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Study of filtering Ag liquid sample by chitosan biomembrane using

laser-induced breakdown spectroscopy (LIBS)

Ni Nyoman Rupiasih, Hery Suyanto, Made Sumadiyasa, Christine Prita Purwanto, and Rendra Rustam Purnomo

Citation: AIP Conf. Proc. 1555, 32 (2013); doi: 10.1063/1.4820987

View online: http://dx.doi.org/10.1063/1.4820987

View Table of Contents: http://proceedings.aip.org/dbt/dbt.jsp?KEY=APCPCS&Volume=1555&Issue=1

Published by the AIP Publishing LLC.

Additional information on AIP Conf. Proc.

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Study of Filtering Ag Liquid Sample by Chitosan

Biomembrane Using Laser-Induced Breakdown

Spectroscopy (LIBS)

Ni Nyoman Rupiasih


, Hery Suyanto


, Made Sumadiyasa



Christine Prita Purwanto


and Rendra Rustam Purnomo



Biophysics Laboratory, 2Applied Physics Laboratory, Department of Physics, Faculty of Mathematics and Natural Sciences, Udayana University, Denpasar, 80361, Indonesia

*Email: rupiasih69@yahoo.com

Abstract. The capability of Laser-Induced Breakdown Spectroscopy (LIBS) to resolve filtration process of Ag liquid sample by chitosan biomembrane is demonstrated. The biomembrane was prepared by inversion method used to filter Ag liquid using pressurized technique samples which were then analyzed by monitoring the emission corresponding to Ag (I) at wavelength of 328 nm. The experiment was conducted by varying the laser energy i.e. 80, 120, and 160 mJ, where, subsequently, and its effect on the depth-profile from 20 - 200 μm was characterized by LIBS. The results showed that the physical processes of pressurized filtration led a homogeneous Ag in the membrane from the surface to a depth of 200 μm. The optimum condition was obtained at laser energy of 120 mJ. The adsorption occurred only on the surface of the membrane i.e. 20 μm depth, but there was no inclusion. Improvement of the detection performance of

adsorption process was done by heating the dripped membrane at 35 oC and was resulting in increase in emission

intensity as expected.

Keywords: Chitosan biomembrane; pressurized filtration; liquid Ag; Laser-Induced Breakdown Spectroscopy



Chitosan is the most abundant natural polymer after cellulose. It is a partially deacetylated product of chitin, which has many useful features such as non-toxic, biocompatibility, biodegradability, and antibacterial property. Due to its features, chitosan has been widely applied in many industries including weastewater treatment. Chitosan has the ability to form complexes with metals. It exhibits higher adsorption capacity for metal ion compared to that of chitin owing to the amino group content. However, the serious drawback of chitosan for metal ion adsorbent from practical utilization is that it is soluble in acidic media [1-2].

Laser induced breakdown spectroscopy (LIBS) or laser induced plasma spectroscopy is a useful method to determine the chemical composition of a wide range of materials including metals, liquids, aerosols, plastics, minerals, biological tissues, etc. [3]. As an analytical technique, LIBS presents some advantages to other techniques: no sample preparation, real time analysis, contactless analysis, apparatus or experimental simplicity, inexpensiveness, robustness, and quickness are interesting properties which makes LIBS an attractive analytical technique. In many cases is a non destructive technique [1]. In this technique

one requires a pulsed laser for generating micro-plasma on the target surface and elemental analysis is accomplished by studying the emission of the plasma plume. The performance of LIBS depends on several parameters including laser wavelength, pulse energy, pulse duration, time interval of observation, and geometrical configuration of collecting optics, target features, and properties of ambient medium. Extensive work has been devoted to optimize these parameters for the best experimental and commercial realization of this technique.

The main disadvantage of LIBS is the high limit of detection, about 500 ppm but 1ppm can be reached for some elements [4].

LIBS is a very versatile technique and have been used in siderurgy, industrial process control [4-7], environmental geochemistry, biohazard material detection, forensic science, microbiology, odontology, archaeology, cultural heritage and art conservation [8-12].

Several papers dealing with LIBS applications in depth-resolved analysis have also reported [5, 9-13]. In their reports, the laser was focused to a different extent resulting in high irradiances (typically in the order of 109 - 1011 Wcm-2).


(LIBS) to sample by technique. varying la 200 μm d process of carried ou Sample-1; by heating Sample-4;


The m characteris solubility sodium hy grade and

b. Prep

The ch by dissolv 1% acetic for 8 hou solution. T plate and d membrane 1% sodiu uncharged 3 times hydroxide membrane

In this been treat control (w ppm dropp naturally ( ppm dropp (adsorption membrane ppm (ads membrane filtration (adsorption

o resolve filtr y chitosan bio Depth profile ser energy from depth. Various f Ag solution ut i.e. control (w

natural adsorp g as Sample-3

and adsorption


a. Ma

materials used a stics i.e. 87,9

in acetic acid ydroxide p.a. A were used with

paration of C

hitosan solution ving 10 g of chi acid solution urs at room te The dope soluti dried at room t e was in the NH um hydroxide d amino form, w

to eliminate , then dried e was around 2

c. Membr

study, the chi ted in 5 diffe without treatm

ped on the me (natural adsorp ped on the mem

n by heatin e to 35°C the sorption after e exposed to A

method with n with pressure

ration process omembrane us e analysis wa m 80 to 160 m s methods of in the membr without treatm ption as Samp 3; adsorption a

n with pressure



are Chitosan p % deacetylate

is 99,4%; ace All reagents we hout further pu

Chitosan M

n of 4% (w/v) w itosan powder n. The mixture emperature to ion was poured temperature for H3+ form. It w

e solution to washed with di the excess d.The thickne

36 μm.

ane Treatm

itosan biomem erent ways i.e ment), Sample-embrane and a ption), Sample mbrane and he ng), Sample-4 n dropped wi heating), and Ag 1000 ppm

h pressure e).

s of Ag liqui sing pressurize s conducted b mJ each for 20 t f the adsorptio ranes were als ment) is called a ple-2; adsorptio after heating a e as Sample-5.


powder with ed and their etic acid and ere analytical urification.


was prepared in 250 ml of e was stirred obtain dope d into a glass r 6 days. The was dipped in o reach the

istilled water of sodium ess of the


mbranes have e. Sample-1: to prob treated the sur uses N there i


pressur scanned 329 nm

d. Laser-In


ser induced br be the present d chitosan biom

rface. The LIB Nd-YAG Lase width), 200 m spectrometer w spectrum 200-tion of 0,1 n

nt linier silicon

pixels. The ou


onitor. the present stu es of each sca essary scan). T

yed in the exp he pulse to pul rements perfor laced approxim and a relativel

n the LIBS m entative avera ion spectra w f successive la zed.


gure 1 shows L pressurized t ple-5) scanned w

327 - 329 nm. nm in Sample

on line of Ag ntrol membran s Ag in the Sam

RE 1. LIBS sp rized treated ch d with laser ene m.

nduced Brea

troscopy (


reakdown spec of Ag elemen membrane at v BS 2500-7 plus

er (1064 nm mJ (max. energ

with specificat -980 nm, with nm using 7 de

n CCD arrays

utput of the spe

ICOR software

udy, the delay t an, and 0 pulse The laser energ periments was

lse energy vari rmed, was no > mately 2 cm in ly wide spot (a measurement in age of the ma ere recorded aser pulses and


LIBS spectra of treated chito with laser ener It shows a pe e-5 which is

(I), whereas n ne (Sample-1) mple-5 that adm

pectra of contro hitosan biomem ergy of 120 mJ




ctroscopy was nt in the pressu various depths s model was us (wavelength), gy)) and echell

ions such as, 7 channels, FW etectors with

s that given to ectrometer ana es that displey

time used was e cleaning (to gy density (flu in the range 60 ation througho > ± 5%. The sa n front of the approx. 1 mm n order to obt aterial compos separately for d were subsequ


f control (Samp osan biomem

rgy of 120 mJ ak at waveleng

known as at no peak observ . This explain mitted by press

ol (Sample-1) a mbrane

(Sample-in the range 327

used urized from alyzed yed on sition.

each uently



biomembra laser energi spectrum is for the com

Figure chitosan b 329 nm fo 160 mJ. C of 120 mJ that the increasing of electron excited he The spectr signal as l continuum these resu analyzed optimal co

Figure Ag (I) at (with laser of depth fr biomembr emission w Ag has be the higher This mea increase, t process tak

For fu deviation measuring adjacent a standard d 2% for las mJ.

2. LIBS spectra

ane (Sample-5) i ies 80, 120, and s presented (kep mparison.

2 shows LIB biomembrane ( or varies of lase Control (Sampl J was also kept intensity of A g laser energy.

ns from the ato ence more em rum also shows laser energy in m emission of

ults, further ex on laser energ ondition for the

3 shows the in wavelength o r energies 80, 1 from the surfac rane (Sample-5 was observed een evenly dist r laser energy ans that the i the peak becom

ke place. urther examina

of the LIBS g the intensity

areas on the deviation in th ser energy 80 a

a of the pressur in the range 327 d 160 mJ. Contr pt at laser energ

BS spectra of (Sample-5) in er energies 80 m le-1) spectrum t for the comp Ag (I) peak This describe oms and more mission of spec s increasing in ncreases, whic the plasma fo xperiments we gy of 120 mJ e chitosan biom ntensity of atom of 328 nm obt

120, and 160 m ce, of the press 5). The graph for all depths tributed within y, 160 mJ sho intensity of t mes broad and

ation of Fig. intensity was from three ide sample surfac he intensities o and 120 mJ, an

rized chitosan 7 - 329 nm for rol (Sample-1) gy of 120 mJ)

the pressurize the range 327 mJ, 120 mJ, an m at laser energ arison. It show increases wit es more numbe

ions have bee ctrum obtaine

the backgroun ch is due to th orm [14]. From ere focused an

J and stated a membrane.

mic emission o tained by LIB mJ) as a functio surized chitosa shows that th s indicating th n the sample. A

ows fluctuation the backgroun d self adsorptio

3, the standar s calculated b entical series o ce. The overa of Ag (I) was for the

To after h before the las Ag (I) other a


RE 3. Intensity ngth of 328 nm 0, and 160 mJ as pressurized chit

study about th an biomembr

ent are introdu natural (Samp μm) by laser e obtained was second shot) ion process oc mance of t ption by heati d membrane w ated to 35°C

sed to ~ 8.75 a nfluenced by t d shot was also heating method

dripping it ple-4), gave int

ity of Sampl d) was the high ese results des rane properly w ure method).

cally and phy ces strong cova providing a s ser shot and pr at wavelength adsorption met

0 20 40 60 8

y of atomic em obtained by LIB s a variation of d tosan biomembra

he adsorption p rane, four m uced. The resul ple-2) after first energy of 120

~ 6.67 a.u, wh was null, i ccurred. To im the adsorptio ing method w with the same p (Sample-3) an a.u. This indica the temperatur o zero. Further d was used. He with 1000 tensity as low le-5 (adsorpti hest at ~ 21.5 a scribe Ag liqui when pressuriz This causes ysically with t alent bonds in t strong rebound roduced plasma h of 328 nm is h


80 100 120 140 16

Depth (µm) Samp



mission of Ag BS with laser en depth from the s ane (Sample-5).

process of Ag methods mem lts are shown in

t shot (shot-1, mJ, the intens hile at a depth indicating tha mprove the dete on processes was introduced

process of Sam nd the intensi ates that the pr re. Result from rmore an adsor

ating the mem ppm Ag sol w as, ~ 5.5 a.u

ion with pre a.u.

id penetrate int zed (adsorption Ag interact the membrane the membrane d momentum d a emission inte high compared

0 180 200 220 ple-5, 80mJ

ple-5, 120mJ

ple-5, 160mJ

(I) at nergies


in the mbrane n Fig. depth ity of of 40 at no ection

, an d, the mple-2

ity is rocess m the rption mbrane lution u. The essure

to the n with both e and



328 nm for

The ad biomembr ions which with N in only a pai bond is ca ion is an donor. Th sufficiently relatively results of carried ou relatively (Sample-2 produced caused a membrane N that acte a low inten

The p

breakdown of Ag ele biomembr was analy (waveleng process re the membr laser ener process oc without in treatment a

0 various membra

dsorption proce rane can be de h were chemica [Ag (NH3)2]+

ir of electrons lled a coordina electron acce herefore, the fo

y strong when low emission f this adsorpt

ut by heatin higher emis 2). The adsor low emission damage to th e and eliminati

ed as Ag adsor nsity.


present study n spectroscopy ement in the rane at various yzed by monit gth of 328 nm esulted in a hom

rane up to a de rgy was 120 m ccurred only at nclusion. Impro

at 35qC.


Sample-3;shot-1Sample-4;shot-1Sa 5;s

mission of Ag (I) ane treatments.

esses occurred escribed as fo ally adsorbed t as a covalent b s shared by at ation covalent b eptor, while N

ormed adsorpt the laser shot

(Sample-2). T tion, the rein ng (Sample-3) sions than w rption after h ns. In this cas he physical s ing or reducing

rption media, t


demonstrated y (LIBS) to pr pressurized t s depths from toring the em m). The pressu

mogenously d epth of 200 μm mJ. The chem t the surface o ovements can b


Sample-2;shot-2Sample-3;shot-2Sa 4;s

) at wavelength

d in the chitosa llows. The Ag through bondin bond resulted i toms N. Such

bond. Here, Ag N is an electro ion layer is no

and hence gav To enhance th nforcement wa ) and produc without heatin heating metho se, heating ha structure of th g the number o thus resulting i

laser induce robe the presen treated chitosa m the surface. mission of Ag

urized filtratio istributed Ag i m. The optimum mical adsorptio

f the membran be done by he



e authors w matics and rsity for the LI


R. Popuri, Y. V

ioresour. Techno

. Zieliska, A. Adsorption of ca inetics and equ

hemistry and App olume XV, edite olish Chitin Soci . Ahmed and M.

ioanal Chem385

Maravelaki-Kal . Zafiropulos,


. Ahmed and M

8, No. 8, August, .C. Garcia, J. M

aserna, Spectroch

W.-B. Lee, J. Wu

pectrosc. Rev39, St-OngeU and 99-308 (2000).

St-OngeU a reakdown Spe haracterization”, ational Institute, M. R. Leahy-Ho urnett, Y. Dikm

ensors10, 4342-M. Vadillo, C aserna, J. Anal. A

J. Radziemski

lasma and Appl



wish to thank Natural S IBS facility.


Vijaya, V. M. B

ol100, 194-199 G. Chostenko admium ions on uilibrium studi

plication of Chit

ed by M. M. Ja iety, 2010, pp. 73 . A. Baig, J. App

A. Brysch, M. K

Sturm, Spectroc

oehne, R. Noll

5, 225–233 (200

laitzaki, D. Angl

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M. A. Baig, IEEE

, 2052-2055 (20 M. Vadillo, S. Pal

him. Acta B56, u, Y. –I. Lee and

, No. 1, 27-97 (2

M. Sabsabi, Spe

and M. Sabsa ectroscopy Stu , Ph.D. Thes

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At. Spectrom13, and D. A Cre

lications, New Y


k the Facult ciences, Uda


Boddu and K. A (2009).

and S. Truszko chitosan memb

es” in Progre

tin and Its Deriv

aworska et. al., 3-78.

pl. Phys106, 03

Kraushaar, I. M

him. Acta B 56

and V. Sturm, 6).

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EE. Trans. Plasm


lanco, J. Ruiz an , 923-931 (2001) d J. Sneddon, J.


ectrochim. Acta

abi, “Laser In udies for M sis, Homi B

iotta, R. Osiand nis and J. B. S

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emers, Laser In

York: Marcel D

ty of ayana


owski, branes:

ess on vatives


nduced aterial Bhabha

der, J. Spicer,

d J. J. 8).



FIGURE 2biomembralaser energispectrum isfor the com2. LIBS spectraane (Sample-5) iies 80, 120, ands presented (kepmparison
FIGURE 4328 nm for 4. Intensity of emvarious membramission of Ag (I)ane treatments. ) at wavelength of


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