Hindawi Publishing Corporation

e Scientific World Journal

Volume 2015, Article ID 574201, 12 pages
http://dx.doi.org/10.1155/2015/574201

Research Article
Improving Ammonium and Nitrate Release from
Urea Using Clinoptilolite Zeolite and Compost Produced from
Agricultural Wastes

Latifah Omar,1 Osumanu Haruna Ahmed,1,2,3 and Nik Muhamad Ab. Majid3
1
Department of Crop Science, Faculty of Agriculture and Food Sciences, Universiti Putra Malaysia,
Bintulu Sarawak Campus, 97008 Bintulu, Sarawak, Malaysia
2
Agriculture and Environment, Borneo Ecosystem Science Research Centre, Faculty of Agriculture and Food Sciences,
Universiti Putra Malaysia, Bintulu Sarawak Campus, 97008 Bintulu, Sarawak, Malaysia
3
Institute of Tropical Forestry and Forest Product (INTROP), Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia

Correspondence should be addressed to Osumanu Haruna Ahmed; [email protected]

Received 18 November 2014; Accepted 27 January 2015

Academic Editor: Ayako Oyane

Copyright © 2015 Latifah Omar et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Improper use of urea may cause environmental pollution through NH3 volatilization and NO3 − leaching from urea. Clinoptilolite
zeolite and compost could be used to control N loss from urea by controlling NH4 + and NO3 − release from urea. Soil incubation
and leaching experiments were conducted to determine the effects of clinoptilolite zeolite and compost on controlling NH4 + and
NO3 − losses from urea. Bekenu Series soil (Typic Paleudults) was incubated for 30, 60, and 90 days. A soil leaching experiment
was conducted for 30 days. Urea amended with clinoptilolite zeolite and compost significantly reduced NH4 + and NO3 − release
from urea (soil incubation study) compared with urea alone, thus reducing leaching of these ions. Ammonium and NO3 − leaching
losses during the 30 days of the leaching experiment were highest in urea alone compared with urea with clinoptilolite zeolite and
compost treatments. At 30 days of the leaching experiment, NH4 + retention in soil with urea amended with clinoptilolite zeolite and
compost was better than that with urea alone. These observations were because of the high pH, CEC, and other chemical properties
of clinoptilolite zeolite and compost. Urea can be amended with clinoptilolite zeolite and compost to improve NH4 + and NO3 −
release from urea.

1. Introduction of soils (e.g., clay and humus); therefore, NH4 + leaches less
in mineral soils which are particularly high in clay [3].
Depending on soil pH, moisture, and application methods, In contrast, NH4 + leaching is significant in coarse-textured
urea undergoes chemical transformation to produce either sands and some muck soils [4]. Thus, agricultural systems
NH4 + or NO3 − [1]. Nitrogen from urea is subject to loss from research leading to management practices that improve N
a number of pathways of which leaching of NO3 − is one of the utilization efficiency and decrease N losses is essential [5].
most important pathways because NO3 − is extremely mobile. Nitrogen leaching loss in soils is a risk because if NO3 −
Leaching of NO3 − from urea leads to increase in NO3 − is not absorbed by the plant root system, it is leached below
concentrations in surface and ground water [2]. Leaching the root zone of plants, thus contaminating groundwater
losses of N occur when soils have more incoming water [6]. According to Paramasivam et al. [7], optimization of
than they can hold. As water moves through the soil, NO3 − irrigation and avoidance of fertilization during rainy seasons
in the soil solution moves along with the water. Because could minimize leaching loss of N. However, this approach
NH4 + is positively charged, it is held by the negative sites can be difficult to achieve because rapidly growing crops
2 The Scientific World Journal

require adequate N fertilizer. Leaching loss of N can be 2. Materials and Methods

reduced by minimizing the amounts of NH4 + and NO3 −
in soils. However, this is a challenge because it requires 2.1. Selected Chemical Properties of Soil, Clinoptilolite Zeolite,
simultaneous management of N fertilizers and water. Loss and Compost. The soil used in this study was Bekenu Series
of mineral N from agricultural systems is difficult to achieve (Typic Paleudults). The soil was sampled at 0–20 cm depth
through reduction of N fertilizers use [8]. One of the better from an uncultivated area at Universiti Putra Malaysia,
methods of reducing losses of mineral N is the use of Bintulu Campus Sarawak, Malaysia. The soil was air-dried
clinoptilolite zeolite. and ground to pass a 2.0 mm sieve for initial characterization,
Clinoptilolite zeolite can be used to control N loss from incubation, and leaching experiments. Field capacity and
urea because of the small molecular size of the open-ringed bulk density of the soil were determined by the method
described by Tan [26]. Soil field capacity was measured using
structure of clinoptilolite zeolite which physically protects
a graduated cylinder. This procedure involves calculation of
NH4 + ions against microbial nitrification [9]. Clinoptilolite
the water percolate in a measuring cylinder. A 10 g soil was
zeolite is a mineral with a unique structure which allows
weighted into a funnel, the base of it filled with Whatman
entrapping or releasing various cations due to its high cation filter paper number 2 to avoid losing of soil. Afterwards, a
exchange capacity [10]. Adoption of management techniques 100 mL of distilled water was poured onto the soil in cylinder
such as clinoptilolite zeolite utilization, which maximizes N and let to drain. All the water drained from the soil by gravity
use efficiency and water use efficiency, may decrease the was considered the field capacity of the soil [26]. Soil bulk
excessive and unbalanced use of N fertilizers in agriculture. density was determined using the core ring method [26]. The
Unbalanced use of N fertilizers could cause environmental core ring was placed with the sharpened side down, on top
pollution [11]. Studies have shown that the use of clinoptilolite of the soil after which the core ring was gently hammered
zeolite and N fertilizers improves N use efficiency [12–15]. into the soil with hammer. Afterwards, a piece of hard wood
The increased efficiency of N utilization when urea is used was placed over the core ring until the top of it was flushed
together with clinoptilolite zeolite has been demonstrated by with the soil surface. A scoop was used to dig a small trench
a number of researchers [16–18]. on one side of the core ring. It was slightly deeper than the
As the third largest producer of chicken products in ring. Afterwards, the soil sample with the core ring was placed
Asia, chicken manure disposal is becoming a challenge in in an oven at temperature of 105∘ C for 24 hours and cooled
Malaysia. In 2012, 674 million and 637 million day-old in a desiccator. The bulk density was calculated considering
chicks and broilers, respectively, were produced [19]. Wastes the mass of oven dry soil, soil volume, diameter, weight, and
generated in the poultry farms are increasing as the poultry height of ring sampler, as well as weight of soil and ring
farming grows. The daily manure production by a laying sampler [26].
hen has been estimated as 138 g day−1 (25% dry substance) Soil texture was determined using the hydrometer
and 90 g day−1 (40% dry substance) by a broiler [20]. Large method [27]. The hydrometer method determines the texture
of soil by measuring total sand (2.0–0.05 mm), silt (0.05–
quantities of rice straw are produced every harvesting season
0.002 mm), and clay (<0.002 mm). A 50 g of soil sample was
in Malaysia. Managing this waste in Malaysia is a challenge.
weighed and placed in a blender cup. Distilled water was
In Malaysia, there is 684,000 ha of paddy fields from which added to the sample within 10 cm of the top and mixed with
1.3 million tonnes of rice straw is produced every year [21]. 4 drops of 3 M NaOH. The mixture was stirred continuously
Cocomposting these wastes to produce organic amendments until the soil suspension had a pH of 10. Then the mixture
such as compost is essential. was stirred mechanically for 15 minutes, after which it was
Cocomposting is a simple method which converts, for transferred into a 1000 mL measuring cylinder. The remain-
example, chicken manure and rice straw into valuable organic ing soil residue in a blender cup was sprayed with distilled
amendments. The process of cocomposting is essential for water until volume of the sample in a 1000 mL measuring
aforementioned wastes to be safely, conveniently, and effi- cylinder was made up to 1130 mL. The soil suspension was
ciently used as soil organic amendment [22]. This is because stirred continuously for a homogenous mixture. Afterwards,
during cocomposting, a large part of the original organic a hydrometer was used to measure first reading after 40
matter is mineralized and the residual organic matter is seconds. The suspension was stirred six times and after 40
transformed into new organic materials (e.g., humic-like seconds, the hydrometer was inserted in the suspension
substances such as humic and fulvic acids). Application to obtain second reading. The suspension temperature was
of compost in agriculture is very desirable worldwide as recorded after removing the hydrometer from the suspension.
compost is most often used to improve soil structure and Average of two readings gave the amount of silt and clay
content of soil organic matter [23]. However, the effects in grams of the soil sample. The suspension was stirred
of compost addition to soil on the fate of mineral N are thoroughly after 2 hours of settling time and the third
scarcely studied. For example, there is dearth of information reading was obtained to get the amount of clay in grams. The
on improving NH4 + and NO3 − release from urea using temperature of the suspension was recorded shortly after the
clinoptilolite zeolite and composts. Thus, the objective of this hydrometer was dipped into the suspension for every reading
study was to determine the effects of clinoptilolite zeolite and because the hydrometer was calibrated at 20∘ C [27].
compost (produced by cocomposting rice straw and chicken The pH of the soil was determined in a ratio of
manure) on controlling NH4 + and NO3 − loss from urea. 1 : 2 (soil : distilled water suspension) using a digital pH
The Scientific World Journal 3

meter [28]. A 10 g of soil was weighed and placed in plastic 5 min. A 10 mL of boric acid with bromocresol green and
vials. Distilled water of 20 mL was added and shaken at methyl red indicator was used to trap NH4 + . Afterwards,
180 rpm for 15 minutes [28]. The reading for pH in water the distillation was continued by adding 0.2 g Devarda’s alloy
was recorded after 24 hours. A digital pH meter (Seven Easy to the sample and the process of distillation proceeded for
Mettler Toledo) was used to record pH reading. Soil organic another 5 minutes. The distillates of NH4 + and NO3 − were
matter, C, and N were determined using LECO CHNS titrated with 0.01 M HCl. The texture of the soil was sandy
Analyzer (LECO Truspec Micro Elemental Analyzer CHNS, loam with a bulk density of 1.51 g m−3 . The texture of the soil
New York). A 2.2 mg ground soil (250 𝜇m) was placed on and bulk density are consistent with those reported in Soil
the loading head of the machine. Samples were combusted at Survey Staff [33]. The selected chemical properties of the soil
1075∘ C and the reading of total C and N was obtained directly are summarized in Table 1. The soil pH, total N, and total C
from computer software. The loss of weight represented the were consistent with those reported for Bekenu Series [24].
weight of C and organic matter content was estimated by The exchangeable Ca, Mg, and K in this study were higher
multiplying organic matter value; 58% of organic matter is than the reported values [24].
C [29]. Soil available P was extracted using the double acid The clinoptilolite zeolite used in this study was in powder
method [26] followed by the blue method [30]. A 5 g of soil form. Total N of the clinoptilolite zeolite was determined
was weighed and placed in a 250 mL Erlenmeyer flask. A using Kjeldahl method [31]. 0.5 g of clinoptilolite zeolite was
20 mL extracting solution was added and shaken mechani- mixed with 5 mL concentrated sulfuric acid (H2 SO4 ) and
cally at 180 rpm for 10 minutes. Afterwards, the supernatant digested. A tablet of selenium catalyst was added, shaken,
was filtered using Whatman filter paper number 2. and left to equilibrate for 30 minutes. The samples were then
Acid molybdate stock solution (Reagent A) and ascorbic digested at 180∘ C for 1 h and then at 320∘ C for 4 to 5 h until
acid stock solution (Reagent B) were prepared for colour samples were colourless. 10 mL of the digested sample was
development procedure. A standard P solution (standard pipetted into 50 mL distillation flask and added with 10 mL
solution 1) and standard solution 2 were prepared and used 40% NaOH. 10 mL of boric acid plus indicator solution was
to prepare working solutions ranging from 0 to 0.6 ppm. 0, placed at the end of the condenser in the distillation apparatus
1, 2, 3, 4, 5, and 6 mL of standard solution 2 were pipetted to trap NH3 released. The mixture was distilled until the boric
into 50 mL volumetric flask using micropipette and added acid-indicator solution doubled the original volume. The
with 8 mL of Reagent B to develop the blue colour. A 4 mL distillate solution was titrated with 0.01 M HCl to estimate
of the supernatant was pipetted into 50 mL volumetric flask. N content in the clinoptilolite zeolite. The pH, exchangeable
Reagent B of 8 mL was added to develop the blue colour. NH4 + , and available NO3 − of the clinoptilolite zeolite were
This solution was diluted to mark with distilled water and determined using the method described previously [28, 32].
maximum blue colour was allowed to develop [30]. The The CEC of the clinoptilolite zeolite was determined using the
absorbance was measured at 840 nm. Standard curve was CsCl method [34]. The procedure is similar to the procedure
prepared by pipetting 0, 1, 2, 3, 4, 5, and 6 mL of the P of soil CEC determination as outlined previously but 1 M of
standard solution into 7 series of 50 mL volumetric flasks. CsCl instead of 1 M NH4 OAc was used. The CsCl method
Samples including standard solution were read using UV-VIS was used to avoid underestimation of CEC of the clinop-
spectrophotometer (Perkin Elmer Lambda 25, USA). tilolite zeolite as the method does not lead to entrapment of
Exchangeable cations were extracted using the leaching ammonium ions in the channels of the clinoptilolite zeolite.
method [26]. A 10 g soil was placed in a leaching tube and The exchangeable K, Ca, and Mg of the clinoptilolite zeolite
leached with 100 mL NH4 OAc solution for 5 hours. Their were extracted using the method of Ming and Dixon [34] and
concentrations in the extract were determined using Atomic their concentrations determined using Atomic Absorption
Absorption Spectrophotometry (Analyst 800, Perkin Elmer, Spectrophotometry (Analyst 800, Perkin Elmer, Norwalk,
Norwalk, USA). Soil CEC was determined by leaching the USA). The chemical composition of the clinoptilolite zeolite
soil samples with 100 mL of 1 M NH4 OAc for 5 hours [26]. used in this study is summarized in Table 2.
Afterwards, the soil sample was washed with 30 mL of 95%
The selected chemical characteristics of the compost were
ethanol. The leachate was collected in a 100 mL volumetric
determined using standard procedures as outlined previously
flask and distilled water was added to make up volume of a
100 mL volumetric flask. A 10 mL of sample from leachate was [26–32]. The selected chemical properties of the compost
pipetted into distillation flask and added with 10 mL of 40% produced by cocomposting rice straw and chicken manure
NaOH. The samples were distilled for 5 minutes and collected are summarized in Table 3. Values were obtained from our
with 10 mL of 2% boric acid with bromocresol green and previous study on cocomposting rice straw and chicken
methyl red indicator [31]. Then, the distillate was titrated with manure (paper under review). Total N of the compost was
0.01 M HCl [26]. The method of Keeney and Nelson [32] was 1.80% (Table 3). Carbon to N ratio of the compost was
used to extract exchangeable NH4 + and available NO3 − after 15.17. Humic acid content, ash content, NH4 + , NO3 − P, Ca,
which their concentrations were determined using steam Mg, and K concentrations increased after the cocomposting
distillation. A sample of 5 g soil was extracted with 50 mL of process (Table 3). The lower concentrations of Cu, Fe, Mn,
2 M KCl solution and shaken for 1 hour. Afterwards, it was Zn, and microbial biomass of the compost suggest that
filtered using Whatman filter paper number 2. Exchangeable the compost is stable, mature, and not toxic. The seeds
NH4 + was determined by pipetting 20 mL of extractant into germination rate of maize (Zea mays L.) tested on compost
distillation tube, added with 0.2 g of MgO, and distilled for and distilled water (control) using the method described by
4 The Scientific World Journal

Table 1: Selected chemical properties of Bekenu Series.

Value obtained
Property Standard data range∗
(mean ± SE)
CEC (cmolc kg−1 ) 7.43 (±0.15) 8.0–24
pHwater 4.66 (±0.10) 4.60
Exchangeable calcium (cmolc kg−1 ) 1.41 (±0.05) 0.01
Exchangeable magnesium (cmolc kg−1 ) 1.53 (±0.05) 0.21
Exchangeable potassium (cmolc kg−1 ) 0.60 (±0.02) 0.19
Total nitrogen (%) 0.15 (±0.01) 0.04–0.17
Organic matter (%) 2.06 (±0.10) nd
Total carbon (%) 1.20 (±0.60) 0.57–2.51
Available phosphorus (mg kg−1 ) 4.16 (±0.13) nd
Exchangeable ammonium (mg kg−1 ) 19.85 (±0.68) nd
Available nitrate (mg kg−1 ) 5.16 (±0.09) nd
Note. ∗ Standard data range reported by Paramananthan [24]; nd = not determined.
Values in parenthesis represent standard error of the mean.

Table 2: Selected chemical properties of clinoptilolite zeolite. Table 3: Selected chemical properties of compost by cocomposting
rice straw and chicken manure.
Present study
Property Reference∗ Property Value obtained∗ (mean ± SE)
(mean ± SE)
pH 6.80 (±0.03) 8-9 pH value 7.66 (±0.07)
CEC (cmolc kg−1 ) 100.33 (±0.35) 160 Humic acid (%) 15.20 (±0.32)
Total nitrogen (%) 1.18 (±0.04) 1.36 EC (ds m−1 ) 1.15 (±0.02)
Calcium (mg kg−1 ) 18,400 (±19.09) 25,600 Total carbon (%) 27.32 (±0.42)
Magnesium (mg kg−1 ) 11,200 (±4.48) 15,000 Organic matter (%) 47.09 (±0.73)
Potassium (mg kg−1 ) 14,850 (±10.17) 22,600 Total nitrogen (%) 1.80 (±0.06)
Ammonium (mg kg−1 ) 12.60 (±0.43) nd C/N ratio 15.17∗∗
Nitrate (mg kg−1 ) 11.58 (±0.18) nd Ammonium (mg kg−1 ) 294 (±2.84)
Nitrate (mg kg−1 ) 161 (±5.23)
Note. CEC = cation exchange capacity, nd = not determined. ∗ Data were
obtained from Luxurious Empire Sdn. Bhd., Kulaijaya, Malaysia. Values in Total phosphorus (mg kg−1 ) 458.20 (±5.50)
parenthesis represent standard error of the mean. Calcium (mg kg−1 ) 14,080 (±6.91)
Magnesium (mg kg−1 ) 15,350 (±3.92)
Potassium (mg kg−1 ) 27,720 (±2.72)
Zucconi et al. [35] and spinach (Spinacia oleracea) growth on Iron (mg kg−1 ) 13.10 (±0.42)
peat-based growing medium (control) [36] and compost was Zinc (mg kg−1 ) 11.80 (±0.15)
not significantly different, suggesting that the compost is not
Copper (mg kg−1 ) 12.40 (±0.21)
phytotoxic.
Manganese (mg kg−1 ) 2.10 (±0.05)
The humic acid fractions after the composting process
were extracted with 0.5 M NaOH, precipitated at pH 1.0 Note. ∗ Values were obtained from our previous study on cocomposting
rice straw and chicken manure (paper under review). Values in parenthesis
with 6 M HCl, and then purified with 100 mL distilled water represent standard error of the mean. ∗∗ Carbon to N ratio was calculated by
[37]. The carboxyl and phenolic contents of the humic acid dividing the percentage of C by the percentage of N.
extracted from the compost were determined according to
the method described by Stevenson [38]. 20 mg of humic acid
was dissolved in 4 mL of 0.08 M NaOH and shaken for 30 on solution of 3 mg of each humic acid in 10 mL of 0.05 M
minutes at 180 rpm. The solution was titrated against 0.01 M NaHCO3 . The ratio of absorbance at 465 nm and 665 nm gave
HCl to pH 2.5. Phenolic content was determined based on the E4 /E6 ratio [25]. The selected chemical properties of the
the amount of acid required to titrate the solution from pH humic acid extracted from the compost are shown in Table 4.
10 to pH 8 and it was estimated that 50% of the phenolic
group dissociates from pH 10 to pH 8 [39]. Carboxylic content 2.2. Soil Incubation Experiment. A soil incubation experi-
was calculated based on the amount of acid needed to titrate ment was carried out for 90 days in the Soil Science Labora-
the solution from pH 8 to pH 2.5 and the total acidity was tory of Universiti Putra Malaysia, Bintulu Sarawak Campus,
calculated by the summation of carboxylic and phenolic Malaysia. The treatments evaluated in this experiment were
content [39]. To obtain the E4 /E6 ratio of the humic acid,
the absorbance at 465 nm and 665 nm was measured using (i) 250 g soil (no urea) (T0),
UV-Vis spectrophotometer (Perkin Elmer Lambda 25, USA) (ii) 250 g soil + 7.40 g urea without additives (T1),
The Scientific World Journal 5

Table 4: Selected chemical properties of humic acid extracted from zeolite + compost). The experimental design of the soil leach-
compost. ing experiment was completely randomized design (CRD)
with three replications. Analysis of variance (ANOVA) was
Property Value obtained Tan∗ [25] used to detect treatment effects whereas Tukey’s test was used
(mean ± SE)
to compare treatment means at 𝑃 ≤ 0.05. The Statistical
E4 /E6 7.73 (±0.07) 7-8
Analysis System version 9.2 was used for the statistical tests.
Phenolic (cmolc kg−1 ) 300 (±6.42) 240–540
Carboxyl (cmolc kg−1 ) 450 (±10.39) 150–440
Total acidity (cmolc kg−1 ) 750 (±8.08) 500–700 3. Results and Discussion
∗
Note. Values in parenthesis represent standard error of the mean. Value
obtained from previous study [25]. 3.1. Soil Incubation Study. Days of incubation significantly
affected total N, exchangeable NH4 + , and available NO3 − but
did not affect soil pH at 30 DAI, 60 DAI, and 90 DAI (Table 5).
(iii) 250 g soil + 7.40 g urea + 6 g clinoptilolite zeolite (T2),
(iv) 250 g soil + 7.40 g urea + 6 g compost (T3), 3.2. Soil Total Nitrogen and pH as Affected by Treatments and
Period of Incubation. The effects of urea without additives
(v) 250 g soil + 7.40 g urea + 6 g clinoptilolite zeolite + 6 g (T1) and urea with additives (T2, T3, and T4) on total N at 30
compost (T4). DAI were not significantly different (Figure 1). However, total
N in the soil was significantly higher in T4 compared with
The rates of urea [40], clinoptilolite zeolite [41], and
T0 and T1 at 60 DAI. Soil total N was significantly higher in
compost were scaled down from the standard fertilizer
T3 and T4 compared with urea without additives (T1) at 90
recommendation for Zea mays L. cultivation [42]. The soil,
DAI (Figure 1). These results suggest that mixing urea with
urea, clinoptilolite zeolite, and compost used in the incuba-
soil resulted in greater urea mineralization at 30 DAI and 60
tion experiment were thoroughly mixed manually. Beakers
DAI, but urea mixed with compost (T3) and the combination
(500 mL) with treatments were sealed with a parafilm. The
of clinoptilolite zeolite and compost (T4) were more effective
parafilm was perforated to enable good aeration. The sam-
in retaining N at 90 DAI. The higher total N in T3 and T4
ples were incubated for 30 days, 60 days, and 90 days at
as compared with T1 at 90 DAI is consistent with the higher
26∘ C, respectively. Each treatment had 3 replications (i.e., 15
organic matter (47.09%) of the compost used in this study
samples for 30 days of incubation, 15 samples for 60 days
(Table 2). This is possible because, in composts, N is present
of incubation, and 15 samples for 90 days of incubation). At
in the form of stable organic N which is slowly but steadily
30 days, 60 days, and 90 days of incubation (DAI), the soil
released over time through mineralization. Mineralization of
samples were air-dried and analyzed for pH in water [28],
organic N in composts involves the conversion of organic
total N using the Kjeldahl method [31], whereas NH4 + and
forms of N to NH3 or NH4 + and NO3 − [1].
NO3 − contents were determined using the method of Keeney
and Nelson [32]. The retention of soil total N in T4 could also be due to
absorption of NH4 + and NO3 − into the clinoptilolite zeolite
lattice [9, 16]. This is possible because of the high CEC
2.3. Soil Leaching Experiment. The soil leaching experiment
comprised the same treatments as in the incubation experi- (100 cmolc kg−1 ) of the clinoptilolite zeolite used in this study.
ment. All treatments were thoroughly mixed and scaled down According to Ferguson and Pepper [9], zeolites decreased
to the amount of 64 g soil. The mixture was then filled in N concentration in soil solution by trapping NH4 + through
leaching tubes and leached with distilled water after which the cation exchange. Besides retaining large quantities of NH4 + ,
leachates were collected at three-day interval based on five- these minerals also interfere with the process of nitrification
year rainfall data obtained from the Sarawak Meteorological [9, 16].
Department, Malaysia [43]. Afterwards, the leachates were Urea with clinoptilolite zeolite (T2) significantly
analyzed for NH4 + and NO3 − using the method of Keeney increased soil pH compared with those of soil alone (T0) and
and Nelson [32] whereas the pH of the leachates was deter- urea without additives (T1) at 30 DAI and 90 DAI but not at
mined using a digital pH meter (Seven Easy Mettler Toledo). 60 DAI (Figure 2). The soil pH was higher in T3 (urea mixed
The volume of the distilled water used was based on rainy days with compost) and T4 (urea mixed with clinoptilolite zeolite
over 30 days. The volume of the distilled water used every and compost) compared with T0 (soil alone) and T1 (urea
three days in the leaching experiment was 36 mL. The soil alone) at 30 DAI, 60 DAI, and 90 DAI, respectively. The
samples at 30 days of the leaching experiment were analyzed higher pH in T2, T3, and T4 was because soil pH increases
for total N, exchangeable NH4 + , and available NO3 − using the with urea hydrolysis. As urea hydrolyzes, NH4 + , OH− , and
standard procedures as outlined previously [31, 32]. CO3 2− ions are released to increase soil pH [44]. The pH
of the compost (7.66) may have partly contributed to the
2.4. Statistical Analysis. The soil incubation experiment was a increase in soil pH (Figure 2). Conversion of organic N to
split-block experimental design in triplicate with two factors, NH4 + for instance is very slow when pH is in the range of 5
namely, time of incubation (30 days, 60 days, and 90 days) and to 6 [45]. According to Weier and Gilliam [45], nitrification
treatments (soil alone, soil + urea, soil + urea + clinoptilolite decreases when soil pH is low (pH 5 to 6). This explains the
zeolite, soil + urea + compost, and soil + urea + clinoptilolite lower total N in T0 and T1 at 30, 60, and 90 DAI (Figure 1).
6 The Scientific World Journal

Table 5: Significant levels from analysis of variance (ANOVA) to determine the effects of treatments and time on total N, soil exchangeable
ammonium, and available nitrate.
Mean square
Source of variation Degree of freedom
Total N NH4 + NO3 −
Time 2 0.291∗ 15728.8∗ 2625.4∗
Replication 2 0.002ns 132.9ns 152.9ns
Error a (time ∗ replication) 4 0.001ns 126.7ns 57.4ns
Treatment 4 0.080∗ 79170.1∗ 33608.7∗
Time ∗ treatment 8 0.004∗ 1543.4∗ 282.5∗
Error b 24 0.001 112.7 73.1
Note. ∗ indicates significance at 𝑃 ≤ 0.05. ns indicates no significance.

0.6 󳰀 󳰀 󳰀󳰀 󳰀󳰀
8
a a a a a a a 󳰀 ab󳰀 a a a󳰀󳰀 a a
7 b 󳰀󳰀
0.5 b b
6
a󳰀
Total N (%)

0.4 󳰀
b󳰀 b󳰀 ab a󳰀󳰀
5 c c󳰀 c 󳰀󳰀

Soil pH
0.3 b 4
󳰀󳰀
b
bc󳰀󳰀 3
0.2 cd󳰀󳰀
c󳰀 2
0.1 d󳰀󳰀 1
0 0
T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 T0 T1 T2 T3 T4
30 60 90
30 60 90
Days of incubation
Days of incubation

Figure 1: Effects of treatments (T0, T1, T2, T3, and T4) and periods Figure 2: Effects of treatments (T0, T1, T2, T3, and T4) and periods
(30, 60, and 90 days) of incubation on soil total N. Note. T0: 250 g soil (30, 60, and 90 days) of incubation on soil pH. Note. T0: 250 g soil
(no urea); T1: 250 g soil + 7.40 g urea (no additives); T2: 250 g soil + (no urea); T1: 250 g soil + 7.40 g urea (no additives); T2: 250 g soil +
7.40 g urea + 6 g clinoptilolite zeolite; T3: 250 g soil + 7.40 g urea + 6 g 7.40 g urea + 6 g clinoptilolite zeolite; T3: 250 g soil + 7.40 g urea + 6 g
compost; T4: 250 g soil + 7.40 g urea + 6 g compost + 6 g clinoptilolite compost; T4: 250 g soil + 7.40 g urea + 6 g compost + 6 g clinoptilolite
zeolite. Means with the same letter are not significantly different by zeolite. Means with the same letter are not significantly different by
Tukey’s test at 𝑃 ≤ 0.05. Note. Letters without prime represent 30 Tukey’s test at 𝑃 ≤ 0.05. Note. Letters without prime represent 30
DAI, single prime superscript represents 60 DAI, and double prime DAI, single prime superscript represents 60 DAI, and double prime
superscript represents 90 DAI. superscript represents 90 DAI.

3.3. Effects of Treatments and Period of Incubation on Soil as the small molecular size of the open-ringed structure of
Exchangeable Ammonium and Available Nitrate in Soil Incu- clinoptilolite zeolite (10−6 –10−9 m) physically protects NH4 +
bation Experiment. Soil exchangeable NH4 + was signifi- against microbial nitrification [9]. The absorption of soil
cantly higher in the urea with clinoptilolite zeolite and exchangeable NH4 + in urea with compost treatments (T3
compost treatments (T2, T3, and T4) than in urea without and T4) was possible because of the humic acid content
additives (T1) and soil alone (T0) at 30 DAI, 60 DAI, and (15.20%) of the compost used in this study. The carboxyl,
90 DAI, respectively (Figure 3). The higher concentrations of phenol, and total acidity of the humic acid of the compost
soil exchangeable NH4 + in T2, T3, and T4 were partly due used in this study were 450 cmolc kg−1 , 300 cmolc kg−1 , and
to increase in the pH of the soil (Figure 2) as mineralization 750 cmolc kg−1 , respectively (Table 4).
of organic N to NH4 + is enhanced by the higher pH [46]. All the mixtures (T2, T3, and T4) significantly increased
This observation could be one of the reasons why the soil soil available NO3 − at 30 DAI, 60 DAI, and 90 DAI compared
total N of T2, T3, and T4 decreased with increasing period with urea without additives (T1) as demonstrated in Figure 4.
of incubation (Figure 1). It is also possible that some of The compost reduced leaching of NO3 − from the soil because
the NH4 + released during urea hydrolysis were adsorbed of its C/N ratio (15.17) (Table 2). As reported by Kristensen
onto the exchange surfaces of clinoptilolite zeolite (T2 and et al. [48], incorporation of N rich compost, (low C/N
T4) and humic substances of compost (T3 and T4). The ratio composts) led to rapid mineralization with associated
retention of soil exchangeable NH4 + could be attributed increase in soil mineral N. At C/N ratio of 15 or less,
to the high CEC of the clinoptilolite zeolite. According to mineralization occurs, whereas above a C/N ratio of 15, N
Kithome et al. [47], NH4 + retained by clinoptilolite zeolite is is immobilized [48]. In a related study in which biosolids-
generally released slowly because of the CEC of this zeolite yard waste compost was used to hinder NO3 − leaching, Xia et
and nitrification in the soil. Retardation of nitrification in al. [49] reported that the concentrations of NO3 − -N in their
this study may have occurred due to clinoptilolite zeolite, first leachates were high but they decreased in the subsequent
The Scientific World Journal 7

350 3.4. Leaching of Ammonium and Nitrate at Three-Day Interval.

Exchangeable NH4 + (ppm)

300 a a The three-day interval losses of NH4 + and NO3 − from soil in
a
250 󳰀 a
󳰀 the leaching experiment for 30 days are presented in Figures
b󳰀 ab 5(a) and 5(b). As summarized in Figures 5(a) and 5(b), all of
200 b a󳰀󳰀 a󳰀󳰀 a󳰀󳰀
c󳰀 󳰀󳰀 the mixtures (T2, T3, and T4) significantly reduced leaching
150 b
100 of NH4 + and NO3 − from soil compared with soil alone (T0)
50
and urea alone (T1). Treatments 2 and 4 (mixtures of urea
c d󳰀 c 󳰀󳰀 and clinoptilolite zeolite) reduced NH4 + leaching because the
0
T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 clinoptilolite zeolite has high affinity for NH4 + (adsorption of
30 60 90 NH4 + in the mineral lattices of clinoptilolite zeolite) whereas
Days of incubation NO3 − was absorbed into the channels of the clinoptilolite
zeolite. Huang and Petrovic [50] found that application of
Figure 3: Effects of treatments (T0, T1, T2, T3, and T4) and periods clinoptilolite zeolite to a sandy soil reduced NH4 + and NO3 −
(30, 60, and 90 days) of incubation on soil exchangeable ammonium. concentrations in leachate and increased moisture retention
Note. T0: 250 g soil (no urea); T1: 250 g soil + 7.40 g urea (no in the soil due to increased soil surface area and CEC. Thus,
additives); T2: 250 g soil + 7.40 g urea + 6 g clinoptilolite zeolite; T3: applying clinoptilolite zeolite to soils may reduce leaching
250 g soil + 7.40 g urea + 6 g compost; T4: 250 g soil + 7.40 g urea + 6 g
of NH4 + and NO3 − . The significant reduction in leaching
compost + 6 g clinoptilolite zeolite. Means with the same letter are
of NH4 + and NO3 − in T2 and T4 reported in this study
not significantly different by Tukey’s test at 𝑃 ≤ 0.05. Note. Letters
without prime represent 30 DAI, single prime superscript represents (Figures 5(a) and 5(b)) was comparable with those reported
60 DAI, and double prime superscript represents 90 DAI. by Zwingmann et al. [51] whereby in a column experiment,
clinoptilolite zeolite was used to reduce N leaching losses in
a sandy soil.
For T3 and T4, leaching of NH4 + and NO3 − was reduced
180 a
a a a󳰀 a󳰀󳰀 (Figures 5(a) and 5(b)) because of the affinity of the functional
160
ab󳰀 a󳰀󳰀 groups such as carboxyl and phenolic in the compost for
Available NO3 − (ppm)

140 b󳰀
120 b 󳰀
b󳰀󳰀 NH4 + and NO3 − . An evidence of this is the high contents
c 󳰀󳰀
100 c of these functional groups of the humic acid (Table 4). The
80 striking effects of urea amended with clinoptilolite zeolite and
60 compost (T2, T3, and T4) on leaching of NH4 + and NO3 −
40 compared with urea alone (T1) are clearly demonstrated in
20 Figures 6(a) and 6(b) whereby the contribution of T0 (soil
c d󳰀 d󳰀󳰀
0 alone) was deducted from those of T1, T2, T3, and T4 over the
T0 T1 T2 T3 T4 T0 T1 T2 T3 T4 T0 T1 T2 T3 T4
30 days of leaching experiment (i.e., leaching losses of NH4 +
30 60 90
and NO3 − from T1, T2, T3, and T4 only).
Days of incubation

Figure 4: Effects of treatments (T0, T1, T2, T3, and T4) and periods 3.5. Cumulative Losses of Ammonium and Nitrate for Thirty
(30, 60, and 90 days) of incubation on soil available nitrate. Note. Days of Soil Leaching. Another evidence to support the
T0: 250 g soil (no urea); T1: 250 g soil + 7.40 g urea (no additives); effectiveness of T2, T3, and T4 in controlling NH4 + and NO3 −
T2: 250 g soil + 7.40 g urea + 6 g clinoptilolite zeolite; T3: 250 g leaching loss compared with T1 is presented in Figure 7. All
soil + 7.40 g urea + 6 g compost; T4: 250 g soil + 7.40 g urea + 6 g the treatments with clinoptilolite zeolite and compost (T2,
compost + 6 g clinoptilolite zeolite. Means with the same letter are T3, and T4) significantly decreased NH4 + and NO3 − leaching
not significantly different by Tukey’s test at 𝑃 ≤ 0.05. Note. Letters losses compared with urea without additives (T1). Treatments
without prime represent 30 DAI, single prime superscript represents
3 and 4 significantly minimized NH4 + and NO3 − leaching
60 DAI, and double prime superscript represents 90 DAI.
losses partly because the compost served as a source of
organic matter for N stabilization in the soil. This is because N
is stored in soils in organic form; thus the quantity and nature
leachates for all compost amended media. The higher soil of organic matter and its decomposition in the soil have effect
available NO3 − at 30 DAI, 60 DAI, and 90 DAI in T2 and on the long-term availability of N. The clinoptilolite zeolite in
T4 compared with urea alone (T1) as presented in Figure 4 T2 and T4 was able to retain NH4 + because of the specific
was because of the presence of clinoptilolite zeolite. This is selectivity of the clinoptilolite zeolite for NH4 + [9]. This is
possible because of the clinoptilolite zeolite’s ion exchange one of the reasons why clinoptilolite zeolite is widely used as
system which enables absorption of anions such as NO3 − and absorbent agent to capture N, after which the captured N is
phosphates [10]. The significant increase in the soil available stored and released slowly for plant use [47].
NO3 − at 30 DAI, 60 DAI, and 90 DAI in T4 Figure 4 was also
partly because of the increase in soil pH (due to pH of the 3.6. Retention of Soil Exchangeable Ammonium and Available
compost). It is widely accepted that high pH has significant Nitrate at Thirty Days of Leaching Experiment. At the end
effect on availability of NO3 − as it influences nitrification of the leaching experiment (30 days of leaching), urea with
and denitrification. Loss of NO3 − to N2 O and NO emissions clinoptilolite zeolite and compost (T2, T3, and T4) showed
increase under low soil pH [45]. significant concentrations of soil exchangeable NH4 + and
8 The Scientific World Journal

70 25

Ammonium (ppm)
60
20

Nitrate (ppm)
50
40 15
30 10
20
10 5
0 0
3 6 9 12 15 18 21 24 27 30 3 6 9 12 15 18 21 24 27 30
Days of leaching Days of leaching
T0 T3 T0 T3
T1 T4 T1 T4
T2 T2
(a) (b)

Figure 5: Ammonium and nitrate leached at three-day interval over 30 days of leaching experiment. Note. T0: 64 g soil (no urea); T1: 64 g
soil + 7.40 g urea (no additives); T2: 64 g soil + 7.40 g urea + 6 g clinoptilolite zeolite; T3: 64 g soil + 7.40 g urea + 1.54 g compost; T4: 64 g soil
+ 7.40 g urea + 1.54 g compost + 6 g clinoptilolite zeolite. Note. Bar represents standard error of the mean.

50 14
Ammonium (ppm)

40 12

Nitrate (ppm)
10
30 8
20 6
4
10
2
0 0
3 6 9 12 15 18 21 24 27 30 3 6 9 12 15 18 21 24 27 30
Days of leaching Days of leaching
T1 T3 T1 T3
T2 T4 T2 T4
(a) (b)

Figure 6: Ammonium and nitrate leached at three-day interval over 30 days of leaching for T1, T2, T3, and T4 effects only. Note. T1: 64 g soil
+ 7.40 g urea (no additives); T2: 64 g soil + 7.40 g urea + 6 g clinoptilolite zeolite; T3: 64 g soil + 7.40 g urea + 1.54 g compost; T4: 64 g soil +
7.40 g urea + 1.54 g compost + 6 g clinoptilolite zeolite. Note. Bar represents standard error of the mean.

available NO3 − compared to urea without additives (T1) application of compost to soils improved soil physical prop-
(Figure 8). Soil exchangeable NH4 + and available NO3 − were erties by increasing water holding capacity and porosity.
lower in urea without additives (T1) at the end of leaching
study because they were leached as discussed previously 3.7. Soil Total Nitrogen after the Leaching Experiment. The
(Figure 7). The availability of NH4 + and NO3 − in the soil soil total N after the leaching experiment without subtracting
with clinoptilolite zeolite is possible because the channels in the contribution of T0 from T1, T2, T3, and T4 is shown in
clinoptilolite zeolite effectively absorbed NH4 + and NO3 − and Figure 9(a) and after subtracting the contribution of T0 is
released them slowly. The high affinity of the clinoptilolite presented in Figure 9(b). The higher concentrations of soil
zeolite for NH4 + in particular is due to the small size of total N in T2, T3, and T4 (urea with clinoptilolite zeolite and
channels that protect NH4 + from excessive nitrification [9]. compost) than in T1 suggest that both clinoptilolite zeolite
In a related study, clinoptilolite zeolite was used to improve and compost ensured slow release of urea-N. For T1 (urea
soil retention of NH4 + . The use of clinoptilolite zeolite also alone), retention of total N was lower compared with urea
minimized the conversion of NH4 + to NO3 − [16]. with clinoptilolite zeolite and compost (T2, T3, and T4)
The compost in T3 and T4 improved retention of soil because N was lost due to leaching of NH4 + and NO3 − as
exchangeable NH4 + and available NO3 − compared with urea discussed previously in Figures 5, 6, 7, and 8.
without additives (T1) partly due to the ability of the compost
to increase water holding capacity of soils. Due to this, 3.8. The pH of Leachate over 30 Days of Leaching. The
leaching of NH4 + and NO3 − is reduced. This is possible pH of leachate over 30 days of leaching is summarized in
because leaching losses of N occur when soils have more Figure 10. The lower pH in T1 (urea alone) compared with
incoming water than the soil can hold. It was also reported the treatments with clinoptilolite zeolite and compost (T2,
that the slow release nature of compost-N renders leaching of T3, and T4) observed in this study explains the loss of N as
NO3 − -N [52]. As reported by numerous researchers [53, 54], discussed previously. The pH of leachate in T1 was lower from
The Scientific World Journal 9

500 200 a
a
b b b
400 b
b b 150
Ammonium (ppm)

Nitrate (ppm)
300
c
100
200
c
50
100

0 0
T0 T1 T2 T3 T4 T0 T1 T2 T3 T4
Treatments Treatments
(a) (b)
350 100
a a
300
b 80
250 b
Ammonium (ppm)

b
b b
Nitrate (ppm) 60 b
200

150 40
100
20
50

0 0
T1 T2 T3 T4 T1 T2 T3 T4
Treatments Treatments
(c) (d)
Figure 7: Cumulative amounts of ammonium and nitrate leached over 30 days of leaching experiment (a, b). Cumulative amounts of
ammonium and nitrate leached (after subtracting the contribution of T0) over 30 days of leaching experiment (c, d). Note. T0: 64 g soil
(no urea); T1: 64 g soil + 7.40 g urea (no additives); T2: 64 g soil + 7.40 g urea + 6 g clinoptilolite zeolite; T3: 64 g soil + 7.40 g urea + 1.54 g
compost; T4: 64 g soil + 7.40 g urea + 1.54 g compost + 6 g clinoptilolite zeolite. Means with different letters indicate significant difference
between treatments by Tukey’s test at 𝑃 ≤ 0.05. Note. Bar represents standard error of the mean.

45 35
a
40 a a ab
30
a b
35
25
Ammonium (ppm)

30
Nitrate (ppm)

25 b 20
c
20 15
15
10
10
c 5 d
5

0 0
T0 T1 T2 T3 T4 T0 T1 T2 T3 T4
Treatments Treatments
(a) (b)
Figure 8: Retention of soil exchangeable ammonium and available nitrate after 30 days of leaching experiment. Note. T0: 64 g soil (no urea);
T1: 64 g soil + 7.40 g urea (no additives); T2: 64 g soil + 7.40 g urea + 6 g clinoptilolite zeolite; T3: 64 g soil + 7.40 g urea + 1.54 g compost;
T4: 64 g soil + 7.40 g urea + 1.54 g compost + 6 g clinoptilolite zeolite. Means with different letters indicate significant difference between
treatments by Tukey’s test at 𝑃 ≤ 0.05. Note. Bar represents standard error of the mean.
10 The Scientific World Journal

0.9 0.8
a
0.8 a 0.7 a
a a
0.7 a 0.6
0.6

Total nitrogen (%)

Total nitrogen (%)

0.5
0.5
0.4
0.4 b
b
0.3
0.3
0.2
0.2

0.1 0.1
c

0 0
T0 T1 T2 T3 T4 T1 T2 T3 T4
Treatments Treatments
(a) (b)

Figure 9: (a) Total nitrogen retained in soil at 30 days of leaching and (b) total nitrogen retained in soil after 30 days of leaching (after
subtracting the contribution of T0). Note. T0: 64 g soil (no urea); T1: 64 g soil + 7.40 g urea (no additives); T2: 64 g soil + 7.40 g urea + 6 g
clinoptilolite zeolite; T3: 64 g soil + 7.40 g urea + 1.54 g compost; T4: 64 g soil + 7.40 g urea + 1.54 g compost + 6 g clinoptilolite zeolite. Means
with different letters indicate significant difference between treatments by Tukey’s test at 𝑃 ≤ 0.05. Note. Bar represents standard error of the
mean.

9 compost use. Only few experiments have led to a pH decrease

8 after compost application [52].
7
pH in leachate

6
5 4. Conclusion
4
3 Urea amended with clinoptilolite zeolite or compost, or
2
combination of clinoptilolite zeolite and compost, reduced
1
0 nitrogen (leaching of ammonium and nitrate) loss by retain-
3 6 9 12 15 18 21 24 27 30 ing ammonium and nitrate in soil. The findings in this
Treatments present study suggest that urea can be properly managed
if it is amended with clinoptilolite zeolite or compost or
T0 T3
combination of clinoptilolite zeolite and compost. Field
T1 T4
T2 application of our findings is being evaluated in our ongoing
field experiment.
Figure 10: pH in leachate at three-day interval over 30 days of
leaching experiment. Note. T0: 64 g soil (no urea); T1: 64 g soil
+ 7.40 g urea (no additives); T2: 64 g soil + 7.40 g urea + 6 g Conflict of Interests
clinoptilolite zeolite; T3: 64 g soil + 7.40 g urea + 1.54 g compost; T4:
64 g soil + 7.40 g urea + 1.54 g compost + 6 g clinoptilolite zeolite. The authors declare that there is no conflict of interests
Note. Bar represents standard error of the mean. regarding the publication of this paper.

Acknowledgments
The authors would like to acknowledge the financial support
the third day of the leaching experiment and stayed above pH (Fundamental Research Grant Scheme) from the Ministry of
6 for 15, 18, 21, and 24 days after which the pH was below Education, Malaysia, and Universiti Putra Malaysia for the
6 towards the end of leaching experiment. The formation of collaborative research.
dissolved NH3 could be the reason for lower leachate pH
in T1. This is because H+ released from NH4 + lowered pH
of the leachate. The ability of T2 and T4 to maintain the References
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