Introduction to

Polymer Science and Engineering

Badge A: Polymer Chemistry
Lecture A10-E: Size Exclusion Chromatography Experiment
James M. Caruthers
Gerald and Sarah Skidmore Professor of Chemical Engineering
Purdue University
West Lafayette, IN 47907
caruther@ecn.purdue.edu

February 17, 2015

Size Exclusion Chromatography

Experiment

Experiment Objective:
Determine a calibration curve using a series of polystyrene standards in THF. Then,
determine the number and weight molecular weight of a broad polystyrene sample
(called Polystyrene A in the PolySim interface) using the calibration curve.
Procedure:
1.Measure the GPC curve of a series of polystyrene standards in THF. A good
concentration for the GPC experiment is 5 mg/ml.
2.Determine peak point elution volume of each standard from GPC data.
3.Plot the elution volume vs. log(MW) to obtain the calibration curve.
4.Measure the GPC curve of a broad polystyrene sample.
5.Determine the broad PS samples number and weight average molecular weight.

We will now go the PolySim Virtual Polymer

Laboratory to perform the necessary experiment

Measure MWD using GPC

This is the interface of Light Scattering instrument simulator.

Measure MWD using GPC

1. Choose your sample vial
2. Choose Column set (200 mixed THF in this
demo)
3. Set the temperature (30C in this
demo)
4. Set the flow rate (1ml/min in this demo)

5. Set the injection volume (0.1ml in this demo)

6. Choose detectors (RI only in this demo)

6. Hit Run button to see your result

Measure MWD using GPC

Your result shows at the bottom of the interface.

Hit this button to save your data as csv file

Construct Spread Sheet

Saved csv file will look like this.

Construct Spread Sheet

Plot elution volume vs. RI signal and find the peak point elution volume.
30.4 ml in this case.
*Tip : use max and vlookup function to find the peak point volume.
Ex) vlookup(max(RI signal,RI&V table,V column #, false)

Construct Spread Sheet

1) Record MW and corresponding Peak volume.

2) Plot peak volume vs. log(MW)
3) Add linear fit to obtain the calibration curve.

Measure MWD of broad sample

Repeat first step using Polystyrene A.

Obtain the RI curve of the sample.

Construct Spread Sheet

1) Calculate log(MW) using the calibration curve

we obtained from the previous step.
* log(MW)=-0.25V+11.6
2) Calculate MW from log(MW)

Construct Spread Sheet

Calculate weight fraction from RI data.

RI signal is proportional to the concentration,
where the normalized RI signal is the weight
fraction.

Construct Spread Sheet

Calculate number fraction from weight fraction.

The normalized number fraction is
the weight fraction/MW

Result

Calculate number and weight average molecular weight.

Mn = 5, 410 g/mole
Mw = 8760 g/mole
PDI = 1.62