APPLICATION NOTE

Investigating why a

No. AN52673
plastic part failed
Key words
ATR, diffuse transmission, failure analysis, FTIR,
FT-Raman, polymer testing, spectroscopy

Abstract
Manufacturers employing plastic parts routinely face
the challenge of analyzing failed parts to determine the
root cause and corrective actions. The tools used to
perform this analysis often include infrared and Raman
spectroscopy for chemical composition, UV-Visible
spectroscopy for color and optical transmissivity, and
thermal analysis for determination of physical properties.
This paper describes a study utilizing all of these tools to
determine why a plastic part failed. Thermo Scientific Nicolet iS50
FTIR Spectrometer

Introduction
A manufacturer of precision optical equipment designed
a plastic cover for a device with specifications for Shortly thereafter, the product began to fail critical
chemical composition, surface texture, color and optical performance tests. The failures were immediately traced
transmission. Briefly, the cover was to be made from a to ambient light causing elevated backgrounds, strongly
polycarbonate – acrylonitrile butadiene styrene (PC-ABS) affecting low level optical measurements. Visual inspection
blend with sufficient titanium dioxide to provide a slightly of the covers did not reveal apparent differences from the
off-white color and optical transmissivity less than original, but various control experiments led to tracing of
0.01% T over a wide spectral range – from the UV into the the failure to the new cover. A root cause analysis using
near-infrared. The opacity was required to prevent ambient many techniques was undertaken to quickly identify and
(room) light from entering the optical device and interfering contain the issue.
with low light level measurements. Initially, all parts
supplied met the specifications and the product provided
satisfactory performance.

A re-engineering project was subsequently initiated to

reduce costs and make the product more competitive.
Alternate suppliers for various parts, including the cover,
were asked for quotations. A new supplier underbid
the original cover supplier, and the test parts met all
the requirements for opacity. Production was shifted to
incorporate this new supplier.
Experimental results Essentially no transmittance was measurable through the
UV-Visible spectroscopy good cover. In contrast, a significant transmittance through
Diffuse transmission measurements of the original the visible part of the spectrum, greater than 7% T, was
cover and failed cover were performed using a Thermo measured from the failing cover. This clearly explained the
Scientific™ Evolution™ 220 UV-Visible Spectrophotometer poor performance – the light leak – of the device under
and integrating sphere, displayed in Figure 1. ambient conditions, but did not identify the root cause.

Thermogravimetric analysis (TGA)

Small pieces of the two covers were then measured with a
TA Instruments™ thermogravimetric analyzer to determine
bulk composition, with results shown in Figure 3.1 The
samples were heated from ambient to 650 °C at 20 °C/min
under N2 purge, then cooled to 550 °C, and heated again
Figure 1: Evolution 220 UV-Visible Spectrophotometer (left),
and sample compartment integrating sphere accessory (right) to 1000 °C at 20 °C/min with air purge.

The cover by design contained significant quantities of The initial heating ramp under nitrogen pyrolyzes the
particulates, which would efficiently scatter any transmitted organic component of the covers, and the final temperature
light. For this reason, transmittance was measured with an ramp in air burns the remaining organic components
integrating sphere. Pieces of covers from both good and leaving only oxides of the inorganic content.
failing devices were placed at the transmittance port of the
sphere and spectra were collected from 220 to 800 nm, The organic decomposition profiles of the two covers
resulting in the spectra shown in Figure 2. were nearly identical, indicating that both had the same
plastic composition. However, the good cover had residual
inorganic component representing 5.4% by weight, while
the failed cover had an inorganic component of only 2.2%
by weight. This indicated a significant difference in the
inorganic filler amounts between the covers and provided a
strong clue as to the source of the light leak.

Infrared analysis
Infrared spectra of small pieces of the two covers were
collected using the integrated diamond iS50 ATR on a
Thermo Scientific™ Nicolet™ iS50 FTIR Spectrometer, as
shown in Figure 4. The built-in iS50 ATR on the Nicolet iS50
has a dedicated detector which permits the collection of
Figure 2: Diffuse Transmittance UV-Visible spectra of the failed cover combined mid- and far-IR ATR spectra down to 100 cm-1. The
(blue) and good cover (red), collected with an Evolution 220 UV-Visible ability of the iS50 ATR to collect spectra in the far-IR allows
Spectrophotometer and integrating sphere accessory
easy measurement and identification of inorganic fillers in
plastic parts.
iS50 ABX
iS50 FT-Raman Automated
Accessary Beamsplitter
Exchanger

Built-in
Diamond
iS50 ATR

Figure 3: Thermogravimetric analysis weight loss curves for the good

cover (red) and failed cover (blue), showing that the good cover has Figure 4: Nicolet iS50 FT-IR spectrometer with built-in diamond iS50
significantly higher inorganic content than the failed cover ATR, iS50 ABX Automated Beamsplitter exchanger, and sample
compartment iS50 Raman accessory
When combined with the iS50 ABX Automated Beamsplitter
exchanger on the Nicolet iS50 Spectrometer, mid and
far-IR spectra can be automatically collected and stitched
together using a Thermo Scientific™ OMNIC™ Macros\Pro™
Visual Basic Program to provide a single spectrum of a
sample from 4000 to 100 cm-1.2

The ATR spectra of the plastic parts, shown in Figure 5, were

corrected using the advanced ATR correction algorithm3
in Thermo Scientific OMNIC Software. The advanced ATR
correction algorithm accounts for both relative intensity Figure 5: Advance ATR corrected infrared ATR spectra of the good
changes caused by sample penetration depth as a function plastic cover (top), failed plastic cover (middle) and difference
spectra between the two (bottom)
of wavelength and also for peak shifts in the infrared spectra
due to index of refraction differences between the ATR
crystal and sample. Inspection of the infrared spectra of the
two plastic pieces shows the polymer composition to be
similar, but the original plastic part has an elevated baseline
below 800 cm-1, and a sharp peak at 360 cm-1, as shown
in Figure 6, that are absent or very weak in the spectrum
of the replacement part. The peak at 360 cm-1 is below
the range of a typical mid-IR spectrometer equipped with
a KBr beamsplitter. The iS50 ABX with a solid substrate
far-IR beamsplitter makes the far-IR range accessible in this
analysis, while maintaining no compromise high performance
across the entire range.
Figure 6: Overlay of the advanced ATR corrected spectra of the good
cover (blue) and failed cover (red), over the spectral region from
There are additional differences between the spectra which 940 to 100 cm-1. Note the elevated baseline and the absorbance band
at 360 cm-1 in the spectrum of the good cover that are absent or
are emphasized through a spectral subtraction. The difference
highly reduced in the spectrum of the failed cover.
spectrum (Figure 5, bottom) shows small peak shifts in the
polymer bands, indicating a small polymer composition
difference between the two parts, typical when comparing
plastic parts made by different suppliers, but a significant
spectral difference is also observed below 800 cm-1.

A library search of the difference spectrum against a

forensic library of automobile paint pigments and fillers,4
shown in Figure 7, matches rutile, one of the crystalline
forms of titanium dioxide, indicating a formulation difference
between the two covers.
Figure 7: FT-Raman difference spectrum between the good and failed
FT-Raman analysis covers (blue), and top match from a library search against a forensic
automobile paint pigment and fillers library (red), identifying a higher
To confirm the conclusions drawn from the infrared analysis, concentration of rutile (titanium dioxide) in the good cover.
the two samples were also analyzed using the iS50 Raman
sample compartment FT-Raman accessory on the Nicolet
iS50 Spectrometer (shown in Figure 4). The iS50 Raman
accessory snaps into the sample compartment of the
Nicolet iS50 FTIR Spectrometer, not requiring an external
module typical of other FTIR spectrometer systems. The
iS50 Raman accessory permits easy collection of Raman
spectra with a near-infrared beamsplitter and InGaAs
detector mounted inside the spectrometer.
FT-Raman spectra of the good and failed covers, along Summary and Conclusion
with the spectral difference spectrum between them, are Ambient light leaking into the device caused erroneous
displayed in Figure 8. FT-Raman spectroscopy allows measurements for low light level measurements. Diffuse
collection of spectra into the far-IR region, complementing transmission measurement of the parts by UV-Visible
the capability of the Nicolet iS50 FTIR Spectrometer with spectroscopy confirmed that the failed cover did not
the built-in iS50 ATR and ABX gaining access to this region. meet the specification for maximum transmittance.
Again, the two spectra are very similar, demonstrating Thermogravimetric analysis demonstrated that the
similar polymer composition, with small differences in the composition of the original cover contained approximately
spectra observable below 800 cm-1, clearly seen in the 3% more, by weight, of an inorganic filler compared to the
difference spectrum. replacement cover. Infrared ATR analysis over the mid and
far-IR spectral regions showed that the original cover had
A library search of the difference spectrum against a significantly higher rutile (titanium dioxide) content than the
minerals Raman library5 is displayed in Figure 9, identifying replacement cover. The infrared results were confirmed by
the difference between the two plastic parts as rutile, FT-Raman spectroscopy.
confirming the identification from infrared analysis.
This study clearly shows the importance of having several
tools available for root cause analysis. Many of the tools
used can be found on the Nicolet iS50 FTIR Spectrometer.
The Nicolet iS50 is able to collect multi-range spectra
without compromise using the built-in iS50 ATR and
iS50 Raman accessories. The analyses provided by the
Thermo Scientific UV-Vis and FTIR instruments, along with
thermogravimetric analysis, were decisive in determining
the root cause failure of the plastic cover.
Figure 8: FT-Raman spectra of the good cover (top), failed cover References
(middle), and subtraction result between the two (bottom) 1. Thermogravimetric results provided by Jeff Jansen, The Madison Group,
2615 Research Park Drive, Madison, WI, 53711.
2. Mid-Far ATR iS50 collection program available upon request. Requires
Nicolet iS50 FTIR Spectrometer configured with built-in diamond iS50
ATR, and ABX Automated Beamsplitter exchanger with KBr and solid
substrate beamsplitter.
3. Thermo Scientific Application Note 50581, Advanced ATR Correction
Algorithm.
4. An Infrared Spectral Library of Automobile Paint Pigments (4000–250 cm-1),
developed by Dr. Edward H. Suzuki at the Washington State Police Crime
Laboratory, downloadable from the SWGMAT.org website
5. Downs R T (2006) The RRUFF Project: an integrated study of the chemistry,
crystallography, Raman and infrared spectroscopy of minerals. Program
and Abstracts of the 19th General Meeting of the International Mineralogical
Association in Kobe, Japan. O03-13 Minerals 514 Raman Library.

Figure 10: FT-Raman difference spectrum between the good and failed
covers (top), and top library search result against a minerals Raman
library (bottom), identifying a higher concentration of rutile (titanium
dioxide) in the good cover

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specified. AN52673_E 05/19M