Manuscript Details

Manuscript number IJBIOMAC_2019_4250

Title Synthesis and characterization of Nano-zeolite Based Composite Fertilizer and

its Slow release Study

Article type Research Paper

Abstract
In this research work, we have proposed macronutrients incorporated slow release basis nano-fertilizer using nano-
zeolite as carrier. Simple chemical approach was used to synthesis nano-zeolite composite fertilizer (NZCF) and
characterized by different techniques including powder XRD, FT-IR, SEM, and TG/DTA. A considerable increase was
observed in soil quality, water retention capacity, swelling ratio, equilibrium water content of NZCF as compared to the
commercial fertilizer which is favourable for plant growth. A laboratory study on proposed nano-fertilizer and
conventional fertilizer were studied to evaluate their effect on soil quality and plant growth in ambient temperature.
Moreover, the slow release studies of macro-nutrients confirmed the long-term availability of nutrients to the plant
which has a great potential in promoting plant growth. Hence, it can be assumed that the prepared nanocomposite
fertilizer can be safely used as environment friendly nutrients for plant growth.

Keywords Nano-zeolite; micro-nutrients; nano-fertilizer

Manuscript category Carbohydrates, Natural Polyacids and Lignins

Corresponding Author Md. Zaved Khan

Order of Authors Md. Zaved Khan, Md. Riajul Islam, Nazmeen Nahar, Md. Rashid Al-Mamun, Md.
Abu Shamim Khan, Matin MD. A.

Suggested reviewers Md. Ikram Hossain, Md. Aziz, Xiuhua LIU, Zennat Ferdousi

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Editor-in-Chief

International Journal of Biological Macromolecules

Dear Editor,

I wish to submit an original article for publication in your well reputed journal, titled “Synthesis
and characterization of Nano-zeolite Based Composite Fertilizer and its Slow release Study”.

This manuscript has not been published or presented elsewhere in part or in entirety and is not
under consideration by another journal. We have read and understood your journal’s policies, and
we believe that neither the manuscript nor the study violates any of these. There are no conflicts
of interest to declare. The manuscript has been read and approved by all named authors.

Thank you for your consideration. I look forward to hearing from you.

Yours Sincerely,

Dr. Md. Zaved Hossain Khan

Associate Professor
Dept. of Chemical Engineering
Jessore University of Science and Technology
Jessore 7408, Bangladesh
Phone (office): +88 0421 62020 Ext. 282
Fax: +88 0421 61199
Mobile: +8801763387455
 Abstract

In this research work, we have proposed macronutrients incorporated slow release basis nano-
fertilizer using nano-zeolite as carrier. Simple chemical approach was used to synthesis nano-
zeolite composite fertilizer (NZCF) and characterized by different techniques including powder
XRD, FT-IR, SEM, and TG/DTA. A considerable increase was observed in soil quality, water
retention capacity, swelling ratio, equilibrium water content of NZCF as compared to the
commercial fertilizer which is favourable for plant growth. A laboratory study on proposed nano-
fertilizer and conventional fertilizer were studied to evaluate their effect on soil quality and plant
growth in ambient temperature. Moreover, the slow release studies of macro-nutrients confirmed
the long-term availability of nutrients to the plant which has a great potential in promoting plant
growth. Hence, it can be assumed that the prepared nanocomposite fertilizer can be safely used as
environment friendly nutrients for plant growth.
1
2
3
4 Synthesis and characterization of Nano-zeolite Based
5

Composite Fertilizer and its Slow release Study

6
7
8
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10 M. Z. H. Khan1, M. R. Islam1, N. Nahar1, M. R. Al-Mamun1, M. A. S. Khan2, M.
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12
A. Matin3
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1Dept. of Chemical Engineering, Jashore University of Science and technology, Jashore 7408,
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16 Bangladesh
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2Environmental Laboratory, Arsenic Center, Asia Arsenic Network, Jashore-7400, Bangladesh
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19 3Dept.
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of Glass and Ceramic Engineering, Bangladesh University of Engineering and
21 Technology, Dhaka 1000, Bangladesh
22
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24 *Corresponding Author: Dr. Md. Zaved H Khan (zaved.khan@just.edu.bd)
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26
27
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29 In this research work, we have proposed macronutrients incorporated slow release basis nano-
30
31 fertilizer using nano-zeolite as carrier. Simple chemical approach was used to synthesis nano-
32 zeolite composite fertilizer (NZCF) and characterized by different techniques including powder
33
34 XRD, FT-IR, SEM, and TG/DTA. A considerable increase was observed in soil quality, water
35
retention capacity, swelling ratio, equilibrium water content of NZCF as compared to the
36
37 commercial fertilizer which is favourable for plant growth. A laboratory study on proposed nano-
38
39 fertilizer and conventional fertilizer were studied to evaluate their effect on soil quality and plant
40 growth in ambient temperature. Moreover, the slow release studies of macro-nutrients confirmed
41
42 the long-term availability of nutrients to the plant which has a great potential in promoting plant
43
growth. Hence, it can be assumed that the prepared nanocomposite fertilizer can be safely used as
44
45 environment friendly nutrients for plant growth.
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47
48
49
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51 Keywords: Nano-zeolite; nanoparticles; micro-nutrients; nano-fertilizer; sustainable release
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62 1. Introduction
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64
Now a day’s conventional fertilizer using in agriculture to yield excellence production is the
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66 common trade worldwide but the large-scale use of commercial fertilizer decreases the soil nutrient
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use efficiency [1,2]. Heavy metals may enter into the soil, plant system and food chain due to
69 excess application of fertilizer which is a great threat on lives [3]. All over the world the total
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71 demand of nitrogen is calculated to be 112.9 million tons for 2015 but about 60-75% of nitrogen
72 losses in fertilizing section [4]. Therefore, the extent presence of commercial fertilizer pollutes
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74 both underground and surface water causing nitrate contamination and eutrophication. The toxic
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76
chemicals that are releasing from fertilizers by water run off reaches the oceans, river, ponds etc.
77 and causes great damage to ecosystem. The use of conventional fertilizer creates huge wastes of
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79 fertilizer and effects directly or indirectly various health concern and bad impact on economic
80 sector.
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It’s a great challenge to produce sufficient crops with these limited lands for the overpopulation
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84 without damaging soils nutrients. During last decades, nanotechnology create a new era for its
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86 unique properties to controlled delivery of pesticides, fertilizers, nutrients, genetic materials and
87 holding plants essential nutrients for long time [5–7]. The term “Nano” means 10-9 or one billionth
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89 part of a meter with at least one dimension less than 100 nm. Nano fertilizer means nano sized
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fertilizer which contains nanoparticles & encapsulation of nutrients and can release micro and
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92 macro nutrients systematically to targeted sites which is specific in plants. In nano fertilizer the
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94 nanostructured elements incorporated in a carrier complex by absorption or adsorption in a matrix
95 such as chitosan, poly acrylic acid, clay or zeolite [2,8,9]. Nano porous zeolite attracts the attention
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97 in farming to increase the fertilizer use efficiency of crops over the adverse effect of chemical
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fertilizer on the agriculture ecosystems. Due to its high surface area, mesoporous structure, and
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100 nutrients loading capacity, zeolite becomes a noble and slow release nanocarriers to enhance the
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102 nutrient retention capacity of soil [10,11].
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106 In general, macronutrient is used to increase soil fertility which in turn help in plant growth [12].
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108 The addition of macronutrients in the farming land is essential due to lack of minerals and nutrients
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contents. The primary and secondary macronutrient such as potassium, nitrogen, phosphorus,
117 silicon, calcium etc. are important for plant gardening and cultivation. To improve the nutrients
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119 use efficiency and to prevent the loss of nutrients to the environment, nano-fertilizers and
120 nanocomposites widely used as a slow release fertilizer in farming [13]. Incorporation of various
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122 macro and micro nutrients in zeolite effectively reduce nutrients deficiencies of soil as reported by
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many researchers [12–16].
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128 The present work deals with the synthesis and characterization of macro-nutrients incorporated
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nano-zeolite fertilizer. Nutrient uptake capacities and slow release study of proposed composite
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131 fertilizer were also studied. A comparative study of prepared fertilizer with commercial fertilizer
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133 on lettuce plantation was also undertaken.
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2. Materials & method
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142 2.1 Chemicals and reagents
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144 All the chemicals used in the experiment are of analytical grade and used without further
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purification. Deionized water was used for all sample preparations.
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150 2.2 Synthesis of nano-zeolite
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152 Nano-zeolite was prepared by using simple co-precipitation method as described in literature [17].
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154 At first, sodium silicate solution (73.3g/100ml distilled water) and 8.33ml ethylene glycol was
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mixed in a three necked round bottom flask which was fitted with reflux condenser and rapid fit
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157 dropping funnels. Then, the mixer was stirred for 30 min with magnetic stirrer at a temperature of
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50-60°C. After that pre-prepared aluminum sulphate solution (26.23g/83ml) and sodium
160 hydroxide solution (10g/83ml) were added drop wise while stirring and maintaining the same
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162 temperature. After completing the reaction, the solution PH was neutralized. Later, the sample was
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filtered, dried at the temperature of 105°C and finally was annealed at 650°C to get the desired
173 porous grey colored zeolite.
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2.3 Preparation of nano-composite fertilizer
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180 NZCF was prepared by impregnated the macro-nutrients into nano-zeolite. In DI water (150ml),
181 30g of nano-zeolite was added and 5% solution of macro nutrients (Na, P, K, Ca, Mg, S) in the
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183 form of their salts (NaH2PO4. 2H2O, MgSO4. 7H2O, Ca3(PO4)2, KCl, and NaNO3) were added
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which were stirred for 3h. Finally, the solution was filtered, oven dried at 105°C, and blended at
186 12000 rpm to get fine grinded particles of NZCF which was stored in air tight container to avoid
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188 any kind of moisture attachment.
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190 2.4 Treatment of NZCF on plants
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192 To ensure the acceptability of prepared fertilizer, lettuce plants were treated with NZCF. Two other
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194 experiments were carried out with commercial NPK fertilizer and in order to compare the plant
195 growth, development, life span and translocation. All experiments were conducted under outdoor
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197 conditions for 6 weeks. Both experiments were carried out with same quality compost soil and
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standard doses of NPK fertilizer was added according to Agricultural Ministry of local
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200 government.
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202 2.5 Characterization of nanocomposite
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To identify the presence of functional groups, Fourier transform infrared spectra (FTIR) study was
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206 performed having a resolution of 1 cm-1 in the wavelength range 500-4000 cm-1. X-ray diffraction
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208 (XRD) measurement was done to investigate the structural behavior and formation of as-
209 synthesized NZCF. Debye-Scherer equation was used to calculate the size of different
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211 nanoparticles and the surface morphology was investigated by scanning electronic microscope
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(SEM). TG/DTA analyses were done to understand the weight loss and reaction type of
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214 synthesized NZCF.
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2.6 Salt index (SI) analysis
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1g prepared fertilizer was taken in a beaker and 1g of sodium nitrate (NaNO3) in another beaker
229 with 200ml of distilled water. The SI was measured as a ratio of conductivities of two solution [21.
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231 The equation for calculating salt index is:
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electrical coductivitivity of 1g fertilizer in water
233 SI = × 100% (1)
234 electrical coductivitivity of 1g NaNO3 in water
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236
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238 2.7 Swelling ratio (SR) and equilibrium water content (EWC) analysis
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240 Swelling ratio is expressed as the raise in the weight of sample due to water soak. In this study 1g
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242 fertilizer was taken and dipped in 200ml of distilled water. After that the sample was allowed to
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swell for 24 hours at ambient temperature and pressure. Finally, after filtration the weight of wet
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245 sample was monitored.
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247 The SR and EWC of the fertilizer can be determined by
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249 𝑊𝑠 ‒ 𝑊𝑑
250 SR= 𝑊𝑑
(2)
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254 𝑊𝑠 ‒ 𝑊𝑑
255 EWC = 𝑊𝑆
× 100% (3)
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257
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260 Where, Ws = the wet weight of fertilizer
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262 Wd = the dry weight of fertilizer
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2.8 Water absorption capacity (WA) analysis
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269 Water absorption is the percent of water that a plant can absorb the maximum amount of moisture
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for a certain period. To calculate the water absorbance capacity1g of sample was taken (w1). Then
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272 two petri dishes were weighed (w2). Later, the petri dishes with sample was kept in desiccator in
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wet environment for 5 days. After 5 days, the sample (w3) re-weighed with petri dishes and
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calculate the water absorption capacity. The following equation was used to determine the water
285 absorbance capacity of the NZCF.
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287 𝑊3 ‒ 𝑊2
288 WA = 𝑊1
× 100% (4)
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293 2.9 Water Retention Capacity (WR) analysis
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295 Two pre-weighted cups A (WA) and B (WB) was used to measure water retention capacity (WR).
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In cup A, 50.0 g sieved soil was mixed with 30 ml distilled water. Whereas, in cup B, 2.0 g of
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298 NZCF was mixed with 50 g soil followed by addition of 30 ml distilled water. Later, both cups
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300 were reweighed (WA1 andWB1) after water was allowed to seep through them for 24 h. Finally,
301 the cups were weighted daily for next 30 days by keeping in a glass box as described in literature
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303 [31]. To calculate WR, the following equation was followed-
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305
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307 𝑊2
308 WR=𝑊 × 100% (5)
1
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2.10 Slow release studies
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315 Slow release studies were performed for both water and soil to understand the leaching pattern of
316 NZCF for 4 weeks. The experiment was conducted in glass column using 5.0g of NZCF and pre-
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318 analyzed soil and tap water. For slow release study in water, 25 ml water was collected daily and
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the nutrients quantity was determined. On the other hand, for slow release study of soil, 50 ml
321 water was collected daily from a column of soil saturated with180 ml pre-analyzed tap water. The
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323 nutrients release pattern was checked by analyzing collected water and soil samples.
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328 3. Results and Discussion:
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3.1 Characterization of NZCF:
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Powder X-ray diffraction (XRD) analysis was performed to study the effect of different
341 modification on structure stability of modified zeolite-based NZCF and presented in Fig. 1a. The
342
343 intensity peak observed at 2θ values of 23.51,25.7, 28.2 and 31.7 corresponding to low crystalline
344 structure of nano-zeolite. The observed spectrum well matched with CCDC No- 01-074-1183 of
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346 sodium aluminium silicate [18]. Moreover, new peaks appeared in the NZCF are belong to
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incorporated macronutrients.
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367 Fig. 1. Powder XRD (a) and FTIR spectra (b) showing the nature of of NZCF
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The FTIR pattern of HNF shows (Fig. 1b)the characteristic peaks at wave number 1039.2 and
373 776.4 cm-1 are assigned to bending and stretching of Al-O and Si-O in nano-zeolite structure [19].
374
375 The other peaks observed at 1627.7 and 593.4 cm-1 may be attributed to the incorporation of
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macronutrients in the zeolite structure. The wide peak near 3400 cm-1 represents the bridging of
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378 OH- due to the moisture content in the porous structure of nano-zeolite [18].
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380 TG and DTA analysis were conducted to study the stability and thermal degradation pattern of
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382 prepared composites and presented in Fig. 2. The observed smooth weight loss throughout the
383 study is typical for zeolites as reported by other researchers [13,17,18]. A slight weight loss of
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385 about 3% was observed after 100 °C, which could be assigned to loss of physically absorbed water
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and almost no weight loss was observed from 310 to 630 °C. However, slow but continuous
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decrease in weight loss was observed for NZCF till a total weight loss of approximately 9.1%.
397 However, two exothermic peaks were observed in DTA curve at 30 and 600 °C for nano-zeolite.
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419 Fig. 2. TG/DTA spectra of nano-zeolite (a) and NZCF (b) showing minor weight loss.
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424 SEM measurement was performed to study the surface morphology of the as-prepared nano-zeolite
425 and NZCF and presented in Fig. 3. An average size of 40 nm was calculated for zeolite
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427 nanoparticle. Figure 3b represents the image of NZCF which represents the spongy nature of
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prepared samples due to the incorporation of macronutrients in nano-zeolite porous structure.
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Fig. 3. SEM images of as-prepared nano-zeolite (a) and NZCF
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475 3.2 Physical parameters test:
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477 To calculate the potentiality of prepared NZCF to cause plant injury, SI measurement was
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479 conducted. The SI value was found approximately 11.38, which is much lower than that was
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reported for urea fertilizer. The low value of SI shows that the proposed fertilizer is suitable for
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482 the seed row placement. The equilibrium water content (EWC), water absorbance (WA) and
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swelling ratio (SR) were studied for as-prepared NZCF. The measured amount for EWC, WA, and
485 SR is 77.2, 80, and 3.3% respectively.
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Moreover, water retention (WR) value was calculated to study the water holding capacity of NZCF
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489 mixed soil. Figure 4 represents the WR value of blank soil and fertilizer mixed soil. It was
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observed that the WR capacity of NZCF was 83.8, 81.5, and 66.8% on the day of 5th, 10th and 15th
492 respectively, whereas, the value was 59.8, 47.5, and 33.2 % for blank soil on the same days. The
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494 27% higher WR rate for NZCF mixed soil presents its higher water holding capacity which is
495 essential for saving water to improve plants health.
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526 Fig. 4. Water retention capacity of soil with and without NZCF
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Slow release study was conducted both in soil and water separately to observe the release pattern
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530 of specific nutrients from prepared fertilizer. Table 1 represents a 14 days nutrient release studies
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532 in soil and water after addition of NZCF. The observed trend of nutrients release from 1-14 days
533 favors continuous nutrient supply to plants which prevent leaching loses. On the other hand,
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535 Rajaeifar et al. have reported about high leaching loses with traditional fertilizer [18]. The slow
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release of nutrients facilitates the growth of healthy plant by early seed sprouting and germination.
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541 Table 1. Physicochemical properties of soil and water with and without NZCF
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543 Parameter Blank Tap Soil with NZCF Water with NZCF
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545 soil water 24 h 7 days 14 days 24h 7days 14 days
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547 pH 8.9 7.9 8.3 7.8 7.5 7.2 7.0 7.0
548
Conductivity (µs/cm) 675 568 827 720 756 590 582 605
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550 TDS (mg/l) 315 230 374 380 378 330 378 350
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552 Ca2+ (mg/l) 105.8 80.6 109.0 126.6 138.3 99.2 101.3 105.3
553 Mg2+ (mg/l) 0 0 44.7 45.7 47.9 37.9 53.48 60.4
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555 PO43- (mg/l) 4.84 0.25 5.45 5.95 7.23 0.43 0.52 0.73
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NO2- (mg/l) 0.01 0.08 0.5 1.58 1.60 0.2 0.8 1.24
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3.3 Application on plant
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572 To study the application of prepared NZCF on lettuce plantation, different parameters were tested.
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Chemical fertilizers (NPK) in doses recommended by the Local Agriculture Ministry were added
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575 at the rate of 1kg/42m2) and blank soil was used as a control. On the other hand, NZCF was added
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at the rate of 10g/42m2, which is 100 times less than that of rate of commercial fertilizer. Plant
578 height [cm], number of branches/leaves etc. were recorded and presented in Fig. 5. The data
579
580 revealed that NZCF treatment has pivotal effect on plants. They significantly increased all growth
581 parameters of lettuce plants in comparison with control (plants receiving recommended dose of
582
583 NPK fertilizers) as shown in Fig. 6. The beneficial effects of these NZCF treatments on lettuce
584
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plant are due to improved soil’s physical, chemical and biological properties and nutrient
586 availability as evident by decreased soil pH, higher TDS and water retention in addition to
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588 availability of elements to be absorbed by plant roots.
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608 Fig. 5. The comparison of the height and leaves of lettuce plant with different fertilization period
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635 Fig. 6. Images of lettuce plants after different fertilizer treatment; (a) blank soil; (b) commercial
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NPK; and (c) NZCF fertilizer
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638
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641
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643 4. Conclusion
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645
646
Our results suggest that nano-zeolite incorporated with macronutrients leads to a functional nano-
647 fertilizer. It can be demonstrated that nano-zeolite based proposed composite fertilizer allows a
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649 slow release of important nutrients for plants. It was observed that proposed fertilizer shows a
650 better plantation of lettuce at a 100 times lower concentration that of NPK fertilizer due to
651
652 improved soils physical, chemical and biological properties and nutrient availability. It can be
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concluded that introduction of nanotechnology in fertilizer can significantly reduce the amount of
655 chemicals used while maintaining crop yield.
656
657
658
659
660
661
662 References:
663
664 [1] Guo H, White JC, Wang Z, Xing B. Nano-enabled fertilizers to control the release and use
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 Data in brief
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