Designation: C 982 – 03

Standard Guide for Selecting Components for

Energy-Dispersive X-Ray Fluorescence (XRF) Systems1
This standard is issued under the fixed designation C 982; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope 3.2 Standard methods for the determination of materials

1.1 This guide describes the components for an energy- using energy-dispersive XRF5 usually employ apparatus with
dispersive X-ray fluorescence (XRF) system for materials the components described in this document.
analysis. It can be used as a reference in the apparatus section
4. Hazards
of test methods for energy-dispersive X-ray fluorescence
analyses of nuclear materials. 4.1 XRF equipment analyzes by the interaction of ionizing
1.2 The components recommended include X-ray detectors, radiation with the sample. Applicable safety regulation and
signal processing electronics, data acquisition and analysis standard operating procedures must be reviewed prior to the
systems, and excitation sources that emit photons (See Fig. 1). use of such equipment. (See ANSI/HPS N43.2.)
1.3 Detailed data analysis methods are not described or 4.2 Instrument performance may be influenced by environ-
recommended, as they may be unique to a particular analysis mental factors such as heat, vibration, humidity, dust, stray
problem. Some applications may require the use of spectrum electronic noise, and line voltage stability. These factors and
deconvolution to separate partially resolved peaks or to correct performance criteria should be reviewed with equipment
for matrix effects in data reduction. manufacturers.
1.4 This standard does not purport to address all of the 4.3 The quality of quantitative XRF results can be depen-
safety problems, if any, associated with its use. It is the dent on a variety of factors, such as sample preparation and
responsibility of the user of this standard to establish appro- mounting. Consult the specific analysis method for recom-
priate safety and health practices and determine the applica- mended procedures.
bility of regulatory limitations prior to use. 4.4 Sample chambers are available commercially for opera-
tion in air, vacuum, or helium atmospheres, depending upon
2. Referenced Documents the elements to be determined and the physical form of the
2.1 ASTM Standards: sample.
E 135 Terminology Relating to Analytical Chemistry for
5. Energy Dispersive X-Ray Detectors
Metals, Ores, and Related Materials2
E 181 General Methods for Detector Calibration and Analy- NOTE 1—Because of the rapid improvement in detector and electronics
sis of Radionuclides3 technologies, the most up-to-date information on XRF components is
found in manufacturers’ literature. Lists of vendors of XRF equipment can
2.2 Other Document:
be found in compilations such as the “Guide to Scientific Instruments,”
ANSI/HPS N43.2–2001 Radiation Safety for X-Ray Dif- published by the American Association for the Advancement of Science,
fraction and Fluorescence Analysis Equipment4 Washington, DC.

3. Significance and Use 5.1 Energy-dispersive X-ray detectors can be used to detect
X rays with energies from approximately 1 to 100 keV;
3.1 This guide describes typical prospective analytical
however, a single-type detector usually cannot satisfy all the
X-ray fluorescence systems that may be used for qualitative
requirements of efficiency and energy resolution over such a
and quantitative elemental analysis of materials related to the
wide energy range.
nuclear fuel cycle.

1
This guide is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel
Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
5
Current edition approved July 10, 2003. Published September 2003. Originally General References for XRF include Bertin, Eugene P., Principles and
approved in 1988. Last previous edition aproved in 1997 as C 982–88–(1997)e1 Practices of X-Ray Spectrometric Analysis, Second Ed., Plenum Press, New
2
Annual Book of ASTM Standards, Vol 03.05. York-London, 1975, Jenkins, Ron, An Introduction to X-Ray Spectrometry, Heyden
3
Annual Book of ASTM Standards, Vol 12.02. and Sons, Ltd., London, New York, Rhine, 1974, and Woldseth, Rolf, All You Ever
4
Available from American National Standards Institute, Inc. or the Health Wanted to Know About X-Ray Energy Spectrometry, First Ed., Kevex Corporation,
Physics Society. Burlingame, CA, 1973.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 C 982 – 03

Reprinted by permission of Kevex Corporation, Burlingame, CA.

FIG. 1 Function Block Diagram of XES System

5.2 The energy resolution (Terminology E 135) of a detector 5.5 Scintillation detectors such as NaI(T1), or gas-filled
is usually specified by the FWHM (full width at half maxi- proportional counters, may be used in certain applications in
mum) of the full energy peak of an X ray (or g ray) of a which the high resolution of the semiconductor detectors is not
particular energy and at a specified count rate. The FWTM (full required.
width at one-tenth maximum) of the full-energy peak or the 5.6 All types of X-ray detectors have entrance windows of
peak-to-background ratio, or both, may also be specified. a low-Z material (for example, Be on solid-state detectors or
“High resolution” (small values of FWHM) detectors are plastic film on gas-filled counters) to minimize X-ray absorp-
required to separate X rays of similar energy emitted by tion.
different elements. 6. Signal Processing Electronics
5.3 The dimension of the detector “active volume” is 6.1 The bias power supply required to operate X-ray detec-
usually specified for X-ray detection applications, allowing the tors must be capable of delivering sufficient high voltage and
efficiency of the device for detecting a particular energy X ray current for the particular detector. The power shall be regulated
to be estimated. and have ripple and noise content below the 10-mV level.
5.4 XRF analysis systems requiring high-resolution detec- 6.2 A preamplifier converts the charge pulse caused by an
tors employ semiconductor (“solid state”) detectors. ionizing event in the detector to a voltage signal. It must also
5.4.1 Lithium-drifted silicon, Si(Li), detectors are usually minimize electronic noise that would degrade the spectrum
used for applications requiring the detection of X rays from 1 resolution. The preamplifier is typically charge sensitive and
to 40 keV. Si(Li) resolution is commonly specified at 5.9 keV uses a field-effect transistor. The noise content, gain, and
and 1000 cps. Resolutions of 145 to 160 eV (FWHM) are count-rate capability must be compatible with the particular
typical. detector and application. “Resistive feedback” and “pulsed-
5.4.2 Germanium, Ge, detectors or lithium-drifted germa- optical feedback” are two types of preamplifier techniques
nium, Ge(Li), detectors are usually employed to detect X rays suitable for high-resolution spectroscopy. The preamplifier is
usually supplied as an integral part of the detector, and the
in the high-energy region of the X-ray spectrum. Ge resolution
detector manufacturer should be consulted to determine a
is commonly specified at 122 keV and 1000 cps when the
suitable preamplifier.
detector is to be used for X-ray detection. Resolutions of 500
6.3 A shaping amplifier is used to integrate the preamplifier
eV (FWHM) are typical.
pulse for a well-defined duration, differentiate the pulse to
5.4.3 Both Ge(Li) and Si(Li) detectors must be operated at provide an acceptable shape, and amplify the pulse to an
77°K (liquid nitrogen temperature). Si(Li) detectors can be appropriate voltage. Typical shaping times vary from 1 to 40 µs
stored at room temperature. Germanium detectors must be depending on the detector count rate and the required energy
stored at 77°K (Standard E 181). resolution. Amplifier outputs are approximately ten volts maxi-
5.4.4 Improvements in technology can extend the useful mum. The amplification factor is variable so that the output
energy range of a particular detector type or result in the pulse height spectrum corresponds to the desired range of
development of new detector materials. Manufacturers should X-ray energies. Most shaping amplifiers provide power to the
be consulted for the latest information. preamplifier. High-resolution amplifiers are equipped with

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 C 982 – 03
adjustments for signal shaping to optimize the resolution at a volts) of pulse height that can be digitized is often MCA-
given rate. Some high-resolution amplifiers are equipped with controllable. Computer control of MCA data acquisition is a
pileup rejection circuitry. (See 6.4.) Most commercial shaping common mode of operation.
amplifiers in these applications are nuclear instrument module 7.1.2 The most basic form of MCA data analysis involves a
(NIM) standard modules. hand integration of peak areas. MCA memory is frequently part
6.4 Pulse pileup rejection is employed to exclude from the of computer memory or accessible to a computer central
processed data those signals with amplitudes that may be processor. In this case, data analysis can be automated. Most
altered by the close occurrence in time of two detected events. MCA systems contain either preprogrammed software or
Pileup rejection units generally permit the selection of a firmware controlled by mechanical operation of buttons or
resolving time within which the occurrence of two events switches, which perform, for example, peak integration, energy
causes the generation of a logic signal. The logic signal is used calibrations, or resolution measurements. They may also pro-
to reject the time-coincident linear signal in a circuit designed vide programmable memory for increased automation or for
for this purpose. The latter circuit can be incorporated in the more complex or specific data analysis, which may include
pileup rejection module, in the data acquisition unit (multi- fitting peaks and backgrounds. As a third option, the MCA can
channel analyzer), or in a separate gating module. The reduc- be interfaced to a computer for direct access to the analyzer
tion of the influence of pulse pileup can also be obtained with memory and functions or for the transfer of stored data to the
circuits which apply “baseline restoration” to the pulse train, computer for analysis. The analysis software should be acces-
and it is possible to combine both baseline restoration and sible to the user for editing or modification to suit the needs of
pulse pileup techniques. A high overlap of pulses can result in the particular application. Source listings of the analysis
loss of the true zero of reference to give an erroneous measure programs of commercial software packages should be available
of pulse amplitude. Pole-zero cancellation reduces these ef- to the user.
fects, but where a resolution of better than 0.1 % at high rates 7.2 Single Channel Analyzer (SCA):
(;50 kHz) is needed, baseline restoration appears to be a 7.2.1 The function of a single MCA channel is performed by
practical solution. Both passive and active methods have been the SCA. This is an electronic component that generates a logic
developed with the active methods showing greater superiority signal for each linear input signal that the amplitude of the
at higher count rates. These circuits can either be incorporated input signal falls within a window defined by certain voltage
in the main amplifier, or they can be part of the pulse amplitude limits. The range and spacing of the limits are adjustable on the
analyzer system. SCA. An SCA rather than an MCA might be employed for
6.5 Counting losses caused by pulse pileup or electronics reasons of economy, portability, or space constraint. Its use is
deadtime increase with increased counting rates. Accurate limited to measurements of relatively simple spectra from
quantitative X-ray analysis requires that data be normalized to samples with well-defined components or for survey measure-
correct for these variable losses. Corrections are performed by ments where high accuracy is not required. A scaler is normally
counting the number of events accumulated in a peak generated used to count the SCA logic output signals.
by a fixed-frequency electronic pulser, or a radioisotopic 7.2.2 The simplest form of SCA data analysis involves
source in fixed counting geometry, or by increasing the counting the number of events in a window that brackets a peak
counting time of the data acquisition system based on an of interest. In this case a peak must be well resolved from
electronic analysis of counting losses. Commercial units are neighboring peaks and have negligible background. When
available for automatic correction for count rate losses. background is nonnegligible, two measurements of equal count
6.6 Gain stabilization to maintain a constant relationship duration can be made with a fixed-width window set to bracket
between X-ray energy and electronic pulse height or multi- the peak in one case and the background in the other. The
channel analyses channel may be required for applications in background count can then be subtracted from the peak count.
some environments. The overall system gain can be stabilized This procedure can be simplified to a single measurement if
using electronic means or computer software techniques. two SCAs are em-ployed. The use of multiple SCAs and
logical summing units can give directly the number of
7. Data Acquisition and Analysis background-subtracted counts in one or more well-resolved
7.1 Multichannel Analyzer (MCA): peaks from a single measurement.
7.1.1 The most frequently employed unit for storage and
counting of pulses from the shaping amplifier is the MCA. 8. Photon Excitation Sources
MCA memory consists of a minimum number of locations 8.1 Radioisotopic sources are convenient and low-cost
(channels) to which counts are assigned based on the ampli- methods of producing X-ray photoexcitation. The choice of
tudes of pulses associated with detected events. Each linear radioisotope, source strength, and geometry is dependent on
amplified signal is digitized (assigned a numerical value) application. 1 09 Cd for L X-ray excitation and 57Co for K X-ray
proportional to its amplitude. One count per event is stored in excitation of nuclear material are typical sources. Useful
the channel corresponding to the digital quantity. Since the source strengths are generally determined by system count rate
number of channels is finite, the channels store the counts of capability. Sources in an annular geometry provide excellent
events within (continuous) energy bins of the amplified pulse uniformity of intensity across the sample surface and a tight
height distribution. A two-dimensional display of the number counting geometry. (See Fig. 2.) Point sources are also used.
of counts versus channel shows peaks in the appropriate 8.2 X-ray generators provide a source of photons with
channels corresponding to the X-ray energies. The range (in variable energy and intensity. The X-ray generator should

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 C 982 – 03

Reprinted by permission of Kevex Corporation, Burlingame, CA.

FIG. 2 Schematic Representation of Radioisotope Excitation System with Annular Source Configuration, (a) Direct Irradiator; (b)
Secondary Target Irradiator

provide X rays of energy at least slightly greater than the 9. Keywords

absorption edge energy of interest. The X-ray tube, available
9.1 energy dispersive x-ray fluorescence; instrument
with a target(s) of various high-purity elements, should be
components
capable of uninterrupted operation up to the potentials and
currents required for the particular application.
8.3 The radiation from radioisotopic sources and X-ray
generators can be modified by the use of filters or secondary
sources or can be utilized in the direct mode.

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