Nutrient release properties of a urea–magnesium–natural
rubber composite coated with chitosan ⇤ Muhammad Adlim , Fitri Zarlaida, Ratu Fazlia Inda Rahmayani, Rauzaton Wardani Chemistry Department, FKIP, Universitas Syiah Kuala, Darussalam Banda Aceh, 23111, Indonesia
The most effective nutrient source in modern agriculture are urea-based fertilizer. However, excessive release of nutrients from fertilizers containing urea, and soluble salts may cause water pollution due to the escape of ammonia and nitrates and dissolved salt into water (Conrad and Fohrer, 2009; Qiao et al., 2016). Urea decomposes in water subsequently converted into ammonia, ammonium hydroxide, and finally into nitrate before absorbed by the plant. Some nutrients were washed out by rain or drifted away from the plant. During the decomposition process, some of the ammonia evaporates before hydrolyzed into ammonium ions, undergoing nitrification and finally being absorbed by the plant. Nitrogen loss from urea decomposition is affected by elevated temperature and soil’s pH. Only 38.2–44.8% of nitrogen fertilizer is taken up by the rice crop (Rahman et al., 2014). In addition to nitrogen, plants also require magnesium, which is involved in the formation of chlorophyll, carbohydrates, fats, oils, and it also plays a role in phosphate transport. Magnesium is also an activator for various enzymes involved in photosynthesis, respiration, and DNA and RNA reactions (Guo et al., 2016). Magnesium sulfate (kieserite) is commonly used as magnesium fertilizer. This salt is water soluble, which is needed to control the release. One of the alternatives to increase fertilizer efficiency, to reduce soil toxicity is the use of slow release fertilizers (SRFs) (Xiang et al., 2008) including sulfur-coated urea (SCU). Other SRFs are prepared by coating them with synthetic polymers, which are potentially pollutant (Azeem et al., 2014). SRFs are reported to have drawbacks such as complicated manufacturing, expensive production costs, non-biodegradable polymer matrices, and non-environmentally friendly mixtures (Naz and Sulaiman, 2016).
Studying the green fabrication for SRFs is crucial (Wang et al., 2017). Some materials that are environmentally friendly and compatible with urea and magnesium compound are chitosan, latex, and rice husk ash (Adlim et al., 2018a). We studied the appropriate composition and the compatibility in previous works (Adlim et al., 2018b, 2017). Studies on the magnesium–chitosan pair were reported by Mansour et al. (2017) and Zima et al. (2017). Karunanayake and Perera (2006) studied the magnesium-latex composite; chitosan–rubber interaction was demonstrated by Paoribut et al. (2015). Studies on urea–chitosan mixture was performed by Hussain et al. (2012). Interaction between urea and Mg was previously reported in case of coating urea with dolomite (Babadi et al., 2016). However, the interactions within single composite of SRFs have not been fully understood. This study aims to explore the effect of magnesium and chitosan coating on release characteristics of urea, ammonium, nitrate and magnesium ions in water.
2. Material and methods
2.1. Materials and equipment
Chitosan medium molecular weight (⇠400,000, Sigma, Singapore), urea (prilled/crystal), rice husk ash (from rice milling waste). Liquid natural rubber latex from Havea bracileansis, and magnesium sulfate heptahydrate (p.a grade. Merck) were used in this study. The experiments were performed using a UV/Vis Spekol 2000 spectrophotometer, a trinocular Olympus CX41 microscope with camera DP12, a microscope stereo bellstone with optical camera, a Kjeldahl equipment and the chemicals for N total analysis for Kjeldahl method.
2.2. Experimental procedures
Preparation of rice husk ash (RHA) and Liquid natural rubber (LNR) from Havea bracileansis (rubber plant grown in Aceh, Indonesia) was done following the previous reports, including the tablet formula (Adlim et al., 2017). The formula of urea–Mg slow release (UMgSR) tablets contained 60 gram of RHA, 20.8 g of urea, and 9.6 g of MgSO4 .7H2 O. The mixture was stirred with a mixer to obtain homogeneous matrix, which was then inserted into a tablet dies and pressed with a hydraulic press at 100 N m2 . Air-dried tablets were dipped into chitosan solution (0.6 g of chitosan in 100 ml of 1.5% v/v acetic acid) for 2 min and filtered off. Then the UMgSR tablets were dried at 105 C for 1 h. Three randomly selected dried tablets were weighed and each tablet was then dipped into 25 mL water for 30 min, air dried for 1 h and weighed with an analytical balance. The mean difference between the weights of dried and wet tablets was counted as the water absorption by tablets. Randomly, one UMgSR tablet was immersed into 250 mL distilled water, which is known as static soak or incubation. The incubation was maintained the ambient temperature (around 28 C) and covered up with plastic film to avoid evaporation. Sampling was carried out in every three days with probes being previously stirred gently by using a mechanical stirring rod. Five milliliters of the aliquots was taken for urea determination using a spectrophotometric method using p-dimethylamino-benzaldehyde as complexing agent and the absorbance was recorded at 420 nm (Husain et al., 2002). Three UMgSR tablets were randomly selected and each tablet was immersed into 250 mL distillated water. Every 3 days it was taken 5 mL of the aliquots was taken and diluted up to 25 mL. A phenol solution (1 mL), sodium nitropruside (1 mL), and sodium hypochlorite (2.5 mL) were added into the sample. The mixture was stirred until it adopted a yellowish color and was then incubated for one hour. Finally the absorbance was recorded by using Spectrophotometer-UV, Perkin Elmer Lambda XLS. The same tablet-immersion procedure followed in ammonia-release experiment was repeated for studying the nitrate release. The dilute solution (10 mL) was pipetted and added 1 sachet nitraVer-5-reagent into a sample bottle. The mixture was then shaken homogeneously before being analyzed using a DR/850 colorimeter. Tablet-immersion procedure was repeated in magnesium release experiment. A 5-mL of aliquot every 3 days and diluted up to 25 mL before being analyzed by using atomic absorption spectroscopy method. A tablet was sampled, ground, and dissolved in 5 mL of concentrated HCl to determine the total magnesium content in tablet. The excessive HCl was evaporated in a water-bath before transferring, filtering and diluting up to 250 mL.
3. Result & discussion
The UMgSR tablets had cylinder shape with thickness and diameter of 1 cm. The materials and the composition were suitable for creating tablets and some LNR droplets formed micro-aggregations with diameter of ±2 µm in the tablet surface, as shown in scanning electron microscope (SEM) image in Fig. 1. The UMgSR tablets were stable in water at least for 12 days of incubation, and they were physically stable during a friction test in rotary evaporator. The mean water content of each dried UMgSR tablet of UMgSR was 20.6±0.5 wt%. After immersed in water, each tablet absorbed water up to 71.8±1 wt%. M. Adlim, F. Zarlaida, R.F.I. Rahmayani et al. / Environmental Technology & Innovation 16 (2019) 100442 3
Fig. 1. SEM images of slow release UMgSR tablet; (a) surface of rice husk ash in the tablet (b) some of LNR aggregated droplet ( ± 2 µm) within the tablet.
3.1. Urea release
The amount of urea release from tablet per day during immersion in water was defined as dissolution rate (DR), and urea DR from various SR-urea-tablets was not significantly different for the tablets with different formula during 12 days of incubation, as shown in Fig. 2. Generally, the urea release was around 0.5–1.5% in 12 days. After 12 days of incubation a significant different percentage of urea was released from tablets with different formula, and the urea DR increased to 3– 5% after 17 days of immersion. Without any magnesium inside the tablet, the percentage of urea release from the chitosan coated samples was higher than that of the uncoated one. In presence of magnesium, the reverse trend was observed. The urea release from uncoated tablets (5%wt) was much higher than that the coated ones (1.5%wt). The highest urea DR was 0.992%wt per day. This rate is slower than DR of commercially available slow release polymer-coated sulfur coated urea, which releases up to 30–60% in 7 days of incubation (http://www.agri-nutrients.com/msds/xcu.pdf). The DR of prill urea was much faster, namely, 75 wt% loss in >0.5 h (Xiaoyu et al., 2013; Sempeho et al., 2014). The rate of urea release in this study is considered to be slow because the standardize value for slow release urea was below 15% in 24 h or <75% release in 28 days (Naz and Sulaiman, 2016). Controversy on urea DR as the effect of chitosan coating and magnesium presence in the composite might be referred to these the following theories. In absence of magnesium ions, urea in LNR matrix inside the tablets is absorbed by chitosan coating and is then released faster into water (Xue and Wilson, 2016; Johns and Rao, 2009). This implies that chitosan coating apparently is not effective, although urea DR is still considered to be slow compared to slow-release standard (Naz and Sulaiman, 2016). However in presence of magnesium, the urea DR was slower due to interaction between trace of ammonium hydroxide in LNR with magnesium ions in the composite. Ammonium hydroxide reacted with magnesium ions and subsequently make LNR become solid (Mansour et al., 2017). Urea is then trapped in solid rubber matrix, which finally leads to a slower DR. This finding seems to agree with the previous study that showed that magnesium sulfate can hold urea from excessive release due to conversion urea into ammonium hydroxide (Rheinbaben, 1987). The hypothesis described above might be supported by these FTIR spectra. Interaction between LNR and urea however neither obvious differences found among FTIR spectra, except for interaction of Chi–Mg2+ . The interaction between magnesium and chitosan led to shift of FT-IR band from 3450 cm 1 (in pure chitosan) into 3250 cm 1 (a broader band for in chitosan–Mg). This indicates a shift of the stretching-vibration of –NH2 , which overlapped with –OH band, and might be related to possible binding Mg2+ at amino group of chitosan (Chen et al., 2014). The interaction exists but is considered weak as reported previously (Zima et al., 2017; Bodek, 2007).
3.2. Ammonia release
In nature, urea is converted to ammonia then into nitrate.
CO(NH2 )2 + H2 O ! NH2 COONH4 NH2 COONH4 + H2 O ! (NH4 )2 CO3 (NH4 )2 CO3 ! 2 NH3 + CO2 + H2 O NH3 + H2 O ! NH4 OH NH4 OH ! NH+4 + OH nitosomonas nitrobacter NH+ 4 ! NO2 ! NO3 +O2 +1/2 O2 4 M. Adlim, F. Zarlaida, R.F.I. Rahmayani et al. / Environmental Technology & Innovation 16 (2019) 100442
Fig. 2. Urea release from SR-Urea tablets prepared in various compositions.
Fig. 3. Ammonia release from slow release tablets prepared in various compositions.
Without magnesium sulfate, ammonia DR of the chitosan coated tablets was faster than that of the uncoated ones (Fig. 3). The initial release rate first increased with incubation time, but at longer incubation time it tended to be slower. The tablets containing magnesium sulfate coated with chitosan showed a slower ammonia release compared to those without chitosan coat. This is consistent with the effect of magnesium in urea release case as described above. Combination of chitosan coating and addition of magnesium sulfate in tablet formula effectively retarded urea release.
3.3. Nitrate release
The tendency of nitrate release apparently increased with the incubation time as shown in Fig. 4. The highest rate of nitrate release was 0.633 ppm per day. Tablets containing magnesium sulfate and chitosan coat delayed the nitrate release. This trend also followed the release pattern of the nitrogen supply from released urea and the urea conversion into ammonia as describe above. In presence of chitosan coat, magnesium bond to chitosan, which weaken the absorption capacity of magnesium toward ammonia and nitrate from urea conversion (Bodek, 2007). Otherwise, without magnesium ions, the dissolved nitrate was finally absorbed by chitosan coating film and released into water. This theory was supported by previous reports on chitosan-nitrate absorption (Chatterjee and Woo, 2009) & Jaworska (2014). M. Adlim, F. Zarlaida, R.F.I. Rahmayani et al. / Environmental Technology & Innovation 16 (2019) 100442 5
Fig. 4. Nitrate release from slow release tablets prepared in various compositions.
3.4. Magnesium release
Magnesium release from the tablet without additional of MgSO4 .7H2 O was very slow, namely, between 0.1–0.4 ppm in 3–12 days as shown in Fig. 5 (a–c). The only possible source of magnesium in control experiment was from RHA and natural rubber. The release rate was nearly twice as fast as that of control if the tablets were coated with chitosan (Fig. 5c). The effect of urea on magnesium release was not significant (Fig. 5b). In the presence of additional magnesium compounds in the composite, the release was 0.72±0.4 ppm per day or 0.07% per day compared to the mean total magnesium weight within a single tablet in the incubation volume (250 mL) of water, which was 1096 ppm. Chitosan coating in this tablet accelerated magnesium release up to 0.99±0.6 ppm or 0.1% per day within 250 mL of water (incubation medium). However, the rate is slower than that of commercial magnesium fertilizer, which exhibits 16.7% loss magnesium-ions per day in kieserite and 1.47% in per day in slow release synthetic magnesium sulfate (SMS) (Härdter et al., 2004). This DR is in the range of plant uptake for magnesium ions, so fertilizing should be efficient. A typical magnesium-uptake value by ryegrass (Lolium perenne L.) is 0.74 mg per pot per day (which is equivalent to 0.15 ppm per day), assuming the volume of total plant is 5 liters (White and Munro, 1981). Magnesium uptake in rice plant (Oriza sativa L) experiment was 0.25–1.2 nmol h 1 per root or 6.0 ⇥ 10 3 –28.8 ⇥ 10 3 ppm h 1 per root (Tanoi et al., 2011). Since magnesium is one of the components in these slow release tablets, its release is affected by chitosan coating but not significantly affected by presence of urea in the composite. As seen in Fig. 5(a) magnesium release from chitosan coated tablets is much higher than from the control. Magnesium release from tablet containing urea without a chitosan coating was not significantly different from that of control (Fig. 5b). The effect of chitosan coating in accelerating magnesium release was confirmed in urea–chitosan coating composite as shown in Fig. 5(c–d). Whenever the urea slow release tablet were coated with chitosan, the magnesium releases from inside tablet increases significantly. This might be explained by tendency of magnesium ions to act as a Lewis acid in the presence of chitosan, which contains lone pair electrons as Lewis bases but with weak bonding. Chitosan takes magnesium ion from inside to the surface of tablet; these are subsequently released and finally dissolved in water. The preferable formulation for urea slow release tablet containing magnesium involves coating with chitosan to control urea release. Although the chitosan coating cause higher magnesium-ions leaching, the rate is still within range of the plants’ magnesium uptake. In absence of magnesium, chitosan coating did not strongly retard urea release compared to a control sample. Coating also protected the tablet from fungi growth (Adlim et al., 2018a). This finding confirmed a previous study that reported that urea loss from a bentonite matrix was proportional to the increase in chitosan content in the composite (Hamid et al., 2013).
4. Conclusion
Nutrient release from UMgSR tablets was affected by chitosan coat, magnesium content, and by a combination of both. The nutrient release rate was generally slower than the DR of related commercial SRFs, fulfilling the standard rate of SRFs and remaining within the plant-uptake range. The ammonia release followed the same trend of the urea-leaching 6 M. Adlim, F. Zarlaida, R.F.I. Rahmayani et al. / Environmental Technology & Innovation 16 (2019) 100442
Fig. 5. Magnesium release from slow release urea tablet during incubation time. Figure (a–c): tablet without additional magnesium compound, Figure (d): tablet containing additional magnesium compound.
process, and nitrate formation increased with incubation period. The chitosan coating did not strongly retard urea release, unless the composite contained magnesium sulfate. The coating also caused a faster magnesium release but the DR was comparable to plant’s magnesium uptake.
Acknowledgments
We highly appreciated research fundings provided by Universitas Syiah Kuala, Aceh Province Indonesia in 2017 and 2018 financial years with Research Grant number: 1442/UN11/SP/PNBP/2017. Also grant number of 287/UN11/SP/PNBP/2018.
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Characterization of Ammonia Adsorption on Corn Husk Biomass Particles Using Adsorption Isotherm and Mechanical Adsorption Methods_Kelompok 7 (1) (1) (1)
Characterization of Ammonia Adsorption on Corn Husk Biomass Particles Using Adsorption Isotherm and Mechanical Adsorption Methods_Kelompok 7 (1) (1) (1)
