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KARAKTERISASI

POLIMER
First : Uji Pemerian
Use your senses (take pictures to document)
What color? Does it fluoresce
Transparent or opaque?
Homogeneous in appearance?
Solid or liquid
Tacky or sticky or brittle or tough
Mass compare with theoretical yield
Describe the material below
Describe the material below
Second : Uji kelarutan
Water, ethanol, benzene, methylene chloride,
tetrahydrofuran, acetonitrile, hexane,
acetone, diethyl ether, dimethyl sulfoxide, N-
methyl pyrrolidone (NMP)
Leave it at room temp overnight. Look for
swelling if not dissolved.
Boil solvent for 4 hours.
If it doesnt dissolve its probably cross-linked
or really crystalline
Types of Polymers & solubility

Will dissolve Wont dissolve


KARAKTERISASI POLIMER
Solid Content
Particle Size Analyzer (Light Scattering)
Gel Permeation Chromatography
Differential Scanning Calorimetry
Thermogravimetry Analysis
Electron Microscope
Lain-lain
Solid Content
Menentukan banyaknya polimer yang
terbentuk pada polimerisasi dispersi.
Merupakan persen rasio antara material
kering (polimer, stabilizer, inisiator) dengan
massa total sampel.
Solid Content

www.protec-de.com
Particle Size Analyzer (Light
Scattering)
Menentukan ukuran/distribusi Persamaan Stokes-Einstein:
ukuran partikel polimer
kT
D
3d
D = koefisien difusi
k = konstanta Boltzmann
T = temperatur
= viskositas
d = diameter hidrodinamik
www.malvern.com
Particle Size Analyzer (Light
Scattering)

www.polymer.uni-karlsruhe.de

www.medsci.org
Gel Permeation
Chromatography
Menentukan berat/distribusi berat molekul dari polimer.

www.whale.wheelock.edu
Gel Permeation
Chromatography

www.nanoscience.ucf.edu
Thermal characterization of
polymers
Thermal gravimetric analyses (TGA)
determines decomposition temperature

Differential scanning calorimetry (DSC)


detects phase changes (melting or glass
transition temperatures) or chemical
reactions
Differential Scanning
Calorimetry
Menentukan transisi
termal dari polimer.

www.industrysearch.com.au
DSC analysis
DSC analysis
DSC Thermogram

Oxidation
Heat Flow -> exothermic

Crystallisation Cross-Linking
(Cure)

Glass
Transition

Melting

Temperature
Thermogravimetry Analysis
Menentukan kestabilan
termal dan analisa
komposisi dari polimer.
Didasarkan massa
yang hilang selama
suhu dinaikkan.
Thermogravimetry Analysis
Thermal Degradation of Polyhydroxylated
Nylon 6,6
15.0k

0 TG
o
100 C -6.3%
o
150 C -6.9%
-20 o
W eight Loss (TG), %

200 C -19.0% 10.0k


o
235 C -50.0%

DTG
-40
o
205 C
o
-60 425 C 5.0k

-80
DTG
0.0
-100

0 100 200 300 400 500 600


o
Temperature, C
Thermal gravimetric analysis
Morphological Characterization
of polymers
If opaque or transluscent, SEM and optical
microscopy (bifringence)-crystalline or
amorphous & more.
Fracture polymer and look at fracture
surfaces
Look for phase separation (like immiscible
block copolymers)
Look for long range order
Look for pores
Electron Microscope
Melihat morfologi dari
partikel polimer dan
menentukan
ukuran/distribusi ukuran
partikel polimer

TEM
Electron Microscope

www.botany.unimelb.edu.au

SEM
Electron Microscope (TEM)

www.remf.dartmouth.edu
Electron Microscope (SEM)
Lain-lain
Infrared spektrometri
Menentukan struktur ikatan polimer.
Lain-lain
Gas Chromatography
Menentukan konversi
monomer dan
monomer sisa dari hasil
polimer.
Lain-lain
NMR
Menentukan struktur kimia dari polimer dan
mengetahui adanya monomer sisa.
Lain-lain
1H NMR PMMA:
NMR
Lain-lain
X-ray diffraction (XRD)
Menentukan susunan ruang semua atom
Menentukan polimer kristalin atau amorf.
amorphous
materials
shows diffuse
band

Semi-crystalline
polymer shows
diffraction rings
Lain-lain
Pola difraksi XRD
Lain-lain
Lain-lain
XRD : analisis tipe kristal
Not every polymer needs all of these
analyses, but structure is the most basic
and important

Known (described in literature) polymers


need less structural characterization. Often
just IR and Mw from GPC.

New polymers need complete structural


characterization: NMR, IR, Combustion
analysis, GPC, solubility, glass transition
temp and/or melting point.
Morphological and Mechanical studies are
dependent on research interests.

If you are interested in strong polymers,


then morphological, mechanical & thermal
studies are important
Other applications requiring
morphological, mechanical & thermal
studies would include preparation and
testing of 1) membranes, 2) coatings, 3)
paint, 4) polymer foams, 5) organic
photovoltaics, 6) OLEDs, 7) adhesives and
8) low friction coatings
Other polymer properties that are
important for specialty polymers

Coatings, packaging, membranes, Photovoltaics


& OLEDs; gas and water permeability should be
measured.
Battery and fuel cell membranes: gas & water
permeability and ion conductivity
Dielectrics, wiring insulation: dielectric and
electrical conductivity
Fabrics & building materials: fire resistance
Any polymer used in sunlight or radiation or in
the presence of chemicals: resistance to oxidative
degradation.

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