Nuclear Inst.

and Methods in Physics Research B 471 (2020) 63–68

Contents lists available at ScienceDirect

Nuclear Inst. and Methods in

Physics Research B
journal homepage: www.elsevier.com/locate/nimb

Detection and interference of fission-neutron reactions on third period T

elements
a,⁎,1
Abdallah Ali , Elsayed K. Elmaghrabyb
a
Radiation Protection Department, Nuclear Research Center, Egyptian Atomic Energy Authority, Cairo 13759, Egypt
b
Experimental Nuclear Physics Department, Nuclear Research Center, Egyptian Atomic Energy Authority, Cairo 13759, Egypt
they usually coexists in biological and geological samples [1–3]. These
elements are vital ingredient in human body. Isotopes of the third
period elements interact with neutron leaving a short lived isotope
ARTICLE INFO
except for 35S (T1/2 = 87.37 d) and 32P (T1/2 = 14.268 d) beta emitters
Keywords: and 24Na (T1/2 = 14.997 h) gamma emitter. These isotopes on are fluent
Neutron activation analysis Reaction cross section move in the human body and when activated in Neutron Capture
ET-RR-2 Egyptian research reactor Interference Therapy (NCT) technique on an organ [4] they cause spread of radia
Soil and tissue tion dose to untreatable organs. On the other hand, when activated by
neutrons in the technique of Neutron Activation Analysis (NAA), sev
eral nuclear reactions are expected to occur, the most pronounced are
(n,γ), (n,p), and (n,α). The limitation of the interfering of the nuclear
reactions yielding the same product nuclei, and the response to the
changes in the irradiation conditions resulting in many systematic shifts
in the assessment of elemental contents. Among these reactions 27Al
(n,γ)28Al, 28
Si(n,p)28Al, 31
P(n,α)28Al, 30
Si(n,γ)31Si, 31
P(n,p)31Si, 27
Al
1. Introduction
27 26 27 30 27 24 24 23
ABSTRACT (n,p) Mg, Mg(n,γ) Mg, Si(n,α) Mg, Mg(n,p) Na, Na
(n,γ)24Na, and 27Al(n,α)24Na. Though the non-capture reactions may be
The interference among neutron reactions on the third-period elements was used as an analytical tool for the reactor field, these elements cannot
investigated. Fission-neutrons from ET-RR-2 Egyptian research reactor was used be easily assayed by NAA with nuclear reactors as they can cause
to determine the concentration of 24Na, 27Mg, 28Al, and 31Si in a standard
reference material. The determination of the concentrations for elements was
found to be affected by the interference among neighboring elements. 23Na was ⁎
Corresponding author.
found to have apparent concentration as twice as the certified value due to
24 27 26 E-mail address: abdallah.ph999@yahoo.com (A. Ali).
interference reaction with Mg and Al, similar results were noticed for Mg due 1
ORCID iD: https://orcid.org/0000-0002-0611-5285.
to interference reactions with 27Al and 30Si. Determination of 27Al concentration
28 28
was found acceptable as a result of negligible contributions of Si(n,p) Al and https://doi.org/10.1016/j.nimb.2020.03.028
31
P(n,α)28Al reactions. These results showed that there are addi tional sources of sources in neutron activation; capture reactions [6], and charge ex
dose uncertainty for the patient exposed to neutron capture therapy associated change reaction.
with the pro duction of 24Na, 27Mg, 28Al, and 31Si in addition to 35S and 32P beta In the present work, we emphasized the effect of interfering neutron
emitters.
reactions on the third period of elements for the determination of the
concentrations of Al, P, Na, and Mg. We also provided factors that
modulate the integral cross section of neutrons induced reactions on
isotopes of the third period to compensate for the effect of un
determined neutron flux distribution of the fission neutrons.

2. Experimental details

2.1. Material.

Standard reference material containing a known amount of third

analytical interferences in the determination of other elements. The
neutron capture reaction in 30Si is still questionable [5]. 31Si has two
Elements in the third period of the periodic table, which includes
sodium, magnesium, aluminium, silicon phosphorus, sulfur, and
chlorine are heavily abundant in complex environment of biosphere;
period isotopes together with elements that may be used as monitors
was used. The important elemental contents of the sample together
with its confidence range are illustrated in Table 1.
2.2. Irradiation
Irradiations were undertaken at the ET-RR-2 Egyptian research re
actor. The location of the irradiation position is just after the beryllium
Received 2 February 2020; Received in revised form 24 March 2020; Accepted 25 March 2020
Available online 02 April 2020
0168-583X/ © 2020 Elsevier B.V. All rights reserved.
A. Ali and E.K. Elmaghraby Nuclear Inst. and Methods in Physics Research B 471 (2020) 63–68
Table 1
The elements of interest contents in the standard reference material. Element
Reference Value mg/kg 95% Confidence Interval mg/kg
Al 47,000 44,000–51,000 La 28 27–29
Mn 631 604–650
V 66 59–73
K 12,100 11,300–12,700 Mg 11,300 11,000–11,800 Na 2400
2300–2500
P 460 460–462
Si 180,000 169,000–201,000
reflectors beside the reactor core, design details can be found in Refs.
[7–10]. The beryllium reflects most thermal neutron and the remaining
amount are partially thermalized in the moderator before reaching the
sample position. The irradiation time was adjusted to 1 min in partially
moderated neutron flux distribution. The reactor average thermal
neutron flux of order 1012 n/cm2 s−1.
2.3. Detection
High purity germanium detector (HPGe) was used for detection.
The sample position was adjusted to 5 cm above the detector end-cap.
For the calibration of the HPGe detector, the efficiency calibration was
performed using standard sources with uncertainty less than 7%. The
efficiency of the germanium detector was calibrated using decay from
standard sources of 60Co, (decay data from Ref. [11]), 133Ba (decay
137 152
data from Ref. [12]), Cs (decay data from Ref. [13]) and Eu and
154
Eu (decay data from Refs. [14,15]. The neutron monitoring reactions
were measured through the decay lines of 56Mn, 51V and 140La, decay
data were taken from Refs. [16–18]. The minimum detectable count
was determined by the Currie's equation [19].
T ,min = (4.65 2.71)ACF T ,B +
whereT ,min the minimum mean number of counts is required under the
photo peak andT ,B is the background counts under the photo peak.
ACF is the activity correction factor which represents the total activity
of the sample divided by the total activity of the background (total
counts of sample and background were used instead). For obtaining
the minimum detection limit, irradiation, cooling, and measuring times
are optimized.
2.4. Uncertainty propagation
The experimental uncertainty in our experiment includes several
sources: (1) sample mass, (2) irradiation and cooling time, (3) sys
tematic efficiency shift, and (4) self-shielding for neutrons in the
sample. The experimental uncertainties in the results includes
estimates of the level of confidence associated with all of the used
parameters and were calculated from the spectral data considering the
independence of measurement parameters. The accumulated
uncertainties were added in quadratic fashion [20] as follows:
222
=++++ttm
The mass uncertainty was 0.0003 g. Uncertainty in efficiency calibra
tion depends on the sample shape and was between 7% and 10% (in
cluding the uncertainty in peak statistics plus 5% uncertainty in the
reference sources and 3% of uncertainty introduced as a result of
sample volume and shape). Time uncertainty was less than 1% in ir
radiation time due to the time elapsed during removal of the sample
from the neutron field while being irradiated through perturbed flux. An
absolute uncertaintytc = 10–20 s in cooling time. The irradiation and
cooling times uncertainties becomes of importance for short-lived
isotopes. The uncertainty due to the self-shielding factors was
neglected due to the small size of the sample.
3. Results and discussion
Fission-neutron activation was undertaken using suitable a fast
pneumatic sample transfer system and computer facilities. Neutron flux
inside the reactor is not constant because of the yield of the fissile
material differs throughout the core, including different path of mod
eration and perturbations due to syntheses and decay of neutron poi
sons [21]. The short irradiation time was adjusted for 1 min with high
neutron flux to avoid neutron field perturbation that could affect the
results. The measurements were conducted several times after cooling
times of 8 min, up to 3 days from the end of irradiation to follow
radioactivity in their corresponding half-life scale. Fig. 1 illustrate the
spectra at the limits of this period to emphasize the certainty in the
measurements. The major problem is therefore, both to eliminate and
detect for the interference and to follow-up the decay of the desired
energy peak(s) to find the contribution of the element(s) under ex
amination.
In order to determine the exact value of flux on each sample, the
monitor reactions of elements within the sample was used. The fluency
rate of thermal neutron is calculated using the conventional activation
formula (cf. Ref. [21]):
T
N I 1 e e e 1 . thi i
()()
=
()()
iiiittt
( ) ( ) i i i c ( )i m
()()()()
Here, th is the flux of incident neutron at thermal energies [cm−2 s−1], T( )i
is the photo-peak net area measured during the measuring timetm, ti
andtc are the irradiation and cooling times in [s], respectively.( )i is the
decay constant of the residual nucleus in [s−1] and the probability of γ
ray per decay of the γ-ray line in the decay of the residual nucleus (I( )i
). is the number of nuclei that is subject to irradiation and is obtained by
using the formula:
N=Nfm
A
M,i ii
()()
()
()
i
whereNA is the Avogadro's number, f( )i is the fraction of existence of the
target nuclei in the samples, m( )i is the mass of the element in the
sample [g], and M is the molar mass of the target molecules. The term
is the detector’s efficiency including sample geometry correction factor,
( )i is integral cross section for the reaction. In our measurements we
determined the thermal neutron flux using 55Mn(n,γ)56Mn, 51V(n,γ)52V,
 139
and La(n,γ)140La reactions which yields several gamma lines as given
C 22
eff.
m the flux, the gamma lines from extend the efficiency calibration to
C eff. ( c) ( i) 56
Mn and 140La were used to high energy
in Table 2. After determination of
where m, C, and eff are the mass of the sample, count under peak of [22] by correlating the known efficiencies of low-energy gamma-rays
the γ-line, and efficiency in the detection of the gamma line. Time un with the count rate of their corresponding high-energy gamma-rays of
certainty is a crucial factor for short lived isotopes; here,tc andti are the the same isotope, see Fig. 2. The relative uncertainties associated with
uncertainties in the cooling time and irradiation time, respectively while such practice were the sum of the uncertainties in the original
is the decay constant of the isotope under consideration. An efficiency at low energies and the statistical uncertainty in peak count
uncertainty in the measuring times was negligible. The uncertainty in at high energies.
the efficiency was calculated similarly using the uncertainty of the The activation cross section of any none-capture reactions
standard sources activity and the counting uncertainty of the standard depends on the neutron energy distribution above its reaction
γ-lines. Counting statistics of peak area has uncertainty less than 3%. threshold. Researchers use flux integrated cross section in the form

64
A. Ali and E.K. Elmaghraby Nuclear Inst. and Methods in Physics Research B 471 (2020) 63–68

Fig. 1. Fission-neutron reactions gamma-ray spectra for third-period and monitor elements at cooling time 8 min and 3 days. ~

()()

Table 2
Monitor elements and their reaction parameters.f( )i is the natural abundances
of the target isotope in the element. Thermal neutron cross section data was

taken from Refs. [23]. The value of ~ (sigma-tiled) represents the integrated
cross section over Watt distribution.

Product isotope T1/2 Reactionsf( )i (%) th (b) ~ (mb)

55
Mn 2.5789 h 55Mn(n,γ)56Mn 100 13.28 1.88 52V 3.743 min 51
V(n,γ)52V 99.7
4.917 1.62 140La 1.6755 d 139La(n,γ)140La 99.9 9.039 5.93
 = E E dE
()
E dE

This quantity is usually used in activation with known flux dis

tribution, see Table 2.
At our irradiation location in the fast channel of the ETRR-2, the
high neutron fluence is due to partially moderated flux distribution
follows; it may follow Watt distribution [24,25] having the general
formula:

ab E 2 3
a bbE a ( ) sinh exp 4
WE=+

where E is the neutron energy; values of the parameters a and b were

investigated thoroughly in decade [26,27]. Empirical investigations
showed that the probability of a neutron from fission having an energy
between E and E + dE is the function P(E)dE is empirically approxi
mated asP E( ) 0.4865 sinh( 2 ) = E e E, in the unit of MeV−1. A better
insight can be gained into what happens in a thermal reactor by
plotting this using a log-scale on the x-axis. The neutron flux is just the
neutron density multiplied by the speed.
Fig. 2. Efficiency calibration at the position of the measurement of the standard
comparator and the soil. Energy was extended using the technique of internal ()()EPEE
efficiency calibration. Fitting curve was performed using Genie2k spectral
analysis software. cE 2
E= ( ) 0.4865 E e 939.6 sinh( 2 ) o E 2
Here, c is speed of light while energy is in MeV. Fig. 3 illustrates the
Watt distribution in which 0.04% of the neutrons are below 40 keV,
16.9% of the neutrons have energies between 40 keV and 1 MeV,
27.6% have energies between 1 MeV and 2 MeV, 22.6% have
energies between 2 MeV and 3 MeV, 14.9% between 3 MeV and 4
MeV, 15% between 4 MeV and 6.5 MeV, and 02.96% are above 6.5
MeV. The actual flux distribution in the reactor may vary from reactor to
reactor and even from run to run. The (n,p) reaction usually occurs
between 1 MeV and 2 MeV while the (n,α) reaction occur at neutron
energies above 1 MeV with increasing cross section with energy.
This distribution is modulated in the reactor due to existence of
water, reflectors, and control instruments. The exact distribution cannot
be determined explicitly because it changes with the operation of the
reactor and also oscillates due to continuous production and

65
A. Ali and E.K. Elmaghraby Nuclear Inst. and Methods in Physics Research B 471 (2020) 63–68

Fig. 3. Part a) The Watt distribution of the fission-neutrons. Part b) The cross
section change with energy for the two monitor reactions as given from eval
uated nuclear data files (ENDF) [28].
decay of neutron poison. In earlier measurements [29], the neutron flux
at the irradiation position was determined to be ϕo = 1.10 cm−2 s−1
which was about one-tenth the maximum core flux. Using the monitor
reaction, we were able to determine the thermal flux contribution which
was found to be ϕth = (2.35 ± 1) × 1011 cm−2 s−1 based on
55
Mn(n,γ)56Mn, and 139La(n,γ)140La capture reactions measurements.
Which represent less than the 2.1% of the total flux as represented by
the comparison in Fig. 3. Both of these values shall be used for their
specific contribution in reaction cross section.
The reaction yield of the 24Na is attributed to the 23Na(n,γ)24Na,
24
Mg(n,p)24Na, and 27Al(n,α)24Na reactions with cross sections as pre
sented in Table 3. The contribution of each reaction depends on the
energy spectrum of the neutron. The interference among these reaction
had caused deviation to larger value upon the determined concentra
tion of sodium in the sample; our results was 4.8 ± 0.1 mg/g, which is
approximately twice the reference data refers to 2.4 ± 0.2 mg/g.
Similarly, reaction yield of the 28Al is attributed to 27Al(n,γ)28Al,
28
Si(n,p)28Al, and 31P(n,α)28Al. The interference among these reaction
did not cause a significant deviation upon the determined concentration
of aluminium in the sample; our results 45.9 ± 0.2 mg/g while re
ference data refers to 47+4
−3 mg/g. Noting that the small difference is
within the experimental uncertainty. Reactions of, 28Si(n,p)28Al and 31P
(n,α)28Al would have negligible contribution upon neutron activation.
The reaction which lead to27Mg belongs to the 26Mg(n,γ)27Mg, 27Al
(n,p)27Mg, and 30Si(n,α)27Mg reactions. The interference among these
reaction had caused deviation to larger value upon the determined
concentration of magnesium in the sample; our results was
26.8 ± 3 mg/g, which is more than twice the reference data refers to
11.3−0.3+0.5 mg/g.
The reaction forming 31Si has two sources in soil, the capture re
action 30Si(n,γ)31Si, and the charge exchange ration 31P(n,p)31Si. The
reaction yield may weigh more to the 30Si(n,γ)31Si reaction because the
concentration of Si in the sample was about 180 g/kg which was large
compared to the P concentration which was 0.5 g/kg if the neutron field
was Maxwellian. However, and due to the existence of large contribu
tion of high energy neutrons, as shown in Fig. 3a, both reactions con
tribute effectively at this range of neutron energies. The interference
among these reactions had caused hard deviation upon the determined
concentration of silicon or phosphorus in the sample. Our experiment
were conducted to measure the silicon, our results were (4 ± 0.1) × 105
mg/g, which is more than twice the reference data refers to
(1.8−0.11+0.21) × 105 mg/g.
The flux distribution in the reactor, however, may be affected by
many parameters that change with time, burn-up of fuel, position of
control rods, etc. The reported thermal cross section and integrated
cross section of some reactor averages for the above mentioned reac
tions are mentioned in Table 2 and are based on Watt distribution.
These values are reactor specific, except for thermal cross section,
and need to be determined experimentally for each neutron field. In
order to override this problem, reactor users, routinely, use a
comparator

Table 3

Parameters for the reactions of interest.f( )i is the natural abundances of the target isotope in the element. Thermal neutron cross section data was taken from Refs.
[23]. Eth is the threshold energy for the reaction. The value of ~ (sigma-tiled) represents the integrated cross section over Watt distribution.

Product isotope T1/2 Reactionsf( )i (%) Eth (MeV) Integral Cross section (mb) Thermal cross section (b) [23]

24
Na 14.997h 23Na(n,γ)24Na 100 0 0.528 27Al(n,α)24Na 100 3.25 0.72 ± 0.03 [30]
24
Mg(n,p)24Na 78.99 4.93 1.44 ± 0.10 [30]
28
Al 2.245 min 27Al(n,γ)28Al 100 0.234 28Si(n,p)28Al 92.23 4.0 5.68 ± 0.20 [30]
31
P(n,α)28Al 100 2.01 1.90 ± 0.08[30]
27
Mg 9.458 min 26Mg(n,γ)27Mg 11.1 0 0.038 27Al(n,p)27Mg 100 1.9 3.84 ± 0.20[30]
30
Si(n,α)27Mg 3.09 4.3 0.1350 ± 0.001[30]
31
Si 157.36 min 30Si(n,γ)31Si 3.09 0 0.107 31P(n,p)Si 100 > 1 36.0 ± 10.0[31]
35
S 87.37 d 34S(n,γ)35S 4.21 0 0.224 35Cl(n,p)35S 75.77 ~0 138 [32]
32
P 14.268 d 31P(n,γ)32P 100 0 0.169 32S(n,p)32P 95.02 ~1 101.4 [32]
35
Cl(n,α)32P 75.77 ~0.8 32.8 [32]
 66
A. Ali and E.K. Elmaghraby Nuclear Inst. and Methods in Physics Research B 471 (2020) 63–68
of 27Al(n,γ)28Al, 30Si(n,γ)31Si, 26Mg(n,γ)27Mg, and 23Na(n,γ)24Na reac
samples with known content. The reaction rate for the comparator and tions. It is recommended to perform an elemental analysis of the neu
the sample are determined using the relation: tron activated sample before performing neutron activation to find out
the possibility of interfering reaction in the results.

= R
()() T (C)
R
I e e e 1 1 . ii i 24
(C or S) ()
Na
iittt()
iiicim = + + f N f N f N 23 23 24 24 27 ( ) ( ) ( ( , )) ( ) ( ) ( ( , )) ( ) ( )

Here,R( )i(C or S)is the reaction rate for production of isotope (i), where Na
Na
th Na n Mg
Mg
o Mg n p Al
Al
o
(C) refers to measurement in the comparator and (S) refers to
27
measurement of the sample. i is the decay constant of the isotope (i),Ii ( ( , ))
Al n
is the in tensity of the measured gamma line and i is its absolute
efficiency. The value ofR( )i(C)is the summation of the interfering (C)
reaction rates as follow Declaration of Competing Interest
the same concentration of interfering isotopes, which is a challenging
task. Any use of comparator material to assess sample having The authors declare that they have no known competing financial
unknown concentration of silicon and aluminium may lead to specious
interests or personal relationships that could have appeared to influ
results due to the contribution of 28Si(n,p)28Al, 31P(n,α)28Al, 31P(n,p)31Si ence the work reported in this paper.
30
Si (n,α)27Mg, 24
Mg(n,p)24Na and 27
Al(n,α)24Na reactions to the yield
Si
o 27 26 26 27 27 30
R f N = Al Al Al th Al n ( )
28 ( ) 27 27
() ( ( , ))
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