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PROCEEDING 

INTERNATIONAL SEMINAR ON 

ENVIRONMENTAL SCIENCE 

20111

"lEnWcmment (Jjasedon Science t.Rpearcfifor(BetterLifeII 

October, 8th
2011 

Gedung Seminar E, 

Andalas University 

Publish by: 

Chemistry Department 

AndalasUniversity 

2011
International Seminar on Environmental Science 2011
Environment Based on Science Research for Better Life
Steering and Scientific Committee:
Prof. Dr. Abdi Dharma 

Dr. Mai Efdi 

Dr. Syukri Drajat 

Dr.lulhadjri 

Organizing Committee:
Chairperson: Riko Irwan
Secretariat: Epi Supriwardi, Defina Nasmiaty, Reno Permata Sari, Wilda Lion
Suri
Treasurer: Nuryanti, Ayu Kurnia D.P.S, Sestry Misfadhila, Mega Ulfaningsih
Program: Sisri Handayani, Restiyani Harahap, Liti fitrianny, Unzilla Rahmi,
Rahmatul Hasanah
Publicity: luI Aritin, Maharani Hazar, Yosi Febriani, Rikha Septiani Yuda
Resource and Facilities: Firdaus M, Yuniar Hardiati, Restu Harly Pebriani, Rid
Junaidi, Febrina lamar
Editor: Rikha Septiani Yuda, Maharani Hazar, Zul Arifin
Secretariat:
Chemistry Department
Faculty of Mathematic and Natural Science
Andalas University
Limau Manis, Padang, West Sumatera, Indonesia, 25163
• J (
I
'"
PREFACE 

VICE RECTOR III 

ANDALAS UNIVERSITY 

Assalammu'alaikum Wr. Wb
All praises be to Allah, the Almighty, the creator of the world. May His peace and
blessing be upon our prophet Muhammad SWT, the leader of messengers and guide of
faithful.
Environmental problems are now becoming the hot issues which have need to solve by
all of us, because these issues directly effect the quality of humans life on earth.
Therefore, as scientist we have to give more effort to give solutions on those issues.
This proceeding is useful as a guide to fix those issues, as the first step to keep the
environmental safe for our next generation.
Padang, 2012 

Vice Rector III 

Andalas University 

Prot: Dr. H~arun.MS
NIP, 19620506198811 1001
II. International Seminar on Environmental Science (ISES2011)
~;~~er Sih, 2011
.enlty ofAndal"
PREFACE 

DEAN OF lHE FACULTY MATHEMATICS AND NATURE SCIENCE 

ANDAtAS UNIVERSITY 

AssaJamualikum, wr,b,
All pnuses be to Allah, the Almighty, the ~reator of the world, May His peace and
-blessing be upon our prophet Muhan1mad SWT, the leader of mes~engers and guide of
tbithful.
t would like to thank all of you who participated in this International seminar which is
held he-Ie in Padang, and specially, key note speakl~rs that came here, and organizing
committee with hard work to prepare this seminar. For the students, I think, this event is
learning process that tel be important in the future time.
I am proud that so many experts in the field of this seminar decided to take part in the
event that has been co-organized by our chemistry students,
Iam confident that the seminar will provide a great opportunity for an international and
national gathering for sciences and te(~hnolog)' from different nation,
<5 we know, at the moment environmental and energy are great problem for us. In this
case, research is one of that we can do to solve these problem and important role to
improve the quality of life, [ do hope that, this semmar provided platform for sci.entist
and technologist to meet and share ideas, achievement as well as experiences through
the presentation of papers and discussion,
Wassalamualikum Vw
Pad.'lng, 2012
Dean ofthe Faculty
Mathematics and Nature Science
r;::~j~
Prof Dr, H Emriagi, MS
NIP. 19620409198703}003
, lnternatlonal Seminar on Environmental Science (ISES2011)
,Q. '()ctober 81b~ 2011 

'University of Ancbla!! 
 ii
FOREWORD 

MAJOR HEAD OF CHEMISTRY 

UNIVERSITY ANDALAS 

A.ssalammu'alaikum Wr. Wb
Thanks be to God praise for all the abundance of His grace and guidance. Sa:awat
coincided greet RasuruJlah SAW,
mtemational Seminar on the theme "Environmental Based on Science Research lor a
Better Life", This is proof that we as chemistry scientist aware that environmental
problems are exist, be(:ause the environment is one of subarea in which we understood
better as a chemistry scientist.
The environm(mtal issues now rise up with the rapid of science and technology
development that is not coupled with environmental awareness. The waste that is not
handled properly, carelessly and discarded on the- right spot, tum raises into new
poroble:ms for the environmenL also to the people 'who were around the neighborhood.
Therefore, the presence of this International Seminar, and the summarize of various
studies to address various environmental problems that have been packaged in this
procedding can provide solutions and contribute little to the existing problem. Hopefully
it can be optimized and maximized its use,
P,lCiang, 2012
Chairman of the Chemistry Department
Andalas University
Dr. Adli Santoni 

NIP. 1001 19620506 198811 

International Seminar on Environmental Science (ISES2011)
l()ctober 81ft
, 2011
[University ofAndal8s III
Internationa(Seminar on fÂŁtwironmentafScimce (LS!ÂŁ52011)
OctoBer /pI, 2011
I'XJ/. Ji'Y.M1(J ltuforusia ~ :H1:M'K)4, 'Unaruf
rDepartlfllnt ofCliemistry. 'University 0/_'4rufafas
Content
Preface by Vi~Rector III... .......... ... , ........,....,. ...,...... 1
Preface by Dean ....."................... , ..... ,... ....,...........'.... ,... ,11
Preface Chairperson "" .. ,..".,....,......,.... ,. """""" ,.",.",." '" ,."." .. ,.. ,.,.....,,'..... "",.111
Contents ..........,' ", '"'''' ,..............,.....,.. ,' .. '.... ,....,,'..... """''''..,.."......,... ',,,....."" IV
Presentations by Keynotes
Towards A New Type Of Science For Successfully Addressing The Global
Challenges For Humankind
file C, Gebeshuber...................................................,............................................... 1
Tyrosinase-Immobilized Biosensor Based On Mwnt Supports With
Multifunctional Group
Seong-Ho Choi And Kyo-ll Kim............................................................................. 12
Presentations by Speakers
Agroclimate Cropping Pattern Changes Based On Climate Change Pr~iections
With Hadcm3 A2 And B2 Climate Change Scenario For Reducing The Risk Of
Harvest Failure In Ngijo Watershed, Yogyakarta Special Province,
Gilang Arya D. Andung 8ayu S. Fitria Nucifera, Emi/ya NurjanL .....................22 

Antioxidative Activity Of Lignin From Oil Palm Empty Fruit Bunch. 

Gustini Syahbirin. Vanny Pratl~Yi. Suminar Setiati AchmadL............................. 39 

Biodegradation Of Phenol-Containing Textile Industry Wastewater By Candida
Tropicalis.
Suryani, Laksmi Ambarsari, Aktnal.......................................................................48
Tsunami Hazard Mapping As A Basis Of Spatial Planning In Sadeng Coastal
Area, Gunung KiduJ District
Ahmad Cahyadi, Andungbayu Sekaranom, Fitria Nucifera, 

Dinifeti Anggraini..................................................................................................61 

Photolysis, Sonolysis And Ozonolysis For Degradation Of
2,4Dichlorophenoxyacetic Acid (2,4-D)
ElvilUl'ifati..............................................................................................................70
Karst Groundwater Management Based On Groundwater Recharge And
Vulnerability Mapping: Case Study In Paliyan And Saptosari Subdistrict,
Gummgkidul Regency
Ahmad Cahyadi. Fedhi Astuti Hartoyo. fJenkr Nugraha.....................................76 

iv
1mentationa{Seminar on E,mAronmenta{Science (ISES2011)
October 811i, 2011
1'1(;4 :}fl')t{7(J 1rufonesia r:!l J{J'M1(Jl Vnan4
'Department ofC("mistry, Vniversity of;4.rufuf'as
Study OfFourier Transform Infrared Spectroscopy And Scanning Electron
Microscope OfCellulose Acetate Membrane From Wastewater OfTapioca
Betty Marira Soebrata, Sri Mulijani. /smiaini Nwpatria Purri......,..........".,........8:

Synthesis And Characterization Of Bimetallic Catalyst Mn/Nj fmmobilized On
Moditled Silica
Nuryanti. Syukri, Syukri Ariej...................................................,.........,.........."......9' 

Immobilization Acetonitrile Ligated Cobalt(II) Complexes On Modified Silica
And Its Characterization
Benny Rio Fernandez, Syukrt Arief. Syukri............."........................................... 11
Poster Presentation
The Effect Of Prefilter On Titania Modified Ceramic Membrane Efficiency In
Humic Water Treatment To Provide Drinking Water
Admin AIif. Mat Efdi, Oily Norita Tetra.............................................:................ ]23
The Effect Of Sol-Gel Processing Variables On Structure Changes OfTioz '
Nanopartiles
Ye/ria Rilda...........................................................................,......,......................,127
Preparation And Photocatalytic Property Of Nanoparticle Magnetic Ti0:2-Nifezo4
By Coprecipitation Method
Rahmayeni, Upira Setiani. Syukri Ariej. Rianda.............,.................................... 13':

The Determination OfComposition OfAir Particulate Matter Pollution In
Comparative Study OfN<>x Gas Analysis By Phenol Disultonic Acid And
Saltzmaan Method Using The Cadmium Reduction Column.
Refilda Suhailt. Radhia Putri, Ardeniswan......................................................... 139 

v
Study ofFourier Transform Infrared Spectroscopy
and Scanning Electron Microscope of Cellulose
Acetate Membrane from Wastewater of Tapioca.
Betty Marita Soebrata, Sri Mu!ijanf, 1smiaini Nurpatria Putri
Department o/Chemistry, Faculty o/Mathematics and Natural Sciences, 

BogorAgricultural University 

Email~ bcttymru:it{1@l4lllilII,cQill
ABSTRACT. Wastewater of tapioca is waste product from starch precipitation or
separation process from its water in making tapioca. This wastewater still contains
carbohydrates such as glucose, so it can be used as raw material for making cellulose
and cellulose acetate (CA) membrane, Nata de cassava was made by fermentation
process using Acetobacter xylinum In wastewater of tapioca as the fermentation
media. Then, the nata was dried and grinded to produce bacterial cellulose (Be)
powder. BC powder was reacted with acetic anhydride to produce CA powder. CA
powder was dissolVed to acetone solvent (appropriate with an acetyl degree of CA)
with 1696 w/v composition and then formed to be a membrane. These CA membraM
was characterized with Fourier Transform Infrared (FTIR) and Scanning Electron
Microscope (SEM).. Analysis from FTIR spectrum showed that CA was formed, by the
existence of absorption band of C carbonyl at 1725.92 cm-1 wavenumber and CoO
acetyl at 1061.37 cm-l. The resuh: of SEM analysis showed that the membrane which
has been produced was the mlcrofiltration and asymmetric membrane with the
diameter pore approximately of 0.37-0.95 IJ.m. CA powder that has been prodliJced had
a water content of 21.39% and an acetyl degree of 40.38% (equal with substitution
degree of 2.51).
Keywords: cellulose, cellulose acetate, nata, bacterial cellulose, membrane, , FTIR, SEM
1. Introduction
Cassava (Man/hot esculenta) is a clump of food crops from the Americas and has
another name ubi kayu orsingkong. In Indonesia, cassava is an important source of
carbohydrates after rice, with a carbohydrate content of 34.7% (Soetanto 2001).
Cassava can grow even in infertile soil, in the tropical climate. Indonesia is currently
the third largest cassava producil"'g countries in t.he world after Brazil and Thailand
because many Indonesian people have switched from planting rice to cassava farming
(SumlyatI2009). According to Badan Pusat Statlstik (BPS 2011)J the amount of cassava
production In Indonesia in 2009 was 22,039F145 tons and in 2010 increased to
23,908,459 tons (preliminary figures).
lnternational Seminar on Environmentlll Science (ISES10ll)
October Slh, 2011
University ofAndalas
85
Cassava can be consumed directly as food or used as a raw material of fooe
industry, one of which is the tapioca industry. The process of making the tapioca in thE
industry will generate solid waste' (onggok) and liquid waste. Tapioca liquid waste car
be generated from the washing stage of raw materIals (cassava) and also thE
deposition process to separate the starch from the water. The process of makin~
tapioca in large industries and small industries in general includes the stages of skir
peeling, washing, scrapping, extraction, starch deposition, and drying.
Wastewater from tapioca industry which is still new is creamy color, While the
color of spoiled waste is dark gray. Turbidity that occurs on the waste caused by the
presence of organic materials, such as soluble starch, microorganisms, and other
colloid materials. Tapioca liquid waste from the precipitation has a BOD value of
1450.8-3030.3 mg L -1 with an average of 2313.54 mg L -1, COD of 3200 mg L ·1
dissolved solids 638-2836 mg L -1, and the amount of cyanide (CN ) of 19.58-33.75 mg l
-1 (Vegantara 2009). Therefore, if the waste is discharged into the er:1vironment that
will cause environmental pollution, such as bad smell and some wells are not suitable
for consumption.
The current technology has not been able to separate the starch which
dissolved in water so that liquid waste which is released into the environment stili
contains starch. The liquid waste will decompos~ naturally In water bodies and cause a
bad odor. -rhe smell is generated in the process of decomposition of compounds
containing nitrogen, sulfur, and phosphorus of the protein material (Olive 1999 and
Hanifa et at~ 1999). Another alternative that can be done to treat this wastewater Into
products that can be exploited further is to process them into so-called nata de
cassavo.
Nata formation requires the element C that comes from glucose and Nand 0
elements derived from the addition of ammonium sulfate. These elements are used as
nutrients and carbon sources for bacteria Acetobocter xylinum in order to form a nata.
Tapioca wastewater containing glucose as the carbon element can therefore be used
as a good medium to stimulate the growth of bacteria such as forming nata.
Therefore, tapioca liquid waste could potentially prodl2lce nata. Nata in the' form of
cellulose produced by bacteria that can be referred to as bacterial cellulose (BC). In
addition: nata can be characterized as a composite of carbon fibers Into a solid form
and porous. so nata potential to be utilized as a cellulose membrane. However, the
cellulose membrane did not have a high commercial value. Therefore, further
processing Is needed to turn it into a membrane of cellulose acetate (CA) which Is
more valuable than cellulose membrane.
Celili/lose trlacetate (primary CA) obtained from: the reaction of cellulose with
aatic anhydride and H2S04 as a catalyst. Acetylation is an important stage in the
.fifacture of CA as it relates to its 4lhility to dissolve in certain organic solvents In
'1Ffl'15rocess of membrane manufacture. CA ~olubility in organic solvents is influenced
InteflDational:Seminar on Environmental Science (18ES2011)
October 8t
h, 2011
Uninrsity orAndaln
86
by the levels of acetyl (Desiyarni 2006). Setting levels is carried out by reaction of
acetyl hydrolysis using dilute acetic acid to obtain the appropriate degree of
substitution,
This study aims to make membrane-based CA tapioca liquid waste, and Identify
it by Fourier transform infrared spectroscopy (FTIR) and Scanning Electron Microscope
(SEM). The analysis was performed to characterize the functional groups and types of
CA membrane.
2. Materials and Methods
Preparation of Nata de Cassava
Tapioca liquid waste that has been filtered is taken in increments of 1 l was then
added sugar as much as 10% (w/v) and ammonium sulfate as much as 0.5% (w / v), the
mixture is heated to boiling, stirring frequently, then when it has been boiled it is
poured Into the fermentation container which has been prepared and set pH to 4-4.5
by the add~tlon of glacial acetic acid. Container is covered with sterile paper and tied
with rubber. The next day, as much as 20% (v / v) inoculum incorporated Into the
medium and incubated for 6 days at room temperature to form nata (Arviyanti and
Yullmartanl 2009).
PreparatIon of Dry Powder of BC
Sheet of nata de cassava is washed with water and then boiled to remove remaining
bacteria. Furthermore, nata sheets soaked in a solution of NaOH 1% (w/v} at room
temperature for 24 hours, followed by 1% acetic acid for 24 hours to neutralize its pH.
Nata sheet that has been neutralized then washed with water and squeezed using a
Buchner funnel and vacuum pump to form thin sheets that are still wet. This thin sheet
Is dried In the sun and then crushed in a blender tc make a powder.
Synthesis of Cellulose Acetate
Acetylation of Be powder is done by modified procedure of Arifin (2004) dan Pasla
(2006). 1.8 IS of BC powder was weighed in a plastic bottle with double lid then added
100 ml of acetic acid. Bottle strongly shaken by hand for 1 minute, then shuffled back
to the shaker for 20 minutes. After that, filtered by vacuum pump with a Buchner
funnei and squeezed. The same filtering was repeated once more. Furthermore, the
powder soaked in 50 mt of acetic acid in double lids bottle. After 3 hours, the powder
re-nltered with vacuum pump and squeezed and then Incorporated into a new
container.
Be powder is then added to a solution of glacial acetic acid-H2S04 wftbfeto
100:1 (10:0.1 mL) and stirred strongly. After that, with a ratio of 1:5 acetic anhyddde
Internadonal Seminar on Environmental Science (ISES2011) 

October 8"" lOll 

University ofAndalas< 

87
was added with a pipette drops gradually while stirring with a stirring rod unti
thickened and allowed to stand for 2 hours, starting from the addition of the firs~
drops of acetic anhydride. After the acetylation process is complete, the suspensiof
hydrolyzed with 2.4 ml of glacial acetic acid-distilled water (2:1) and stirred at the firs'
few minutes, then was allowed to stand for 30 minutes, starting from the addition 0
dilute acetic acid. Furthermore, the hydrolysis solution was centrifuged for 15 minute:
at a speed of 4000 rpm. The resulting supernatant was then inserted into a beakel
containing 500 ml of distilled water and stirred as strong as possible with a magneth
stirrer to form white flakes (CA)
CA fragments obtained with the filtered-vacuum BOchner funnel and washed with It-.
NaHC03 until C02 gas bubbles disappear, then washed again with distilled water
These neutral fragments are squeezed and then dried In an oven with a temperature
of 50 2C for: 24 hours until the CA is completely dry. The resulting products were ther
analYzed for CA water content and levels of acetyl.
Preparation of Membranes
Preparation of membranes made with modified procedures of Pasla (2006). The firs1
phase, CA Is dissolved in dry acetone solvent (according to the degree of acetylatior
generated) using ~ magnetic stirrer. Polymer ratio and solvent used by 16% (w / v)'.
The solution Is then poured onto glass plates. Furthermore, the solution is pr.inted b
pressing and interesting s!!llution using the stir bar to obtain a thin layer that sticks tc
the glass and left for 15 minutes to evaporate the solvent. Cross section of glass wa~
then soaked In water until a thin layer of membrane that sticks to the glass apart.
Membrane characterization
FTIR Analysis
FTIR analYSis performed on powdered cellulose and cellulose acetate membranes.
Each sample was prepared to form pellets and then placed in the sample holder.
SEM Analygls
CA membrane Is cut into small then praced on the sample. Then, the sample was
placed In a tube for the gold-coated surface for 20 minutes. Furthermore, samples that
had been coated Is. placed in a SEM tool and look for the best magnification for surface
morphology can be observed, Images obtained tnen photographed and stored.
3. Result and Discussion
The addition of sugar as a carbon source as much as 10%,0.5% ammonium suiphate as
a source of nitrogen, A. xylinum as stofter as much as 20%, and setting the pH to 4
International; Seminar on Environmental Science (ISES201 )) 

Octooer 8th
, 20) 1 

Uninnity orAndalas: 

88
with the addition of glacial acetic acid is the optimum conditions needed to make nata
de cassava from 1 l of liquid waste tapioca (Avriyanl and Yullmartani 2009). The
addition of sugar which Is less than 10% do not provide enough carbon source so that
disrupt bacterial metabolism and bacterial growth would be hampered, whereas the
addition of sugar more than 10% will cause the media is too concentrated so that the
bacteria work to be not optimum. Setting the pH to 4 aims to make the A. xylinum is
superior compared with other bacteria in terms of obtaining nutrients from the media
for its growth, thus preventing the growth of other bacteria that can disturb the
growth of nata.
Nata de cassava (Be) obtained In this study is white with a thickness of about 1
em (Figure 4). Before acetylation" BC Is soaked In NaOH 1% to swell the structure of
cellulose fibers so it can open and reduce the intramolecular hydrogen bond.
Immersion in 1% CH3COOH is Intended to neutralize the alkalinity of the structure of
BC that has been purified. The structure of the swollen cellulose can Increase the
accessibility of·OH group on cellulose to acetylation reagent. BC then dried and
crushed to obtain a brown powder. BC powder produced has a tight structure due to
intermolecular hydrogen bonding of cellulose (Arifin 2004).
Figure 1 Nata de cassava.
Cellulose Acetate (CA)
Manufacture of cellulose acetate include four stages, namely activation, acetylation,
hydrolysis, and purification. Stages of activation using concentrated acetic acid to
attract water remaining in the powder BC because BC is hygroscopic powder. The
process of immersion in acetic acid also Increases the rea~lvlty of cellulose as the Be
matrix which Is difficult to penetrate by chemical reagents will be swollen, so as to
accelerate the penetration of acetic anhydride into the matrix at the time of
acetylation.
International Seminar on Environmental Science (ISES2011)
October 8'h, 1011
University of Andatas
89
Acetylation process intended to substitute BC hydroxyl groups with acet
groups to form CA. Acetylation is an exothermic reaction, the temperature must t
kept low to avoid degradation of the cellulose chain and to avoid evaporation (Windir
and Hasche 1947). This can decrease the resulting yield will be reduced, or CA produc
can not form at all. The addition of ac.etic anhydride dropwise followed by stirrir
during the process of acetylation can maintain the solution temperature remained 10
and avoid It, because the addition of acetic anhydride in significant quantities cc
cause the system temperature to Increase rapidly.
The third stage is hydrolysis, acetylation of the termination process with tr
addition of dilute acetic acid. Hydrolysis with dilute acetic acid can reduce the levels t
acetyl substitution and reduce the degree of CA to the desired value. The reaction
then purified by centrifugation to separate the acylated and BC are not. Parts of tr
acylated form of supernatant subsequently dispersed into distilled water to obtain
tanned white flakes which is cellulose acetate (Figure 2).
Figure 2 Powder cellulose acetate.
Cellulose Acetate (CA) Membranes
CA powder produced has a acetyl content of 40.38%. CA with acetyl (ontent of 37 t
42% soluble in acetone solvent. Therefore, the CA powder produced in this study weI
dissolved In acetone to make the CA membrane. Preparation of CA membrane mad~
by phase inversion method. Polymer solution was printed on glass plates whose sidE
are covered with tape.. CA solution was printed and allowed 15 minutes to evaporat
the acetone until the solution becomes dry and form a membrane sheet. Membran
sheets are then soaked in water to release it from the glass. The resulting membranE
are white-brown (Figure 3),
Inter.national Seminar on Environmental Science (ISES2011) 

October Stll, 2011 

Unk-ersity ofAndals!< 

90
Water levels and levels of Acetyl CA
levels show the abundance of acetyl-OH group in BC that has been acylated or tile
number of acetyl groups contained in the CA.. Factors that may affect the magnitude
levels of acetyl cellulose Is a method of drying, the concentration of NaOH
mercerization on the stage or purification of cellulose, and cellulose ratio between
weight and volume of acetic anhydride (Pasla 2006). The factors above have been
optimized by Arifin (2004) and Yulianawati (2002).
Cultivated bacterial cellulose obtained containing low water levels due to
moisture can affect the course of acetylation reaction. -OH group on the water more
easily reacts with acetic acid anhydride as compared to the-OH groups on cellulose.
Therefore, high accessibility to the cellulose-OH group is required to facilitate
acetylation reaction by acetic acid anhydride reagents.. The higher accessibility of the
cellulose-OH, acetyl levels would be even higher. CA acetyl content obtained In this
study of 40.38%.. The value is equivalent to the levels of acetyl substitution degree of
2:51. The degree of substitution (OS) is the average number of H atoms on the
hydroxyl group (-OH) is converted into acetyl group in each anhydroglucose residue.
OS is associated with the application of CA in the industry. CA with OS 2.2 to 2.7 can be
applied as a yarn and film.
CA with acetyl content of 40.38% can be dissolved In acetone (Kirk and Othmer
1993). Therefore, the solvent used to make the membrane CA in this study is acetone.
According Wenten (1999), the higher the levels of acetyl, membrane pore size will be
smaller and the water permeability will decrease. Based on the statement, the CA
obtained in this study has pores small enough and low enough water permeability
seen from the acetyl vaiue which has high enough levels. This can be evidenced by the
results of SEM analysis on the CA membrane surface that shows the range of
membrane pore size (Fig. 6).
CA water content obtained was 21.49%. The amount of water content can be
caused by the drying time of less CA long time in the oven so it has not gained the
weight that Is really constant. In addition, the cleanliness of the container and place of
measurement can be influential because it can add weight to be weighed. The value of
water content is necessary to calculate the levels of acetyl CA.
FTIR Spectra Analysis
FTIR spectrum analysis performed on cellulose nata de COCO, nata de cassava
powder, and CA, Cellulose nata de coco Is the result of culturing the bacteria A.
xylinum in coconut water medium without any additions.
In the FTIR spectrum of nata de cassava powder (Fig. 4} contained the
absorption band at 3394.46 cm-1
wavelengths which is the stretching absorption band
Internadonal Seminar on Environmental Science (ISES2011)
October Slh, 2011
University ofAndala,
91
of-OH group as well as on the wavelength region 1059.15 cm ·1 which is an absorption
band stretching from the group CO. In addition, there are also absorption band for CH
stretching in the wavelength region around 2900-3000 em -1. Uptake values are not
much differ,ent also found on the FTIR spectrum of cellulose nata de coco (Fig. 5), ie
3367.85 cm -1 for-OH groups, 1059.21 cm -I for CO groups, and around 2900-3000 cm -1
for CH stretching. This indicates that the constituent structure contained on nata de
cassava powder Is similar in structure to the cellulose constituent nata de coco.
Therefore, based on the spectrum, nata de cassava powder can be regarded CIS
cellulose, although there is still a possibility of other substances are impurities.
Figure 3 FTIR Spetttra of Cellulose nata de coco.
I.
Il
laboratory Test R~utt
seiIJlOs~
?lAir'
fI~ , (
Il
,f
~VI
II I
~r lG I
i f, I
,/0
elOOG :006 I!I<! lOOCi
..,1
Figure 4 FT1R Spectra of Powder nata de cassava.
International' Seminar on Environmental Science (ISÂŁ820J I)
University ofAndalns:
October st 2011
92
Nata de cassava powder spectrum compared with the membrane of FTIR CA to
see the success of the acetylation process that has been done. In the FTIR spectrum of
CA membrane (Fig. 5) there is a typical absorption band for carbonyl group or a C= 0,
ie the wavelength region 1754.81 cm ·1. In addition, there are absorption band for CO
acetyl group at the wavelength of 1042.34 cm -1. This indicates already the formation
of acetyl groups in cellulose nata de cassava after diasetilasi to become CA. The
existence of absorption band for-OH group at 3445.12 cm-1 region indicates that there
is some residual hydroxyl groups on each anhidroglukosa are not acylated. This can be
evidenced from the value of OS in CA that does not reach Its maximum value, which is
3.
!~
.; i
I ',; ,
I,
I
, i
I I
i
i
I
o , ! '
o o '00
I iI r! iii ! I i I 1 I I
Ui II t. JJ___ i Itl litH ;Ii
Figure 5 FTIR Spectra of CA Membranes.
Analysis of CA membranes by SEM
Characterization by SEM alms at observing the morphology of the surface membrane,
namely by looking at the existence and size of membrane pores as well as latitude
cross-section. From these observations, membrane type being analyzed be known.
Observations made on two sections of the membrane, ie the surface and cross section
latitude. The results of SEM with magnification of 5000x on the membrane surface
showed the existence of pores that are spread on the membrane (Flg.6). The pore
diameter of about 0.37-0.95 Ilm.. This suggests that the membrane can withstand the
particles larger than 0.95 IJ,m. in other words, permeate formed consisting of partide
size S 0.95 Ilm while rentetatnya be a particle size ~ 0,95 Ilm. According to Mulder
(1996), the membrane has a pore size of 0.1-10.0 IJ,m classified as microfiltratlon
membranes. Therefore, the resulting membrane CA is a microfiltration membrane.
International Seminllron Environmental Science (ISES2011)
October Sill, 2011
University ofAndalas
93
Figure 6 The Surface of CA Membrane With a Magnification of 5000 times.
Based on morphology, the observation of cross section of the membrane with a
magnification of 2500 times (Fig.7) shows that the resulting membrane includes an
asymmetric membrane as composed of several layers. Asymmetric membrane
structure consists of layers of very dense an~ porous layers as a buffer. In asymmetric
membranes, permeation occurs, in a dense layer having a large mass transfer
resistance (Undu et a/2008).
Figure 7 Cross-section latitude CA membranes with 2500 times magnification.
5. Conclusion
Tapioca liquid waste can be mi:lde into nata de cassava. This is evidenced from the
similarity spectrum of celhuiose from nata de cassava with nata de coco. Cellutose nata
de t:tassava can diasetilasi, then the resulting CA made into membranes by phase
inversion technique using acetone solvent. CA formation is indicated by the results of
FTIR analysis on CA membrane indicating the presence of C :::: 0 absorption band at
Intel!national: Seminar on Environmental Science (ISES201 1) 

Od()ber 8l
 2011 

Unh'ersity orAndalas. 

94
wavenumber region 1725.92 cm-1 and CO acetyl at 1061.37 cm-1 region. CA has
acquired the water levels of 21.49% and the acetyl content of 40.38% (equivalent to a
range of degree of substitution of 2:51). SEM observations on CA membrane showed
that the resulting membrane is a m1crofiltration membrane type and asymmetric.
6. References
Andrlansyah M. (2006). The properties of membranes made of pineapple juice fruit
leather [thesis]. Bogar: Faculty of Mathematics and Natural Sciences, Bogar
AgrlcuIturalUnlverslty.
Arifin B. (2004). Optimization of conditions for bacterial cellulose acetylation of nata
de coco [thesis]. Bogar: Faculty of Mathematics and Natural Sciences, Bogor
Agricultural University.
Arviyanti E, Yulimartanl N. (2009). Effect of the addition of tapioca wastewater in the
production of nata [thesis}. Semarang: Faculty of Engineering, University
Diponegoro.
[BPS} Central Bureau of Statistics. (2011). Table-Productivity-Area Harvested Crop
Production Cassava Entire Province [connected periodically].
http://www.bps.go.id [July 24, 2011J.
Desiyarni. (2006). The design process of making cellulose acetate from microbial
cellulose for ultrafiltration membranes. [thesis]. Bogar: Graduate Program,
Bogar Agricultural University.
Fengel D, Wegener G. (1984). Wood: Chemistry, Ultrastructure, Reaction. Berlin:
Walter de Gruyter.
Gosh R. (2003). Protein bioseparatlon Using ultra/iltratlon Theory, Application, and
New Development. Oxford: Imperial College Press.
Hanifah TA,Saeni MS, Ad!juwana H, Bintaro HMH. (1999). Evaluation of heavy metal
content of lead and cadmium In cassava (Manihot esculenta Crantz) is
cultivated municipal solid waste, Gaku-ryoku Scientific Bulletin 1:38-45.
H Hartl lE Craine, OJ Hart. (2003). Organic Chemistry. Achmadi 55, translator; Safitri
A, editors. New York: Erlangga. Translation of: Organic Chemistry.
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York: Interscience.
Lapuz, MM, EG Gallerdo, Palo MA. (1967). The nata organism-cultural characteristic
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and identify requirements. Philippines J Sci 96:91-107.
Lindu M, Puspitasari T, ISMI E. (2008). Synthesis and test the ability of cellulose
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the dye in artificial wastewater. Nuclear Energy Agency 4:107-112.
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cellulose from pineapple waste [thesis]. Bogar: F<'Iculty of Mathematics and
Natural Sciences, Bogar Agricultural University.
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Education and Science Teacher Training, University of Muhammadiyah
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Susanto T, Adhitia R, Yunianta. (2000). Making Nata de pina pineapple fruit from the
skin, the study of carbon sources and dilution of fermentation medium, J
Agricultural Technology 1:58-66.
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anaerobic system [thesis], Bogar: Faculty of Animal Husbandry, Bogar
Agricultural University.
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industry. In the Proceedings of the National Seminar on Chemical and Process
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October gth, 2011
Unh'ersity of Andaills­

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Study of Fourier Transform Infrared Spectroscopy and Scanning Electron Microscope of Cellulose Acetate Membrane from Wastewater of Tapioca.

  • 1.
  • 2. PROCEEDING INTERNATIONAL SEMINAR ON ENVIRONMENTAL SCIENCE 20111 "lEnWcmment (Jjasedon Science t.Rpearcfifor(BetterLifeII October, 8th 2011 Gedung Seminar E, Andalas University Publish by: Chemistry Department AndalasUniversity 2011
  • 3. International Seminar on Environmental Science 2011 Environment Based on Science Research for Better Life Steering and Scientific Committee: Prof. Dr. Abdi Dharma Dr. Mai Efdi Dr. Syukri Drajat Dr.lulhadjri Organizing Committee: Chairperson: Riko Irwan Secretariat: Epi Supriwardi, Defina Nasmiaty, Reno Permata Sari, Wilda Lion Suri Treasurer: Nuryanti, Ayu Kurnia D.P.S, Sestry Misfadhila, Mega Ulfaningsih Program: Sisri Handayani, Restiyani Harahap, Liti fitrianny, Unzilla Rahmi, Rahmatul Hasanah Publicity: luI Aritin, Maharani Hazar, Yosi Febriani, Rikha Septiani Yuda Resource and Facilities: Firdaus M, Yuniar Hardiati, Restu Harly Pebriani, Rid Junaidi, Febrina lamar Editor: Rikha Septiani Yuda, Maharani Hazar, Zul Arifin Secretariat: Chemistry Department Faculty of Mathematic and Natural Science Andalas University Limau Manis, Padang, West Sumatera, Indonesia, 25163
  • 4. • J ( I '" PREFACE VICE RECTOR III ANDALAS UNIVERSITY Assalammu'alaikum Wr. Wb All praises be to Allah, the Almighty, the creator of the world. May His peace and blessing be upon our prophet Muhammad SWT, the leader of messengers and guide of faithful. Environmental problems are now becoming the hot issues which have need to solve by all of us, because these issues directly effect the quality of humans life on earth. Therefore, as scientist we have to give more effort to give solutions on those issues. This proceeding is useful as a guide to fix those issues, as the first step to keep the environmental safe for our next generation. Padang, 2012 Vice Rector III Andalas University Prot: Dr. H~arun.MS NIP, 19620506198811 1001 II. International Seminar on Environmental Science (ISES2011) ~;~~er Sih, 2011 .enlty ofAndal"
  • 5. PREFACE DEAN OF lHE FACULTY MATHEMATICS AND NATURE SCIENCE ANDAtAS UNIVERSITY AssaJamualikum, wr,b, All pnuses be to Allah, the Almighty, the ~reator of the world, May His peace and -blessing be upon our prophet Muhan1mad SWT, the leader of mes~engers and guide of tbithful. t would like to thank all of you who participated in this International seminar which is held he-Ie in Padang, and specially, key note speakl~rs that came here, and organizing committee with hard work to prepare this seminar. For the students, I think, this event is learning process that tel be important in the future time. I am proud that so many experts in the field of this seminar decided to take part in the event that has been co-organized by our chemistry students, Iam confident that the seminar will provide a great opportunity for an international and national gathering for sciences and te(~hnolog)' from different nation, <5 we know, at the moment environmental and energy are great problem for us. In this case, research is one of that we can do to solve these problem and important role to improve the quality of life, [ do hope that, this semmar provided platform for sci.entist and technologist to meet and share ideas, achievement as well as experiences through the presentation of papers and discussion, Wassalamualikum Vw Pad.'lng, 2012 Dean ofthe Faculty Mathematics and Nature Science r;::~j~ Prof Dr, H Emriagi, MS NIP. 19620409198703}003 , lnternatlonal Seminar on Environmental Science (ISES2011) ,Q. '()ctober 81b~ 2011 'University of Ancbla!! ii
  • 6. FOREWORD MAJOR HEAD OF CHEMISTRY UNIVERSITY ANDALAS A.ssalammu'alaikum Wr. Wb Thanks be to God praise for all the abundance of His grace and guidance. Sa:awat coincided greet RasuruJlah SAW, mtemational Seminar on the theme "Environmental Based on Science Research lor a Better Life", This is proof that we as chemistry scientist aware that environmental problems are exist, be(:ause the environment is one of subarea in which we understood better as a chemistry scientist. The environm(mtal issues now rise up with the rapid of science and technology development that is not coupled with environmental awareness. The waste that is not handled properly, carelessly and discarded on the- right spot, tum raises into new poroble:ms for the environmenL also to the people 'who were around the neighborhood. Therefore, the presence of this International Seminar, and the summarize of various studies to address various environmental problems that have been packaged in this procedding can provide solutions and contribute little to the existing problem. Hopefully it can be optimized and maximized its use, P,lCiang, 2012 Chairman of the Chemistry Department Andalas University Dr. Adli Santoni NIP. 1001 19620506 198811 International Seminar on Environmental Science (ISES2011) l()ctober 81ft , 2011 [University ofAndal8s III
  • 7. Internationa(Seminar on fÂŁtwironmentafScimce (LS!ÂŁ52011) OctoBer /pI, 2011 I'XJ/. Ji'Y.M1(J ltuforusia ~ :H1:M'K)4, 'Unaruf rDepartlfllnt ofCliemistry. 'University 0/_'4rufafas Content Preface by Vi~Rector III... .......... ... , ........,....,. ...,...... 1 Preface by Dean ....."................... , ..... ,... ....,...........'.... ,... ,11 Preface Chairperson "" .. ,..".,....,......,.... ,. """""" ,.",.",." '" ,."." .. ,.. ,.,.....,,'..... "",.111 Contents ..........,' ", '"'''' ,..............,.....,.. ,' .. '.... ,....,,'..... """''''..,.."......,... ',,,....."" IV Presentations by Keynotes Towards A New Type Of Science For Successfully Addressing The Global Challenges For Humankind file C, Gebeshuber...................................................,............................................... 1 Tyrosinase-Immobilized Biosensor Based On Mwnt Supports With Multifunctional Group Seong-Ho Choi And Kyo-ll Kim............................................................................. 12 Presentations by Speakers Agroclimate Cropping Pattern Changes Based On Climate Change Pr~iections With Hadcm3 A2 And B2 Climate Change Scenario For Reducing The Risk Of Harvest Failure In Ngijo Watershed, Yogyakarta Special Province, Gilang Arya D. Andung 8ayu S. Fitria Nucifera, Emi/ya NurjanL .....................22 Antioxidative Activity Of Lignin From Oil Palm Empty Fruit Bunch. Gustini Syahbirin. Vanny Pratl~Yi. Suminar Setiati AchmadL............................. 39 Biodegradation Of Phenol-Containing Textile Industry Wastewater By Candida Tropicalis. Suryani, Laksmi Ambarsari, Aktnal.......................................................................48 Tsunami Hazard Mapping As A Basis Of Spatial Planning In Sadeng Coastal Area, Gunung KiduJ District Ahmad Cahyadi, Andungbayu Sekaranom, Fitria Nucifera, Dinifeti Anggraini..................................................................................................61 Photolysis, Sonolysis And Ozonolysis For Degradation Of 2,4Dichlorophenoxyacetic Acid (2,4-D) ElvilUl'ifati..............................................................................................................70 Karst Groundwater Management Based On Groundwater Recharge And Vulnerability Mapping: Case Study In Paliyan And Saptosari Subdistrict, Gummgkidul Regency Ahmad Cahyadi. Fedhi Astuti Hartoyo. fJenkr Nugraha.....................................76 iv
  • 8. 1mentationa{Seminar on E,mAronmenta{Science (ISES2011) October 811i, 2011 1'1(;4 :}fl')t{7(J 1rufonesia r:!l J{J'M1(Jl Vnan4 'Department ofC("mistry, Vniversity of;4.rufuf'as Study OfFourier Transform Infrared Spectroscopy And Scanning Electron Microscope OfCellulose Acetate Membrane From Wastewater OfTapioca Betty Marira Soebrata, Sri Mulijani. /smiaini Nwpatria Purri......,..........".,........8: Synthesis And Characterization Of Bimetallic Catalyst Mn/Nj fmmobilized On Moditled Silica Nuryanti. Syukri, Syukri Ariej...................................................,.........,.........."......9' Immobilization Acetonitrile Ligated Cobalt(II) Complexes On Modified Silica And Its Characterization Benny Rio Fernandez, Syukrt Arief. Syukri............."........................................... 11 Poster Presentation The Effect Of Prefilter On Titania Modified Ceramic Membrane Efficiency In Humic Water Treatment To Provide Drinking Water Admin AIif. Mat Efdi, Oily Norita Tetra.............................................:................ ]23 The Effect Of Sol-Gel Processing Variables On Structure Changes OfTioz ' Nanopartiles Ye/ria Rilda...........................................................................,......,......................,127 Preparation And Photocatalytic Property Of Nanoparticle Magnetic Ti0:2-Nifezo4 By Coprecipitation Method Rahmayeni, Upira Setiani. Syukri Ariej. Rianda.............,.................................... 13': The Determination OfComposition OfAir Particulate Matter Pollution In Comparative Study OfN<>x Gas Analysis By Phenol Disultonic Acid And Saltzmaan Method Using The Cadmium Reduction Column. Refilda Suhailt. Radhia Putri, Ardeniswan......................................................... 139 v
  • 9. Study ofFourier Transform Infrared Spectroscopy and Scanning Electron Microscope of Cellulose Acetate Membrane from Wastewater of Tapioca. Betty Marita Soebrata, Sri Mu!ijanf, 1smiaini Nurpatria Putri Department o/Chemistry, Faculty o/Mathematics and Natural Sciences, BogorAgricultural University Email~ bcttymru:it{1@l4lllilII,cQill ABSTRACT. Wastewater of tapioca is waste product from starch precipitation or separation process from its water in making tapioca. This wastewater still contains carbohydrates such as glucose, so it can be used as raw material for making cellulose and cellulose acetate (CA) membrane, Nata de cassava was made by fermentation process using Acetobacter xylinum In wastewater of tapioca as the fermentation media. Then, the nata was dried and grinded to produce bacterial cellulose (Be) powder. BC powder was reacted with acetic anhydride to produce CA powder. CA powder was dissolVed to acetone solvent (appropriate with an acetyl degree of CA) with 1696 w/v composition and then formed to be a membrane. These CA membraM was characterized with Fourier Transform Infrared (FTIR) and Scanning Electron Microscope (SEM).. Analysis from FTIR spectrum showed that CA was formed, by the existence of absorption band of C carbonyl at 1725.92 cm-1 wavenumber and CoO acetyl at 1061.37 cm-l. The resuh: of SEM analysis showed that the membrane which has been produced was the mlcrofiltration and asymmetric membrane with the diameter pore approximately of 0.37-0.95 IJ.m. CA powder that has been prodliJced had a water content of 21.39% and an acetyl degree of 40.38% (equal with substitution degree of 2.51). Keywords: cellulose, cellulose acetate, nata, bacterial cellulose, membrane, , FTIR, SEM 1. Introduction Cassava (Man/hot esculenta) is a clump of food crops from the Americas and has another name ubi kayu orsingkong. In Indonesia, cassava is an important source of carbohydrates after rice, with a carbohydrate content of 34.7% (Soetanto 2001). Cassava can grow even in infertile soil, in the tropical climate. Indonesia is currently the third largest cassava producil"'g countries in t.he world after Brazil and Thailand because many Indonesian people have switched from planting rice to cassava farming (SumlyatI2009). According to Badan Pusat Statlstik (BPS 2011)J the amount of cassava production In Indonesia in 2009 was 22,039F145 tons and in 2010 increased to 23,908,459 tons (preliminary figures). lnternational Seminar on Environmentlll Science (ISES10ll) October Slh, 2011 University ofAndalas 85
  • 10. Cassava can be consumed directly as food or used as a raw material of fooe industry, one of which is the tapioca industry. The process of making the tapioca in thE industry will generate solid waste' (onggok) and liquid waste. Tapioca liquid waste car be generated from the washing stage of raw materIals (cassava) and also thE deposition process to separate the starch from the water. The process of makin~ tapioca in large industries and small industries in general includes the stages of skir peeling, washing, scrapping, extraction, starch deposition, and drying. Wastewater from tapioca industry which is still new is creamy color, While the color of spoiled waste is dark gray. Turbidity that occurs on the waste caused by the presence of organic materials, such as soluble starch, microorganisms, and other colloid materials. Tapioca liquid waste from the precipitation has a BOD value of 1450.8-3030.3 mg L -1 with an average of 2313.54 mg L -1, COD of 3200 mg L ·1 dissolved solids 638-2836 mg L -1, and the amount of cyanide (CN ) of 19.58-33.75 mg l -1 (Vegantara 2009). Therefore, if the waste is discharged into the er:1vironment that will cause environmental pollution, such as bad smell and some wells are not suitable for consumption. The current technology has not been able to separate the starch which dissolved in water so that liquid waste which is released into the environment stili contains starch. The liquid waste will decompos~ naturally In water bodies and cause a bad odor. -rhe smell is generated in the process of decomposition of compounds containing nitrogen, sulfur, and phosphorus of the protein material (Olive 1999 and Hanifa et at~ 1999). Another alternative that can be done to treat this wastewater Into products that can be exploited further is to process them into so-called nata de cassavo. Nata formation requires the element C that comes from glucose and Nand 0 elements derived from the addition of ammonium sulfate. These elements are used as nutrients and carbon sources for bacteria Acetobocter xylinum in order to form a nata. Tapioca wastewater containing glucose as the carbon element can therefore be used as a good medium to stimulate the growth of bacteria such as forming nata. Therefore, tapioca liquid waste could potentially prodl2lce nata. Nata in the' form of cellulose produced by bacteria that can be referred to as bacterial cellulose (BC). In addition: nata can be characterized as a composite of carbon fibers Into a solid form and porous. so nata potential to be utilized as a cellulose membrane. However, the cellulose membrane did not have a high commercial value. Therefore, further processing Is needed to turn it into a membrane of cellulose acetate (CA) which Is more valuable than cellulose membrane. Celili/lose trlacetate (primary CA) obtained from: the reaction of cellulose with aatic anhydride and H2S04 as a catalyst. Acetylation is an important stage in the .fifacture of CA as it relates to its 4lhility to dissolve in certain organic solvents In '1Ffl'15rocess of membrane manufacture. CA ~olubility in organic solvents is influenced InteflDational:Seminar on Environmental Science (18ES2011) October 8t h, 2011 Uninrsity orAndaln 86
  • 11. by the levels of acetyl (Desiyarni 2006). Setting levels is carried out by reaction of acetyl hydrolysis using dilute acetic acid to obtain the appropriate degree of substitution, This study aims to make membrane-based CA tapioca liquid waste, and Identify it by Fourier transform infrared spectroscopy (FTIR) and Scanning Electron Microscope (SEM). The analysis was performed to characterize the functional groups and types of CA membrane. 2. Materials and Methods Preparation of Nata de Cassava Tapioca liquid waste that has been filtered is taken in increments of 1 l was then added sugar as much as 10% (w/v) and ammonium sulfate as much as 0.5% (w / v), the mixture is heated to boiling, stirring frequently, then when it has been boiled it is poured Into the fermentation container which has been prepared and set pH to 4-4.5 by the add~tlon of glacial acetic acid. Container is covered with sterile paper and tied with rubber. The next day, as much as 20% (v / v) inoculum incorporated Into the medium and incubated for 6 days at room temperature to form nata (Arviyanti and Yullmartanl 2009). PreparatIon of Dry Powder of BC Sheet of nata de cassava is washed with water and then boiled to remove remaining bacteria. Furthermore, nata sheets soaked in a solution of NaOH 1% (w/v} at room temperature for 24 hours, followed by 1% acetic acid for 24 hours to neutralize its pH. Nata sheet that has been neutralized then washed with water and squeezed using a Buchner funnel and vacuum pump to form thin sheets that are still wet. This thin sheet Is dried In the sun and then crushed in a blender tc make a powder. Synthesis of Cellulose Acetate Acetylation of Be powder is done by modified procedure of Arifin (2004) dan Pasla (2006). 1.8 IS of BC powder was weighed in a plastic bottle with double lid then added 100 ml of acetic acid. Bottle strongly shaken by hand for 1 minute, then shuffled back to the shaker for 20 minutes. After that, filtered by vacuum pump with a Buchner funnei and squeezed. The same filtering was repeated once more. Furthermore, the powder soaked in 50 mt of acetic acid in double lids bottle. After 3 hours, the powder re-nltered with vacuum pump and squeezed and then Incorporated into a new container. Be powder is then added to a solution of glacial acetic acid-H2S04 wftbfeto 100:1 (10:0.1 mL) and stirred strongly. After that, with a ratio of 1:5 acetic anhyddde Internadonal Seminar on Environmental Science (ISES2011) October 8"" lOll University ofAndalas< 87
  • 12. was added with a pipette drops gradually while stirring with a stirring rod unti thickened and allowed to stand for 2 hours, starting from the addition of the firs~ drops of acetic anhydride. After the acetylation process is complete, the suspensiof hydrolyzed with 2.4 ml of glacial acetic acid-distilled water (2:1) and stirred at the firs' few minutes, then was allowed to stand for 30 minutes, starting from the addition 0 dilute acetic acid. Furthermore, the hydrolysis solution was centrifuged for 15 minute: at a speed of 4000 rpm. The resulting supernatant was then inserted into a beakel containing 500 ml of distilled water and stirred as strong as possible with a magneth stirrer to form white flakes (CA) CA fragments obtained with the filtered-vacuum BOchner funnel and washed with It-. NaHC03 until C02 gas bubbles disappear, then washed again with distilled water These neutral fragments are squeezed and then dried In an oven with a temperature of 50 2C for: 24 hours until the CA is completely dry. The resulting products were ther analYzed for CA water content and levels of acetyl. Preparation of Membranes Preparation of membranes made with modified procedures of Pasla (2006). The firs1 phase, CA Is dissolved in dry acetone solvent (according to the degree of acetylatior generated) using ~ magnetic stirrer. Polymer ratio and solvent used by 16% (w / v)'. The solution Is then poured onto glass plates. Furthermore, the solution is pr.inted b pressing and interesting s!!llution using the stir bar to obtain a thin layer that sticks tc the glass and left for 15 minutes to evaporate the solvent. Cross section of glass wa~ then soaked In water until a thin layer of membrane that sticks to the glass apart. Membrane characterization FTIR Analysis FTIR analYSis performed on powdered cellulose and cellulose acetate membranes. Each sample was prepared to form pellets and then placed in the sample holder. SEM Analygls CA membrane Is cut into small then praced on the sample. Then, the sample was placed In a tube for the gold-coated surface for 20 minutes. Furthermore, samples that had been coated Is. placed in a SEM tool and look for the best magnification for surface morphology can be observed, Images obtained tnen photographed and stored. 3. Result and Discussion The addition of sugar as a carbon source as much as 10%,0.5% ammonium suiphate as a source of nitrogen, A. xylinum as stofter as much as 20%, and setting the pH to 4 International; Seminar on Environmental Science (ISES201 )) Octooer 8th , 20) 1 Uninnity orAndalas: 88
  • 13. with the addition of glacial acetic acid is the optimum conditions needed to make nata de cassava from 1 l of liquid waste tapioca (Avriyanl and Yullmartani 2009). The addition of sugar which Is less than 10% do not provide enough carbon source so that disrupt bacterial metabolism and bacterial growth would be hampered, whereas the addition of sugar more than 10% will cause the media is too concentrated so that the bacteria work to be not optimum. Setting the pH to 4 aims to make the A. xylinum is superior compared with other bacteria in terms of obtaining nutrients from the media for its growth, thus preventing the growth of other bacteria that can disturb the growth of nata. Nata de cassava (Be) obtained In this study is white with a thickness of about 1 em (Figure 4). Before acetylation" BC Is soaked In NaOH 1% to swell the structure of cellulose fibers so it can open and reduce the intramolecular hydrogen bond. Immersion in 1% CH3COOH is Intended to neutralize the alkalinity of the structure of BC that has been purified. The structure of the swollen cellulose can Increase the accessibility of·OH group on cellulose to acetylation reagent. BC then dried and crushed to obtain a brown powder. BC powder produced has a tight structure due to intermolecular hydrogen bonding of cellulose (Arifin 2004). Figure 1 Nata de cassava. Cellulose Acetate (CA) Manufacture of cellulose acetate include four stages, namely activation, acetylation, hydrolysis, and purification. Stages of activation using concentrated acetic acid to attract water remaining in the powder BC because BC is hygroscopic powder. The process of immersion in acetic acid also Increases the rea~lvlty of cellulose as the Be matrix which Is difficult to penetrate by chemical reagents will be swollen, so as to accelerate the penetration of acetic anhydride into the matrix at the time of acetylation. International Seminar on Environmental Science (ISES2011) October 8'h, 1011 University of Andatas 89
  • 14. Acetylation process intended to substitute BC hydroxyl groups with acet groups to form CA. Acetylation is an exothermic reaction, the temperature must t kept low to avoid degradation of the cellulose chain and to avoid evaporation (Windir and Hasche 1947). This can decrease the resulting yield will be reduced, or CA produc can not form at all. The addition of ac.etic anhydride dropwise followed by stirrir during the process of acetylation can maintain the solution temperature remained 10 and avoid It, because the addition of acetic anhydride in significant quantities cc cause the system temperature to Increase rapidly. The third stage is hydrolysis, acetylation of the termination process with tr addition of dilute acetic acid. Hydrolysis with dilute acetic acid can reduce the levels t acetyl substitution and reduce the degree of CA to the desired value. The reaction then purified by centrifugation to separate the acylated and BC are not. Parts of tr acylated form of supernatant subsequently dispersed into distilled water to obtain tanned white flakes which is cellulose acetate (Figure 2). Figure 2 Powder cellulose acetate. Cellulose Acetate (CA) Membranes CA powder produced has a acetyl content of 40.38%. CA with acetyl (ontent of 37 t 42% soluble in acetone solvent. Therefore, the CA powder produced in this study weI dissolved In acetone to make the CA membrane. Preparation of CA membrane mad~ by phase inversion method. Polymer solution was printed on glass plates whose sidE are covered with tape.. CA solution was printed and allowed 15 minutes to evaporat the acetone until the solution becomes dry and form a membrane sheet. Membran sheets are then soaked in water to release it from the glass. The resulting membranE are white-brown (Figure 3), Inter.national Seminar on Environmental Science (ISES2011) October Stll, 2011 Unk-ersity ofAndals!< 90
  • 15. Water levels and levels of Acetyl CA levels show the abundance of acetyl-OH group in BC that has been acylated or tile number of acetyl groups contained in the CA.. Factors that may affect the magnitude levels of acetyl cellulose Is a method of drying, the concentration of NaOH mercerization on the stage or purification of cellulose, and cellulose ratio between weight and volume of acetic anhydride (Pasla 2006). The factors above have been optimized by Arifin (2004) and Yulianawati (2002). Cultivated bacterial cellulose obtained containing low water levels due to moisture can affect the course of acetylation reaction. -OH group on the water more easily reacts with acetic acid anhydride as compared to the-OH groups on cellulose. Therefore, high accessibility to the cellulose-OH group is required to facilitate acetylation reaction by acetic acid anhydride reagents.. The higher accessibility of the cellulose-OH, acetyl levels would be even higher. CA acetyl content obtained In this study of 40.38%.. The value is equivalent to the levels of acetyl substitution degree of 2:51. The degree of substitution (OS) is the average number of H atoms on the hydroxyl group (-OH) is converted into acetyl group in each anhydroglucose residue. OS is associated with the application of CA in the industry. CA with OS 2.2 to 2.7 can be applied as a yarn and film. CA with acetyl content of 40.38% can be dissolved In acetone (Kirk and Othmer 1993). Therefore, the solvent used to make the membrane CA in this study is acetone. According Wenten (1999), the higher the levels of acetyl, membrane pore size will be smaller and the water permeability will decrease. Based on the statement, the CA obtained in this study has pores small enough and low enough water permeability seen from the acetyl vaiue which has high enough levels. This can be evidenced by the results of SEM analysis on the CA membrane surface that shows the range of membrane pore size (Fig. 6). CA water content obtained was 21.49%. The amount of water content can be caused by the drying time of less CA long time in the oven so it has not gained the weight that Is really constant. In addition, the cleanliness of the container and place of measurement can be influential because it can add weight to be weighed. The value of water content is necessary to calculate the levels of acetyl CA. FTIR Spectra Analysis FTIR spectrum analysis performed on cellulose nata de COCO, nata de cassava powder, and CA, Cellulose nata de coco Is the result of culturing the bacteria A. xylinum in coconut water medium without any additions. In the FTIR spectrum of nata de cassava powder (Fig. 4} contained the absorption band at 3394.46 cm-1 wavelengths which is the stretching absorption band Internadonal Seminar on Environmental Science (ISES2011) October Slh, 2011 University ofAndala, 91
  • 16. of-OH group as well as on the wavelength region 1059.15 cm ·1 which is an absorption band stretching from the group CO. In addition, there are also absorption band for CH stretching in the wavelength region around 2900-3000 em -1. Uptake values are not much differ,ent also found on the FTIR spectrum of cellulose nata de coco (Fig. 5), ie 3367.85 cm -1 for-OH groups, 1059.21 cm -I for CO groups, and around 2900-3000 cm -1 for CH stretching. This indicates that the constituent structure contained on nata de cassava powder Is similar in structure to the cellulose constituent nata de coco. Therefore, based on the spectrum, nata de cassava powder can be regarded CIS cellulose, although there is still a possibility of other substances are impurities. Figure 3 FTIR Spetttra of Cellulose nata de coco. I. Il laboratory Test R~utt seiIJlOs~ ?lAir' fI~ , ( Il ,f ~VI II I ~r lG I i f, I ,/0 elOOG :006 I!I<! lOOCi ..,1 Figure 4 FT1R Spectra of Powder nata de cassava. International' Seminar on Environmental Science (ISÂŁ820J I) University ofAndalns: October st 2011 92
  • 17. Nata de cassava powder spectrum compared with the membrane of FTIR CA to see the success of the acetylation process that has been done. In the FTIR spectrum of CA membrane (Fig. 5) there is a typical absorption band for carbonyl group or a C= 0, ie the wavelength region 1754.81 cm ·1. In addition, there are absorption band for CO acetyl group at the wavelength of 1042.34 cm -1. This indicates already the formation of acetyl groups in cellulose nata de cassava after diasetilasi to become CA. The existence of absorption band for-OH group at 3445.12 cm-1 region indicates that there is some residual hydroxyl groups on each anhidroglukosa are not acylated. This can be evidenced from the value of OS in CA that does not reach Its maximum value, which is 3. !~ .; i I ',; , I, I , i I I i i I o , ! ' o o '00 I iI r! iii ! I i I 1 I I Ui II t. JJ___ i Itl litH ;Ii Figure 5 FTIR Spectra of CA Membranes. Analysis of CA membranes by SEM Characterization by SEM alms at observing the morphology of the surface membrane, namely by looking at the existence and size of membrane pores as well as latitude cross-section. From these observations, membrane type being analyzed be known. Observations made on two sections of the membrane, ie the surface and cross section latitude. The results of SEM with magnification of 5000x on the membrane surface showed the existence of pores that are spread on the membrane (Flg.6). The pore diameter of about 0.37-0.95 Ilm.. This suggests that the membrane can withstand the particles larger than 0.95 IJ,m. in other words, permeate formed consisting of partide size S 0.95 Ilm while rentetatnya be a particle size ~ 0,95 Ilm. According to Mulder (1996), the membrane has a pore size of 0.1-10.0 IJ,m classified as microfiltratlon membranes. Therefore, the resulting membrane CA is a microfiltration membrane. International Seminllron Environmental Science (ISES2011) October Sill, 2011 University ofAndalas 93
  • 18. Figure 6 The Surface of CA Membrane With a Magnification of 5000 times. Based on morphology, the observation of cross section of the membrane with a magnification of 2500 times (Fig.7) shows that the resulting membrane includes an asymmetric membrane as composed of several layers. Asymmetric membrane structure consists of layers of very dense an~ porous layers as a buffer. In asymmetric membranes, permeation occurs, in a dense layer having a large mass transfer resistance (Undu et a/2008). Figure 7 Cross-section latitude CA membranes with 2500 times magnification. 5. Conclusion Tapioca liquid waste can be mi:lde into nata de cassava. This is evidenced from the similarity spectrum of celhuiose from nata de cassava with nata de coco. Cellutose nata de t:tassava can diasetilasi, then the resulting CA made into membranes by phase inversion technique using acetone solvent. CA formation is indicated by the results of FTIR analysis on CA membrane indicating the presence of C :::: 0 absorption band at Intel!national: Seminar on Environmental Science (ISES201 1) Od()ber 8l 2011 Unh'ersity orAndalas. 94
  • 19. wavenumber region 1725.92 cm-1 and CO acetyl at 1061.37 cm-1 region. CA has acquired the water levels of 21.49% and the acetyl content of 40.38% (equivalent to a range of degree of substitution of 2:51). SEM observations on CA membrane showed that the resulting membrane is a m1crofiltration membrane type and asymmetric. 6. References Andrlansyah M. (2006). The properties of membranes made of pineapple juice fruit leather [thesis]. Bogar: Faculty of Mathematics and Natural Sciences, Bogar AgrlcuIturalUnlverslty. Arifin B. (2004). Optimization of conditions for bacterial cellulose acetylation of nata de coco [thesis]. Bogar: Faculty of Mathematics and Natural Sciences, Bogor Agricultural University. Arviyanti E, Yulimartanl N. (2009). Effect of the addition of tapioca wastewater in the production of nata [thesis}. Semarang: Faculty of Engineering, University Diponegoro. [BPS} Central Bureau of Statistics. (2011). Table-Productivity-Area Harvested Crop Production Cassava Entire Province [connected periodically]. http://www.bps.go.id [July 24, 2011J. Desiyarni. (2006). The design process of making cellulose acetate from microbial cellulose for ultrafiltration membranes. [thesis]. Bogar: Graduate Program, Bogar Agricultural University. Fengel D, Wegener G. (1984). Wood: Chemistry, Ultrastructure, Reaction. Berlin: Walter de Gruyter. Gosh R. (2003). Protein bioseparatlon Using ultra/iltratlon Theory, Application, and New Development. Oxford: Imperial College Press. Hanifah TA,Saeni MS, Ad!juwana H, Bintaro HMH. (1999). Evaluation of heavy metal content of lead and cadmium In cassava (Manihot esculenta Crantz) is cultivated municipal solid waste, Gaku-ryoku Scientific Bulletin 1:38-45. H Hartl lE Craine, OJ Hart. (2003). Organic Chemistry. Achmadi 55, translator; Safitri A, editors. New York: Erlangga. Translation of: Organic Chemistry. Kirk RE, Othmer DF. (1993). Encydopedia of Polymer Science and Technology. New York: Interscience. Lapuz, MM, EG Gallerdo, Palo MA. (1967). The nata organism-cultural characteristic International Seminar 011 Environmental Science (ISES2011) October s'b, 2011 University ofAndalas 95
  • 20. and identify requirements. Philippines J Sci 96:91-107. Lindu M, Puspitasari T, ISMI E. (2008). Synthesis and test the ability of cellulose acetate membranes from nata de coco as ultrafiltration membranes to exclude the dye in artificial wastewater. Nuclear Energy Agency 4:107-112. Pasla FR. (2006). Characterization of cellulose acetate membrane-based bacterial cellulose from pineapple waste [thesis]. Bogar: F<'Iculty of Mathematics and Natural Sciences, Bogar Agricultural University. Scott K, Hughes R. (1996). Industrial Membrane Separation Technology. London: Blackle Academic and Professionals. Soetanto E. (2001). Creating Patilo and Cassava Crackers. Yogyakarta: Canisius. Sumiyatl. (2009). The quality of nata de cassava tapioca liquid waste with the addition of sugar and a longfermentation of different [thesis]. Surakarta: Faculty of Education and Science Teacher Training, University of Muhammadiyah Surakarta. Susanto T, Adhitia R, Yunianta. (2000). Making Nata de pina pineapple fruit from the skin, the study of carbon sources and dilution of fermentation medium, J Agricultural Technology 1:58-66. Vegantara DA. (2009). Tapioca processing wastewater using cow manure to an anaerobic system [thesis], Bogar: Faculty of Animal Husbandry, Bogar Agricultural University. Wenten IG. (1999). The presence of membiane technology in food and beverage industry. In the Proceedings of the National Seminar on Chemical and Process Eng;neering~ Sema~ang. F15 (1·10). Winding ce, RL Hasche. (1947).. Chemical Engineering Series: The Technology of High Polymer. London: McGraw-HilI. International Seminar on Emrironmental Science (ISES20i I) 96 October gth, 2011 Unh'ersity of Andaills­