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The Microanalysis System
What makes a Good Detector?
The Pulse Processor
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Role of the pulse processor Analog pulse shaping Time variant shaping Digital pulse shaping Fixed process time Adaptive pulse shaping Resolution & count rate Pulse pile-up protection Comparing different pulse processors Summary
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The pulse
processor
Comparing
Different Pulse Processors
For accurate and efficient EDS
analysis the performance of the pulse processor is as important as the
detector.
EDS detector specifications
typically reveal the best possible performance that the detector can
achieve. Any pulse processor will perform its best at very low count rates,
when the voltage steps on the ramp are widely spaced and easy to measure.
Therefore detector specifications are often quoted at 1000cps. However, this
count rate is well below what is required for efficient analysis and only
the best designs of pulse processor will maintain good and stable detector
performance as the input count rate is varied.
How does performance change when
the count rate is increased? At more commonly used input rates between 2000
and 10000cps, processors may not be able to maintain the best resolution if
resolution degrades with count rate, or process time is shortened to achieve
a useful acquisition rate. Therefore one useful measure of how an EDS
hardware system will perform is the resolution achieved when the input rate
is at least 2500cps, and the acquisition rate is below the maximum for the
process time chosen.
Modern EDS software is designed
to give reliable automatic identification of X-ray peaks and accurate
standardless analysis. This is a relatively straightforward task when peaks
are well separated, but for overlapped peaks where there is no clear valley
between the peaks, accurate energy calibration is vital. Some systems may
appear to have stable performance with count rate because peaks do not move
more than 5eV and X-ray line markers are always in the correct channel at
10eV/channel. However, when quantifying peaks about 35eV apart (e.g. SiKα
and WMα) only a 4eV shift in energy calibration can introduce a 10 weight%
error (Statham 2002). If the resolution also varies and the width of peaks
is wrongly predicted by the software then larger errors may occur.
Analog pulse shaping designs have
difficulty maintaining a stable baseline so the energy calibration may vary
as count rate increases. Time variant shapers or digital pulse shapers
should show much less variation, and provide more reliable results, without
the need to keep input rate constant. Moreover, processors which are able to
constantly monitor the zero level will be able to measure shifts in the
baseline and, in addition, some systems can also monitor resolution changes
for correction by software.
The best method to test how
energy calibrations and resolutions change over a useful operating count
rate range, and how well these changes are compensated, is to analyze real
samples at a useful range of input rates, for example 1000, 2500, 5000 and
10000cps. By doing this the effect of any variation on the ability of a
system to perform reliable analysis can be tested. The ability to resolve a
severe overlap can be tested by analyzing a pure material for elements known
not to be present. For example, by collecting spectra from a pure element
such as Si, at different count rates.
If the spectra are
quantified assuming Si, and Ta and W are present (TaM and WM are very close
to SiK), a system that will provide accurate analysis in this count rate
range should find levels of Ta and W below statistical significance at all
count rates. By overlaying spectra collected at the different rates it may
also be possible to see peak shifts or resolution changes with count rate.
For example Fig. 20 shows four spectra collected from pure silicon at
different input rates using a digital pulse processor where count rate
stability is good. Quantitative analysis of these spectra, assuming Si, Ta
and W are present (Table 1) shows that within statistical significance only
Si is present, whatever count rate is used to collect the data.
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1000cps |
2500cps |
15000cps |
10,000cps |
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Si |
99.68 ± 1.78 |
99.43 ± 1.41 |
99.90 ± 0.97 |
99.23 ± 0.90 |
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Ta |
-0.82 ± 1.56 |
0.31 ± 1.22 |
-0.99 ± 0.85 |
0.04 ± 0.78 |
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W |
1.14 ± 0.89 |
0.26 ± 0.70 |
1.09 ± 0.49 |
0.74 ± 0.46 |
Table 1 Quantitative analysis of pure silicon calculated from the spectra
shown in Fig 20 assuming Si, Ta and W are present. At all input rates Ta and
W are below statistical significance (3 sigma). Note that negative numbers
should be reported, because negative values greater than statistical
significance also indicate incorrect spectrum deconvolution.
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