Analyzing Failure Using Pyrolysis-GC–MS The Column spoke to Peter Kusch of the Bonn-Rhein-Sieg University of Applied Sciences in Rheinbach, Germany, about analyzing failure in the automotive industry. Q: What is the focus of your research at the present time? A: My research at the Department of Applied Natural Sciences at the Bonn-Rhein-Sieg University of Applied Sciences (Rheinbach, Germany) focuses on the application of the analytical pyrolysis-gas chromatography–mass spectrometry (Py-GC–MS) and headspace– solid-phase microextraction-GC–MS (HS-SPME-GC–MS) for characterization of polymeric materials and components from many branches of manufacturing and building industry. Pyrolysis involves thermal fragmentation of the high molecular analytical sample at elevated temperature (500–1400 °C) in the presence of an inert gas (helium). The pyrolysis products are separated by performing GC using a fused-silica capillary column and subsequently identified by interpretation of the obtained mass spectra or by using mass spectral libraries, such as NIST/EPA/NIH, Wiley, MPW, or Norman Mass Bank. 1–3 The HS-SPME-GC–MS technique will be used in our laboratory for determination of residual monomers and other volatile organic compounds (VOCs) and additives (antioxidants, plasticizers) in polymers and copolymers. Q: What are the main objectives of your research group? A: In the first decade of the 21st century there was the EUREKA-project “Boiltreat E! 2426“ in cooperation with the Institute of Heavy Organic Synthesis “Blachownia“ (Kedzierzyn-Kozle, Poland) and other project partners from France, Lithuania, and Romania. The aim of the project was the development and implementation of a new technology for water chemical treatment in the energy industry. Our laboratory was responsible for the GC–MS identification of thermostable long-chain alkyl amines and alkyl Photo Credit: pixhook/Getty Images 17 The Essentials 21 RSC Event Preview 23 Staff 27 CHROMacademy 24 Training & Events 25 Broomell 2 News 9 Incognito 13 Q&A: Kusch 17 9 9 13 3
Transcript
Analyzing Failure Using Pyrolysis-GC–MSThe Column spoke to Peter Kusch of the Bonn-Rhein-Sieg University of Applied Sciences in
Rheinbach, Germany, about analyzing failure in the automotive industry.
Q: What is the focus of your research
at the present time?
A: My research at the Department
of Applied Natural Sciences at the
Bonn-Rhein-Sieg University of Applied
Sciences (Rheinbach, Germany) focuses
on the application of the analytical
pyrolysis-gas chromatography–mass
spectrometry (Py-GC–MS) and headspace–
solid-phase microextraction-GC–MS
(HS-SPME-GC–MS) for characterization
of polymeric materials and components
from many branches of manufacturing
and building industry. Pyrolysis involves
thermal fragmentation of the high
molecular analytical sample at elevated
temperature (500–1400 °C) in the
presence of an inert gas (helium).
The pyrolysis products are separated
by performing GC using a fused-silica
capillary column and subsequently
identi# ed by interpretation of the
obtained mass spectra or by using mass
spectral libraries, such as NIST/EPA/NIH,
Wiley, MPW, or Norman Mass Bank.1–3
The HS-SPME-GC–MS technique
will be used in our laboratory for
determination of residual monomers
and other volatile organic compounds
(VOCs) and additives (antioxidants,
plasticizers) in polymers and
copolymers.
Q: What are the main objectives of
your research group?
A: In the first decade of the 21st
century there was the EUREKA-project
“Boiltreat E! 2426“ in cooperation
with the Institute of Heavy
Organic Synthesis “Blachownia“
(Kedzierzyn-Kozle, Poland) and
other project partners from France,
Lithuania, and Romania. The aim of
the project was the development and
implementation of a new technology
for water chemical treatment in
the energy industry. Our laboratory
was responsible for the GC–MS
identification of thermostable
long-chain alkyl amines and alkyl Ph
oto
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: p
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17 The Essentials21 RSC Event Preview23 Staff27CHROMacademy24 Training & Events25
Broomell2 News9 Incognito13 Q&A: Kusch1799 133
The Column www.chromatographyonline.com
diamines and analysis of boiler water
samples from the power plant by using
the new anti-corrosive and anti-scaling
formulations.4
In recent years, however, the focus has
been on the characterization of polymeric
materials and failure analysis, especially
in the automotive industry. In my work,
besides projects, I am also involved under
the auspices of the German Chemical
Society (Gesellschaft Deutscher Chemiker,
Frankfurt) together with my colleagues
Professor Gerd Knupp and M. Eng.
Johannes Steinhaus in the implementation
of the course “Application of Pyrolysis-Gas
Chromatography/Mass Spectrometry
for Characterization of Plastics“ for
participants from industry, research
institutes, and academia from Germany,
Austria, and Switzerland.
Q: What is “failure analysis” in the
automotive industry?
A: Failure of the structure of materials
or components often results in accidents
and plant shutdowns, resulting in hefty
compensations. Failure analysis is the
process of collecting and analyzing data
to determine the cause of a failure and to
take action to prevent it from happening
again. It is an important discipline in many
branches of the manufacturing industry,
such as the automotive industry. Failure
analyses of automotive materials or
components help to identify root causes
for degradation, malfunction, damage, or
ageing. Various analytical techniques, like
microscopy imaging, scanning electron
microscopy (SEM), energy dispersive x-ray
analysis (EDX), UV–vis spectrometry,
Fourier-transform infrared spectrometry
(FTIR), nuclear magnetic resonance
(NMR), and time-of-flight secondary ion
mass spectrometry (TOF-SIMS) are used
for the clearing of raw material failure,
manufacturing, function, design, or
storage errors of various plastic or
metal components from the automotive
industry.
For more than 10 years, our laboratory
has been involved in failure analysis
projects in the automotive industry using
py-GC–MS. The high success rate for
solving problems and the satisfaction of
our clients have convinced us that this
analytical technique is well suited for
failure analysis in the automotive industry.
The obtained analytical results are then
used for troubleshooting and remedial
action of the technological process. Some
of the results we have obtained have been
presented at international symposia and
published in analytical journals.5–8
Q&A: Kusch
18 The Essentials21 RSC Event Preview23 Staff27CHROMacademy24 Training & Events25
Broomell2 News9 Incognito13 Q&A: Kusch1799 133
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Q: What are the applications of
pyrolysis gas chromatography–mass
spectrometry in failure analysis?
What are the advantages over other
methods?
A: Practical application of these
hyphenated analytical techniques in our
laboratory ranges from: case studies of
automotive components; failure analysis
of failed hydraulic cylinders, membranes,
and packaging of hydraulic cylinders;
sealing rings, tyre materials, and additives;
auto paints, auto wrapping foils, auto
catalysts, mineral oils, and brake fluids
to identification of plastic particles from
industrial filter fins; residues of fittings
of refrigerant compressors; residues from
a valve block of a medical respirator;
identification of dental filling materials;
detection of counterfeits of plastic and
rubber products; modules from building
industry; fouling from a roller bearing;
adhesives; sealing compounds; cesspit
residues from an extruder or polyethylene
re-granulate from mechanical recycling
process; or polymer residues in recycled
aluminum.
Py-GC–MS allows the direct analysis of
very small sample amounts (5–200 µg)
without the need of time-consuming
sample preparation. The identification
of complex mixtures or blends as well as
identification of samples with so-called
“difficult matrix” are also possible in many
cases.
Q: What are the challenges and
difficulties in applying pyrolysis gas
chromatography–mass spectrometry
to failure analysis? How can they be
overcome?
A: The increasing use of polymeric
materials in the automotive industry
requires sensitive and reliable methods
for its analysis. For the failure analysis in
motor vehicles there is often a lack of
information about the component itself,
such as chemical composition, temperature
resistance, possible contaminants, or
mechanical properties. The damage
range is usually limited and not always
homogeneous. There are often only small
amounts of samples available to clarify
the damage, which may be important
for recognizing the cause of damage.
Traditional analytical techniques used for
characterization of polymers/copolymers,
such as thermal analysis (TA) and Fourier
transform infrared spectroscopy (FTIR),
have limitations or are not sufficiently
sensitive to demonstrate the change of the
structure and the resulting dysfunction of
used materials. A lot of information about
dysfunction of automobile parts can be
Q&A: Kusch
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