Neutron Activation Analysis

What is Neutron Activation Analysis

(NAA)?
• NAA is a method for qualitative and
quantitative determination of elements
based on the measurement of
characteristic radiation from radionuclides
formed directly or indirectly by neutron
irradiation of the material.
NAA Method
 NAA Categories
• According to type of emitted γ-ray measured
• If the Prompt γ-ray is the measured radiation
Prompt γ -ray neutron activation analysis
(PGNAA)
• The measurements take place during irradiation.

• If Delayed γ-ray is the measured radiation.

• Delayed γ -ray neutron activation analysis
(DGNAA)
The measurements take place after a certain
decay period.
• (DGNAA) is more common.
 I. PGNAA
• The PGNAA technique is generally performed by using a
beam of neutrons extracted through a reactor beam port.

• detectors are placed very close to the sample compensating

for much of the loss in sensitivity due to flux.

• The PGNAA technique is most applicable to elements with

extremely high neutron capture cross-sections (B, Cd, Sm,
and Gd); elements which decay too rapidly to be measured
by DGNAA; elements that produce only stable isotopes; or
elements with weak decay gamma-ray intensities.
 II. DGNAA
• DGNAA (sometimes called conventional
NAA) is useful for the vast majority of
elements that produce radioactive nuclides.
• The technique is flexible with respect to time
such that the sensitivity for a long-lived
radionuclide that suffers from an interference
by a shorter-lived radionuclide can be
improved by waiting for the short-lived
radionuclide to decay.
• This selectivity is a key advantage of
DGNAA over other analytical methods.
 Instrumental vs. Radiochemical
NAA
• It is generally possible to simultaneously measure more
than thirty elements in most sample types without
chemical processing.

• The application of purely instrumental procedures is

commonly called instrumental neutron activation analysis
(INAA) and is one of NAA's most important advantages
over other analytical techniques.

• If chemical separations are done to samples after

irradiation to remove interferences or to concentrate the
radioisotope of interest, the technique is called
radiochemical neutron activation analysis (RNAA).
 NAA procedure
• Sampling;
• Pre-irradiation sample treatment (such as
cleaning, drying or ashing, pre-concentration of
elements of interest or elimination of interfering
elements, sub-sampling and packing);
• Irradiation (and prompt gamma-ray counting in
PGNAA);
• Radiochemical separation (only in RNAA);
• Radioactivity measurement;
• Elemental concentration calculation;
• Critical evaluation of results and preparation of
the NAA report.
 Irradiation
• There are several types of neutron sources:
reactors, accelerators, and radioisotopic neutron
emitters.

• Nuclear reactors with their high fluxes of

neutrons offer the highest available sensitivities
for most elements.

• Most neutron energy distributions are quite

broad and consist of three principal components
(thermal, epithermal, and fast).
Neutron Energy Distribution
 I. Thermal Flux
• The thermal neutron component consists of low-
energy neutrons (energies below 0.5 eV) in
thermal equilibrium with atoms in the reactor's
moderator.
• At room temperature, the energy spectrum of
thermal neutrons is best described by a
Maxwell-Boltzmann distribution with a mean
energy of 0.025 eV and a most probable velocity
of 2200 m/s.
• In most reactor irradiation positions, 90-95% of
the neutrons that bombard a sample are thermal
neutrons.
 II. Epithermal Flux
• The epithermal neutron component consists of neutrons
(energies from 0.5 eV to about 0.5 MeV) which have been
only partially moderated.
• A cadmium foil 1 mm thick absorbs all thermal neutrons
but will allow epithermal and fast neutrons above 0.5 eV in
energy to pass through.
• In a typical unshielded reactor irradiation position, the
epithermal neutron flux represents about 2% the total
neutron flux.
• Both thermal and epithermal neutrons induce (n,gamma)
reactions on target nuclei.
• An NAA technique that employs only epithermal neutrons
to induce (n,gamma) reactions by irradiating the samples
being analyzed inside either cadmium or boron shields is
called epithermal neutron activation analysis (ENAA).
 III. Fast Flux
• The fast neutron component of the neutron
spectrum (energies above 0.5 MeV) consists of
the primary fission neutrons which still have much
of their original energy following fission.
• Fast neutrons contribute very little to the
(n,gamma) reaction, but instead induce nuclear
reactions where the ejection of one or more
nuclear particles - (n,p), (n,α), and (n,2n) - are
prevalent.
• In a typical reactor irradiation position, about 5%
of the total flux consists of fast neutrons.
• An NAA technique that employs nuclear reactions
induced by fast neutrons is called fast neutron
activation analysis (FNAA).
 Radioactivity Measurement
• The instrumentation used to measure
gamma rays from radioactive samples
generally consists of a semiconductor
detector, associated electronics, and a
computer-based, multi-channel analyzer
(MCA/computer).
• Most NAA labs operate one or more hyper
pure germanium detector (HPGe).
Gamma-Spectroscopy System
 Calibration
• Energy Calibration

• FWHM Calibration

• Efficiency Calibration
Gamma-Ray Spectra (Short
Irradiation)
Gamma-Ray Spectra (Long
Irradiation)
Gamma-Ray Spectra (Long
Irradiation)
 Elemental Concentration
Calculation
• Basically there are two standardizations
methods used in NAA:

- The relative method

- The non-relative method.

 The Relative Method
• Sample and element standards are irradiated
simultaneously and later measured under the
same counting conditions.

• The relative method promises the highest

accuracy when the standard and sample match
each other well in composition, irradiation and
counting conditions.
 The Non-Relative Method
• Multi-element INAA is feasible in the non-
relative method or single comparator
method.
 Detection Limits
• The detection limit represents the ability of a
given NAA procedure to determine the
minimum amounts of an element reliably.
• The detection limit depends on the:
(1)The amount of material to be irradiated and to be counted..
(2) The neutron fluxes.
(3) The duration of the irradiation time.
(4) The total induced radioactivity that can be
(5)The duration of the counting time
(6) The detector size, counting geometry and background
shielding.
 Advantages of NAA
• Very low detection limits for 30–40 elements,
• Significant matrix independence,
• The possibility of non-destructive analysis
(instrumental NAA or INAA),
• The use of radiochemical separation to
overcome interference in complex gamma-ray
spectra (radiochemical NAA or RNAA),
• An inherent capability for high levels of accuracy
compared to other trace element analysis
techniques.
 NAA Applications
• Archaeology
• Biomedicine
• Environmental science and related fields
• Geology and geochemistry
• Industrial products
• Nutrition
• Quality assurance of analysis and reference
materials
 NAA at ETRR-2
- Egypt Second Research Reactor (ETRR-2), a 22
MW light water moderated and cooled open pool
nuclear reactor.
- There are many manually loaded sites for
irradiation of samples for several hours.
- For analysis that require short lived radionuclides
to be measured there are two computer
pneumatic irradiation transfer systems
- The detectors used to measure gamma rays from
irradiated samples are two coaxial HPGe
detectors and a Compton suppression system
 NAA at ETRR-2 (Con.)
• Instrumental Activation Analysis: about 300 samples
(geological, biological, industrial…), per year.
• Measurements of topaz activities: about 1200 samples
(each 1 kg) per year.
• Flux Mapping after core refueling and for the reactor
facilities.
• Reactor waste analysis.
• Measurements of radioisotopes produced at the reactor (100
Co-60 sources in 2005 and 52 sources in 2007).
• Participation in research projects:
- Arab Atomic Energy Authority coordinating project: “ Study
of trace elements in cancerous samples”
- AFRA IV-7 Research Reactor Project for Socio-economic.
- The lab participated in three proficiency tests: (2003, 2005
& 2007)
Samples analyzes by NAA during
the last six years
450
400
350
300
250
200
150
100
50
0
2008 2007 2006 2005 2004 2003
 Large Sample-NAA
• The problem of representativeness of the sample when dealing with
inhomogeneous bulk material affects all currently available analysis
techniques.

• Most techniques do not allow for large samples (kg level) because
the activating signal or the response (or both) cannot penetrate
samples of that size, or the technique is destructive and cannot
handle such large amounts.

• NAA, though, has highly penetrating neutrons as incoming signal

and highly penetrating gamma-rays as signal to be detected. This
makes NAA (in principle) a suitable technique for the analysis of
such large samples.

• The ‘large sample’ in INAA could be defined as a test portion in

which neutron and gamma-ray self-attenuation can not be neglected
in view of the required degree of accuracy. Hence, such a ‘large
sample’ would range from a few grams to several kilograms and
above.
 References
• IAEA-TECDOC-1215, “Use of research
reactors for neutron activation
analysis”, 1998.

• http://web.missouri.edu/~glascock/
naa_over.htm