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Format sampul /cover mengikuti

contoh yang tercantum dalam


Petunjuk pelaksanaan CERCo pada
bagian III.2

Keseluruhan naskah fullpaper


ditulis menggunakan bahasa
Inggris

Chemical Engineering Research Competition 2016

THE INFLUENCED OF ACTIVATED ZEOLITE-CHITOSAN


NANOPARTICLE TOWARDS NUTRIENT RELEASED FROM UREA
FERTILIZER USING ENCAPSULIZED METHOD FOR INCREASED
SLOW RELEASE FERTILIZER EFFICIENCY

Suggested by :

Leader : ANNIZAH RAHMATYA G.21030113120076/ BATCH 2013


Member : ALFIN DARARI 24040112140090/ BATCH 2012
EKO SISWOYO 24030113140100/ BATCH 2013

UNIVERSITAS DIPONEGORO
SEMARANG
2016
Format halaman pengesahan
mengikuti contoh yang tercantum
dalam petunjuk pelaksanaan
CERCo pada bagian III.3 VALIDATION PAGE

CHEMICAL ENGINEERING RESEARCH COMPETITION

halaman pengesahan
ditandatangani oleh ketua tim,
dosen pembimbing, dan
dekan/rektor/yang mempunyai
otoritas (stempel)

Bagian kelengkapan administratif


yang meliputi halaman judul,
nama/daftar anggota kelompok,
halaman pengesahan serta kata
pengantar apabila ada, diberi nomor
halaman menggunakan angka
romawi kecil dan diketik di sebelah ii
Abstrak berisi uraian singkat penelitian yang meliputi: latar belakang, tujuan,
manfaat, metode penulisan, hasil dan saran yang direkomendasikan. Abstrak
ditulis 1 spasi, maksimal 300 kata, berbahasa Inggris
Saran :
*gunakan kalimat aktif (hindari kalimat pasif)
Nama-nama *gunakan kalimat efektif (singkat, padat, dan jelas)
penulis beserta
alamat institusinya
diketik tepat di
The Influenced of Activated Zeolite-Chitosan Nanoparticle towards Nutrient
bawah judul Released from Urea Fertilizer Using Encapsulized Method for Increased
artikel dengan Slow Release Fertilizer Efficiency.
jarak 1,5 spasi Annizah Rahmatya G, Eko Siswoyo, Alfin Darari
Drs. Suhartana, M.Si
Anggota tim terdiri dari
maksimal 3 orang, Jurusan Teknik Kimia, Fakultas Teknik, Universitas Diponegoro
MINIMAL salah satu
berasal dari program studi
Jurusan Kimia, Fakultas Sains dan Matematika, Universitas Diponegoro
TEKNIK KIMIA Jurusan Fisika, Fakultas Sains dan Matematika, Universitas Diponegoro
(dibuktika dengan Semarang
lampiran fotokopi KTM)
Abstrak
Urea is a type of chemical fertilizers that contain macronutrient elements. The
biggest content in urea is nitrogen, potassium and phosphor . Although classified
sebaiknya as a vital nutrient elements, the type of telement is not efficient for utilization.
kalimat abstrak Urea fertilizer efficiency of nutrient release has only 30%-40%. So many are not Latar belakang
dimulai dengan well absorbed by plant. To overcome these problems, author try to give solution (singkat saja)
perkenalan
tentang topik
i.e. modification of urea-activated zeolite encapsulation with Chitosan
yang diteliti nanoparticles to optimize the release of nutrient elements from urea fertilizer.
The purpose of this research is to increase the effectiveness of the formulation
fertilizer urea modification with zeolite-Chitosan-based nanotechnology in
nutrient elments release efficiency. The benefits of this research, to give solutions
Tujuan that capable to optimized absorption of nutrient elements fertilizer of urea against
the absorption by plant. The method used is the sol-gel process on synthesis and
encapsulation in manufacturing formulations. The test results with SEM 4000x Manfaat
Chitosan 182nm particle size is obtained. Results of FTIR and Chitosan shows
cluster (– NH2) at wavenumbers 1650 cm-1 and the cluster (-OH) at 3450
wavenumbers cm-1. Based on the results of study, a combination of urea,
Metode yang activated zeolite-encapsulated Chitosan nanoparticles by comparison with 40%:
digunakan 10%: 50% have is the most active formulations, where on testing content of Hasil
penelitian
nutrient elements has levels of N of 9. 8%, P by 17. 78% of K and 13. 64%.
Analysis of solubility in water obtained late-time for 5. 31 minutes. Test release
fertilizer efficiency seen that elements of the phosphor is experiencing an increase
of releases by 8. 76 at the treatment of urea into 4. 43 using the formulation was
more active. It is also visible from potassium nutrient elements from release 16.
85 down to 4. 12, so that it can be concluded the release efficiency increased 2
times better.
ditutup dengan kesimpulan penelitian

Keywords : Encapsulation, Zeolite- Chitosan Nanoparticle, Slow Release


Fertilizer

Jangan lupa mencantumkan keyword


Note : beberapa naskah abstrak tidak
lolos pada tahap awal hanya karena tidak
mencantumkan keyword

iii
FOREWORD

Praise to the Almighty God for the gift that was given to us, so that we can
solve a scientific paper entitled “The Influenced of Activated Zeolite-Chitosan
Nanoparticle towards Nutrient Released from Urea Fertilizer Using Encapsulized
Method for Increased Slow Release Fertilizer Efficiency”.
This scientific writing proposed in order to follow Chemical Engineering
Research Competition (CERCo) 2016. Hence, we thank you for the opportunity
that has been given by event organizers of CERCo 2016 for us to develop our
interest in competition in this paper. We also thank for our lecturers who have
taken the time to discuss with us and we do not forget to thank the parents that
given the blessing prayers and motivation to solve this scientific paper.
Innovation through scientific papers that we hope the knowledge we gain
from the learning process in these colleges can be more beneficial and can solve
environmental problems existing in the field of Indonesian’s animal husbandry.

Semarang, August 22th 2016


Writer

iv
LIST OF CONTENTS

TITLE PAGE ......................................................................................................... i


VALIDATION PAGE........................................................................................... ii
ABSTRACT .......................................................................................................... iii
FOREWORD ........................................................................................................ iv
LIST OF CONTENTS ...........................................................................................v
LIST OF TABLES ............................................................................................... vi
LIST OF FIGURES ............................................................................................ vii
CHAPTER 1 PRELIMINARY .............................................................................1
Background ......................................................................................................... 1
Problems .............................................................................................................. 2
Writing’s Goals ................................................................................................... 2
Writing’s Benefit ................................................................................................. 2
Systematically Writing ........................................................................................ 3
CHAPTER 2 LITERATURE ................................................................................3
Problems Release Urea Fertilizer ........................................................................ 3
Chitosan Nanoparticle ......................................................................................... 3
Activated Zeolit ................................................................................................... 4
The Method Of Encapsulation Of Urea .............................................................. 4
Mechanism of Slow Release Fertilizer ................................................................ 5
CHAPTER 3 RESEARCH METHOD.................................................................5
Writing’s Approachment ..................................................................................... 5
Writing’s Source.................................................................................................. 5
Writing’s Variable ............................................................................................... 5
Writing’s Step...................................................................................................... 6
CHAPTER 4 RESULT AND RESEARCH .........................................................8
Chitosan SEM (Scanning Electron Microscopy) Analysis ................................. 8
FTIR (Fourier Transform InfrRed) Data Analysis .............................................. 9
The Result of Activated Zeolit Analysis ........................................................... 10
Encapsulation Process of Chitosan Nanoparticle .............................................. 11
Analysis of Nutrient Content in Fertilizer ......................................................... 11
Analysis of Nutrient Elements Release with Energy Dispersy Spectroscopy ... 13
Analysis of Soil Chemical Properties ................................................................ 14
Analysis of The Solubility in Water .................................................................. 15
Analysis of Nutrient Release Efficiency .......................................................... 15
Conclusion ......................................................................................................... 16
Suggestion ......................................................................................................... 16
BIBLIOGRAPHY ................................................................................................16

v
LIST OF TABLES

Table 1. The Characterization Results of Freeze-Dried Nanoparticles Eggshell


Powder .................................................................................................................... 9
Table 2.Content Elements in Zeolit ...................................................................... 10
Table 3.Nitrogen Content ..................................................................................... 12
Table 4. Phosphorus Content................................................................................ 12
Table 5.Potassium Content ................................................................................... 12
Table 6. Analysis of Soil Physical Properties After Fertilization Process ........... 14
Table 7.Fertilizer Solubility in Water ................................................................... 15

vi
LIST OF FIGURES

Figure 1.Encapsulation Technology....................................................................... 4


Figure 2.Mechanism of Slow Release Fertilizer .................................................... 5
Figure 3.Step of Experiment .................................................................................. 6
Figure 4. a) The results of examination with SEM magnification of 1000x
chitosan, b) SEM magnification of 3000X, c) SEM magnification of 4000x......... 8
Figure 5. FTIR Chitosan Spectra ......................................................................... 10
Figure 6.Analysis of Nutrients EDS.................................................................... 13
Figure 7. EDS Analysis After Watering Them with Water for 2 Weeks ............. 14

vii
Chapter I Pendahuluan berisi: latar belakang, rumusan masalah, Bagian utama (naskah artikel)
tujuan penulisan, manfaat penulisan, sistematika penulisan. diberi nomor halaman
menggunakan angka arab 1
yang dimulai dengan nomor
Penulisan Bab dan
halaman 1 (satu) dan diketik
Subbab tidak
di sebelah kanan atas dengan
menggunakan
sistem numeral, CHAPTER 1 PRELIMINARY jarak 3 cm dari tepi kanan dan
artinya tidak ada 1,5 cm dari tepi atas
penomoran Bab dan Background
Sub-bab.
Indonesia is a country with a very large agricultural commodities. As an
agricultural country, fertilizer is the main support in the field of agriculture.
Indonesia is one of the large consumer of urea fertilizer, that is of 3.2 million
Latar belakang : berisi
tonnes per year (Ministry of agriculture, 2010). Urea is one type of chemical
informasi, data, dan
penelitian-penelitaian fertilizers used in agriculture i.e. about 3.6 million tons. Many farmers, especially
terdahulu serta for food crops using fertilizers irrationally anymore especially urea fertilizer
kelemahannya usage that range between 100 – 600 kg/ha. The efficiency of fertilization until
(maksimal 10 tahun recently perceived in agriculture is still low, especially for rice crops due to loss
terakhir, disertai sitasi),
of nutrient elements. Craswell, et al (1991) reported that the use of urea fertilizer
mengapa dilakukan
that is spread to the surface of the soil in the long time can cause the soil become
acidic and dependency to chemical fertilizers. In addition, the efficiency of
nutrient release by urea only 30%-40% , so that it becomes its own problems in
agriculture.
Beri argumen-argumen Therefore, it is necessary to other innovations to improve the efficiency of
mengapa penelitian ini nutrient release urea fertilizer. One of the efforts to reduce the loss of nutrient
penting dilakukan elements is to make nutrient elements be slow (slow release). Efforts to slow the
release of fertilizer can decrease the environmental pollution of agriculture
because of release of nutrient elements being controlled. One of the efforts to
improve the efficiency of urea fertilizer is by modifying the slow release fertilizer
fertilizers (SRF). One of the efforts is by mixing urea with ingredients that have a
cation exchange capacity (CEC) high as zeolites and Chitosan nanoparticles. By
making the fertilizer-based urea, zeolites, and Chitosan is expected to improve the
efficiency of nitrogen fertilizers. In addition, modification of zeolite and Chitosan
nanoparticle size will be very effective in nutrient absorption by plants.
According to Suwardi (1999) the addition of zeolite on nitrogen fertilizers will be
issued by ammonium menjerap fertilizer. At a time when the concentration of
nitrates in the soil decreased ammonium that have been dijerap by zeolite will be
released back into the soil solution.
tunjukkan kelebihan Chitosan is a polymer that is most abundant biodegradable. Source of
dan inovasi dari chitin and Chitosan is present on most types of crustaceans with a population of
penelitian about 70% (Muzzarelli, 1977). Some of the benefits of the Chitosan among
others: slowing the release of fertilizer nutrients by covering a large part of the
pore-water porinya so can stay signed in to dissolve through the pores that are not
covered. Therefore, Chitosan as selected upholstery because Chitosan can not
water soluble and able to coat the fertilizer (Liu, 2014), has biodegradibel,
biocompatible bonding agent, nontoxic and eco-friendly. Modification of
Chitosan application as a aims to penyalut in fertilizer, because of its ability to
withstand the release of nutrient elements gradually. Chitosan has many benefits
in a variety of fields, including agriculture. One of the benefits of chitosan in the
field of agriculture, namely increasing nitrogen fixation, where nitrogen fixation
affects plant growth. In addition to other material which has the effect on the
effectiveness of release of nutrient elements i.e. zeolite. Benefits of zeolite of
which contains many minerals that are abundant, the ability of the CEC, and keep
the pH balance of the soil (Gufron, 2013). As for the Chitosan is made in sizes

Naskah diketik 1 (satu) spasi pada kertas berukuran A4 dengan font 12,
Times New Roman, jarak pengetikan 4 cm dari samping kiri, 3 cm dari
samping kanan, 3 cm dari batas atas, dan 3 cm dari batas bawah
Jangan lupa sitasi pada setiap
kalimat yang merujuk pada
tulisan/sumber yang diperoleh 2
dari penulis lain

nano with the goal of keeping the required elements of this plant can be
appropriately absorbed by the cells of the target, because nanoparticles have a
much larger surface area against the comparative volume (Szeto, 2007).
Starting from the above problem, then research highlights against testing
the efficiency of urea nutrient release in combination with Chitosan nanoparticles
activated zeolite as a controller release nutrient elements. Blend of urea-activated
zeolite with Chitosan nanoparticles as a development of nano-fertilizers on the
expected release of nutrient enhancement capable in fertilizer. It will have an
effect on the nature of the physical, chemical, and biological in farmland. The
advantages of this fertilizer is the ability that a slow release nutrient elements
which is released slowly and continuously in a certain period of time, thereby
losing due to nutrient leaching by water.
Rumusan masalah tunjukkan
Problems penelitian memberi
banyak manfaat
The problems formulation in this study include :
1. How to improve the effectiveness of release nutrient elements from urea
fertilizer.
2. How to design method of modification urea fertilizer development
zeolite-Chitosan nanoparticles as a controller release nutrient elements.
3. How to know the effectiveness of fertilizer testing the nano as a slow
release fertilizers.

Writing’s Goals Tujuan penelitian menjawab rumusan masalah

The purpose of this study include :


1. Able to resolve the issue of release of nutrient elements fertiliser of urea
by the less than optimal
2. Improve the effectiveness of the fertilizer formulation of nano-
modification of urea fertilizers with zeolite-Chitosan-based
nanotechnology
3. Modifying urea fertilizer with Chitosan nanoparticles and zeolite as a
slow release in the release of nutrient elements
4. Perform testing slow release fertilizers,
Manfaat dari penelitian dalam pangaplikasiannya,
Writing’s Benefit
lebih ke manfaat untuk jangka panjang

The benefit of this study include:


1. Provide an alternative to the use of natural resources that are abundant
in Indonesia.
2. Provide a solution to the lack of optimal absorption of urea fertilizer
nutrients to absorption by plants.
3. Demonstrate the application of science and technology in addressing
the problem of the lack of effectiveness of the release of nutrients.
4. Patents
3

Sistematika
Systematically Writing penulisan

The systematically writing of this study include :


1. Title’s page
2. Validation Page
3. Abstract
4. Foreword
5. List of Contains
6. List of Tables
7. List of Figures
8. Chapter 1 Preliminary
9. Chapter 2 Literature
10. Chapter 3 Research Method Writing’s
11. Chapter 4 result and research
12. Bibliography
13. Attachment
Chapter II Tinjauan pustaka
merupakan kerangka konseptual berisi
CHAPTER 2 LITERATURE batasan/konsep/teori yang mendukung
penulisan yang dapat diperoleh dari
jurnal penelitian, buku, atau sumber-
Problems Release Urea Fertilizer sumber lainnya.

Indonesia is one of the largest agricultural country in the world. Fertilizer


is one of the factors supporting agriculture, where chemical fertilizers the most
widely used by farmers. In 2012, the total demand for fertilizers reached 11.1
million tons. Therefore, fertilizer is a big issue for Indonesia. The high demand
for chemical fertilizers due to the womb of high fertilizer nutrient elements and
have an important role of the field of agriculture. Although these elements are
important, but belongs to the nitrogen, potassium and phosphor is is the most
inefficient use. It is because nitrogen is easily lost through leaching in the form of
nitrate (Prima, 2009). The case occurred on potassium and phosphor is, where it
had nutrient levels high solubility in water. The ability of release of nutrient
elements in fertilizer only about 35% and in the form of long-term acid soil will
make it so that it will lead to a dependence of the use of chemical fertilizers

Tinjauan pustaka yang dimasukkan cukup singkat, tidak bertele-tele, hanya


Chitosan Nanoparticle mencakup hal-hal terkait dasar teori/konsep yang mendukung tulisan

Chitosan is a biopolymer materials that are abundant in Indonesia. This


material is easily biologically degraded, non-toxic and is good as a coagulant and
flocculant as well as easy to form the membrane or film. Chitosan is a natural
biopolymer which is a reactive chemical can make changes. Because it's much
Chitosan derivatives can be made easily. Therefore the selected ingredient
Chitosan as fertilizer because of water insoluble Chitosan and possess
biodegradable, biocompatible bonding agent, nontoxic and eco-friendly.
Modification of Chitosan application as a aims to surround in fertilizer, because
4

its ability to withstand the release of nutrient elements gradually. Chitosan has
many benefits in a variety of fields, including agriculture. One of the benefits of
chitosan in the field of agriculture, namely increasing nitrogen fixation, where
nitrogen fixation affects plant growth (Tolaimate, 2003)

Activated Zeolit

Zeolite is a crystalline mineral from the Group of tectosilicate, i.e.


alumino-silicate hydrated with alkaline and alkaline earth cations such as
potassium, sodium, calcium and magnesium that fills the cavity-cavity frame
aluminosilikat and have a three-dimensional structure. The arrangement of the
structure is (Si, Al) O4 tetrahedral, have pore containing water molecules and
cations are interchangeable. Zeolite is characterized by its ability to absorb and
excrete water and Exchange parts of kationnya without changing the structure of
the Crystal (Mumpton, 1977). The ability of the zeolite which are as agents of
the absorption and cation exchanger. In this case, the adsorbate molecules in
diameter is equal to or smaller than the diameter of the cavity can be adsorbed,
whereas the molecular diameter is larger than the pores of zeolite will be halted.
Result of a warm-up then the water will evaporate, in the circumstances of the
case, both channels cavities in the zeolite will be able to function as molecular
filters (Astiana, 1993). Zeolite which has lose water from the sockets called
zeolite that has been activated that can serve as an effective cation adsorber. In
addition to this cation exchange capability of zeolite this will lead to a level of
soil’s fertility will increase due to cation exchange of zeolite from fertilizer with
minerals that are found in agricultural land.

The Method Of Encapsulation Of Urea

Encapsulation technology is rapidly growing with many potential


applications including in the field of agriculture. Encapsulation is a process,
where small particles on the core material packaged in a wall to form a layer to
cupsle. Encapsulation method was developed to protect the bioactive components
or materials in encapsulation (Ezhilarasi, 2012).
Gambar baik dalam bentuk grafik/foto diberi
judul dengan penomoran gambar sesuai dengan
urutan kemunculannya dalam naskah
(perhatikan walaupun gambar tercantum pada
chapter 2, karena muncul pertama dalam naskah
maka diberi nomor Figure 1.). Judul gambar
ditulis di bawah gambar dengan nomor gambar
menggunakan angka arab (1,2,3,... dst). Figure 1.Encapsulation Technology
Nanoencapsulation is an encapsulation technique development innovations
are being made to get the size of enkapsulan that belongs to the very small-sized
nanometers. The application of nanotechnology is carried out as an effort to
increase the solubility of a material that is used as encapsulant, stabilize the
condition of thermal, as well as facilitate the digestibility of compound ingredients
are contained in the dienkapsulasi. Size of microencapsulation diameter between
5

3-800 µm, whereas in nanoencapsulation materials ,encapsulation only has a size


of 10-1000 nm. (Ezhilarasi, et al., 2012).

Mechanism of Slow Release Fertilizer

Fertilizer off slow (Slow Release Fertilizers) is a fertilizer with the release
mechanism of nutrient elements at regular intervals following a pattern of
absorption by the plant nutrient elements. Several mechanisms that can be
applied in the production of the SRF that is the mechanism of coating fertilizer.
The main principle of the mechanism is to create an obstacle in the form of
molecular interactions so that a fertilizer granules in the nutrient substances not
easily off to the environment. Slow release fertilizer can increase the efficiency
of absorption of fertilizer by plants to 75-80% if compared with the usual 40%
only fertilizer, fertilizing SRF applications only once done in one growing season.
Compared to chemical fertilizer urea given 2-3 times (Akelah, 2006).

Figure 2.Mechanism of Slow Release Fertilizer


Metode penulisan menyajikan langkah-langkah/prosedur yang
benar yang digunakan dalam penulisan karya ilmiah yang
CHAPTER 3 RESEARCH METHOD menguraikan secara cermat cara/metode pengumpulan
Pendekatan penulisan informasi dan atau data, analisis informasi dan atau data,
penarikan kesimpulan, serta merumuskan saran.Metode
Writing’s Approachment penulisan mencakup: pendekatan penulisan, sumber, sasaran
penulisan, tahapan penulisan.
This study using research methods which are conducted for 6 months in the
laboratory of analytical chemistry, Faculty of science and mathematics the
University of Diponegoro, Semarang.
Sumber penulisan
Writing’s Source

The source of the data used in this study i.e. from experimental results or test data
laboratoium as well as the study of literature, journal and previous research in a
comprehensive manner.
Sasaran penulisan

Writing’s Variable

Fixed Variable :
1. The main raw materials (Urea, Chitosan and Zeolite)
Independent Variable :
1. Urea composition-zeolite: Chitosan nanoparticle
Measuring Variables :
6

1. Particle size Chitosan encapsulation Agent


2. Effectiveness of release of nutrient elements

Writing’s Step Tahapan penulisan/penelitian.


Umumnya dibuat dalam bentuk bagan

Menjelaskan proses penelitian dari


bahan yang digunakan, proses yang
digunakan, cara dan metode untuk
memperoleh data, cara analisa data Figure 3.Step of Experiment

Materials
Commercial urea fertilizer, natural zeolite come from klaten, Central Java,
waste of skin shrimp, filter paper, pH paper universal comes from Hepilab, HCl
NaOH technical, aqudest, HF 1% Tween 80, NH4Cl, and ethylene glycol.

Nanoparticle Chitosan Sythesis


The process of demineralization, the first shrimp skin already mashed into
powder and then added HCl, and the mixture is heated at 80oC for 4 hours while
stirring with a 50 rpm agitator, and filtered. Solids obtained were then washed
with a solution of akuades to eliminate the remaining HCl. Then this floured
solids were dried in an oven at a temperature of 70oC for 24 hours.
Deproteination is the next stage of the process, where the skin dried shrimp
powder process results demineralization NaOH is added and stirred at a
7

temperature 90oC. Furthermore, the skin dried shrimp then muted and stirred then
dried chitin, and the result is then washed with aquades until the pH becomes
neutral. Chitin already washed coupled with ethanol 70% and continued with
filtering, then washed sediment with akuades heat and acetone to remove color,
done twice. Chitin-shaped solid powders, dried at the temperature 80oC for 24
hours. Deasetilasi is the last stage in the manufacture of Chitosan. Marinated
shrimp skins and stirred in the NaOH 60%, then the mixture is stirred and heated
at the temperature is 120oC for 4 hours. The mixture is filtered through filter
paper wollfram, the next solution titrated using HCl to precipitate back Chitosan
back into the solution so that it will be formed Chitosan

Activated Natural Zeolit


Zeolites are soaked in a solution of HF 2% for 10 minutes stirring occurs,
accompanied by discoloration of the substance originally nodes becomes white
grayish and turbid. This indicates the existence of a content of oxide-oxide
dopants and organic compounds in zeolites. Then soaked in a solution of HCl
zeolite 6 M for 30 minutes, changing color to the solution that was initially a clear
yellow. This indicates that the reaction between HCl with metal contained in the
zeolite. In accordance with the theory that the HCl will change to yellow when
contaminated metal content. While soaking the zeolite with 0.1 M NH4Cl
solution, a solution that was initially a clear turn green. It is caused due to the
aluminum oxide which reacts with chlorine-containing hydrates and colored
green. Soaking also aims to reaffirm the structure of zeolites,then zeolite do the
calsination. calsinated Zeolite results look whiter and brighter than zeolite before
calsinated. Then after that is done using the energy characterization of dispersy
spectroscopy to find out the content of SiO2 and AlO3 component constituent of
zeolite.

The Process of Urea-Encapsulated Nanoparticles Activated Zeolite-Chitosan


This research has been carried out in the laboratory of analytical chemistry
and inorganic Chemistry Laboratory, Faculty of science and mathematics,
University of Diponegoro. Testing and analysis of samples carried out in Lab.
Terpadu UNDIP. This slow release fertilizer is a combination of a modified urea
with zeolite nanoparticles Chitosan edible coating. Urea used was urea prill
circulating in the community and the zeolite used is a natural zeolite has been
activated and the result of the synthesis of Chitosan nanoparticle skin shrimp. For
Chitosan previously done milling for 5 hours in order to minimize the size of the
particles of Chitosan. After the synthesis process has been completed, then the
combination process is done by using the method of encapsulation. From process
research conducted three variations, and then taken the formulation of active
composition: with 40 grams of urea: 10 grams of activated zeolite: 50 ml of
Chitosan nanoparticles previously reconstituted with 1% acetic acid. procedure
i.e. urea with smoothing mortar and then modified with activated zeolite with
granulation process materials, further in doing the process of encapsulation. Then
do the test with the characterization of content of nutrient elements in fertilizer,
8

fertilizer solubility in water analysis, analysis of Energy Dispersy Spectroscopy,


analyzing the chemical properties of soil and nutrient release efficiency.
cantumkan
alat apa
Testing the efficiency of nutrient elements with Atomic Absorpsion Spectroscopy yang
digunakan
Testing this out in Analytical Chemistry Laboratory is doing at the untuk
University of Diponegoro started from March until June 2016. Characterization analisa hasil
penelitian
to be conducted includes the testing of SEM-EDS and AAS (Atomic Absorption
Spectroscopy). Fertilizer SRF who previously has been made will be applied to
agricultural land to find out the nutrient absorption by plants. The land that will
be used as a medium for planting rice paddy soil taken from the temperate
Tembalang. Taken as a composite soil at a depth of 0 – 50 cm. In the prepared
media planting amounted to 3 media, then distinguished from the media created
jangan lupa untuk
the third variation of allotment of fertilizer. At the first planting media are given
menulis cara fertilizer urea, urea fertilizer combination given the second with zeolite
analisa secara nanoparticles and the third planting in the media give a combination of urea
detail dan fertilizers with zeolite-Chitosan nanoparticles. Time measurement is carried out
mencantumkan during 2 weeks. The parameters used are the nutrient elements content in growing
setiap variabel
kontrol (misalnya
media.
waktu, suhu, dll)
Chapter 4 kumpulan dan kejelasan
penampilan data, proses/teknik
CHAPTER 4 RESULT AND RESEARCH pengolahan data, ketajaman analisis
dan sintesis data, perbandingan hasil
dengan hipotesis atau hasil sejenis
Chitosan SEM (Scanning Electron Microscopy) Analysis sebelumnya

Hasil The SEM microscope work principle is the wave nature of the electron
penelitian/analisis diffraction in the form of very small angles (Samsiah,2009 and Wulandari,2010).
data ditulis urut
Information on particle surfaces can be obtained with the introduction of the
sesuai yang
tercantum pada probes in the path of the electron beam or on the surface of the particle.
metode penelitian. Information can also be carried by the probe captures the electrons on the surface
of the tunnel between the particles of the specimen with the tip of the probe or a
probe that capture the thrust between the surface with the tip of the probe (Poole
and Owens,2003). The SEM characteristics of Chitosan nanoparticles results
showed the particles that form a circle resembling a ball. Particle size can be
determined by measuring the diameter of the ball. SEM was used to observe the
morphology of a materials. Following are the results of the analysis:

Hasil penelitian
sesuai dengan
kejadian yang
sebenar-benarnya /
tidak dimanipulasi
seuai keinginan.
Sertakan gambar dan
grafik.
Figure 4. a) The results of examination with SEM magnification of 1000x
chitosan, b) SEM magnification of 3000X, c) SEM magnification of 4000x
Tabel diberi judul dengan penomoran tabel sesuai dengan
urutan kemunculannya dalam naskah. Judul tabel ditulis di
atas tabel dengan nomor tabel menggunakan angka arab 9

Table 1. The Characterization Results of Freeze-Dried Nanoparticles Eggshell


Powder
Charateristic Result
Organoleptis White-Brown, Odorless
Water Content (%) 2,75 ± 0,16
SEM Magnification 1000x 268 nm
SEM Magnification 3000x 124 nm
SEM Magnification 4000x 84 nm

The SEM characterization result of Chitosan nanoparticles showed the


particles that form a circle resembling a ball. Particle size can be determined by
measuring the diameter of the ball. Magnification used i.e. 1000 times obtained
the size 268nm, 124nm size 3000x zoom and magnification 4000x sized 84nm.
SEM was used to observe the morphology of a materials. SEM characterization
of the above results showed the presence of vapour-shaped ball. The BLOB is a
merger between Chitosan with sodium tripolifosfat. SEM using electron and
visible light as a source of light. The electrons produce shorter wavelength light
photons with a size of 5 nm and produces images with better resolution (Balaz,
2008). However, the above is not clearly visible. This is because the coating is
not done when shooting. The upholstery used i.e. upholstery that is the conductor.
Coating commonly used include Platinum, gold, and silver (Poole and Owens
2003).
Nanotechnology application was done as an attempt to increase the
solubility of a material that is used as encapsulant, stabilize the condition of
thermal, as well as facilitate the digestibility of compound ingredients are
contained in the encapsulation. Size mikroenkapsulasi diameter between 3-800
µm, whereas in nanoencapsulation materials has a size of 10-1000 nm.
(Ezhilarasi, et al., 2012). Based on photographic images of SEM in Figure 4 can
be seen in the process of homogenization for 60 minutes using sodium
tripolyphosphat can solve an aggregate nanocrystal formed at the dry process is
frozen. Aggregation occurred due to increase of the surface free energy of the
particles, so the particles tend to be mutually interacting particles that cause
changes (Sinko, 2006). Solution of Tween 80.1% that is used as a medium
dispered serves as the steric stabilizer and impede the merger between particles to
prevent the growth of aggregate (Shi, 2002).

FTIR (Fourier Transform InfrRed) Data Analysis

The infrared spectrum is able to detect the presence of functional groups


that are used for the identification of compounds in a sample. FTIR analysis can
be used to know the functional group in an organic compound or polymer
compound at wavenumbers of 400-4000 cm-1. FTIR test can be used to know the
functional groups in organic compounds or compounds of polymers on the
wavenumbers of 400-4000 cm-1. Those wavenumbers accordance to the
10

determination of the functional groups of organic compounds (Nuance


Rachmania, 2004).

Figure 5. FTIR Chitosan Spectra

The curve shows the FTIR transmitter results of chemical profile pattern
spectrum. In this study, there is 1 sample tested, namely powder Chitosan results
synthesis. Firdaus et al. (2008) Chitosan has specific clusters, namely (NH2 –
and – OH). Can be seen on the curve of the FTIR Chitosan cluster Amine (NH2 –
) are on the wave number 1650 cm-1, whereas the hydroxyl (– OH) are on the
wave number 3450 cm-1. According to Pebriani et al. (2012) absorption wave
numbers of functional Amine (NH2 –) and hydroxyl (– OH) on commercial
Chitosan is at wavelength 1655 cm-1 and 3450 cm-1. So it can be conclude that
synthesis of results has been detected pure Chitosan.

The Result of Activated Zeolit Analysis

Identification of activated zeolite results using EDS (Energy Dispersy


Spectroscopy). The goal is to find out whether or not there are SiO4 and AlO4.
With the analysis of the EDS then can know the material content or element that
is in the sample results synthesis. On the process of activation will occur the
dissolving process of silica which is one of component that framework the zeolite.
Dissolving silica zeolites structure changes will cause as well as a reduced ratio of
Si/Al. The decline in this ratio will increase capacity and selectivity adsorption
zeolite against polar molecules. Based on the results of the analysis with EDS can
be known that a compound of alumina and of silica is a constituent component of
the zeolite. The content elements in t zeolite can be seen in Table 2.

Table 2.Content Elements in Zeolit


The element in the Concentration(%)
11

form of oxides
SiO2 61,86 %
Al2O3 10,42 %
Fe2O3 3.93%
CaO 4.53
MgO 0.74
TiO2 0.24
Na2O 0.14
K2O 1.06
MnO 0.03
H2O 5.33
K2O 13.8

Comparison of Si and Al from the zeolite describing its cation exchange


capacity function . XRF analysis results data indicate that the percentage
comparison between SiO2 and A12O3. This comparison is theoretically
demonstrated that its cation exchange capacity is large relatively

Encapsulation Process of Chitosan Nanoparticle

Main research includes the stages of Chitosan manufacture nanoparticles


that refers to a method of Wahyuono (2010), namely magnetic stirring at room
temperature with 3% (b/v) Chitosan in acetic acid 1% as many as 100 mL, then
cutting the gel bonding method using software namely magnetic stirrer for 2 hours
with a speed of 1400 rpm. Then add a solution of tween 80 0. 01% added as
much as 2 sprays that can separate between the gel one with another, in gel-stirrer
for 30 minutes. After that, 100 mL tripoliphospat 0. 1% added aims so that the
resulting particle size remained stable, in-stirrer for 30 minutes. A solution of
urea fertilizers add Chitosan nano as much as 8% of the use of Chitosan, then in-
stirrer for 15 minutes. Mixed solution of terahkir phase in spray drying. Then do
the characterization of Chitosan nanoparticles with SEM (Scanning Electron
Microscopy) and FTIR (Fourier Transform InfraRed).

Analysis of Nutrient Content in Fertilizer

The testing method used is the Kjeldahl method for Nitrogen content,
while for N, P and K method used AAS, and uv-vis Spektrofotometeri. In this
study the most optimum composition in the get on urea-zeolite: comparison with
Chitosan nanoparticle 40%: 10%: 50%. This active formulations to make
12

fertilizer urea into solid and gel that changes color from white to black because of
the influence activated zeolite addition. Here are the results :
Table 3.Nitrogen Content
Sample Parameters Results
Urea N Total 7,73 %
Urea : Chitosan N Total 10,35 %
Urea : Chitosan : N Total 9,8 %
Zeolite

Nitrogen content analysis using methods kjehdahl. From the test results ,
most optimum composition on a combination of urea: chitosan which the nitrogen
content of 10. 35%, while the composition of urea-zeolite: chitosan had lower
levels of the grading of 9. 8%. The decline caused by zeolite in the composition of
the fertilizer. The decline in the percentage of the total N of the most active
formulations caused by the amount of urea is reduced and replaced by zeolite,
while the main source of nitrogen is from fertilizer urea. This is what causes the
nitrogen content is reduced. But on the other side with the addition of the raw
material zeolite in the womb of fertilizer will cause the cation exchange capability
of the mineral fertilizers contained in the soil increase as well as the nature of
other zeolite support the absorption capacity.
Table 4. Phosphorus Content
Sample Parameters Result
Urea Phosphorus 15,32 %
Urea : Chitosan Phosphorus 17,13 %
Urea : Chitosan : Phosphorus 17,78 %
Zeolite

Then the further testing is the content of phosphorus. The method used is a
UV-VIS spectrophotometer. From the analysis of testing can be seen an increase
of urea, urea: chitosan and urea-zeolite: chitosan. Most visible results on the
content of urea-zeolite composition: chitosan namely phosphorus content of 17.
78%. While the urea-chitosan composition has a content of 17. 13%. Increased
levels of phosphorus is caused because andanya cation exchange ability of zeolite.
Phosphor itself is one mineral that have a good cation growth for processes in
plants, with the addition of zeolite will certainly lead to the cation exchange
process of mineral nutrients will be increased.

Table 5.Potassium Content


13

Sample Parameters Result


Urea Potassium 10,69 %
Urea : Chitosan Potassium 12,86 %
Urea : Chitosan : Potassium 13,64 %
Zeolite

The third test is a test of potassium content. From the results of nutrient
elements content testing in potassium using SSA-Flame method. The test results
look that urea fertilizer combination of chitosan and zeolite have higher levels i.e.
potassium levels amounted to 13. 64%. While in urea: chitosan amounted to 12.
86% and urea control with 10 levels. 69%. The increase in the level of potassium
is caused due to the addition of chitosan and zeolite, activated. Potassium is the
same as with the phosphor is, it is still related to cation exchange capability and
the absorption properties of the zeolite content in fertilizers which are able to fix
the nutrient content of potassium in the fertilizer. So the presence of chitosan is
able to enhance the capabilities of release of potassium from manure, whereas
zeolite acts against power of fertilizer absorbs.

Analysis of Nutrient Elements Release with Energy Dispersy Spectroscopy

Analysis using EDS (Energy Dispersy Spectroscopy) aims to find out the
content of nutrient elements contained in the soil. In the analysis by using energy
dispersy spectroscopy shows all of the material contained in the sample will be
detected, but only at the results of this analysis show the nutrient psospor and
potassium, while for the element nitrogen cannot be detected by testing samples.
This is caused because the gaseous nitrogen, whereas samples which can be
analysis only at solid phase. Here the following analysis results:

70 25.91
60 21.31
18.24
50
14.42 34.52
40 32.1
Nilai

29.1
30 21.86
20
10
0
Kontrol Urea Kitosan-Urea Urea-Kitosan-Zeolit

Nilai K Nilai P

Figure 6.Analysis of Nutrients EDS


14

In this EDS analysis, nutrient observed only potassium and phosphorus,


Treatment test using four variations of the 1 box of soil as a control. Box 2 in
treatment with the addition of urea, box 3 with the addition of urea in combination
with chitosan nanoparticles and box 4 with urea treatment combination with
zeolite-chitosan nanoparticles. After it let stand for 2 weeks then testing. In the
test , sample is taken from 1-10 cm soil depth. But in the analysis of the second
energy spectroscopy dispersy do the watering with water in advance for 2 weeks,
with the aim to determine the level of influence of water on the solubility of
fertilizer in the water. In addition to. determine the effect of chitosan on the ability
of resistance to degradation by water fertilizer. Here the following analysis
results:
60 21.48
18.49
50
40
30.4
Nilai

30 9.84 27.16
6.91
20
12.25
10 9.42

0
Kontrol Urea Kitosan-Urea Urea-Kitosan-Zeolit

Nilai K Nilai P

Figure 7. EDS Analysis After Watering Them with Water for 2 Weeks

The fourth variation of the difference that can be seen on the nutrient
elements such as P and K. On the variation of urea-zeolite: chitosan slowdown in
the release rate of the most effective nutrients. The test results Potassium content
of 34. 52% down to 30. 4% while the phosphor of 25. 91% down to 21 to 48%.
From the observation charts can be seen a significant increase in the addition of
zeolite and chitosan nanoparticles in the formulation of slow release urea
fertilizer. Decreasing the release of fertilizer efficiency lead to the release of
nutrients will run longer and in the long term. This is because the pores of urea
will be coated with chitosan nanoparticles, resulting in degradation of the ability
of water to urea will be smaller. This will impact on the ability of urea nutrient
release better.

Analysis of Soil Chemical Properties

Analysis of soil properties made after 1 month of fertilizer in the soil. The
goal is to determine the effect of fertilizers on the physical properties of the soil.
There are 4 samples in the analysis of control, urea, urea and urea-chitosan-
zeolite: chitosan. Here the following analysis results:

Table 6. Analysis of Soil Physical Properties After Fertilization Process


15

Sample pH Condition Texture


Sample 1 5,2 Loose Dry
Sample 2 5,8 Clot Dry and Hard
Sample 3 6,1 Unclotted Quite Wet
Sample 4 6,6 Unclotted Quite Wet

In the analysis of the chemical properties in sample 4 shown that the


composition of urea in combination with zeolite-chitosan has the highest pH 6.6
and included soil conditions are good, then consistency rather moist soil
conditions and does not clot while on the texture of the soil slightly moist. From
these results we can conclude that the most active formulations demonstrate
consistency and the texture is most excellent among all four variables.

Analysis of The Solubility in Water

Fertilizer Solubility in Water = Fertilizer Wt/ V Water


= 2 gr/ 900 ml
= 2.2 x 10-3

Table 7.Fertilizer Solubility in Water


NO Sample Difference of Solubility Solubility in Water
(Menit/gram)
1 Control 3,12 2.2 x 10-3
2 Urea : Chitosan 5,58 2.2 x 10-3
3 Urea : Chitosan-zeolite 5,31 2.2 x 10-3

Analysis of solubility in water is done by dissolving the sample in water,


and stirrer the process to determine the level of fertilizers solubility. From the test
results, when added chitosan as a coating material, the urea is the longer dissolve,
because chitosan is used as the coating insoluble in water so as to slow down the
release rate of fertilizer nutrients. However, the zeolite then a soluble fertilizer to
be reduced due to a slight inhibiting coating of chitosan in fertilizers.

Analysis of Nutrient Release Efficiency

EDS of the chart data can be analyzed the efficiency of nutrients release
from fertilizers. Comparative test in use is the control of urea with urea-modified
zeolite: chitosan nanoparticles. The element phosphorus has increased from
release of 8.76 to the treatment of urea to 4.43 by using the most active
formulations, it is also evident from nutrient release of potassium from 16.85
down to 4.12. The decline in the release of nutrients will increase the power
16

absorption of nutrients by plants. This is caused within the same release of


nutrients, slowly release fertilizer would be better if compared with release
fertilizer with significant amounts and are not necessarily able to be released into
the soil well. So, with the urea-modified zeolite formulations: chitosan
nanoparticles release fertilizer process becomes less, so the release of nutrients
that it can run longtime term and will not be degraded by the presence of water.

Conclusion Kesimpulan penelitian

The development of urea fertilizer nano-zeolites: chitosan nanoparticles


combination with a ratio of 40%: 10%: 50% is the most active formulations. The
test results from the slow release formulation of the most active in obtaining that
release nutrients increased better than with the use of urea fertilizer. Increasing the
nutrient release efficiency in the fertilizer is caused by the ability of chitosan to
minimize the pores of urea and resist the dissolution of the water, plus the
activated zeolite which has a cation exchange Traffic, power of absorption and
maintain the pH balance of the soil. From these results it can be concluded that
with the improvement process relase it will make the release of nutrients from
Saran untuk penelitian
selanjutnya,
fertilizer more effective. So it is expected to improve the absorption of nutrients
mengaplikasikan by plants that will have an impact on increasing the productivity of agriculture.
manfaat dari hasil
penelitian untuk Bagian kesimpulan sangat penting. Tunjukkan bahwa gagasan atau ide
komersial, dll. Suggestion dapat menyelesaikan solusi dari permasalahan yang ditelaah dengan lebih
kreatif dan inovatif dibandingkan penelitian terdahulu
For the further research need to concerning the development of the
fertilizer effectiveness of slow release against absorption by plant, so it will be
better prepared in the scale of production and commercial market. In addition a
need for cooperation with the relevant agencies to support the implementation of
sustainability research.

Referensi/sumber acuan yang digunakan dalam karya tulis ilmiah.


BIBLIOGRAPHY Disesuaikan dengan sitasi-sitasi yang disertakan dalan tulisan.

Akelah, A. 2006. Novel Utilizations of Conventional Agrochemicals by Controlled


Release Fertilizer. Materials Science and Engineering. C4. 83-98.
Astiana. S. 1993. Perilaku Mineral Zeolit dan Pengaruhnya terhadap
Perkembangan Tanah. Disertasi. Program Pasca Sarjana IPB. Bogor.
Ezhilarasi, et al. 2012. Nanoencapsulation Techniques: A Review. J Food
Bioprocess Technology. Volume 6. Issue 3. 628-647.
Fujinuma, R. and Balster, N. j. 2010. Controlled-release Nitrogen in Tree
Nurseries. Research Communication. 2. 123-126.
Liu, M. 2014. Preparation and Properties of Chitosan-coated NPK Compound
Fertilizer with Controlled Released Nano. College of Chemical
Engineering. Northwest Minorities University Polymer 55. 1964-1976.
Muzzarelli, R.1997. Chitin Perngamon Press. Oxford. NewYork.
17

Pebriani et al. 2012. Modifikasi Komposisi pada Proses Sintesis Komposit TiO2-
Chitosan. Jurnal Kimia Unand Vol. 1 (1).
Poole & Owens FJ. 2003. Introduction to Nanotechnology. New Jersey: John
Wiley & Sons Inc.
Prima. 2009. Permasalahan Pupuk dan Langkah-langkah Penanggulangannya di
Indonesia. Kementrian Sekertariat Negara Indoneisa. Jakarta. Vol 14.
24-34.
Rachmania D. 2012. Karakterisasi Nano Chitosan Cangkang Udang Vanamei
dengan Metode Gelasi Ionik. Bogor: FPIK, Institut Pertanian Bogor.
Suwardi. 1999. Pemanfaatan Zeolit sebagai Media Tumbuh Tanaman
Hortikultura. Prosiding. Temu Ilmiah. 1-3 September 1995. PPI.
Tokyo. Jepang.
Szeto, et al. 2007. Exploring Nanochitosan. ATA-Journal for Asia on Textile &
Apparel. China.
Wahyono D. 2010. Ciri Nanopartikel Chitosan dan Pengaruhnya pada Ukuran
Partikel dan Efesiensi Penyalutan Ketoprofen. Bogor: Pascasarjana
IPB.
Wulandari T. 2010. Sintesis Nanopartikel Ekstrak Temulawak (Crucuma
xanthorrhiza Roxb.) Berbasis Polimer Chitosan-TPP dengan Metode
Emulsi [Skripsi]. Bogor: Fakultas MIPA, Institut Pertanian Bogor.
Yanti, S. 2014. Pengaruh Penambahan Berbagai Dosis Aplikasi Pupuk Urea
terhadap Produksi Tanaman Sawi. Junal Ornaline Argoteknologi ISSN
No. 2337-6957.
18
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karya, Biodata peserta, Biodata dosen
pembimbing, Fotokopi Kartu
Mahasiswa/KTM yang masih berlaku, dan
ATTACHMENT Lampiran lain jika diperlukan

1. VALIDATION PAGE
19

2. ORIGINALITY PAGE
20

3. MEMBER GROUP BIOGRAPHY

PARTICIPANT
A. Identity
a. Full Name : Annizah Rahmatya Gerhana
b. Birth Date and Place : Jayapura, 24 Oktober 1995
c. NIM : 21030113120076
d. Department/Faculty : Teknik Kimia/ Teknik
e. Phone Number : 085713541575
f. Adress : Jl. Gatotkoco 2 Pancaarga 2 Magelang
g. Email : anisa.gerhana@che.undip.ac.id
h. Awards :-

All the data I input and biographical data contained is correct and legally
defensible . If later on it turned out to be found different with reality, I should
accept the sanctions. Thereby I created this biographical data to fulfill the
requirements of Chemical Engineering Research Competition.

Semarang, 22 Agustus 2016


Team Leader

Annizah R. Gerhana

B. Identity
a. Full Name : Alfin Darari
b. Birth Date and Place : Semarang, 17 Februari 1994
c. NIM : 24040112140089
d. Department/Faculty : Fisika/ Sains dan Matematika
e. Phone Number : 085713541575
f. Adress : Puri Anjasmoro, Semarang
g. Email : Alfin.darari@st.fisika.undip.ac.id
h. Awards :-

All the data I input and biographical data contained is correct and legally
defensible . If later on it turned out to be found different with reality, I should
accept the sanctions. Thereby I created this biographical data to fulfill the
requirements of Chemical Engineering Research Competition.

Semarang, 22 Agustus 2016


Member

Alfin Darari
21

C. Identity
a. Full Name : Eko Siswoyo
b. Birth Date and Place : Pati, 2 Agustus 1995
c. NIM : Ekosiswoyo37@gmail.com
d. Department/Faculty : Kimia/ Sains dan Matematika
e. Phone Number : 085740763575
f. Adress : Pati, Jawa Tengah
g. Email : Ekosiswoyo37@gmail.com
h. Awards :-

All the data I input and biographical data contained is correct and legally
defensible . If later on it turned out to be found different with reality, I should
accept the sanctions. Thereby I created this biographical data to fulfill the
requirements of Chemical Engineering Research Competition.

Semarang, 22 Agustus 2016


Member

Eko Siswoyo
22