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I NSTITUT S UPÉRIEUR

I NDUSTRIEL DE B RUXELLES
R UE R OYALE 150, 1000 B RUXELLES (B ELGIUM )

Physics laboratory
Quantitative determination of copper
in a coin by neutron activation

Students
Evan P OKET Supervising teacher
Dr. Eng. Isabelle G ERARDY
(58024@etu.he2b.be)
Sabri M ANAÏ
(58305@etu.he2b.be)

academic year 2022 - 2023


Contents

1 Introduction 1

2 Theoretical fundations 2
2.1 Reminder about the units [3] . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.2 Gamma transition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.3 Activation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.4 Gamma rays detection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

3 Modus operandi 5

4 Physical Analysis [7] 6

5 Measurements and analysis 7


22
5.1 Calibration with 11 Na . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
5.2 Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
5.2.1 Standard and sample . . . . . . . . . . . . . . . . . . . . . . . . . . 8
5.3 Verification of the absence of unstable copper after 15 minutes . . . . . . 9
5.4 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
5.4.1 Uncertainties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
5.4.2 Determination of the percentage of copper present in the sample 10

6 Conclusion 10

7 Bibliography 11

8 Appendix 12
22
8.1 Characteristics of the 11 Na source . . . . . . . . . . . . . . . . . . . . . . . 12

i
Abstract

This work focusses on the determination of a certain element in a sample, in


this case, a copper coin, by neutron activation. The sent neutrons react with the
sample and make the copper unstable, leading to an emission of gamma particles
allowing to determine the proportions of copper isotopes in the coin. After the
calibration of the detector with a 22 Na source and the analysis of a pure copper
standard of equivalent size to the sample, it is demonstrated that, based on the
activities of the sample and the standard as well as the mass of the latter, it is
possible to determine the mass, and therefore the percentage of copper in the coin.

1 Introduction
Neutron activation is an analytical technique that allows the qualitative and quantita-
tive determination of elements based on the measurement of gamma radiations emit-
ted during the decay of radioactive nuclei. Those are formed by neutron irradiation of
a material, such as a copper coin. Samples that are suitable for this analysis method
can come from various fields such as medicine, biology but also mineral detection and
environment [1].
Although neutron activation analysis can be done in several ways, most of the meth-
ods used are based on the detection of gamma rays emitted by the irradiated material.
In addition, these methods are mainly non-destructive as they do not require sample
reduction and can be performed on very small amounts of sample material. It is also
one of the most widely used applications of the decay of radioactive nuclei measure.
To date, neutron activation analysis is mainly used for specific cases, such as verifying
results obtained by other faster methods that are not as reliable. However, one of the
main disadvantages is the response time that some radioisotopes can have, sometimes
slowing down the process to several days [2].

1
2 Theoretical fundations

2.1 Reminder about the units [3]


It is good to specify/remind the nature of the different units inherent to the present
manipulation, in order to ensure a good understanding of the subject.

1. 1 Becquerel ( Bq) = 1 desintegration/s ; characterizes the activity of the source.

2. 1 Curie (Ci ) = 3, 7.1010 Bq ; Older activity unit still often used in source data
sheets.

3. 1 electronvolt (eV ) = energy acquired by an electron subjected to a potential


difference of 1 V or 1, 6.1019 J ; Measurement of the energy of radiation.

2.2 Gamma transition


The present manipulation is based on the emission of gamma particles. This emission
differs from alpha and beta radiation in that no particles are ejected from the nucleus
when it undergoes this type of decay. Gamma rays are highly ionizing photons and, as
such, have no associated mass or charge. This is why gamma rays do not change the
structure or the composition of the atom in presence. Gamma radioactivity is caused
by the excitation of a proton or neutron in the atom, which attempts to return to a more
stable state. In the same way as in the excitation of an electron, this return to stability
is done by energy emission, in this case by means of a gamma photon. The return of
an excited nucleus to stability is done according to the following equation :

A∗ → A + γ (1)
Where A∗ is the nucleus in an excited state, A is the nucleus in a stable state and γ is
the emitted gamma particle.

As in the case of electron excitation, it is also possible to determine the frequency of the
emitted radiation (corresponding to the energy carried by the gamma photon) based
on the initial and final states of the nucleon considered, as shown in equation (4):

Ei − E f = h. f (2)
Where Ei is the initial state of the nucleon, E f is the final, h the planck constant and f
the frequency of the emitted radiation [4].

2
2.3 Activation
As mentioned in the introduction, activation in this laboratory is called "neutron ac-
tivation". Target atoms are bombarded with so-called slow neutrons. Basically, thos
are free neutrons (not bound to an atomic nucleus) whose average kinetic energy cor-
respond to the average energy of the surrounding particle. A thermal neutron has a
large fission cross section, which means that they are often useful in chain reaction
applications, such as our case or even in nuclear fission [5].
As shown in the figure 1, thermal neutrons are produced by slowing down the more
energetic neutrons (resulting from nuclear fission in the figure 1) in a substance called
a moderator (such as water or graphite) after they have been ejected from atomic nu-
clei.

Figure 1: Slow neutron formation in a thermal reactor [6]

In this case, the reaction that allows the ejection of these neutrons is performed by a
neutron source Am − Be. The latter is shown in the equation below.

9
Be + α →12 C + nth (3)
Where the α particles come from the decay of americium present in the source.

Both the sample and the pure copper standard are composed of 2 main copper iso-
topes, namely 63 Cu and 65 Cu. These react with the thermal neutrons they encounter
and form the following activation products:

63
Cu + nth →64 Cu ( β/γ) (4)
65
Cu + nth →66 Cu ( β/γ) (5)

3
These two activation products are, as seen in equations (4) and (5), Beta and Gamma
emitters with respective half-lives of 12.7 hours and 5.1 minutes [3]. In this manip-
ulation, only the gamma rays will be detectable, since, the coins being placed in the
multi-channel analyser’s container (figure 2), the beta rays do not pass the thickness
of the container.

Figure 2: Container where the sample to be analyzed is placed

2.4 Gamma rays detection


The detection of gamma rays emitted by the unstable sample (or standard) is done by
means of a hit detector, connected to a counting chain. This one is presented as follows
on the figure 3.

Figure 3: Counting chain and multi-channel detector [3]

1. Sensor / detector : Material called scintillator capable of emitting photons under


the influence of received radiation. These same photons are collected by a photo-
cathode which emits electrons amplified by a pair of electrodes undergoing a
potential difference (High Voltage HV).

2. (Pre)amplifier : Allow the amplification of the received pulse through the col-
lected electrons. The energy of the radiation causing the scintillation is propor-
tional to the amplitude of this pulse.

4
3. Multi-Channel Analyzer : Classifies the pulses according to their amplitudes (ac-
cording to the energy of the radiation perceived by the detector). The memory
of the analyzer is divided into 512 channels (in this case) whose counter is in-
cremented by 1 for each pulse perceived within the limits of amplitude. The
computer interface allows to observe the evolution of the detection in real time
for each channel.

3 Modus operandi
The different steps to go through in order to perform this manipulation are listed
chronologically below.

1. Place the standard and sample (successively) for 25 minutes in the irradiator to
obtain the maximum activity of 66 Cu.

2. Energy calibration of the detector (meanwhile step one) using the source of 22 Na.
It is therefore necessary to establish a relationship between the channel of the
peak and the energy of the corresponding radiation.

3. Perform an acquisition of the sample, then observe and identify the peaks ob-
tained.

4. In order to allow the determination of copper in the sample, make a region of


interest (ROI) around the copper peak and take the area in number of shots.

5. Repeat an acquisition 10 minutes later, the half-life of 66 Cu being 5.1 minutes,


this new measurement allows to validate that there is no more unstable 66 Cu in
the sample.

6. Perform an acquisition with the standard and take the value of the region of
interest.

7. Compare the results obtained for the sample and the standard and determine the
mass of copper present in the sample thanks to the equation (10).

5
4 Physical Analysis [7]
We know that the activity (number of radioactive atoms that decay per unit time) is
proportional to the number of atoms Nat that decay, to the X-ray flux passing through
the element ϕRX and the cross section σact which is equivalent to the probability of
interaction of a particle as shown on the equation (6):

A ∝ Nat .ϕRX .σact (6)

This equation for the pure copper standard is:

Astd ∝ Nat std .ϕRX .σact (7)

And for the sample of the 50 cents coin:

Asam ∝ Nat sam .ϕRX .σact (8)

If we consider that the sample and the standard are of the same dimensions, then
the X-ray flux will be the same since it is defined as being a physical property pass-
ing through a surface. The cross sections are also identical. Indeed, given that their
surfaces are equal, the probabilities of interaction are equivalent. So if we split the
equation (8) by the equation (7), we arrive at the following relationship :

Asam Nat sam


= (9)
Astd Nat std

Proportionality turned into equality by removing the terms ϕRX .σact which cancel each
other out. Moreover, the number of atoms testifies to a quantity in the same way as
the mass. Since we have a division, the ratio remains the same and, the standard being
hypothetically composed of 100% copper, there is only one unknown left:

Asam M
= Cu sam (10)
Astd MCu std

6
5 Measurements and analysis

5.1 Calibration with 22


11 Na

The computer interface of the detector is presented as a graph divided into a certain
number of channels, 1024 in this case, as well as a number of measured hits associated
with each of them. Initially, the channels are numbered in order and it is therefore very
difficult to draw conclusions as to the presence of a certain element based solely on the
number of measured hits. However, by using a source whose γ emission energy values
are known, the detector can be calibrated so that each channel corresponds to a specific
energy. After the analysis of the unknown sample, it is then possible, by searching the
theoretical tables, to determine to which element the characteristic energies mesured
correspond. The approach for the calibration (with a 2211 Na source whose characteristics
are given in section 8, table 2) is the following:

1. Place the 22
11 Na source in the detector container and start the acquisition

2. Note the different energies associated with the peaks obtained and the corre-
sponding channels.

3. Enter the values in the program to perform an energy calibration

4. Check the accuracy of the calibration by analyzing another sample with known
characteristic energies, such as pure copper in our case.

It is possible to plot the calibration line associating each channel with the measured
energy as seen in figure 4, we then obtain the equation that links the two values :

Figure 4: Calibration line with 22


11 Na

7
5.2 Measurements
Before moving on to the actual measurements, it is necessary to specify that the uncer-
tainties inherent in the manipulation are given by the program used, namely "Génie2000".
This program consists of a complete environment for the acquisition, display and anal-
ysis of gamma and alpha spectrometry data.

5.2.1 Standard and sample

The first acquisition was done on the pure copper standard, with a mass of 10, 590 ±
0, 006 g. The results obtained are unequivocal and show the presence of copper. By
examining the regions of interest around the characteristic peaks, it is possible to de-
termine the activity of the standard. Figure 5 shows the results of the acquisition as
well as the regions of interest present around the major peak.

Figure 5: Acquisition by γ spectrometry for the standard

The second one was made on the coin of unknown copper mass for a total mass of
7, 790 ± 0, 006 g. The graph of the acquisition as well as the region of interest around
the copper peak are shown in figure 6.

Figure 6: Acquisition by γ spectrometry for the sample

8
Only the second respective peaks of the two acquisitions were retained, since they
are those to which are associated the characteristic energy of copper. The results and
characteristics of the curves (net area, energy and uncertainty) are shown in the table
1 below.

Table 1: Acquisition results for the sample and the standard

5.3 Verification of the absence of unstable copper after 15 minutes


As explained in the procedure, it is possible to verify the absence of 66 Cu in the sample
by launching an acquisition far enough away from the first one. Indeed, the half-life
time of this 66 Cu is 5.1 minutes and, after a quarter of an hour, the acquisition should
return 0 Hits for the characteristic energy slice of the 66 Cu.
The spectrum obtained for this verification analysis is shown in Figure 7 below:

Figure 7: Spectrum of the sample 15 minutes after its activation by slow neutrons

For the same characteristic channels as those used in the previous acquisitions, the area
under the curve calculated is unequivocal, its value is 17 strokes which corresponds to
the background noise inherent in the manipulation.

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5.4 Results
5.4.1 Uncertainties

During the manipulation, several errors coming from different quantities implemented
in the calculations were identified. An uncertainty is linked to the balance measuring
the mass. These uncertainties are present intrinsically to the element, they are type B
(UB ). Thus the relation (11) will be applied by taking as k, a value of 2 for a confidence
level of 95%. While the resolution ∆r of the scale is 0.01 g :
∆r 10−2
UB = k √ ⇒ UB = 2 √ = 0, 006 g (11)
12 12
Again, it is important to remember that, as explained in section 5.2, the other poten-
tial uncertainties inherent in the manipulation are directly provided by the computer
which calculates them automatically.

5.4.2 Determination of the percentage of copper present in the sample

Based on Table 1 showing the acquisition results, and by isolating MCu sam in formula
8 demonstrated in section 4, the following result emerges in equation (12) aswell as in
equation (13) for the percentage value of copper in the coin:
Asam 879
MCu sam = .MCu std = .10, 590 = 6, 860 g (12)
Astd 1356
MCu sam 6, 860
Copper percentage = .100 = .100 = 88, 12% (13)
Msam 7, 790

6 Conclusion
In conclusion, neutron activation is a powerful analytical method that allows the qual-
itative and quantitative determination of the composition of a sample in its entirety
(and not just on the surface). In the present case, this activation was carried out using
an americium berilium source and the subsequent analysis was done using a scintilla-
tor connected to a computer managed by the program Génie200. The results obtained
show a composition equal to 88.12%, which is exact in view of the theoretical average
value of copper composition of a 50 cents coin which is 89%. The notable variation of
the results between this method of analysis (88,12%) and the X-ray fluorescence (95%)
is explicable by the physical properties on which the two analyses rely.
Indeed, X-ray fluorescence only allows a surface analysis, X-rays not having a suffi-
ciently high penetrating power to allow an in-depth analysis of the sample. Neutron
activation, on the other hand, allows an analysis of the sample in its entirety, since it is
based on the emission of gamma particles, which can pass through the sample.

10
7 Bibliography
Resources:

[1] IAEA - International Atomic Energy Agency, Neutron activation analysis,


<online on 20/04/23>,
Available on : https://www.iaea.org/topics/neutron-activation-analysis

[2] Voix du nucléaire, L’analyse par activation neutronique,


<Online on 20/04/23>, Published on 04/03/2022,
Available on : https://www.voix-du-nucleaire.org/lanalyse-par-activation-neutronique/

[3] Dr. Eng. GERARDY Isabelle, Syllabus de laboratoire de physique nucléaire,


ISIB - Institut Supérieur Industriel de Bruxelles HE2B, 2022-2023

[4] Encyclopédie énergie, Désintégration gamma,


<Online on 27/04/23>, Review dated 11/08/22 at 18:00 by Jmdonev ,
Available on : https://energyeducation.ca/Encyclopedie_Energie/index.php?title=D%
C3%A9sint%C3%A9gration_gamma&oldid=1116

[5] GAUR Aakansha, Encyclopaedia Britannica, Thermal Neutrons,


<Online on 22/04/23>, Reviewed on 05/11/18 by the author,
Available on : https://www.britannica.com/science/thermal-neutron/additional-
info#history

[6] NUPEX - Nuclear Physics Experience, Modérateurs,


<Online on 22/04/23>,
Available on : http://nupex.eu/index.php?g=textcontent/nuclearenergy/
nuclearreactors&lang=fr

[7] Dr. Eng. GERARDY Isabelle, Oral course dated 19/04/23 at 150, Rue Royale 1000
Brussels, Nuclear Physics Laboratory

11
8 Appendix

8.1 Characteristics of the 22


11 Na source

Source T1/2 [Years] Emitter E [keV]


22 Na
11 2,60 β+ , γ 511,00 & 1274,50

Table 2: Characteristics of the 22 Na source (T1/2 , emitter type and emission energy
11
theoretical value)

12

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