Characterization Lab

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Polymer Analysis and Characterization
20 MTEN 7032C
Semester: Spring, 2014-15
LEVEL: Dual (Required Graduate; Undergraduate Elective)

Wednesday 2:00-5:00 TBD

Occasionally Tuesday and Thursday Baldwin 648 2-3


  1. Courses typically taught in Materials Engineering at the undergraduate level as follow.
  2. A Course similar to Introduction to Polymers
  3. A background in rheology and fluid dynamics
  4. An introductory course in mechanical properties of materials and failure analysis
  5. Background in x-ray diffraction.
  6. Some understanding of the morphology of polymers.
  7. The ability to write a simple computer program.
Prof. Gregory Beaucage
492 Rhodes/551 ERC and 410 Rhodes (Labs)
Teaching Assistant:
Lucas (Yuan Zhao

First Last Lab Group Day Time Reverse Engineering Topic
Jehan Kothari A Wednesday 2:00 Unknown
Robert Kramer        
Kunal Kumar        
Adam Meador        
Vi Phan        
Devesh Shreeram        



Week 1 Week 2 Week 3 Week 4 Week 5 Week 6 Week 7 Week 8 Week 9 Week 10 Week 11 Week 12 Week 13 Week 14 Week 15
Finals Week
Aug. 22

Aug. 29

Sept. 6

Sept. 19

Oct 24

Sept. 12

Sept. 26

Oct. 3

Oct. 10

Oct. 17 Oct. 31 Nov. 7 Nov. 14 Nov. 21
Nov. 28
Dec. 5


Tues Thursday Baldwin 648

Lab 1 Lab 2 Lab 4 Lab 9 Lab 3 Lab 5

Lab 6


Lab 7 Lab 8
Lab 10
Lab 11
Lab 12

Lab 13

Ayers Lab Rievschl 704

Lab 14

Computer ProgramERC 435 (Nov 28) ERC 405 (Nov 30)

12 to 2 pm ERC 435
Lab Notebook,

Report Format,

Error Analysis,

Significant Figures,

Reverse Engineering

Overview of
Polymer Analysis

Notes on Lab Reports 2013
Notes Lab 1A
Notes Lab 1B
Notes Lab 2
Notes Lab 3

Notes Viscometer Lab 1 2014 Spring
Rheology Instron GPC/IV


Rheometer           Computer Program          
Baldwin 660
Rieveschl Hall
Rhodes 505
 Due Friday at
 5 PM in
Rhodes 410

Crosley Tower First Floor

Dr. Keyang Ding 

Rhodes 410B
Char. Center
Rievschl 704 Ayres Lab 
ERC 435 (Nov 28) ERC 405 (Nov 30) 

Reverse Engineering Group Report

Presentation 12-2
ERC 435


15 students are registered for Polymer Characterization. The class will be divided into 3 groups of  5 students. Groups will meet on Monday, Wednesday, or Friday at 2:30 (see table above) to be instructed on each lab. The 3 credits of lab for this course convert to 9 hours of lab time which the students can complete at any time that access to the instruments is available. A take home quiz on the lab write-up and supporting documentation will be required at the start of each lab.

The numbers in the table above correspond to the lab number given below. Students are expected to be familiar with the lab prior to the specified instruction period.

Parts: (html)
Background Class on Analysis.html

Computer Program Problem.html
Free Mac Software that may be useful for Computer Program Project
(A free PC version called Scion Image for Windows, is available from Scion Corporation
Password Name="computer" password="yoyo".)

Parts of a Marco in Scion that may be of some use
(Keep in mind that there are many ways to work this program. e.g. you could use scions graphic interface commands to pick circular pieces.)

Reverse Engineering Project.html



Lab html file Background Notes: Sample Data:
Lab 1

Jan. 21

Melt Viscosity

(Complete prior to lab)

Polymer Melt Rheology/Viscometric Flow.html
Melt Viscosity Option A (OLD).html
Temperature Dependence of Viscosity (Wiki)

Text for Lab:
(Change first "Middleman" in link to "Mm")
Middleman Chapter 5: Viscometric Flows

Middleman Chapter 3: Introduction to Polymer Flow

Viscometer Manual (Buchanan)

Toledo Lecture Notes on Viscosity

Vainessa Ng Plots for PDMS

Group A 2016; Group B
Group A 2014; Group B 2014; Group C 2014; Concentration Data; Viscosity vs MW Plot

Group A 2013; Group B 2013

Data 2005 Winter

Collected Fall '01
Excel MW in g/mole and viscosity in cp for PDMS
WLF Parameters for PDMS

2001 Eric, Ayush, Tingtai Data
Group 5 (Jim Chen et al) 2000
PDMS Reaction Data
Viscosity Versus Shear Rate and Temperature for Final PDMS Reaction
Viscometer Data 2000

Lab 2

Jan. 28

Tensile / Impact

Quiz (Complete prior to lab)

Polymer Stress Strain Notes
Morphology of Polymer Deformation
Mechanics of Materials

Instron 4465 Manual
Instron 4400 Manual (1 of 2)
Instron 4400 Manual (2 of 2)

Roland NRL Viscoelastic Behavior of Rubbery Materials
(Mooney Rivin and Gent Equation)

Paper on MR plot
Jim Mark Polymer Encylopedia MR Plot
Herve Marand Rubber Elasticity Talk

Typical Values of Young's Modulus for PS, PE, PP, Rubber
Chi and Rubber Elasticity Polyurethane Rubber

Instron Data 2016 Swollen Rubber

Instron Data Group B/A 2014; Group C/A 2014
Zip of Instron Data 201

Data Winter; Picture of Samples

Fall 2001 Data
Group 1, Group 2, Group 4, Group 6,
Impact Test
Older Data
1999 Instron Data and Several Groups from 2000 Data

Lab 3

Feb. 4

Rieveschl Hall)

GPC/Intrinsic Viscosity.html
(Please bring a stopwatch to lab)

Quiz (Complete prior to lab)

Intrinsic Viscosity and MW distribuitons.html
Physics of Coil: dilute.html
Physics of Coil: semi-dilute.html

GPC With Light Scattering Training Manual (79 Mb)

Watt Hardware and Software Manual and Intro Slide

Bridge Viscometer Paper

Data 2015 ; Multimodal PMMA on DMF GPC

Data 2015; Multimodal Sample 2015

Group A 2014: PolyLactose .txt; .afe6; .xml; .docx; .jpg1; .jpg2; .jpg3; .jpg4; .csv (excel)
Group B 2014: PolyUrethane .pdf; .afe6; .xml; .csv (excel); .jpg1
Group C 2014: Polystyrene .afe6; .xml; .docx; .csv (excel)
Pictures of Lab: .jpg5; .jpg6; .jpg7; .jpg8; .jpg9
The instrument gives an error for some values. You need to explain the origin of these values and your reason to use them.
"Taylor, Leeanne (tayloln)" <>

GPC Data Group A 2013
GPC Data Group B 2013

Data Winter 05

GPC Curves for PE.xls
Intrinsic Viscosity F01 (Check for updates to file)
Groups 6 and 3 (2000) Data
38C and 25C PS/Toluene

Lab 4

Feb. 11


Quiz (Complete prior to lab)

EM Radiation.html
FTIR Tutorial and quiz
Raman Tutorial
Raman Tutorial B
Raman Review.html

Polybutadiene IR/Raman.pdf
Nylon IR/Raman.pdf
Nylon IR/Raman.jpg

IR Absorption Frequencies
ATR Lecture
Sample Prep for FTIR
MIRacle PDS 2013

Raman Spectrum of Graphene

2014 Group A IR; Group A Raman
2014 Group B IR; Group C IR; Group B Raman
Pictures: 23.jpg; 24.jpg; 25.jpg; 26.jpg; 27.jpg

2013 Group A IR; Group A Raman
2013 Group B IR; Group B Raman

W05 IR Data Group A, Group B, Group C

F01 Combined IR Data

IR Data Group 3.xls

Proton NMR patterns from Elwood Brooks 10/23/01 Demonstration for Class

Polymethylacrylate (missing "Meth" but close...)
Some IR data in Excel Spreadsheet

Lab 5

Feb. 18


Quiz (Complete prior to lab)

Thermal Analysis.html
Semicrystalline Morphology.html
DSC Southern Misissippi
Modulated DSC TA Instruments.pdf
Modulated DSC Summary.pdf

PET Crystallization Paper.pdf, HoffmanWeeksNumbersFromPaper
Artifacts in DSC.pdf
TA DSC and PET Modulated DSC.pdf
TA Modulated DSC and PET.pdf

TGA for Tires TGA A.pdf , TGA B.pdf

TGA for BioCharTalk; Paper on Bamboo TGA

2016 Data
2015 Data
2014 Data Group A; Group B; Group AB; Group C and Combined Plots

Group A 2013
Group B 2013 File 1 File 2, File 3

W05 DSC Data PET and PP

TGA Scans F01 (Check for Updates)
DSC Scans F01 (Please check for updates)
Isothermal Crystallization Analysis
DSC Trace for PET

Lab 6

Feb. 25


Quiz (Complete prior to lab)

d-spacing to a,b,c,alpha,beta,gamma

Common Polymer XRD Peaks

Polymer XRD.html

X-ray Diffraction Class (Undergraduate/Cullity)

2 Theta Positions for Polymers

Taiwan PPT.pdf

PC in Solvent Crystallization Kinetics.pdf

PC Crystallization Dissertation VPI had sigma e and DH for Hoffman Lauritzen/Gibbs Thompson Equation

How to Calculate DOC.html

XRD Data 2016 Monday, Wednesday

XRD Data 2014 asc = txt; XRD Data Spring 2014

Radial Average Data for Hermans Orientation Function Calculation.xls

XRD Data

W05 Data (Raw data, xls file)

PET Recrystallization Data
XRD Date F01.xls
XRD Pinhole Photos F01

Groups 1, 2, 4, 5 and 6: 2000 data

Radial and Azimuthal Averages of 2-d PE file for Orientation and DOC

Large 2-d file for computer program
2-d gif for computer program
1-d slice for computer program
Oriented Polyhydroxybutyrate (PHB) Film

Lab 7
March 4
(Computer Program Due Friday 5 pm)
SAXS Lab.html
Quiz SAXS (Complete Prior to Lab)
(Computer Program Project Due this Week Friday at 5 pm)
Ilavsky SAXS software for Igor Pro (Irena)

Semi-crystalline Polymer Morphology

XRD of Semi-Crystalline Polymers

SAXS Notes

Beaucage Review Article

Old Small-Angle Scattering of X-rays.html

RAR Expander Program for Mac

SAXS Data 2009.rar
SAXS Data 2006
2004 Data
2001 Data
q* vs Temp data for Hoffman Analysis
Aerogel 2D
PE isotropic 2D HDPE
Aerogel 2D
All 1-d files are columns of q (1/Angstrom), I (counts), Standard Deviation (counts)
Aerogel 1D
PET (Bad) 1D

Processing Data LDPE
2d SAXS and XRD of Blown LDPE Films

Lab 8

March 11


(NMR Quiz)

EM Radiation.html

Preparation of NMR samples
Spincore Software Downloads

Tacticity Determination of PMMA.pdf
Tacticity of PMMA Talk.pdf

MestReC Program
(beaucage mestrec)

MestReC (8Mb)
1) Open the fid file in mestrec.
2) Do Fourier transform under process option on toolbar.
3) Under Process-Phase Correction-Automatic Phase Correction (Simplex Method).
4) This gives the spectrum ready for analysis from the tools menu. (Pick the peaks before you integrate them.)

Spinworks PC program for NMR
How to run spin works video


NMR Data 2015
Program from Chemistry for NMR

NMR Data.rar (need to download rar expander for the Mac people) Please contact Lucas (Yuan Zhao) <> if there is confusion about the samples.

To open the NMR data you need to download the MestReC Program which takes some time and several e-mails.  When you finally have it loaded you should open the "1r" files to see the data.  This should be in ppm on the x-axis.

Group A 2013; Group B 2013

Spectra From E. Brooks W05: 1, 2, 3, 4, 5, 6 (open with MestReC Lite)

Proton NMR patterns from Elwood Brooks 10/23/01 Demonstration for Class

Polymethylacrylate (missing "Meth" but close...)
NMR data (of Prof. Elwood Brooks, Chemistry) for PMMA
Gif's of NMR scans (of Prof. Elwood Brooks, Chemistry) for Commercial and Aldrich Samples

NMR data (of Prof. Elwood Brooks, Chemistry) for PMMA
Gif's of NMR scans (of Prof. Elwood Brooks, Chemistry) for Commercial and Aldrich Samples

Lab 9

Mar. 25

Optical Microscopy Lab.html

(Quiz Microscopy)

(OLD Lab NOT DONE: Microscopy.html)

Morphology of Complex Materials

EM Radiation (Analysis).html
Morphology Class.html
Semicrystalline Morphology.html
Deformation Morphology.html
Phase Morphology.html



Group A 2013.rar

Group B (no videos)

W05 Data

Group 1 F01 50C; 62C; 69C; 72C

Group 4 F01 60C;65C

Group 6 F01 77C

Groups 1, 3 and 6 (2000) PHB-co-5%-PHV Micrographs 25, 53, 81 Deg C

Lab 10

November 7

DLS Lab.html

DLS Quiz.doc

Prof. Schaefer DLS and DMA Igor Procedures
1) Load the ENTIRE Ilavsky Igor Code Package (takes 10 minutes)
2) Put the Schaefer Macros in the appropriate folders (Place in Igor Procedure and User Procedure folders in Igor Pro Folder)
3) Under Macros, First: "Load UC Macros",
4) Then: Macros: Other Macros: "AVL Light Scattering"
5) Then under: Plot Fits: "ALV DLS Panel"
6) Click Load
7) Then you can plot, fit etc.
You need to set the viscosity yourself

Schaefer code does not load the error for the correlation function, or the raw data I versus time. You need I versus time to get the average static intensity for I vs q plot. This can be obtained by opening the file as a notebook in Igor, finding the two columns of time and intensity, copy and paste into a table then do "wavestats" on the intensity wave to get average and standard deviation.

Igor Program where I have read in some DLS data. You can copy from the history section to read in other data.

Some Russo data in Igor

ALV/CGS3 DLS Instrument

Paul Russo's LSU (Now Georgia Tech) DLS Lab.pdf
Old Russo Lab

Paul Russo's LSU Lab Course
Russo Final Exam (difficult)
Example Data Set for Exam

Russo Insights on Guinier's Law

Dynamic Light Scattering
             HiemenzRajagopalan DLS 

Diffusing Wave Spectroscopy (DWS) Mason, Gang, Weitz 1997
    1993 paper

ZimmPlot.png Strobl
Zimm Equation.pdf

ZimmPlot IAS

Kirkwood 1954 RH calculation

David Boas Dissertation

Group B 2014 Milk, Almond Milk, Cream, SELS/NaCl in Water

Group C 2014 Same Samples at 34 and 45°C also High Concentration SELS/NaCl in Water 21% and Graphene Solution in Water from Kuppa

Russo Data Set mixed Spheres (Exam)
Russo Data Set Milk
Russo Data Set Polymer in Solution

Lab 11
November 7


Prof. Schaefer DLS and DMA Igor Procedures
1) Load the ENTIRE Ilavsky Igor Code Package (takes 10 minutes)
2) Put the Schaefer Macros in the appropriate folders (Place in Igor Procedure and User Procedure folders in Igor Pro Folder)
3) Under Macros, First: "Load UC Macros",
4) Then: Macros: Other Macros: "DMA"
5) Figure out how to use his macros for DMA.

Polymer Dynamics Course

DMA 861 Examples.pdf
Mettler Toledo DMA 861 Video
DMA 861 Manual.pdf
Star Software Manual.pdf

DMA Instrument Comparison
DMA TA Instruments.pdf
Lab on DMA from Iowa State.pdf
TA slides.pdf
More DMA.pdf
VT dissertation chapter.pdf
Cole-Cole Plot and Debye Relaxation.ppt

DMA Data 2014
Unknown (3 point bend), PET (tensile), and Ketchup Bottle(tensile)
Use 2013 data if necessary

Group A 2013 Data; Group B 2013 Data

Lab 12 November 14


(Old Lab SEM Lab.html)


Needle Throwing.pdf
ImageJ Plugin for Correlation Function

AFM Image processing from ETH

Igor Pro Procedures for AFM/SPM:
Web Site Source
Folders to Put in Igor Pro
Data:Load Waves:Load NanoScope Image
There are other procedures you can get by
File:Open File: Procedure go to folder you just put in

AFM/SPM Software List for Download from Mel

NIH Image

AFM Sites
UGuelph Canada
Bristol, UK
Hobbs Site

AFM Polymers.pdf
Polymer AFM Bruker.html
AFM How it works NKU.pdf

SEM Sites
SEM Wikipedia
SEM Video
ESEM UQueensland Australia
Iowa State site
UK site
ESEM Cambridge, UK

EM Radiation (Analysis).html
Morphology Class.html
Semicrystalline Morphology.html
Deformation Morphology.html
Phase Morphology.html

2014 Group A (Various Paper)
Group B
Group C

2013 Group A Photographs and Micrographs
2013 Group B Photographs and Micrographs

TEM Images of pressed polypropylene from Ayush Bafna
Micrographs from the SEM Lab (Zipped File)

Lab 13 November 21
Oscillatory Rheometry Lab

(Quiz Torque Rheometer)

Faith Morrison Lab Notes Lecture 4 2013

Faith Morrison Video of Classes on Rheology (goes with her book)

Discovery HR Hybrid Rheometer (Ayres Lab) video Operating Procedure

Polymer Dynamics Class


Rheology of Gels

Dynamic Viscoelasticity (NIST)

Larson Polymers (add f to end for pdf)

Larson Gels (add f to end for pdf)

Larson Particulate Gels (add f to end for pdf)

Thermal Analysis Data 2016

Software to read .tri files
(Requires windows/779Mb)

Click "TRIOS for Rheology"

Lab 14
Nov 28
Computer Simulation Lab

A) Simulation of Chain Distribution in Branched Polyethylene

B) Simulation of Ising Model

Most Probable Distribution

Dealy & Larson (2006), Soares & Hamielec (1996), Costeux, Wood-Adams & Beigzadeh (2002), and Costeux (2003)    Read and McLeish (2001)  Ramachandran (2005)  Beigzadeh, Soares & Duever (1999)

Description of Ising Model

Lab xx

April xx

X-ray Reflectivity Lab.html
Quiz Reflectivity (Complete Prior to Lab)
Reflectivity Tom Russell.pdf
UC Schaefer Notes 2013.pptx
Northeastern Univ. Power Point.pdf
Colorado State Power Point.pdf
Roger Pynn IU.pdf
Reflectivity SOP How to Run Reflectometer.pdf
Reflectivity Paper
Reflectivity Paper 2

Data Fitting Procedure for Igor (Irena)
Example Igor Experiment with one data set.pxp
(you need to load Irena before you look a this experiment)

Vapor Swelling 1.pdf
Vapor Swelling 2.pdf

2013 Group A Data; Igor Experiment with Data.pxp
2013 Group B data; Igor Experiment with Data.pxp

Lab xx
April xx

"out of time"

Impedance Spectroscopy

Finals Week
Monday December 5
12-2 pm

ERC 435

Reverse Engineering Presentation and Report
Reverse Engineering Group Report Due Friday April 18 5 pm

Files: (Click to Down Load)
.zip file of Text Data for Computer Program
Free Mac Software that may be useful for Computer Program Project
(A free PC version called Scion Image for Window, is available from Scion Corporation
Password Name="computer" password="yoyo".)

Course Requirements:

The focus of this course is analysis and characterization of polymers and plastics. Polymer Characterization is a lab course which is intended as a compliment to a lecture classes in the polymer curriculum such as Polymer Analysis.

Polymer Characterization involves

- a sequence of 13 labs which are performed by groups of 3 to 4 students

- a required computer program written individually

- a reverse engineering project based on a commercial product which is presented as a written report and as a class presentation by each group.

The grade for the class is an equally weighted sum of grades for each of the 13 reports, the 1 computer program, the group presentation and the group write-up for the reverse engineering project. That is, each component of the grade is weighted 1/16.

Students are expected to keep a lab notebook which will make up a portion of the individual grades for the lab reports.

Lab reports are due 6 days after completion of the lab. This means that the first lab done on Wednesday January 21 is due at 5 pm on Monday January 26 in 410 Rhodes at 5 pm. One lab will be due every week until 12 have been completed. Late reports will not be accepted.

The computer program is due at midterm (Friday March 6 at 5pm in 410 Rhodes) no late computer programs will be accepted.

The written report on the reverse engineering project is due the Monday of Finals Week. No late reports will be accepted.  The group presentations for the reverse engineering project will be given during Finals Week.

(Deliver All Reports to 410 Rhodes Lab or Directly to Beaucage)

Final letter grades will be based on class grade using the following scale:
A is between 90.0 and 100.0; B is between 80.0 and 89.9; C is between 70.0 and 79.9; D is between 60.0 and 69.

Grade Sheet

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