Analysis of Chlorine in Rubber and Windshield Wiper Blades Using

ASOMA
Application Note
®
PROCESS INSTRUMENTS
ASOMA® PHOENIX II
Analysis of Chlorine in Rubber and Windshield Wiper Blades
Using Direct Excitation
Introduction
Summary
This report demonstrates
the suitability of the
PHOENIX II using Direct
Excitation (DE) XRF
analyzer for determining
the concentration of
chlorine in rubber and in
finished windshield wiper
blades. It will show that
use of this instrument
will deliver improvements
in product quality by
accurately and rapidly
determining the chlorine
content, which affects the
rigidity of the rubber and
the wiping smoothness of
wiper blades.
The PHOENIX II DE is an excellent benchtop XRF analyzer for at-line
QC analysis or the laboratory alike. The PHOENIX II DE offers a fast,
precise, simple and non-destructive analysis technique well suited for
the determination of chlorine in bulk rubber stock and finished rubber
products. Monitoring the chlorine is important in several applications. For
example, the chlorine content helps determine the stiffness or rigidity of
the rubber. In the finished windshield wiper blades, a proper chlorine level
helps minimize wear and the blade squeaking against the window.
The PHOENIX II DE is a powerful tool for monitoring chlorine in rubber.
The analyzer uses a rugged, time-proven proportional counter as its
detection system and a direct excitation X-ray tube. This combination of
ruggedness and simplicity using a small benchtop analyzer enables fast
and precise results.
The PHOENIX II DE uses an integrated computer system with a userfriendly touch screen interface. (An external computer is not required.)
Data handling and results storage can be obtained on a thermal paper
print out and are also stored in the hard drive of the PHOENIX II DE.
The data can be readily transferred to a USB thumb-drive or a network
Ethernet connection.
Calibrations are readily carried out using assayed standards, usually
of flat rubber sample panels. This ensures easy traceability of results
for quality purposes. This initial calibration process is a “once only”
procedure. Subsequently, the curve can be restandardized, if required, by
the touch of a button on the main analysis screen.
The PHOENIX II DE offers power, versatility and performance all in a
small, compact, easy-to-use design.
The advantages can
be seen in easily and
quickly measuring the
chlorine. Namely, ensuring
proper chlorine levels to
control product quality and
minimize waste of over
use of chemicals. Thus,
the PHOENIX II DE can be
used to minimize costs and
maximize profitability.
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Experimental Portion
Equipment
Windshield Wiper Blade Preparation
Unique Phoenix II sample holder
All measurements were conducted using a
PHOENIX II DE XRF analyzer. Performance is
shown for using a total measurement time of 200
and 100 seconds.
Sample Preparation
Sample preparation is minimal. For bulk rubber
samples simply cut a coupon approximately 2X2
inches square and place it over the aperture in the
analysis chamber. For wiper blade samples, lay the
section of blade in the specially designed sample
holder for windshield wiper blades and screw down
the sample holder top. This ensures the blade is
kept flat for analysis. Once the sample is in place
simply press the green ANALYZE button..
Flat Sample Preparation
White paper sample shown for better viewing
2
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Measurement Parameters
The results can be reported using a variety of
different options: results are reported on the display
screen; on a thermal paper printout; on an optional
external printer; and in the database history within
the analyzer.
Correlation Plot
2.0
Measured ( % )
All measurement parameters are easily controlled
through the touch screen on the display panel.
Operators simply choose the correct method from
the analysis screen (there may be more than one
method stored, e.g. to measure bulk rubber samples
or windshield wiper blades) and then press the green
ANALYZE button.
1.5
1.0
0.5
Instrument Configuration
ASOMA® PHOENIX II using Direct Excitation
0.0
Excitation: Direct Excitation 30 kV 9 W Air-cooled
X-ray tube
Detection: Gas-filled Proportional Counter
Analytes: Cl
Optimization: X-ray voltage, current and X-ray filter
Atmosphere: Air
Options: Detector filter; Mylar 4 µm film
0.5
1.0
Results
Empirical calibrations are built using assayed
standards supplied by customers. The most
accurate results are obtained when using such
“matrix-matched” calibration technique and
calibration standards using the rubber formulation of
interest.
Precision for Chlorine in Rubber
10 repeat analyses at 200 seconds per
measurement
Units: %
Sample
Given
Mean
Std.
Dev.
% Rel.
1
1.92
1.927
0.0044
0.2
4
0.48
0.487
0.0021
0.4
10 repeat analyses at 100 seconds per
measurement
Element: Cl
Chlorine in Rubber
Calibration for Chlorine in Rubber
Element: Cl
Std. Error of Estimate: 0.0037
Sample
Given
Measured
1
1.92
1.921
2
1.45
1.449
3
0.97
0.967
4
0.48
0.484
5
0.00
-0.001
3
1.5
Given ( %)
Element: Cl
Note: No helium purge is required.
Units: %
0.0
Units: %
Sample
Given
Mean
Std.
Dev.
% Rel.
1
1.92
1.920
0.0048
0.3
4
0.48
0.484
0.0032
0.7
2.0
Analysis of Chlorine in Rubber and Windshield Wiper Blades
Using Direct Excitation
Element
Count Time
LOD
Cl
200 sec
0.003 %
Cl
100 sec
0.005 %
Calibration for Chlorine in Windshield Wiper
Blades
Element: Cl
Std. Error of Estimate: 0.018
Sample
Given
Measured
1
1.0
0.99
1b
1.0
1.02
2
2.0
2.04
2b
2.0
1.99
3
3.0
3.00
Sample
Given
Mean
Std.
Dev.
% Rel.
1
1.0
0.99
0.005
0.5
2
2.0
2.01
0.008
0.4
3
3.0
3.02
0.011
0.4
3b
3.0
3.01
The Limit of Detection (LOD) for an element is
determined as three times the standard deviation
of ten analyses of a blank sample. The following
LOD was derived using this empirical method and
applies to this matrix and concentration range.
Element
Count Time
LOD
Cl
100 sec
0.018 %
Conclusion
As can be seen from the above data, the use of
the PHOENIX II DE gives excellent performance
when applied to the determination of chlorine
in rubber and finished windshield wiper blades.
Results are rapid, precise and analysis is easily
carried out, even by non-laboratory personnel.
Because no consumable chemicals are used, the
relative “cost of ownership” is much lower than
other analytical techniques.
Correlation Plot
3.5
3.0
Measured ( % )
Units: %
Limit of Detection (LOD)
Chlorine in Rubber in Windshield Wiper Blades
Chlorine in Windshield Wiper Blades
Units: %
Element: Cl
2.5
2.0
1.5
1.0
0.5
0.5
1.0
1.5
2.0
2.5
3.0
3.5
Given ( %)
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The Limit of Detection (LOD) for an element is
determined as three times the standard deviation
of ten analyses of a blank sample. The following
LOD was derived using this empirical method and
applies to this matrix and concentration range.
Precision for Chlorine in Windshield Wiper
Blades
10 repeat analyses at 100 seconds per
measurement
Application Note
Limit of Detection (LOD)
Chlorine in Rubber
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