XF50 indicating the weight ratio of (90:10), (75:25), (67:33) and (50:50) of XG and Fe3O4 nanocrystals respectively. The known amount of XG and Fe3O4 nanocrystals in defined ratio were dispersed in ethanol and subjected to sonication for 30 min at 5 kHz. In sonicated solution, 5 g succinic acid was added followed by further sonication up to 60 min. The solution was left under stirring conditions overnight. The synthesized magnetic nanocomposites were separated from the mother liquor using centrifugation (5000 rpm, 10 min) and washed several times with ethanol. All the samples were prepared under same conditions and dried at 45–50 °C in an oven for further use (Liu et al. 2009).


The Bruker diffractometer (D8 Discover) was used to record the powder X-ray diffraction (PXRD) patterns of the nanocomposites employing Cu Kα radiation (λ = 1.5418 Å) in the range of 2θ = 10°–60° (Chuev 2009). The Philips Tecnai G2 30 transmission electron microscope (TEM) operating at an accelerating voltage of 300 kV was used to take images and the energy dispersive X-ray (EDX) measurements (Naseem and Farrukh 2015). The field emission scanning electron microscopy (FESEM) images were taken by using the FEI QUANTA 200 FEG scanning electron microscope in accordance with Prodan et al. (2013). The Perkin–Elmer FT–IR spectrometer (model 2000), at a resolution of 4 cm−1 and 32 scan collections, was used for the Fourier-transform infrared spectroscopy (FTIR) analysis of the nanocomposites, employing KBr as dispersal medium (Suhas et al. 2014). The vibrating sample magnetometer ( VSM) (Microsense EV9) was used under magnetic fields up to 10 kOe at room temperature for the magnetic measurements (Mahdavi et al. 2013).

Removal of methylene blue (MB) dye

In case of photocatalytic degradation of dye, the method adopted was as described by Lassoued et al. (2018) and in case of adsorptive removal of dye, the method followed was as given byXu et al. (2016). The decolorization experiments by both the methods were carried out using 100 mL aqueous solution of MB (10 mg/L), and nanocomposite (100 mg/L) in an Erlenmeyer flask of 250 mL capacity. The content was shaken at 110 rpm and 30 °C in light using an incubator shaker (NSW-159, New Delhi, India). The UV–Vis spectrophotometer [Single beam, model no. 290, Labtronics, India)] was used to evaluate the removal of MB by recording the absorbance of the reaction mixture at 668 nm at various time intervals. The percent removal value for MB was calculated using the following formula:
$$\% {\text{ MB removal }} = {\text{ C}}_{0} - {\text{ C}}_{\text{e}} /{\text{ C}}_{0} \times 100$$
where, C0 and Ce were the concentrations (mg/L) in the initial state and the concentration at equilibrium respectively. Each experiment was conducted three times to get exact result.

Results and discussion

The PXRD patterns of the products (XF10, XF25, XF33 and XF50) obtained from the reaction of XG with Fe3O4 are shown in the Fig. 1. The magnetite structure of all the four products showed peaks and intensities matched well with the JCPDS File no: 76-1849. This finding indicated that the crystalline structure of Fe3O4 nanoparticles remained almost the same even after the formation of the composites; however, a slight shift of the reflections to the higher 2θ side was also observed. All the four samples of nanocomposites, XF10, XF25, XF33 and XF50 showed the value of cubic lattice constant ‘a’ as 8.328 (3) Å, 8.358 (4) Å, 8.340 (2) Å and 8.332 (1) Å, respectively. These ‘a’ values were lower than the standard value (8.400 Å) and were derived from the PXRD patterns through the Le Bail refinements using space group Fd-3 m No. 227. This reduction of the unit cell was attributed to the presence of oxygen vacancies due to the introduction of carbon and hydrogen ions during the formation of nanocomposites. The broadness of the observed Bragg reflections also confirmed the low-crystallite size of the nanocomposites. The average crystallite size of the nanocomposites as estimated by the Scherrer analysis was in the range of 17–20 nm (Londoño-Restrepo et al. 2019). This size range indicated that there was not any significant difference in mean particle size on changing the ratios of Fe3O4 and XG. In addition, an apparent broad diffraction peak of XG could also be identified at 15°–25°, whose intensity suppressed with Fe3O4 concentrations in the XG–Fe3O4 nanocomposites samples, indicating that the Fe3O4 nanocrystals were efficiently deposited on the XG surface. Taylor and Atkins (1985) have reported similar results for β-1,4-linked polyglucose backbone (twofold flat ribbon type helical structure) based on cyclicity indexing on a distance of 2.06 nm along the chain direction.
Fig. 1

PXRD patterns of the XF10, XF25, XF33 and XF50

The TEM images of these magnetic nanocomposites showed agglomeration of crystallites which was attributed to the high surface area of the Fe3O4 nanocrystals (Fig. 2a). Nanorod like shape was observed for the synthesized Fe3O4 nanoparticles. The high resolution (HR) TEM image analysis proved the good crystallinity in composites due to the presence of lattice fringes of individual crystallites (Fig. 2b) and a distance of 0.29 nm was found to be present between the lattice fringes. This distance corresponded to the d spacing for the (220) lattice plane of the cubic Fe3O4 structure. The selected-area electron diffraction (SAED) pattern of the crystallites (Fig. 2c) also proved its cubic Fe3O4 structure as these patterns could be indexed to the (111), (220), (311), (222), and (400) planes. Remarkably, the SAED pattern of the XG has also been observed at 0.589 nm and 0.440 nm which clearly indicated the formation and stability of the magnetic nanocomposites.
Fig. 2

a TEM image and b HR-TEM image, c SAED pattern and d EDX of the XF25 nanocomposites

The formation of uniform magnetic nanocomposites was proved by the EDX spot analysis on various locations in TEM images (Fig. 2d). The FESEM of the nanocomposites clearly showed the different surface morphologies from the XG (Fig. 3a). The surface of the XG particles (Fig. 3a) demonstrated a small crinkle-like pattern (Li et al. 2018). In fabricated nanocomposites, this pattern showed homogeneously dispersed crystals of XG–Fe3O4 (Fig. 3b–d). The average crystal size of pure Fe3O4 nanocrystals was 22.4 nm. Several researchers (Mamania et al. 2014; Tancredi et al. 2017; Li et al. 2017) have also reported the size of Fe3O4 nanocrystals between the range 10–64 nm. Since XG is a polymer and an amorphous compound, its average crystal size cannot be evaluated, however, its particle size ranged from 0.19 to 29 µM.
Fig. 3

FESEM image of a Xyloglucan and bd XF25 nanocomposites

The FTIR spectra of the nanocomposites confirmed the interaction of functional groups in XG with the Fe3O4 nanoparticles at the surface (Farias et al. 2018; Allafchian et al. 2019). The vibrations characteristic of Fe3O4 at 630–631 cm−1 for Fe–O from a tetrahedral site was observed at 646 cm−1 while the band for Fe–O from an octahedral site shifted at 617 cm−1 from 570-580 cm−1 (Fig. 4). This shifting towards higher wave numbers could be explained on the basis of the formation of Fe–O-C bonds replacing Fe–O–H groups on the surface of the Fe3O4 nanoparticles (Hsieh et al. 2010). More electronegative character of C than that of H might have led to the enhancement of bond force constant for Fe–O bonds, consequently shifting of the absorption bands to high wave numbers. The spectra also exhibited absorption bands around the 450 cm−1 which might be due to the vibration mode of Fe–O bond (Zhang et al. 2008). Additionally, the strong peaks at 2922 (νasCH2) and 2853 (νsCH2) cm−1 might be attributed to the presence of XG on the particle surfaces (Nakamoto, 2008). The broad peaks between 1135 and 1027 cm−1 might be due to C–O–C and C–O group of XG. The bands centred at around 3430 cm−1, 1635 cm−1 and 1385 cm−1 were assigned to the O–H stretching, banding and deforming vibrations of adsorbed water, respectively (Kacurakova et al. 2002; Ahmad et al. 2011).
Fig. 4

FTIR spectra of XF10, XF25, XF33 and XF50

The magnetization curve of XG–Fe3O4 nanocomposites at room temperature under the influence of applied magnetic field has been depicted in Fig. 5. The magnetic properties seemed to depend on the amount of Fe3O4 in the nanocomposites. The values of saturation magnetization (Ms) were 2.65, 4.42, 5.65 and 8.58 emu/g for the samples XF10, XF25, XF33 and XF50, respectively. The results indicated that the saturated magnetization value is directly proportional to the content of Fe3O4 in the nanocomposites. The average crystallite size of the nanocomposites as estimated by the Scherrer analysis varied in a very narrow range (17–20 nm), hence, the change in average crystallite size was not significant to alter the saturation magnetizations (Londoño-Restrepo et al. 2019). Moreover, a tiny hysteresis loop in all of the XG–Fe3O4 nanocomposites was observed which proved that the XG–Fe3O4 nanocomposites exhibited small ferromagnetic behavior (Rabel et al. 2019). The extent of hysteresis loop was maximum for the nanocomposite sample, XF50. On increasing the Fe3O4 content from 10 to 50%, the coercivity (Hc) values increased from 81 to 102 Oe distinctively, and the remnant magnetization (Mr), also increased from 0.33 to 1.18 emu/g. The magnetic properties of the nanocomposites were found lower than that of the bulk Fe3O4 particles which showed the value of Ms as 84 emu/g and of coercive force as 500–800 Oe. The magnetic properties of any material is influenced by its particle size and for mono-domain particles, the Ms goes down with decrease in crystallite size due to the surface spin canting and disorder; thermal fluctuation; and distribution of cations. In the present study, the decrease of Ms and Hc values in nanocomposites as compared to the bulk sample might be attributed to the surface disorder (Kanwal et al. 2019). At room temperature, the nanocomposites of 20 nm diameter seemed behaving almost like the supermagnets. In present study, magnetic coercivity was found to be negligible insinuating no more magnetization after withdrawal of extraneous magnetic field. It firmly established that the synthesized XG–Fe3O4 were of superparamagnetic in nature (Hoan et al. 2016; Maldonado-Camargo et al. 2017).
Fig. 5

VSM spectra of XF10, XF25, XF33 and XF50

MB dye removal potential of XF50

Preliminary study on MB removal using XG–Fe3O4 magnetic nanocomposites showed promising results for its potential use in wastewater treatment. The photocatalytic activity of XF50 to degrade MB dye was evaluated under visible light irradiation at 664 nm. The color disappeared completely after about 30 min. In the case of adsorptive removal of MB dye, it was seen that the dye removal was time-dependent (Fig. 6) and the color of the dye almost disappeared after an incubation period of 75 min. These results were comparable to the results obtained by other researchers with the magnetic nano-adsorbents similar to reported in this study (Hua et al. 2018; Li et al. 2018).
Fig. 6

Removal of MB by XF50


The synthesis of magnetic nanocomposites of XG and Fe3O4 has been done using a nonhazardous sonication method. The PXRD results of all the four nanocomposites suggested that the small size carbon and hydrogen has been incorporated at the surface of ferric oxide. Both the TEM and SEM images validated the change in the morphology while their EDX confirmed the formation of uniform nanocomposites. The XG–Fe3O4 nanocomposites exhibited small ferromagnetic behaviour and the saturation magnetizations were in the range of 2.65–8.58 emu/g. This unique combination of XG and Fe3O4 made this as multifunctional nanocomposites. Preliminary studies showed that the material is capable of removing the hazardous organic dye, MB, from water; however, the material may also be used for many other classes of dyes. Hence, xyloglucan based magnetic nanocomposites are proposed as a promising newer material and eco-friendly sustainable approach for remediation of wastewater containing synthetic dyes.



One of the authors, Shahzad Ahmad, expresses his sincere thanks to UGC, New Delhi, India, for Dr D S Kothari Post Doc Fellowship.

Compliance with ethical standards

Conflicts of interest

There is no conflict of interest to declare.


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Copyright information

© Society for Environmental Sustainability 2019

Authors and Affiliations

  1. 1.Department of Applied Chemistry, School of Vocational Studies and Applied SciencesGautam Buddha UniversityGreater NoidaIndia
  2. 2.Department of Environmental Science, School of Vocational Studies and Applied SciencesGautam Buddha UniversityGreater NoidaIndia

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