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Foundation GPC Training Course

Theory
Nomenclature

Gel Permeation Chromatography GPC

Size Exclusion Chromatography SEC

Gel Filtration Chromatography GFC


Types of Liquid Chromatography
Interactive adsorption, partition, ion exchange, etc

Non-interactive GPC, SEC, GFC


Why do GPC ?

GPC is the only technique for MWD determined by GPC


characterising polymer molecular
weight distribution
As Mw/Mn decreases the strength
and toughness of the polymer
increases
However as Mw/Mn decreases the
polymer becomes more difficult to
process
GPC provides key information to
predict the processability and material
properties of a polymer
Size Exclusion Mechanism
GPC Separation Mechanism

Polymer is prepared as a dilute solution in the


eluent and injected into the system
The GPC column is packed with porous
beads of controlled porosity and particle size
Large molecules are not able to permeate all
of the pores and have a shorter residence
time in the column
Small molecules permeate deep into the
porous matrix and have a long residence time
in the column
Polymer molecules are separated according
to molecular size, eluting largest first,
smallest last
GPC Column Technology

Columns are packed with porous particles, controlled pore


size and particle size
Columns are produced by slurry packing technique, packed
at pressures in excess of 2000psi
Column dimensions typically 7-8mm i.d., 250-600mm in
length
Synthesis of Porous Particles
High cross-link content
gives a rigid, low swelling
product with a well-
defined pore structure
SEM Images of Porous Particle of PLgel
10m Media
Elution Profile of Different Molecular Sizes
Elution Profile Nomenclature

Exclusion volume (Vo) - Upper MW limit


(also known as void volume)

Total permeation volume (Vt) Lower MW limit

Pore volume (Vp) Working resolving range of MW

Vp = Vt - Vo
PLgel Individual Pore Size Column
Calibration Curves
PLgel MIXED Column Calibration Curves
Plate Counts
A measure of the efficiency of
a chromatographic system is the
plate count
Column is divided into a
number of theoretical plates
Plates are defined as the
smallest cross-sectional slice in
which the mobile and stationary
phases are in equilibrium
The smaller the width (known
as height) of the plate, the
quicker the system comes to
equilibrium and the greater the
efficiency
Plate counts controlled by the
Van Deemter relationship
Determination of Column Performance
tR = retention time
W = peak width at 50% peak
height
W5s = peak width at 4.4% peak
height
L = column length in meters

Efficiency ( height)
N=5.54(tR/W)2
L

Plate count efficiency (5s)


N=25(tR/W5s)2
L

Symmetry =W1/W2
Resolution in GPC
Resolution Rs = 2(V1-V2)
(W1+W2)

Specific Resolution per Molecular


Weight Decade

Rsp = 0.25
sD

Elution Volumes of peaks 1 and 2


are V1 and V2

Peak Widths of peaks 1 and 2 are


W1 and W2

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