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Some applications of neutron activation analysis: A review

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 REVIEW

Journal of Radioanalytical and Nuclear Chemistry, Vol. 265, No. 1 (2005) 141–150

Some applications of neutron activation analysis:

A review
E. Witkowska,* K. Szczepaniak, M. Biziuk
Department of Analytical Chemistry, Chemical Faculty, Gdansk University of Technology, 11/12 Narutowicza Str., 80-952, Gdansk, Poland
(Received August 3, 2004)

Basic information on neutron activation analysis (NAA) and its application in environmental studies is presented. The fundamentals of the
technique are shown while various methods of neutron activation analysis are briefly characterized in order to depict the most important
information. A rich set of NAA applications for human and biological samples is given together with the short description of the results. The
problems associated with the quality assurance and control are also pointed out and discussed. The information is addressed to researchers
interested in the applications of neutron activation analysis or to those who are searching for a suitable alternative analytical technique for
environmental studies on human and other biological samples, where other techniques are not the best choice.

Introduction substance to ensure that the radioactivity will behave

Determining the elemental composition of different
types of materials is an important task in a wide range of
disciplines such as biomonitoring, human and other
biological analysis, environmental research and
materials science.1 There are many analytical techniques
capable of detecting very small quantities of elements.
One such technique is the neutron activation analysis
(NAA).
The principle of the method is given elsewhere.2–5
normally in all subsequent chemical and physical
processes.14 Before separation, samples have to be
chemically decomposed. Usually samples are digested
using various acids (HNO3, H2SO4, HF, HClO4) or
burnt in an oxygen atmosphere. Although RNAA has the
advantage of high sensitivities to many elements and the
obtained data are accurate. The method has also
disadvantages: it is rather time consuming and the
radiochemical procedures can often be very
complicated.11

Characteristics of different types of neutron Instrumental neutron activation analysis (INAA)

activation analysis
There are many ways to subdivide the types of the
neutron activation analysis. One of them is based on the
way radionuclides are analyzed and distinguish two
types of neutron activation analysis.
Radiochemical neutron activation analysis (RNAA)
RNAA is used in the case where the induced
radionuclides of trace elements are masked by matrix
activity. The resulting radioactive sample is chemically
decomposed and the radionuclides are isolated by
chemical separations into a single or several fractions
free of interfering radioactivities, each with one or
relatively few radionuclides. The most frequently used
separation techniques are: liquid extraction,6,7 ion
exchange,8,9 precipitation,10,11 electrolysis12 and
chromatography.13
Generally a carrier is added during the chemical
separation. According to IUPAC, a carrier is an inactive
material deliberately added to a specified radioactive
When applying instrumental neutron activation
analysis (INAA)2–4,15,16 the decomposition of the
radioactive sample is not necessary. The radionuclides
are determined on the basis of the differences in decay
rates via measurements at different decay intervals using
high-resolution detectors.
Below is a list of the essential physical and chemical
characteristics of INAA.
The method is nondestructive. It does not require
complicated handling. All problems related to the
decomposition of the sample and separation (dissolution,
contamination and losses) are avoided. This aspect is
very important when unique or valuable materials must
be analyzed, e.g., archeological and art objects or in the
case of materials that are difficult to dissolve, e.g.,
silicon based samples or ceramics.
It is multielemental, suitable for sample sizes from
@g to kg, which allows one to obtain low detections
limits (at µg/kg to mg/kg level) for up to fifty elements.
Various amounts of elements from sub-ng/g up to %
level give linear responses.

* E-mail: emwitko@poczta.onet.pl

0236–5731/USD 20.00 Akadémiai Kiadó, Budapest

© 2005 Akadémiai Kiadó, Budapest Springer, Dordrecht
 E. WITKOWSKA et al.: SOME APPLICATIONS OF NEUTRON ACTIVATION ANALYSIS
Better detection limits of desired elements can be
achieved by optimizing irradiation parameters (energy,
fluence rate of the neutrons, and irradiation, decay and
counting times).
The influence of the matrix is usually negligible.
Most matrices appear to be transparent, because the
atoms of which most of them are composed (H, C, O, N,
P, and Si) hardly form any radioactive isotopes. This
makes the method highly sensitive for measuring trace
elements.
The sensitivity obtained by neutron activation
analysis is a function of nuclear parameters of the
element in question (neutron cross section, isotope
abundance, half-life, and gamma-ray abundance),
available neutron flux, length of irradiation, detector
efficiency, matrix composition, and the “total” sample
size.
It is self-validating: two or more analytical -lines
may be used for the determination of the same element
allowing a crosscheck of the process.
Some environmentally important elements, e.g., Cd,
Cu, Ni and Pb cannot be determined, at least not at low
concentrations.
The method is rather time-consuming. It takes about
2–4 weeks to obtain information about elements
involving radionuclides with long half-lives.
NAA only gives the information on the total element
concentrations. Information on chemical compound
structure and physical state cannot be immediately
acquired.
Less widely applied than other analytical techniques
due to necessity of having access to a nuclear reactor.
Thermal, epithermal and fast neutron activation
analysis
Thermal neutron activation analysis (TNAA)
NAA is often called thermal NAA (TNAA) to
emphasize that thermal neutrons play the main role in
the activation process. More than 70 natural elements
can induce radionuclides by means of (n,J) reactions.
The main advantages of the TNAA are: high-activation
cross sections and no interfering reactions exist. The
main drawback is the perturbation of thermal neutron
flux by highly absorbing samples.17
Epithermal neutron activation analysis (ENAA)
Mainly non-thermal neutrons are used to improve
detection limits and precision of element determination
such as U, Tl, In, Au, Ta, Ag, Br, Co, I and Sb. ENAA is
mainly applied when elemental content can be
determined via a nuclide with high ratio of resonance
activation integral (I0) to thermal neutron cross section
142
( 0): I0/ 0. To reduce the activity of nuclides where the
ratio of resonance activation integral to thermal neutron
cross section is low, thermal neutron filters of cadmium
or boron are used. Therefore, this method is particularly
useful for geological samples because many interfering
nuclides (i.e., 24Na, 38Cl 42K, 46Sc, 51Cr, 59Fe) have low
I0/ 0 ratios.18,19 ENAA is also very often used to
determine Br and I in biological samples.20,21
Fast neutron activation analysis (FNAA)
Also called 14 MeV neutron activation analysis, it
utilizes not only nuclear research reactor fast neutrons,
but also fast neutrons produced by a neutron generator
or by an isotopic neutron source.4,22 In neutron
generators 14 MeV neutrons are produced by the
reaction between deuterium and tritium nuclei. They are
produced by creating deuterium ions and accelerating
these ions into a tritium or deuterium target. The D-D
reaction is used only in special circumstances because
the neutron yield from the D-T reaction is ~100 times
higher.23 In isotopic neutron sources the most common
source of neutrons is the spontaneous fission of
californium-252 (252Cf). The average energy of neutrons
from 252Cf is 2.3 MeV.24 Neutrons may also be
produced by a reaction between -particles and low Z-
elements (the most common element is Be). The -
particle is emitted during radioactive decay of 238Pu,
226Ra or 241Am. Isotopic neutron sources although
having a long useful life and producing a relatively
constant flux of neutrons, have several disadvantages
including the fact they cannot be turn off when not in
use. Isotopic neutron sources cannot be pulsed and the
energy spectrum of the emitted neutrons is broad and
peaks at energies below the threshold for some
important reactions.25 One of the advantages of the
FNAA lies in the fact that the use of fast neutrons from a
neutron generator enables to perform field
measurements, e.g., detections of metal contamination in
soil.26 The most important application of FNAA is the
analysis of oxygen content in a wide variety of matrices
including metals, geologic materials, coal, liquid fuels,
ceramic materials, petroleum derivatives and fractions
and chemical reaction products.22,26–29 The determi-
nation of nitrogen in biological materials, including
nitrogen as a measure of protein content30 as well as
nitrogen determination in fertilizers, explosives, and
polymers are also important applications. Other
elements that are routinely analyzed by FNAA include
Ag, Al, Au, Si, P, F, Cu, Mg, Mn, Fe, Zn, As, and
Sn.31,32
Other types of neutron activation analysis
The major and trace quantities of most elements in
variety of samples matrices can be determined by
 E. WITKOWSKA et al.: SOME APPLICATIONS OF NEUTRON ACTIVATION ANALYSIS
conventional INAA. However, in some cases there is a
need for special irradiation, counting and data treatment
conditions.
Cyclic neutron activation analysis (CNAA)
Cyclic neutron activation analysis is based on
repetitive short irradiation and measurement cycles,
whereby the measurements are summed. CNAA is used
for the measurements of the concentrations of very
short-lived isotopes (half-life <10 s) to improve their
detection limits. However, it is limited by the transfer
times of the sample from the irradiation unit to the
counting place. These times should be shorter in time
than the half life of the radioisotope of interest.33,34 The
method has been applied for the determination of, e.g.,
Au, Ag, Cl, F, Hf, Sc, Se in biological samples. 2,4,35
In vivo neutron activation analysis (IVNAA)
In vivo neutron activation analysis is a well-
established technique used to measure the major
elements such as C, Ca, K, N, O and P, or trace element
content in the human body.36–40 However, the
fundamental principles include that the body is exposed
to neutron from either a neutron generator, isotopic
neutron source, or a nuclear reactor. IVNAA allows
reliable and reproducible reconstruction of molecular
level components such as total body fat, protein and
minerals.
Prompt gamma neutron activation analysis (PGNAA)
Prompt gamma neutron activation analysis as
mentioned in the first paragraph, is based on the
measurement of -rays emitted during nuclear reactions
rather than -rays emitted from radioactive decay.
PGNAA is used for the determination of low Z elements
like B, H, N, P, S, and Si in various types of samples
(geological samples, biological samples, and
alloys).41–45 These elements are unusually determined
by typical neutron activation analysis or detected with
low sensitivity. However, PGNAA has been also applied
for heavier elements, e.g., uranium.46 PGAA is also
valuable for elements with large capture cross section
and high gamma-ray yield, especially cadmium,
samarium, and gadolinium.47
Quality assurance and quality control
According to IUPAC, the quality control is the
maintenance and statement of the quality of the data set
specifically that it meets and exceeds some minimum
standard based on known, testable criteria.48 The basic
quality control principle is to ensure that the
measurement methods are sufficient to assure
conformance to specified requirements. Practically, the
quality control implies analysis of reference materials,
spiked samples, blanks, duplicates and other control
samples. Another important aspect in quality control is
the necessity of documentation of all experimental
conditions connected with the reactor operation,
statistical analysis, safety analysis and the quality of the
irradiated material.
Quality assurance is the guarantee that the quality of
an analytical data set is claimed on the basis of the
quality control applied in creating that product.48
Practical quality assurance in neutron activation analysis
is a complex problem and requires taking into account
many aspects connected with:49
Reactor operation and NAA facilities, like:
characterization of irradiation positions (an evaluation is
required for the thermal, epithermal and fast neutron
fluxes in the irradiation positions); pneumatic transfer
system (the system should be operated, characterized,
and maintained in accordance with adequate
procedures); reactivity effects of in-core experiments;
pressure build-up due to radiolysis.
Preparation for irradiation: impurities in irradiation
containers or sample encapsulation (impurities should be
evaluated by irradiating and analyzing several of the
capsules); estimation of induced radioactivity and
radiation dose rate (for radiation protection purposes it is
important to estimate the induced radioactivity and
associated dose rate after irradiation); encapsulation of
liquids (a procedure for leakage testing of containers
used for liquid samples should be developed); moisture
content and moisture uptake during weighing;
evaporation losses during drying; quality of
homogeneity (to ensure the quality of samples
homogeneity tests should be carried out); quality of
standards (verification of the purity and the
stoichiometry of standards); quality of the used balance
(the balance should be routinely inspected and
calibrated); pipette calibration; effect of differences
between samples and standards.
Irradiation process: irradiation requests containing
the relevant information needed for the facility used,
sample characteristics and container/capsule contents
should be completed by the user); integrity and
identification of sample holders; routine and non-routine
samples (a list of routine samples should be prepared;
non-routine samples are required to be subjected to a full
safety evaluation).
Analysis process: synchronization of clocks (to
accurately correct for radioactive decay it is important to
know the synchronization of the clocks used for
registration of the irradiation time beginning, its
duration and the start of the counting); sample and
standard physical dimensions (development of standard
operating procedures for the preparation of the sample
and standard in the same geometry is needed); undefined
143
 E. WITKOWSKA et al.: SOME APPLICATIONS OF NEUTRON ACTIVATION ANALYSIS
geometry of sample and/or standard (the development of
a technique for fixing small pieces of material in a well a
defined position in a capsule is necessary); dead-time
effects; variable count rate during counting; pile-up
corrections; coincidence or cascade summing effects;
gamma ray self-absorption effects; background,
shielding and contamination problems; nuclear reaction
interferences and gamma-ray spectrum interferences;
differences in irradiation geometry between samples and
standards; malfunctioning gamma-ray spectrometers.
Standardization in neutron activation analysis
Standardization in neutron activation analysis can be
divided into absolute and relative methods. The absolute
standardization method is based on the calculation using
the activation equation. This method has some
drawbacks described elsewhere.4,50,51 In relative
standardization an unknown sample is irradiated
together with a sample containing a known amount of
elements of interest. In one application of this method a
certified reference material (CRM) is used as a standard.
There is one serious problem with this case, the
availability of CRMs of various matrices is limited. In
the second application a multielemental prepared
standard is used. The last example of relative
standardization is a single comparator method called the
k0-method. In this case the unknown sample is irradiated
together with a neutron flux monitor such as Au. The
rate of induced activity from stable atoms of interest is
related to the activation rate of gold through the k0-
constant. This constant is independent of irradiation and
measuring conditions. Compared to relative method with
multielemental standard k0-NAA is simpler but requires
more complicated calculations.50 The k0-NAA
procedure is nowadays widely used in numerous
laboratories performing NAA all over the world.52–54
Applications of the neutron activation analysis
The neutron activation analysis is a powerful
analytical technique with application in a broad range of
disciplines such as: archeology,55–57 environmental
monitoring, geology, human sample analysis, materials
science29,58,59 and many others.
For a long time NAA has been used in many
countries for the characterization of candidate reference
materials or in certification of elements in existing
reference materials.47,60,61 Nowadays, there is a trend to
use NAA to validate other methods of elemental
analysis.62,63 In this paper we focus on the analysis of
environmental and human samples.
144
Human sample analysis
Human samples analyzed by neutron activation
analysis can be divided into hard tissue, soft tissue and
body fluids. In the case of bones usually Ca and P are
determined to estimate the bone strength.64–70 For
example TZAPHLIDOU et al.70 took rib bones at post-
mortem, cleaned them of soft tissue and blood and
analyzed them, by NAA. It was found that the Ca/P ratio
is more reliable for diagnosis of bone disorders than the
individual concentrations of Ca and P.68–70
A next example of hard tissue, which is widely
analyzed by means of NAA, is hair. Hair analysis is the
most frequently used for assessing human environmental
and occupational exposure.71-75 For example, KUPERA
and co-workers71 found increased levels of Cr and Mo
in hair of workers in the stainless steel industry. Similar
studies were done in a galvanizing factory and results
suggest that hair reflects the impact of the polluted
environment on workers’ health.76 Hair analysis has also
been applied to estimate the correlation between
concentration of elements in hair and the health status.
For instance it was found that children suffering from
asthma showed increased concentration of Au, Cs and
Sb in hair.72 Before analysis, hair samples are washed
with a detergent, acetone and deionized water.
Another application of NAA for hard tissue analysis
is the determination of elements in nails. This type of
analysis is also used for assessing human environmental
and occupational exposure.35,71,77–79 An interesting
application is the one proposed by TING-PANG and co-
workers.35 They used cyclic neutron activation analysis
to improve detection limits of Ag, F and Sc determined
in nails samples collected from construction workers.
The detection limits were significantly improved and
interferences from sodium in the determination of F
were eliminated.35 The purpose of another study was to
investigate whether Ca and Mg content in nail clippings
correlates with bone mineral density. The correlation
between concentrations of Ca and Mg and bone mineral
density was very low, so the conclusion was that Ca and
Mg measurements in nail clippings could not be used for
screening purposes in the prevention of osteoporosis. 77
Another type of samples analyzed is soft tissue, e.g.,
brain, breast tissue, liver, neural tissue and thyroid. The
determination of elemental concentration in brain is
usually used for investigating diseases, for example
Alzheimer’s. Two independent groups found the
increased concentration of Fe and Zn in one part of brain
and they surmised that elevated Fe could possibly play a
role in neuronal degeneration in Alzheimer’s
disease.80–82 DEIBEL and co-workers,83 in turn,
 E. WITKOWSKA et al.: SOME APPLICATIONS OF NEUTRON ACTIVATION ANALYSIS
developed an NAA method modification involving a
short epithermal irradiation and counting with a
Compton suppression system for determination of Cu in
brain. They showed that Cu can be determined by either
64Cu and coincidence counting, or 66Cu and counting
with Compton suppression. NAA was also used for the
investigation of optimal brain samples digestion.84
Preparation of brain samples consisted of removing
surface fluids by pressing between sheets of Whatman
No. 541 filter paper and/or freeze-drying.80–87
Considerably more rarely brain analysis is used for
exposure assessment. For example, BARREGÅRD and
coworkers86 applied RNAA for Hg determination in
brain samples of thermoether workers exposed to
mercury vapors. Unexpectedly, the Hg level was found
to be the same as that found in brains of not exposed
people.
Breast tissue analyses were performed to check if
there were differences in the elemental composition of
histologically normal tissue and tissue exhibiting
malignant lesions. It was found that the concentration of
all determined elements were higher in the malignant
tissue.88–89
In the case of human liver analysis NAA is often
used combined with biochemical techniques. This
combination of neutron activation analysis with
physical, chemical or biological separation is sometimes
called molecular activation analysis.90,91 This technique
gives information on chemical speciation of trace
elements. Biochemical separation are: size-exclusion
chromatography, precipitation, extraction and SDS
polyacrylamide gel electrophoresis. By means of
separation techniques and NAA it is possible to study
the distribution pattern of rare earth elements and their
binding species with proteins or the concentration and
chemical species of Al, Cl, Cu, K, Mg, Mn, Na in
human liver and its subcellular fractions.92–95 Another
interesting application of NAA is that proposed by
ARNOLD and co-workers.96 They used in vivo NAA to
study the concentration of Mn in liver. A small dose of
neutrons was delivered to the organ of interest, the
neutrons were readily captured by the target nuclei, and
the gamma rays emitted were detected outside the body.
This solution can be applied to monitor manganese
levels in individuals occupationally exposed to the
element.
Platinum in neural tissue was determined to
investigate if Pt accumulates in neural tissue of patients
treated with cisplatin. The method was radiochemical
neutron activation analysis. Tissue samples were
decomposed after irradiation using a mixture of
hydrochloric, nitric and perchloric acids. Gold
(including 199Au indicator of Pt) was separated by
electrolysis of a hydrochloric acid solution.12,97,98
Another application of NAA is the determination of I
in thyroids. The concentration of 129I and the ratios of
129I/127I in regular human thyroids were determined by
radiochemical neutron activation analysis. Before
irradiation iodine was pre-concentrated from thyroids
using steps as follows: incinerating the thyroid samples,
leaching the iodine with hot water, extraction with CCl4
and evaporation of the solution. After irradiation iodine
was separated by extraction with CCl4 and precipitation
of PdI2.99–101
Another application of NAA in human samples
analysis is the determination of elements in human body
fluids like blood, serum or urine. There are many
purposes for urine and blood analysis. One of them is
the occupational exposure assessment, for instance the
determination of chromium and manganese collected
from workers in the stainless steel industry.71 OUGH and
co-workers102,103 applied NAA for the determination of
U in urine collected from active and retired Canadian
Forces personnel, who served in the Gulf War and
Kosovo. The total uranium concentration was relatively
low so the conclusion was that isotopic (238U/235U ratio)
assay could not have been performed. Radiochemical
neutron activation analysis was applied to the
determination of As, Co, Mo and Se in urine collected
from a healthy, unexposed group of British people. In
assessing the health risk posed by toxic elements, the
knowledge of the current levels of trace elements in
human populations is essential. Dried urine samples
were irradiated, next mineralized by microwave
digestion and finally separated on a series of ion
exchange resins.104,105 Determination of element
concentration in blood is also used in health studies. For
example, BAKIR and co-workers106 investigated the
relationship of selenium concentration in blood
components and tumor tissues of breast cancer patients
and healthy volunteers in Syria. They found that the
selenium concentration in serum and RBC was
significantly lower among breast cancer patients
compared to healthy volunteers. The results also showed
that selenium concentration was significantly higher in
the cancer tissues compared to adjacent regular tissues.
Environmental samples
Air samples play a dominant role in environmental
studies. The analysis of elemental concentrations in
samples such as aerosols, ash and particulate matter are
used for assessing air pollution.107–130 In the case of
aerosol analysis an interesting application is the one
proposed by PROBST and co-workers.112,113 They
determined gold, calcium and platinum concentration in
aerosol samples without application of sample digestion.
NAA of Pt using the 199Au daughter of 199Pt was
performed. This analysis was affected by Au and Ca
concentrations, but both interferences on Pt
determination were corrected by applying suitable
calculations. Platinum concentrations in air were the
145
 E. WITKOWSKA et al.: SOME APPLICATIONS OF NEUTRON ACTIVATION ANALYSIS
highest ever published for environmental investigations.
The estimation of potential toxicity of ashes emitted by
various types of incinerators was the aim of another
study. Extractable organohalogens (EOXs) were
determined after extraction with toluene in a Soxhlet
apparatus. EOX analysis suggested that ash samples
contained many of organochlorine compounds. In
addition, medical waste incinerator ashes were
considered to have relatively higher amount of
organoiodine compounds than other ashes.114–117 The
study of airborne particulate matter, especially the
distribution and multielement composition of PM2.5
(fine particles with diameter <2.5 µm) and PM10 (coarse
particle with diameter between 2.5 and 10 µm), is
gaining worldwide attention because of its health
effects. This type of analysis was performed in Portugal,
China, Belgium, Italy and Greece.120–129 Particulate
matter samples are usually collected by means of Gent
stacked filter unit sampler consisting of two Nuclepore
filters with 0.4 and 8 µm pore sizes. A new procedure
for cadmium determination in air particulate matter was
done using the 336.2 keV gamma-ray line of 115mIn in
addition to the gamma-ray line of 527.9 keV used for
115Cd detection. It was found that the measurement of
336.2 keV gamma-ray line of 115mIn significantly
improved the determination of Cd.126,127
A good alternative to the characterization of air
particulate matter is the use of plants as environmental
pollution biomonitors. Biological materials used for air
pollution monitoring include mosses, lichens, tree
leaves/needles and bark.131–143 In the case of plant
analysis sample preparation is rather simple and
involves washing, drying and grinding. In order to
remove fluctuations of absolute values and give a clue to
sources of metals found in plants, raw concentrations are
sometimes normalized to the soil or the earth’s crustal
abundance pattern by calculating the enrichment factor
(EF).145 Elements with EF values that are significantly
higher than considered not originating from the local
soil background may be attributed to long transportation
phenomena from other natural and/or anthropogenic
sources.136
The use of moss as atmospheric metal deposition
biomonitors has been widely accepted. FRONTASYEVA et
al.144 studied atmospheric deposition of heavy metals
and other toxic elements in the Chelyabinsk region in
Russia. Epithermal NAA appeared to be a convenient
analytical technique for assessing the environmental
situation in the given area. They also found higher
concentration of Cu and As in an area within a distance
of about 30–40 km from the copper smelter.
GALSOMIÉS133–135 reported that P. schreberi and S.
purum accumulate slightly more to much more than H.
cupressiforme for the majority of thirty six elements
investigated.
146
Lichens are also suitable biomonitors of
environmental pollution for a variety of elements and
radionuclides. FREITAS and co-workers137,138 studied
the distribution of some pollutants in lichens in Portugal.
They were able to identify elements as emitted by some
anthropogenic sources. COSTA et al.125 found correlation
between lichen and PM10 samples element content, but
only for a few elements. An interesting application of
lichens as biomonitors was presented in another
paper.136 Element concentrations and enrichment factors
found in Himalayan lichens suggested that Cu, Zn, Cd,
As, Sb and Br may be derived not only from the local
soils but also from long transport phenomena of other
natural and/or anthropogenic sources. Because of the
fact, that moss and lichens do not occur in all parts of
the Czech Republic, oak tree bark was chosen as
biomonitor of air pollution. It is less sensitive but
available almost everywhere and easy to collect.141
In some cases two or three types of biomonitors are
used simultaneously. Tree-bark, lichens and moss were
used for evaluating trace elements bioavailability in
different regions of Morocco.131 It was found that using
elemental analysis of lichens, moss and tree bark
coupled with enrichment factors is a powerful tool for
atmospheric pollution detection. Also in another study
moss, lichens and tree bark were used to assess air
pollution.132 In this case, however, fast neutrons
produced via the 3H(d,n)4He reaction with a neutron
generator were used for irradiation. It was found that
Mg, Al, Si, Cl, K, Ca, Ti and Fe can be easily
determined by 14 MeV NAA with good precision while
results for Zn, Rb, Sr, Ba and La are less precise or
below the detection limit.
There are also other plants used as environmental
pollution biomonitors, like cotton, white beet, or species
typical for a given country area (e.g., Solanum
lycocarpum in Brazil).143,146,147 Another example of a
plant widely used in biomonitoring are algae.
Macrophytic algae, especially green and brown seaweed
concentrate metal ions from seawater to levels many
times higher than those found in the surrounding water.
That is why algae have been widely used as an indicator
of marine water pollution.75,148–152 Preparation of algae
samples involves washing, drying and homogenization.
HOU et al.152 applied NAA for the characterization of
major and trace element composition of Chinese algae.
They found that the concentrations of halogens, rare
earth elements and many transition metals in marine
algae were remarkably higher than those in terrestrial
plants. Similar studies were done in Mexico. It was
reported that brown algae showed a tendency to
incorporate elements at higher concentration levels than
red and green algae. It was also found that a significant
correlation existed between measurements in algae and
their corresponding average elemental concentrations in
oceanic water.150
 E. WITKOWSKA et al.: SOME APPLICATIONS OF NEUTRON ACTIVATION ANALYSIS
Other types of samples, widely analyzed by NAA,
are soil and sediment. The interest in analyzing sediment
and soil samples for their metal contents lies in the fact
that they concentrate these analytes, exhibiting higher
concentrations than other adjacent samples, such as air,
water or plants. Concentrations of elements in river, lake
and marine sediments are determined to evaluate how
different sources of pollutants influence heavy and trace
elements accumulation.153–155 NAA was also used as
reference technique for evaluating the right digestion
method of zircon-bearing samples for REEs
determination. It was found that HF digestion resulted in
unsatisfactory recovery of REE. Instead a relatively
simple, fast and safe partial digestion using
HClO4+HNO3 was used to extract REE mainly from
clay minerals.156 An interesting application was the
determination of Se(IV) forms in marine sediments.
After drying and powdering, sediment samples were
dissolved with a mixture of HNO3, HClO4 and HF in a
microwave digester. The quantitative determination of
Se(IV) was performed by co-precipitating its
dibenzyldithiocarbamate complex with phenolphthalein
(DBDTC-Pp) followed by neutron irradiation of the
Se(IV). The distribution of Se(IV) concentrations along
the South Johore coastal area showed some variations
with locations and strata.157 Soil samples are often
analyzed to find if there is a correlation between soil and
plant element content.146,147,158,159 SHINONAGA and co-
workers,158 for instance, were looking for correlation
between iodine content in cereal grains and soil samples.
For iodine determination they used RNAA after
irradiation and dissolution of soil samples and iodine
precipitation as PdI2. It was found that the soil-to-grain
transfer factor was correlated negatively with iodine
concentration in soils. This can be due to weaker
adsorption of iodine in the soil matrix, which leads to a
lower content in soil and at the same time to higher
content of iodine in soil solution which is available for
plants. Another interesting application of RNAA for soil
samples analysis is presented by HOU and co-
workers,160 who determined 137Cs and 129I in soil
contaminated by the Chernobyl accident. Before
irradiation iodine was separated from soil samples by
extraction and back-extraction.161 It was found that in
129I
most Chernobyl-contaminated soils, the
concentration in the upper few centimeters layer has a
significant positive correlation with the corresponding
137Cs concentration.
Water sample analysis by means of NAA is not very
popular due to the need of sample pretreatment. One
way of sample pretreatment is preconcentration on
activated carbon. The method proposed by YUSOF and
co-workers162 is based on preconcentration of analytes
on activated carbon and zirconium loaded activated
carbon using specific conditions of pH and oxidation
states. It was found that zirconium loaded activated
carbon is capable of adsorbing As(V), Se(VI), Cr(VI)
and Hg(II) at any pH while activated carbon adsorbs
As(III), Se(IV), Cr(III) and Hg(I) at a higher pH. HOU
and co-workers160,163–166 developed a method for the
determination of iodides, iodates, organic iodines and
total iodine in seawater. Iodides were separated from
other iodine species and other ions by passing seawater
through an anion-exchange column. Organic iodines
were separated by passing seawater through an ion-
exchange column after iodates had been converted to
iodides by KHSO3. The iodine content was determined
with postirradiation separation using CCl4 extraction
and PdI2 precipitation. In another case, RNAA was
applied for the determination of Ba and Tl in water
samples. After irradiation Ba and Tl were separated
using cerium(IV) molybdate as inorganic ion-
exchanger.167 One more interesting application of NAA
is the analysis of uranium in drinking water. Before
irradiation uranium was separated by means of a chelate-
forming anion-exchanger with thiourea groups. By the
described procedure it is possible to measure uranium in
the range of µg/l.168
Conclusions
Neutron activation analysis has been applied in many
fields of science. However, developments of other non-
nuclear techniques such as ICP and ICP-MS have
caused the decline of NAA usage, especially in human
and other biological samples. Nevertheless, there are
still some fields where NAA is irreplaceable, e.g.,
analysis of solid materials which are difficult to
dissolve, analysis of samples with low trace element
concentrations, where the risk of contamination is very
high, and analysis in which a high degree of accuracy is
needed. Moreover, contrary to other techniques, this one
does not require in general any special sample
pretreatment and is a non-destructive. In many cases this
is of great importance.
*
The Department of Analytical Chemistry constitutes “Centre of
Excellence in Environmental Analysis and Monitoring” which is a
research project supported by the European Commission under the
Fifth Framework Programme and contributing to the implementation
of the Key Action “Sustainable Management and Quality of Water”
within the Energy, Environment and Sustainable Development
(Contract No.: EVK1-CT-2002-80010). The authors acknowledge this
generous support.
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