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Keywords: Use of agriculture waste to develop value-added products has helped in resolving the waste management con-
Corncob biochar cernsalong with addressing the cost-effectiveness issues. Utilization of bio-char derived from agriculture waste
Biochar based nano-composite back to the agriculture field marks the new strategy to improve crop yield and reduce environmental issues of
Macronutrients conventional fertilizers. In addition to that it helps in improving soil condition by balancing the soil organic
Micronutrients
carbon, pH, water holding capacity and soil ion exchange potential. The present research work is based on the
Impregnation
Slow release fertilizer
development of nano-composite based on biochar derived from corn cob and to check the suitability of corncob
biochar(CB) as support material for providing macro and micro-nutrients to the plants on slow release
basis.CBand its nano-composite (BNC) were synthesized by pyrolysis and simple impregnation method, re-
spectively and characterized by FT-IR,SEM/EDX, powder XRD,AFMand TGA/DSC. Proximate analysis and
physical properties were also examined by standard procedures whilestudies on water retention, water absor-
bance, swelling ratio and equilibrium water content of pointed to increased values of BNC as compared to CB.
Slow release studies indicated release pattern of nutrients for prolonged period which is helpful in improving
plant growth and yield. The experimental results indicated that the synthesized nano-composite is eco-friendly
material and can be used as slow release fertilizer for sustainable agriculture.
1. Introduction mated to be reached 9.6 billion by the year 2050 (DeSA, 2013). In
addition to that use of conventional fertilizer leads to huge economic
Agriculture is now-a-days greatly impacted by climatic change issue losses because of leaching issues (40–70%) which is critical for the
which is aggregated by global warming, urbanization and unbalanced developing countries where agriculture is backbone of the economy
use of resources and environmental problems like eutrophication and (Ditta and Arshad, 2016).To combat with this situation, there is need to
run off, related to use of conventional fertilizers. These problems are introduce new fertilizers which provide nutrients to plants slowly
increasing day by day with rapid increase in population which is esti- thereby reducing nutrient loss and promoting enhanced crop yield (Liu
Abbreviations: AFM, atomic force microscopy; BNC, biochar based nano-composite; CEC, cation exchange capacity; CB, corncob biochar; DSC, differential scanning
calorimetry; EDX, Energy-dispersive X-ray Spectroscopy; EWC, equilibrium water content; FT-IR, fourier transforms infrared spectroscopy; SI, salt index; SR, swelling
ratio; SRF, slow release fertilizer; SEM, scanning electron microscope; TGA, thermal gravimetric analysis; TDS, total dissolved solids; TH, total hardness; WR, water
retention; WA, water absorbance; XRD, X-ray diffraction
⁎
Corresponding author.
E-mail address: rabiapcsir@yahoo.com (R. Nazir).
https://doi.org/10.1016/j.enmm.2019.100212
Received 18 April 2018; Received in revised form 27 January 2019; Accepted 15 February 2019
2215-1532/ © 2019 Elsevier B.V. All rights reserved.
A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
Table 1 nutrient loss and improve crop production. This research work focus on
Analysis of Tap Water. the synthesis of biochar based slow release ecofriendly fertilizer on
Parameters Results nano-scale with aim to make use of its porous structure to incorporate
both macro and micro nutrients that can be made available to crops and
pH 7.6 soil on slow release basis. This approach will not only help in waste
Conductivity (μs cm−1) at 25°C 288.50
reduction and management but will also aid pollution prevention by
TDS (mg L−1) 418.5
TH (mg L−1) 0.69
conversion of waste into value added product and resolving the
Na1+ (mg L−1) 1.98 leaching issues of conventional fertilizers. This will hence help in mi-
Cl1− (mg L-1) 16.69 tigating the environmental problems and provision of nutrients to
K1+ (mg L−1) 1.08 plants to promote enhanced yield.
Ca2+ (mg L−1) 0.38
Zn2+ (mg L−1) 0.08
Mg2+ (mg L−1) 0.35 2. Experimental
PO43− (mg L−1) 1.96
NO31− (mg L−1) 1.2 2.1. Chemicals
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A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
Fig. 1. FT-IR spectra of CB (A) and BNC (B) representing shifting of peaks in BNC, which affirms the adsorption of nutrients.
The material was characterized by different techniques comprising conductivities (He et al., 2007).
FT-IR (Thermo Nicolet spectrometer) to access the organic moieties
present, powder XRD (PANanalyticalX’pert pro diffractometer via a
Philips X-ray generator) to determine phase and crystallinity, SEM/EDX 2.3.3. Swelling Ratio (SR) and Equilibrium water content (EWC)
(Nova NanoSEM 450 and EDX, Nova 450 at 5.00 kV) to define mor- 1.0 g of CB and BNC was submerged in 200 mL of distilled water
phology and elemental composition samples, AFM (AFM 5500 Agilant, separately for 24 h to swell and then filtered. Calculate SR and EWC
USA) to obtain particle size and topography and TGA ((SDT- Q600, using Eqs. 1 and 2, respectively (He et al., 2007).
Germany) to check thermal stability. Ws Wd
SR =
Wd (1)
2.3.2. Salt Index (SI)
Take 1.0 g each of BNC and sodium nitrate (NaNO3) in separate Ws Wd
beakers and add 200 mL of distilled water. Conductivities of both the EWC (%) = × 100
Ws (2)
solutions were measured by conductivity meter model CM-40S TOA
after 24 h. The value of SI was calculated, as ratio of these Where, Wd and Ws are the dry and wet weights of CB or BNC.
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A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
2.3.4. Water absorbance studies (WC) studies which were analyzed previously (Table 1) to set blank reading.
Water absorbance studies were conducted, by taking 1.0 g of CB and First studies of slow release of nutrients in water from BNC were
BNC (W1) in petri-plates which were previously weighted (W2). These performed for 7 days. The experiment employed glass column (30 ̋ ×
petri-plates were placed for 5 days in desiccator filled with water to 0.5 ̋ ) containing 5.0 g of BNC and tap water which volume was main-
create moist environment. The petri-plates were weighted again (W3) to tained at 50 mL mark during the whole experiment. 25 mL of water was
measure water absorption capacity of sample using Eq. 3(Hamid et al., draw from column on daily basis after every 24 h for 7 days to monitor
2013). the leakage of nutrients (Jamnongkan and Kaewpirom, 2010).
Second studies were conducted for 14 days in soil (400 g) + BNC
(W3 W2 )
WC = × 100 (10 g) filled glass column (62 ̋ × 5 ̋ ) to which 180 mL of tap water was
W1 (3)
added to soak the soil. Withdrawal of 50 mL water was done for 14 days
and after that 100 mL water added to maintain moisture level in
2.3.5. Water retention studies (WR) column. Water samples collected from column were analyzed to
Water retention studies (WR) were conducted in pre-weighted cups, monitor the release behavior of nutrients in soil from nano-composite.
add 50.0 g of sieved soil in cup A (weighed as WA) as control or blank Under similar conditions 400 g of soil was also run to monitor leaching
and in cup B (weighed as WB) add 2.0 g of BNC + 50 g soil. Add 30 mL from soil only (Kottegoda et al., 2011).
of distilled water in both cups, allowed to seep and reweighed (as WA1 The water samples collected were analyzed for NO31− by Ion
and WB1) after 24 h. The cups were then retained in a glass box, Selective Electrode 930, PO43- by UV Visible Spectrophotometer,
weighted as WA2 and WB2 on daily basis for 30 days (Hassan and (Na1+and K1+) by Flame Photometer Tenway PSP7 and metals (Zn2+,
Mahmoud, 2015). Water retention was calculated using Eq. 4. Ca2+, Mg2+, Fe2+/3) by Perkin Elmer Flame Atomic Absorption
W2 Spectrometer (FAAS).
WR%= × 100
W1 (4)
2.4. Statistical analysis
2.3.6. Slow release studies Data was explored and processed using MS Excel and Origin-Pro 8.
Slow release studies were done in 1) tap water and 2) soil, to Data is reported as average of three replications and in case of slow
monitor the nutrient leaching pattern. Tap water was used in both release studies, readings were adjusted for blank.
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A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
Fig. 3. SEM images of CB and BNC at resolutions of 5 μm (A & B), 1 μm (C & D) and 500 nm (E & F), respectively, showing porous structure of CB while white color
represents the impregnation of nutrients.
3. Results and discussion support material for macro and micro nutrients to result in BNC. CB has
a porous structure (Budai et al., 2014) which supports and facilitates
The research work describes a simple process to synthesize BNC the impregnation of nutrients. Earlier studies had also shown potential
using impregnation method, to incorporate macro and micro nutrients of biochar to store nutrients by either chemisorption and/or physio-
onto CB. sorption (Ding et al., 2016). Therefore, this property of biochar can be
exploited to use this as slow release fertilizer as it not only improves soil
3.1. Synthesis of BNC quality but also ensures the availability of nutrients, for prolonged
period of time to plants.
Pyrolysis approach was followed to prepare CB, which was used as
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A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
Fig. 4. Elemental analysis of CB (A) and BNC (B) represents the detailed composition of micro and macro nutrients.
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A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
Fig. 5. 2D (A) and 3D (B) AFM images of BNC indicating formation of nano sized composite.
3.2.4. Scanning electron microscopy (SEM)/energy dispersive X-ray particle size of BNC from two and three dimensional images as in Fig. 5
spectroscopy (EDX) and atomic force spectroscopy (AFM) which confirms the formation of nano-sized material having average
SEM gives information about morphology of synthesized samples particle size of 55.9 nm (Fig. 5B). The AFM image (Fig. 5A) also points
(CB and BNC). The images of CB and BNC (Fig. 3) taken at different to the regular spherical shape of the particles and narrow particle size
resolutions of 5 μm (A and B), 1 μm (C and D) and 500 nm (E and F) distribution in the prepared nano-composite; giving assurance about
represented the porous structure of CB. This porous structure augments the feasibility of synthetic protocol to result in particles with less dis-
the surface area and hence can enhance the adsorption capacity of CB tribution in particle size.
by providing more sites for chemical reactions (Lehmann, 2007;
Yuet al., 2014), as indicated by high MB value of BNC. The factors like 3.2.5. Thermal gravimetric analysis (TGA)
pyrolysis temperature and conditions depicted the final composition of Thermal stability of prepared samples (CB and BNC) was de-
biochar in addition to its source (Spokas, 2010). White color coating on termined by TGA/DSC analysis. The interlinked spectra of TGA and DSC
the surface of CB represented the doping of salts into CB as shown in are presented in Figs. 6 and 7. The thermogram of CB (Fig. 6) was
Fig. 3B. characterized by steady weight loss with three non-distinctive steps
Elemental analysis of CB and BNC was conducted by EDX (Fig. 4) after which constant decrease in weight was observed. The first peak at
which confirmed the impregnation of both macro and micro nutrients 147.52 °C (Wt. loss 94.54%) was probably due to loss of moisture, as
into the BNC structure. The variation in this wt. % can be attributed to affirmed by the proximate analysis while second (335.13 °C; wt. loss
affinity of these ions with the carbon structure and organic moieties 82.63%) and third peak (481.25 °C; wt. loss 63.85%) accounted to
presents as suggested by FT-IR (Fig.1). AFM is used to measure the pyrolytic decomposition stage, where maximum mass loss occurred due
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Fig. 6. TGA thermogram (black line) and DSC curve (blue line) depictingthermal stability of CB.
Fig. 7. TGA thermogram (black line) and DSC curve (blue line) describingthermal stability of BNC.
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Fig. 9. Release pattern of nutrients (Fe2+/3+, Zn2+, Ca2+,Mg2+,NO31−, Na2O,P2O5 and K2O) for 7 days in tap water.
available cations in soil (Xu et al., 2014). The trends observed can help impregnated with macro and micro nutrients to prepare
in continues supply of nutrients to plants as per their requirement and nanocomposite,BNC, having neutral pH and spongy structure of
prevented leakage of nutrients, when compared to conventional ferti- 55.9 nmas indicated by SEM and AFM while EDX analysis confirmed
lizers (Costa et al., 2013). CB absorbs nutrients because of its high the adsorption of nutrients.Results of salt index, slow release column
surface area and porosity and physiochemical binding that ensures re- studies, water absorbance and retention studies indicated that BNC has
duced leaching of nutrients (Steiner et al., 2008) thereby facilitating great potential to be used as nano-fertilizer. BNC can not only enhance
enhanced plant growth (Hunt et al., 2010). All these reasons favor the the plant growth by providing nutrients for prolong period of time,
use of biochar for enhancing soil fertility and increasing plant growth. improvingsoil fertility and also mitigating environmental issues of
Thus, initially the nutrients supplied by the BNC can enhance the seed global warming and land contamination that arises due to volatilization
germination which ultimately improves the plant growth and yield. and leaching of nutrients from conventional fertilizers. Hence, synthe-
sized BNC can be considered as economical, viable and ecofriendly
4. Conclusion material for sustainable agriculture.
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A. Lateef, et al. Environmental Nanotechnology, Monitoring & Management 11 (2019) 100212
Fig. 10. Release pattern of nutrients (Fe2+/3+, Zn2+, Ca2+,Mg2+,NO31−, Na2O,P2O5 and K2O) for 14 days in soil.
Acknowledgment Ding, Y., Liu, Y., Liu, S., Li, Z., Tan, X., Huang, X., Zeng, G., Zhou, L., Zheng, B., 2016.
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