Radioactive and Chemical Pollution Evaluation in Coastal Sea

Sediments

FRANCESCO CARIDI1, GIUSEPPE PALADINI2, ALBERTO BELVEDERE3,

MAURIZIO D’AGOSTINO3, SANTINA MARGUCCIO3, MAURIZIO MESSINA3,

GIOVANNA BELMUSTO3, GIOVANNA STILO4, VALENTINA VENUTI1,

DOMENICO MAJOLINO1

1Department of Mathematical and Computer Sciences, Physical Sciences and Earth Sciences,

University of Messina,

V. le F. Stagno D’Alcontres, 31-98166 Messina,

ITALY

2Department of Physics and Astronomy “Ettore Majorana”, University of Catania,

Via S. Sofia, 64-95123 Catania,

ITALY

3Department of Reggio Calabria,

Regional Agency for Environmental Protection of Calabria (ARPACal),

Dipartimento di Reggio Calabria, Via Troncovito SNC, 89135 Reggio Calabria,

ITALY

4Department of Medical and Surgical Sciences and Advanced Technologies “GF Ingrassia” ENT

Section, University of Catania,

95123 Catania,

ITALY

Abstract: - In this article, coastal sea sediments from three different selected sites of Reggio Calabria and Vibo

Valentia districts, Calabria region, Southern Italy, were picked up to quantify natural and anthropogenic

radioactivity content and metal concentrations. The aim was to assess any possible radiological health hazard

for human beings due to external exposure to gamma rays, as well as the level of pollution due to anthropic

radionuclides and metals in the investigated area. To this purpose, High Purity Germanium (HPGe) gamma

spectrometry was employed to quantify specific activities of 226Ra, 232Th, 40K, and 137Cs radioisotopes. The

absorbed gamma dose rate in air (D), the annual effective dose equivalent (AEDE) outdoors, the external hazard

index (Hex) and the excess lifetime cancer risk (ELCR) were also estimated to assess any possible radiological

health risk for the population, mainly due to the use of coastal sea sediments for the beach nourishment.

Moreover, Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were carried out for the

quantitative elemental analysis of the samples, to assess any possible chemical pollution by metals, that could

be released into the environment by both natural and anthropogenic sources, through a comparison with the

limits set by the Italian Legislation. Finally, the results reported in this paper can be used as a baseline for

future investigations concerning a more complete mapping of the radioactivity levels in coastal sea sediments.

Key-Words: - Coastal sea sediments, radioactivity, radiological risk, metals, chemical pollution, High Purity

Germanium (HPGe) gamma spectrometry, Inductively Coupled Plasma Mass Spectrometry (ICP-

MS).

Received: April 12, 2023. Revised: September 11, 2023. Accepted: November 5, 2023. Published: December 6, 2023.

1 Introduction

Naturally occurring radioisotopes from the Earth's

crust and cosmic radiation, as well as artificially

produced radionuclides from nuclear weapons

experiments and nuclear facility failures, are a

permanent environmental occurrence and constitute

notable sources of radiation exposure for human

beings, [1], [2], [3], [4], [5]. In particular, natural

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Francesco Caridi,

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radionuclides are uranium (238U and 235U) and

thorium (232Th) decay chain products and 40K,

primordial and with variable concentrations based

on local geological landforms, [6]. Their

significance resides in the fact that they account for

more than half of the radioactive exposure to which

the population is subjected, [7], [8]. Besides these

natural radionuclides, man-made ones such as 137Cs,

being released into the environment by different

anthropogenic practices and being deposited in soils

as fallout, also play a significant role in radiation

exposure, [9], [10]. Hence, the knowledge of natural

and anthropogenic radionuclides-specific activity in

environmental matrices is important for establishing

background levels of radiation and assessing the

effects of radioactive exposure for humans, [11],

[12].

In sediments, naturally occurring radioisotopes

mainly tend to be accumulated by weathering,

erosion, and depositional processes of different

geological materials, exhibiting concentrations

generally growing as grain size becomes smaller,

[13], [14]. The investigation of natural radioactivity

in coastal sea sediments may give valuable

information on the source and fate of radionuclides

in aquatic habitats, helping to establish their

distribution and the potential risk to public health

from radio contamination of rivers and coastline

areas and the use of sea sediments for nourishment

of beaches, [15], [16].

Going on, the unregulated urban development

surrounding many towns and coastal areas has led to

an increasing level of pollutants that have

contaminated these aquatic habitats to an alarming

degree. Among them, metals are of the greatest

concern because of their long-lasting and bio-

accumulative character, [17], [18], [19], [20]. They

can be delivered to the aquatic environment and

accumulated in sediments through the disposal of

liquid effluents, chemical leachates, and runoff from

residential, manufacturing, and farming activities,

and also through atmospheric deposition, [21], [22].

These metals can be leached from sediments to

overlying waters through either natural or man-

made processes, resulting in a potential hazard to

ecosystems, [23].

In this article, coastal sea sediments from three

different selected sites of Reggio Calabria and Vibo

Valentia districts, Calabria region, Southern Italy,

were analyzed to quantify natural (226Ra, 232Th and

40K) and artificial (137Cs) gamma-emitting

radionuclides, by using High Purity Germanium

(HPGe) gamma spectrometry, to record

radioactivity background levels and to check for any

possible anthropic radionuclides’ pollution, [24].

Moreover, Inductively-Coupled Plasma Mass

Spectrometry (ICP-MS) was employed for the

quantitative analysis of metals, to evaluate any

possible chemical pollution through a comparison

with the limits set by the Italian Legislation, [25].

2 Materials and Methods

2.1 Samples Collection and Preparation

Five samples of coastal sea sediments, around 1 kg

everyone, were collected for each of the three

selected locations (Figure 1), at a depth of 8-10 m.

In detail, the GPS coordinates of the sampling

points are 38°28’28.3” N and 15°54’32.7” E for

ID1, 38°30’27.3” N and 15°55’04.73” E for ID2,

38°32’25.9” N and 15°55’50.4” E for ID3,

respectively. Sampling was performed according to

the following process: the sampler was cocked and

depressed at a steady speed to enable it to contact

the seabed in the proper position. Upon contact with

the seabed, the operator scored the GPS coordinates

and recovered the sampling instrument. As soon as

the sampler touched the surface, it was rapidly

retrieved to prevent any stresses that would alter its

content, externally rinsed to ensure no

contamination, and its content was drained into a

tank and stored in well-sealed and labeled 1 L

acidified polyethylene containers to prevent

radionuclide precipitation and absorption on the

container sides.

In the laboratory, all sediments were oven-dried

at 105° C, sieved to a particle size of less than 2

mm, and placed into 1 L capacity Marinelli airtight

containers. After 40 days, secular radioactive

equilibrium was reached between 226Ra and its

daughter products, and sediments were ready to be

analyzed by High Purity Germanium (HPGe)

gamma spectrometry, [26].

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Fig. 1: Location of the sampling sites, in Reggio

Calabria (ID1 and ID2) and Vibo Valentia (ID3)

districts

2.2 HPGe Gamma Spectrometry

Measurements

For the HPGe gamma spectrometry analysis, coastal

sea sediments were counted for 70000 seconds, to

reduce the statistical uncertainty, and spectra were

analyzed to obtain the activity concentrations of

226Ra (by using the 295.21 keV and 351.92 keV

214Pb and 1120.29 keV 214Bi gamma-ray lines), 232Th

(by using the 911.21 keV and 968.97 keV 228Ac γ-

ray lines), 40K (through its gamma-line at 1460.8

keV) and 137Cs (through its gamma-line at 661.66

keV), [27].

The experimental set-up was a positively biased

detector (GEM), with FWHM of 1.85 keV, peak-to-

Compton ratio of 64:1, and relative efficiency of 40

% at 1.33 MeV (60Co), placed inside lead wells to

shield the background radiation environment. It is

worth noting that, for the sample holder geometry of

1 L, efficiency and energy calibrations were carried

out with a multipeak Marinelli geometry gamma

source (AK-5901) of 1 L capacity, covering the

energy range 60-1836 keV, customized to reproduce

the exact geometries of samples in a water-

equivalent epoxy resin matrix. The Gamma Vision

software was used for data acquisition and analysis,

[28].

The specific activity (Bq kg-1 dry weight, d.w.)

of the detected radionuclides was given by, [29]:

𝐶 = 𝑁𝐸

𝜀𝐸𝑡𝛾𝑑𝑀 (1)

where NE indicates the net area of a peak at energy

E, εE and γd is the efficiency and yield of the

photopeak at energy E, respectively, M is the mass

of the sample (kg) and t is the live time (s), [30].

The quality of the gamma spectrometry

experimental results was certified by the Italian

Accreditation Body (ACCREDIA), [31].

2.3 ICP-MS Measurements

The concentration of As, Cd, Cu, Hg, Ni, Pb, Sb, Tl,

Zn, and Crtot was obtained through ICP-MS analysis

using a Thermo Scientific iCAP Qc ICP-MS.

Particles with a size smaller than 2 mm, previously

served, were further minced at a size of about 100

µm through an agate ball mill. After, a quantity of

0.5 g of this sample, together with 9 mL of ultrapure

(67-69%) HNO3 and 3 mL of ultrapure (32-35%)

HCl were directly introduced into a 100 mL TFM

vessel. Acid digestion was performed using a CEM

microwave unit system, Mars 6 touch control, in one

step, at 1000 W and 175 ºC, with a maintenance

time of 4 minutes and 30 seconds, followed by a 20-

minute cooling, [32]. After cooling, vessel contents

were filtered and filled up to 50 mL with distilled

H2O. The final sample was then diluted at a

concentration of one order of magnitude lower than

the initial value.

The sample introduction system consisted of a

Peltier cooled (3 ˚C), baffled cyclonic spray

chamber, PFA nebulizer, and quartz torch with a 2.5

mm i.d. removable quartz injector. The instrument

was operated in a single collision cell mode, with

kinetic energy discrimination (KED), using pure He

as the collision gas. All samples were presented for

analysis using a Cetac ASX-520. The iCAP Qc ICP-

MS was operated in a single KED mode using the

following parameters: 1550 W forward power; 0.98

L/min nebulizer gas; 0.8 L/min auxiliary gas; 14.0

L/min cool gas flow; 4.5 mL/min collision cell gas

He; 45 s each for sample uptake/wash time;

optimized dwell times per analyte (0.1 s, except 0.5

s for As, Hg, Cr and Se); one point per peak and

three repeats per sample.

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2.4 Evaluation of Radiological Hazard

Effects

Radiological parameters, such as the absorbed

gamma dose rate in the air (D), the annual effective

dose equivalent (AEDE) outdoors, the external

hazard index (Hex) and the excess lifetime cancer

risk (ELCR), were estimated to assess any potential

radiological health risk to humans, [33], [34].

In particular, the absorbed dose rate calculation

is the first major step to evaluating the health risk,

[35]:

D (nGy h-1) = 0.462CRa + 0.604CTh + 0.0417CK (2)

where CRa, CTh, and CK are the specific activities, in

Bq kg-1 d.w., of 226Ra, 232Th, and 40K, respectively.

Going on, the annual effective dose equivalent,

received by an individual, is given by, [36]:

AEDEout (mSv y-1) = D (nGy h-1) · 8760 h · 0.7 Sv

Gy-1 · 0.2 · 10-6

(3)

where 0.2 is an outdoor occupancy factor and 0.7 Sv

Gy-1 is the conversion coefficient from the absorbed

dose to the effective dose received, [37].

Moreover, the external radiation hazard index,

to set the radiation dose to a value lower than 1 mSv

y-1 was defined, [38]:

Hex = (CRa/370 + CTh/259 + CK/4810) ≤ 1 (4)

Finally, the excess lifetime cancer risk index

gives the probability of cancer development during

a lifetime at a certain amount of exposure. It

accounts for the number of extra cancers that are

expected in a defined population as a result of

exposure to a carcinogen at a particular dose, [38]:

ELCR = AEDEout · DL · RF (5)

where DL is the mean human life duration (estimated

to be 70 years) and RF the risk factor (Sv−1), i.e. fatal

cancer risk per Sievert, equal to 0.05 for the public

according to the International Commission on

Radiological Protection (ICRP) recommendation,

[39].

3 Results and Discussion

3.1 Radioactivity Analysis and Radiological

Hazard Effects Assessment

The average activity concentrations of detected

radionuclides, 226Ra, 232Th, 40K, and 137Cs, in the

investigated samples, are reported in Table 1 for

each sampling site.

Table 1. The average activity concentrations CRa,

CTh, CK, and CCs (average value ± standard

deviation) of, respectively, 226Ra, 232Th, 40K, and

137Cs, were evaluated for each sampling site.

CRa

(Bq kg-1

d.w.)

CTh

(Bq kg-1

d.w.)

(Bq kg-1

d.w.)

CCs

(Bq kg-1

d.w.)

(19.6 ± 2.7)

(32.3 ± 4.9)

(800 ± 112)

< 0.2

(13.5 ± 2.2)

(23.4 ± 2.9)

(543 ± 81)

< 0.1

(13.2 ± 2.1)

(24.3 ± 3.1)

(825 ± 91)

< 0.1

The observed variability, location by location,

can be due to the large changes in chemical and

mineralogical properties and rare-earth elements of

the marine backdrop, [40].

As far as natural radionuclides are concerned,

the 40K specific activity is more than one order of

magnitude greater than that of 226Ra and 232Th

radionuclides, as usually occurs in soil samples. In

detail, the specific activities range from (13.2 ± 2.1)

Bq kg-1 d.w. to (19.6 ± 2.7) Bq kg-1 d.w., from (23.4

± 2.9) Bq kg-1 d.w. to (32.3 ± 4.9) Bq kg-1 d.w. and

from (543 ± 81) Bq kg-1 d.w. to (825 ± 91) Bq kg-1

d.w. for 226Ra, 232Th, 40K, respectively. It is worth

noting that the highest specific activity of 226Ra and

232Th were found in site ID1, while 40K was in site

ID3.

Furthermore, taking into account that worldwide

average concentrations of 226Ra, 232Th, and 40K in

soils, as reported by [31], are 35 Bq kg-1 d.w., 30 Bq

kg-1 d.w. and 400 Bq kg-1 d.w., respectively, we can

notice that, in our case, the specific activity

concentration is lower than the average world value

in all cases for 226Ra. Moreover, it is higher than the

mean worldwide value only for site ID1 for 232Th,

while it is higher than the worldwide one in all cases

for 40K. These results are strictly related to the

mineralogical composition of the coastal sea

sediments themselves, as widely reported in the

literature, [41], [42], [43], [44].

Regarding anthropogenic radioactivity content,

we notice that the activity concentration of 137Cs is

lower than the minimum detectable activity value in

all cases, excluding radioactive contamination of

anthropic origin for the investigated samples.

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Going on, radiological hazard indices are reported in

Table 2 for all the investigated sampling sites.

Table 2. Radiological hazard indices for all the

investigated sampling sites.

(nGy h-1)

AEDEout

(µSv y-1)

Hex

ELCR

(x10-3)

61.9

75.9

0.34

0.27

43.0

52.8

0.24

0.18

55.2

67.7

0.30

0.24

In detail, the absorbed dose rate, as evaluated by

using equation (2), is higher than the world average

value (57 nGy h-1), [37], only for site ID1. The

annual effective dose equivalent, received by an

individual and obtained through equation (3), never

exceeds 1 mSv y-1, which is set as the maximum

limit by, [45]. Moreover, the external radiation

hazard index, as resulting from equation (4), is

lower than unity for all investigated samples. Thus,

in light of the aforementioned results, radiological

health risks for the population due to external

exposure to gamma rays, mainly due to the use of

coastal sea sediments for beach nourishment, can be

considered negligible. Finally, excess lifetime

cancer risk values, as obtained by using equation (5)

the AEDEout values calculated by equation (3), are in

very good agreement with the literature, [46], [47],

[48]. It is worth noting that the assessment of the

radiological health hazards for the population only

based on the calculated ELCR is not possible,

because trustworthy and standardized mortality and

morbidity statistics are not affordable.

3.2 Metals Analysis

Table 3. Average contents (mg kg-1 d.w.) of metals

detected in the investigated samples by ICP-MS

analysis, were evaluated for each sampling site. In

the last column, the threshold limit set by the Italian

legislation is reported for comparison.

Table 3 reports the average contents (mg kg-1

d.w.) of metals detected in the investigated samples

by ICP-MS analysis, evaluated for each sampling

site.

It can be noticed that in all cases the

experimental values remain below the

contamination thresholds set by, [49], [50].

Consequently, these metals cannot be treated as

pollutants, they do not cause unpleasant effects

neither compromise the well-being of the

environment nor pose a risk to human health, [51].

4 Conclusion

The specific activity of natural and anthropic

radioisotopes, i.e., 226Ra, 232Th, 40K, and 137Cs, was

quantified through HPGe gamma spectrometry for

coastal sea sediments picked up from different

sampling points of Reggio Calabria and Vibo

Valentia districts, Calabria region, Southern Italy.

Moreover, to assess any possible radiological health

risk for the population, mainly due to the use of

coastal sea sediments for beach nourishment, the

absorbed gamma dose rate in air, the annual

effective dose equivalent outdoors, the external

hazard index, and the excess lifetime cancer risk

were calculated. Obtained results put into evidence

low levels of radioactivity, thus discarding any

significant radiological health risk for the

population.

Going on, the presence of potentially hazardous

elements (such as As, Cd, Cu, Hg, Ni, Pb, Sb, Tl,

Zn, and Crtot) was assessed through ICP-MS

measurements. To estimate the degree of pollution

by these metals, their concentrations were compared

with threshold limits set by the Italian Legislation.

Obtained results indicate that metal concentrations

are much lower than the contamination reference

values, thereby ruling out pollution.

Noteworthy, as a direction for future research,

this study can be used as a baseline for

investigations about radioactivity background levels

in coastal sea sediments of the investigated area.

Furthermore, it should be remarked that the

approach stated in this article might be applied, in

principle, for the assessment of any potential

radiological hazard for human beings due to the

presence of radioactive elements in sediments, by

constituting a guideline for investigations focused

on the monitoring of the radiological and chemical

quality of these samples, with a strong impact on the

real life. No Artificial Intelligence methods can be

applied to this study.

Site ID

Threshold limit

CAs

1.07

1.49

1.21

CCd

< 0.1

0.3

CCu

1.83

2.61

1.93

CHg

< 0.05

0.3

CNi

1.69

2.54

1.33

CPb

2.85

3.01

1.87

CSb

0.09

0.06

0.05

CTl

< 0.1

0.3

CZn

6.93

25.5

33.1

124

CCr-tot

2.61

4.64

2.42

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