NED – PAF Collaboration

Assoc. Prof. Dr. Saud Hashmi (Chairman)

Asst. Prof. Dr. Rafiq Ahmed
Lect. Engr. Asra Nafees
Dept. Polymer & Petrochemical Engineering
NED University of Engineering & Technology

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Why Reverse Engineering?

 To replace parts that are obsolete and no longer available

from the original manufacturer or are worn and broken.
 High cost, notably proprietary item, is another factor

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Rubber Compounding Ingredients

Homo(or co-) Polymer(s):

Fillers
Protective Agents
Vulcanizing Chemicals
Activators
Accelerators
Retarders
Antidegradants …………………………

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Principal Chemical and Analytical Methods

A. Major Characterization:
1. Infrared Spectroscopy (FTIR) (PPD)
2. Thermal Analysis (e.g. TGA & DSC) (PPD)
3. Pyrolysis- GCMS Analysis
4. Atomic Force Microscopy (AFM) Analysis
5. Soxhlet Extraction (PPD)
6. Crosslink Density (ASTM D 471-97(1998)) and Distribution
7. Dispersion Test (ASTM D7723 and ISO 11345) and Scanning
Electron Microscopy (SEM)
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Principal Chemical and Analytical Methods

8. X-ray Diffraction (XRD) (Materials Engg., NED)

9. X-ray Fluorescence (XRF)
10. Nuclear Magnetic Resonance (NMR)
11. Optical Microscopy (Materials Engg., NED)

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Principal Chemical and Analytical Methods

A. Major Characterization:
1. Infrared Spectroscopy (FTIR): Reveals a spectrum in which
every peak represents a particular chemical compound
• Tricky for multivariable compounds

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FTIR: Example

Chemical structure of an EPDM molecule

FTIR scan of an EPDM compound

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Comparative Analysis using FTIR

The graph above was produced by FTIR scans on two EPDM compounds. We
can tell by the graph that they are both EPDM material but they are not the
same compound as shown by the two peaks present at wavenumber 1539
cm-1 and 1397 cm-1 in Sample 2 that are not in sample 1.
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Principal Chemical and Analytical Methods

2. Thermal Analysis (e.g. Thermal Gravimetric Analysis)

Sample specimen is subjected to a controlled temperature
program in a controlled atmosphere
• To determine the level of content of polymer or additives, or,
look for changes in constituents after use in service
• Thermal stability of samples
• Decomposition kinetics
• Etc. A smart design of experiment can
reveal desired informations

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TGA: Example of rubber samples

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Principal Chemical and Analytical Methods

3. Pyrolysis- GCMS analysis

Pyrolysis combined with Gas Chromatography (GC) and Mass
Spectroscopy (MS) is an ideal approach to analyze rubber
samples.
• Pyrolysis volatiles the rubber components, which are then
separated by GC. The use of Mass Spectroscopy enables the
Pyrolysis products to be positively identified.

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Principal Chemical and Analytical Methods

3. Pyrolysis- GCMS analysis of rubber – cont’d

• Furthermore, GCMS analysis itself can be used to identify any
extractable components of a rubber material. It can be used i.e.
to determine with what kind of media the rubber has been in
contact with or what is the composition of the materials which
have migrated out of the rubber.

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Principal Chemical and Analytical Methods

4. Atomic Force Microscopy (AFM) analysis:

Atomic Force Microscopy can be used to determine the surface
roughness of rubber materials and i.e. to get insight in the
dispersion of fillers or to find out whether the rubber product
contains a polymer blend.

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Principal Chemical and Analytical Methods

5. Soxhlet extraction
• The content of extractable matter (low volatile materials) can
be determined by means of Soxhlet extractions.
• Rubber samples may be extracted by different solvents
during different times at different temperatures to know how
much content migrates or can be extracted out of the rubber
products.

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Principal Chemical and Analytical Methods

6. Crosslink density and distribution

The crosslink density and distribution analysis is a combination
of chemical probe reactions and Flory-Rehner equilibrium
swelling experiments. 
• This analysis shows the total crosslink density, but more
specifically the mono, di and polysulphidic distribution.

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Principal Chemical and Analytical Methods

7. Dispersion Test (ASTM D7723 and ISO 11345) and Scanning

Electron Microscopy
Fillers dispersion, size (30-50 ◦A) and shape e.g. Carbon black
dispersion
8. X-ray Diffraction:
• Filler type and quantitative measurement
• Particle size (nanometer) Etc.
9. X-ray Fluorescence (XRF)
• Elemental analysis of rubber samples (e.g. Zn, Mg, Cl2 etc.)
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Principal Chemical and Analytical Methods

10. Nuclear Magnetic Resonance (NMR)

• Determining the crosslink-density or the aged state of
elastomers
• Rubber-carbon black interactions
• Homogeneity of rubber compounds
• Etc.
11. Optical Microscopy:
• Dispersion and size (0.1 – 0.2 μm)of particles

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Mechanical Testing (Supporting Tests)

B. Supporting Test:
1. Density (ASTM D1817 - 05(2016))
2. Tensile Properties (ASTM D-412) (PPD)
3. Tear Resistance (ASTM D-624) (PPD)
4. Air Over Aging (ASTM D-573) (PPD)
5. Heat Buildup (ASTM D-623)
6. Fluid Immersion Properties (ASTM D-471) (PPD)
7. Compression Set (ASTM D-395) (PPD)
8. Durometer Hardness (ASTM D-2240) (PPD)
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Principal Chemical and Analytical Methods

9. Abrasion Resistance (ASTM D-2228)

10. Low Temperature Properties (ASTM D-1053)
11. Ozone Resistance (ASTM D-1171)
12. Stress Relaxation (Life time prediction) (ASTM D6048 -
07(2018)) (PPD)

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 Thank You!

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