Journal of Environmental Radioactivity 189 (2018) 202–206

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Journal of Environmental Radioactivity

journal homepage: www.elsevier.com/locate/jenvrad

Geochemical signature of NORM waste in Brazilian oil and gas industry T

a,∗ a a b
G.T. De-Paula-Costa , I.C. Guerrante , J. Costa-de-Moura , F.C. Amorim
a
Department of Radioactive Waste Management and Transport, Brazilian Nuclear Agency (CNEN - Comissão Nacional de Energia Nuclear), General Severiano Street 82,
22290-901, Rio de Janeiro, RJ, Brazil
b
Department of Mechanical Engineering, Federal Center for Technological Education of Rio de Janeiro, CEFET-RJ, UnED, Itaguaí, RJ, Brazil

A R T I C LE I N FO A B S T R A C T

Keywords: The Brazilian Nuclear Energy Agency (CNEN) is responsible for any radioactive waste storage and disposal in the
Geochemical signature country. The storage of radioactive waste is carried out in the facilities under CNEN regulation and its disposal is
Geochemical fingerprints operated, managed and controlled by the CNEN. Oil NORM (Naturally Occurring Radioactive Materials) in this
Radioactive waste management article refers to waste coming from oil exploitation. Oil NORM has called much attention during the last decades,
Oil NORM
mostly because it is not possible to determine its primary source due to the actual absence of a regulatory control
TENORM
mechanism. There is no efficient regulatory tool which allows determining the origin of such NORM wastes even
among those facilities under regulatory control. This fact may encourage non-authorized radioactive material
transportation, smuggling and terrorism. The aim of this project is to provide a geochemical signature for oil
NORM waste using its naturally occurring isotopic composition to identify its origin. The here proposed method
is the modeling of radioisotopes normally present in oil pipe contamination such as 228Ac, 214Bi and 214Pb
analyzed by gamma spectrometry. The specific activities of elements from different decay series are plotted in a
scatter diagram. This method was successfully tested with gamma spectrometry analyses of oil sludge NORM
samples from four different sources obtained from Petrobras reports for the Campos Basin/Brazil.

1. Introduction
Among other nuclear and radioactive subjects, the Brazilian Nuclear
Energy Agency (CNEN) controls the storage and transportation of
radioactive waste. Naturally Occurring Radioactive Material (NORM)
from oil exploration has been an issue along the last decades. Gas and
oil exploration processes produce waste contaminated with NORM. The
main concern with such NORM occurrences is the difficulty to de-
termine the primary source of such waste, especially, in the absence of
regulatory control. Such oil NORM occurs by precipitation or in-
corporation of these materials in the oil sludge, pipe cleaning, in scales
inside pipes, vessels, heat exchanger, pieces of pumps, and others (Afifi
and Awwad, 2005).
One of the main responsibilities of the CNEN as the official ruler is
to develop efficient tools to control the radioactive waste in the
country. Due to the dynamics and versatilities of gas and oil production
as well as the amount of oil productive wells, it is hard to determine the
origin of the many so-called NORM wastes produced by such facilities.
Regarding this, the CNEN-8.01 act regulates as follows (CNEN, 2004):
Art. 42 All facilities must keep an updated record system of the radio-
active waste, including:
I – The radioactive waste type identification, origin and the location of its
container;
II – The radioactive waste origin and destination.
Concerning waste management of oil production, “the hazardous
characteristics of such waste depend on the type of oil produced” (Cunha,
2009). Thus, origin and provenance of oil wastes are extremely im-
portant subjects in determining the risk levels for the environment and
the people.
Nowadays, there is already a serious regulatory control issue re-
garding metal scraps containing NORM. These scraps are sold by oil
producers to scrap-dealers who resell the scrap to the steel industry.
The steel industry has installed radiation detectors at the entrance ac-
cess of their plants. Because of this the CNEN is constantly requested to
verify and investigate warnings about the presence of radioactivity in
steel oil tubes. In most of the cases it is impossible to identify the pri-
mary source of these scrap tubes contaminated with NORM and thus the
effective control and notification of the primary seller cannot be done.
The goal of this project is to develop a geochemical signature for
each specific NORM waste enabling to identify the radioactive waste
source using its naturally occurring radiochemical components and
support the CNEN in its activities of regulation. This article presents a

∗
Corresponding author.
E-mail addresses: gilberto.costa@cnen.gov.br, gilbertothiago2000@gmail.com, gilbertothiago@id.uff.br (G.T. De-Paula-Costa).

https://doi.org/10.1016/j.jenvrad.2018.04.014
Received 8 November 2017; Received in revised form 12 February 2018; Accepted 16 April 2018
Available online 23 April 2018
0265-931X/ © 2018 Elsevier Ltd. All rights reserved.
G.T. De-Paula-Costa et al. Journal of Environmental Radioactivity 189 (2018) 202–206

Table 1 of columbite-tantalite (coltan) ores in Brazil. It was found out by

2014 and 2015 oil and natural gas volume production and proved reservoirs modeling the relations (Nb/Ta; U/Th) that such elemental ratios pro-
(CIPEG, 2016). vide fingerprints of the original source location of such ore. This result
2014 helps and allows the CNEN to improve the control of the economical
circulation of those ores in the country.
OIL in millions of offshore onshore Total Graupner et al. (2010) and Melcher et al. (2015), following an UN
barrels (MMbbl) Production 761.35 61.58 822.93
request to create a way to avoid the commerce of what is called “blood-
Proved 15,350.06 832.22 16,182.29
reservoirs coltan”, described geochemical signatures for coltan (columbite group
NATURAL GAS in offshore onshore Total minerals) ore mined in Africa. Combining U-Pb mass relations with
millions of cubic Production 23.,39 8.50 31.90 associated rare earth elements (REE), geochronological data, REE ra-
meter (MMm3) Proved 399,920.02 71,228.17 471,148.19
tios, and mineralogy they obtained individual signatures for coltan ore
reservoirs
2015
in Africa.
OIL in millions of offshore onshore Total Balboni et al. (2016) presented a methodology for geochemical
barrels (MMbbl) Production 831.30 58.37 889.67 signatures of uranium ores demonstrating the importance of geo-
Proved 12,366.90 666.34 13,033.70 chemical signatures in the investigation on the origin of intercepted
reserssvoirs
nuclear material, both in local community or cross-border transport.
NATURAL GAS in offshore onshore total
millions of cubic Production 26.74 8.39 35.13 This study provided a detailed chemical characterization of 11 samples
meter (MMm3) Proved 358,702.31 70,754.75 429,457.10 of USA uranium ore. The authors plotted Th versus Y and U versus Th
reservoirs contents and the total REE concentration normalized to chondrite REE
standards demonstrating that these chemical indicators can be used to
distinguish depositional areas. The results showed the necessity of
study on the project's viability based on literature data. combining multiple chemical features to determine the origin of ur-
anium ore.
2. NORM in oil industry El Mamoney and Khater (2004) applied a relation between 226Ra
and 228Ra to determine the highest radiological impact zones involving
2.1. Location of oil wells in Brazil oil industry and its waste of the Red Sea region, Egypt. The authors
indicated the regions where radiological impacts would be bigger in
Brazil is the world's 12th largest oil producer (CIPEG, 2016). Bra- case of accidents involving NORM waste coming from oil facilities in
zilian production fields comprise onshore and offshore oil and gas wells this region.
spread out in all country territory. The biggest volumes are produced Yet, there is no methodology available in the literature for the de-
offshore. Table 1 shows the volume of oil and gas produced in 2014 and termination of geochemical signatures in oil NORM waste. However,
2015. 93% of the oil and 76% of the gas produced in the country came Shawky et al. (2001), in their work about oil NORM waste character-
from offshore plants. Besides that, pre-salt production represented 40% ization in the oil industry in Egypt, concluded that each oil formation
of offshore oil production in 2016. In addition, it is expected that many will produce distinct NORM waste with different NORM concentrations.
new wells start production in the near future (Petrobras, 2017). The authors identified that the NORM waste characteristics depend not
only on the extraction manner but mainly on the original characteristics
2.2. Oil NORM history and on the chemical arrangement of those elements in the mineral
matrix. They also highlighted the importance of such knowledge for
Since the thirties the occurrence of NORM in the oil extraction tubes regulation and the development of management techniques for those
inlays is well known. It is usually associated with sulfate and carbonate wastes.
of barium. During the seventies large companies sponsored research to
evaluate risks relative to radon in oil production plants. In the eighties, 4. Method and materials
researchers in the USA detected relatively high concentration of NORM
in the oily inlays, scale and sludge coming from the oil platforms. Here presented is a preliminary study based on literature data and
Therefore, the US government and the oil industry initiated research to on Petrobras gamma spectrometry analysis reports to verify the viabi-
characterize and map the main locations where oil NORM occurs lity of a more complex project that, if continued, will include collection
(Attallah et al., 2012). and multiple analyses of oil NORM samples.
In Brazil this issue started in the 80s, when Petrobras identified the The determination of radionuclides and the measurement of specific
presence of radiation in the oil sludge of pipes coming from the activities in the 238U and 232Th series is done by gamma spectrometry
Namorado field (Campos basin). During many years Petrobras had to (Knaepen and Bergwer, 1995; Kolb and Woick, 1984). It consists of
store pipes with NORM scales due to the absence of a cleanup tech- quantifying radioactive elements by gamma-ray emission spectrum
nology for decontaminating such pipes. The problem continued until using a high-purity germanium detector (HPGe). Below it is shown how
the early 2000s, when Petrobras developed a process to remove the some radionuclides are determined by this method:
inlays from the tubes. After this the scales and oil sludge were stored in Gamma-spectrometry for radioisotopes of the 238U decay series:
barrels to attend the demands imposed by the CNEN (Matta and Reis,
2002). Nowadays, as already mentioned in section 1, the oil NORM a Ra is indirectly measured by the γ-emission peak of 609 keV and
.226

wastes status inside the country is under control. However, the CNEN, 1120 keV of the 214Bi.
as the only and official responsible of the government, still needs an b .210Pb is directly determined by measuring its γ-emission of
appropriate tool that allows identifying the precise source origin of 46.5 keV.
those wastes.
232
Gamma-spectrometry for radioisotopes of the Th decay series:
3. Geochemical signatures in nuclear regulation
a Ra is indirectly measured by the γ-emission peak of 911.2 keV
.228

The idea of geochemical signatures in nuclear applications is rela- and 969 keV of the 228Ac;
tively new. Costa-de-Moura et al. (2013) and Costa-de-Moura (2009, b .224Ra is indirectly measured by 212Pb or 212Bi.
2013) determined geochemical signatures that indicate the provenance

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G.T. De-Paula-Costa et al. Journal of Environmental Radioactivity 189 (2018) 202–206

Table 2 Table 5
214 214
Comparison between Pb and Bi in NORM waste coming from oil/gas Specific activity (Bq/g) of 46 samples from Garoupa-1 Platform (PGP-1) and
fields. 214
Bi/228Ac ratio. Adapted from (Petrobras, 2006a,b,c, 2007a,b, 2008).
Namorado field Abu Rudeis (Egypt) Egypt Desert (Shawky Platform Material 214
Bi S. D. 228
Ac S. D. 214
Bi/228Ac Error
(Brazil) (Matta and (Afifi and Awwad, et al., 2001)
Reis, 2002) 2005) PGP-1 Oil sludge 1.020 0.06 0.71 0.08 1.44 0.25
PGP-1 Oil sludge 1.030 0.04 0.66 0.04 1.57 0.17
Sample A3 (oil sludge) Sample before Sample (oil sludge) PGP-1 Oil sludge 1.520 0.06 0.70 0.05 2.18 0.22
specific activities (Bq/ treatment (oil sludge) specific activities (Bq/ PGP-1 Oil sludge 1.400 0.06 0.58 0.05 2.41 0.32
g) specific activities (Bq/ g) PGP-1 Oil sludge 0.655 0.03 0.26 0.02 2.49 0.29
g) PGP-1 Oil sludge 3.020 0.07 1.18 0.03 2.56 0.13
PGP-1 Oil scale 6.900 0.16 2.23 0.06 3.09 0.15
214
Pb 15.63 ± 2.34 66.5 ± 0.5 19.39 ± 0.019 PGP-1 Sand 8.690 0.21 2.74 0.07 3.17 0.16
214
Bi 15.22 ± 2.39 66.8 ± 2.5 18.32 ± 0.050 PGP-1 Oil scale 11.800 0.27 3.63 0.09 3.25 0.15
PGP-1 Oil scale 19.400 0.44 5.79 0.14 3.35 0.16
PGP-1 Oil sludge 4.800 0.12 1.43 0.04 3.36 0.18
PGP-1 Oil sludge 1.750 0.06 0.42 0.03 4.17 0.44
Table 3
PGP-1 Oil sludge 6.830 0.16 1.62 0.04 4.22 0.20
Specific activity (Bq/g) of 7 samples from Cherne-2 Platform (PCH-2) and
214 PGP-1 Oil sludge 13.600 0.31 3.21 0.09 4.24 0.21
Bi/228Ac ratio. Adapted from (Petrobras, 2006a,b,c, 2007a,b, 2008). PGP-1 Oil sludge 12.400 0.29 2.85 0.07 4.35 0.21
Platform Material 214
Bi S. D. 228
Ac S. D. 214
Bi/228Ac Error PGP-1 Oil sludge 13.400 0.29 2.92 0.07 4.59 0.21
PGP-1 Oil sludge 21.900 0.49 4.33 0.11 5.06 0.24
PCH-2 Oil sludge 1.18 0.04 0.64 0.03 1.83 0.15 PGP-1 Oil sludge 33.000 0.74 6.32 0.17 5.22 0.26
PCH-2 Oil sludge 36.90 0.29 11.80 0.09 3.13 0.05 PGP-1 Oil sludge 26.400 0.06 4.96 0.12 5.32 0.14
PCH-2 Not available 56.70 1.18 18.00 0.38 3.15 0.13 PGP-1 Oil sludge 39.500 0.85 7.23 0.17 5.46 0.24
PCH-2 Sand 62.80 1.34 18.60 0.40 3.38 0.15 PGP-1 Sand 76.500 1.72 13.60 0.36 5.63 0.28
PCH-2 Not available 71.40 1.47 20.90 0.44 3.42 0.14 PGP-1 Oil sludge 48.700 1.07 8.62 0.19 5.65 0.25
PCH-2 Rock 84.20 1.75 23.30 0.50 3.61 0.15 PGP-1 Oil scale 66.900 1.49 11.40 0.29 5.87 0.28
PCH-2 Oil sludge 1.73 0.05 0.44 0.02 3.97 0.29 PGP-1 Oil scale 134.000 2.92 22.80 0.55 5.88 0.27
PGP-1 Oil sludge 71.000 1.56 12.00 0.30 5.92 0.28
PGP-1 Sand 136.000 2.93 22.80 0.53 5.96 0.27
PGP-1 Oil scale 83.400 1.88 13.90 0.42 6.00 0.32
Table 4 PGP-1 Sand 108.000 2.30 17.90 0.40 6.03 0.26
Specific activity (Bq/g) of 11 samples from Namorado-1 Platform (PNA-1) and PGP-1 Sand 155.000 3.36 25.60 0.61 6.05 0.27
214
Bi/228Ac ratio. Adapted from (Petrobras, 2006a,b,c, 2007a,b, 2008). PGP-1 Oil scale 75.200 1.69 12.40 0.34 6.06 0.30
214 228 214 PGP-1 Sand 199.000 4.21 32.70 0.73 6.09 0.26
Platform Material Bi S. D. Ac S. D. Bi/228Ac Error
PGP-1 Oil scale 137.000 3.07 22.40 0.61 6.12 0.30
PGP-1 Oil scale 138.000 3.01 22.30 0.54 6.19 0.29
PNA-1 Oil sludge 7.14 0.08 4.61 0.07 1.55 0.04
PGP-1 Oil sludge 93.000 2.07 15.00 0.40 6.20 0.30
PNA-1 Oil sludge 9.01 0.10 5.63 0.08 1.60 0.04
PGP-1 Oil scale 170.000 3.63 27.40 0.62 6.20 0.27
PNA-1 Oil sludge 10.50 0.13 6.49 0.11 1.62 0.05
PGP-1 Oil scale 128.000 2.81 20.60 0.53 6.21 0.30
PNA-1 Oil sludge 10.50 0.09 6.37 0.05 1.65 0.03
PGP-1 Oil scale 196.000 4.07 31.50 0.68 6.22 0.26
PNA-1 Oil sludge 12.50 0.10 7.42 0.05 1.68 0.02
PGP-1 Oil scale 177.000 3.88 28.30 0.69 6.25 0.29
PNA-1 Oil sludge 11.50 0.10 6.77 0.05 1.70 0.03
PGP-1 Oil scale 177.000 3.84 28.00 0.65 6.32 0.28
PNA-1 Oil sludge 12.20 0.11 7.14 0.06 1.71 0.03
PGP-1 Oil scale 155.000 3.38 24.40 0.59 6.35 0.29
PNA-1 Oil sludge 12.50 0.13 7.25 0.09 1.72 0.04
PGP-1 Oil scale 174.000 3.59 27.30 0.58 6.37 0.27
PNA-1 Cleaning water 1.55 0.08 0.82 0.08 1.88 0.28
PGP-1 Oil sludge 154.000 3.36 24.10 0.59 6.39 0.30
PNA-1 Cleaning water 1.36 0.04 0.70 0.03 1.93 0.13
PGP-1 Oil scale 222.000 4.75 34.60 0.79 6.42 0.28
PNA-1 Cleaning water 1.72 0.04 0.84 0.02 2.05 0.11
PGP-1 Oil scale 95.200 2.14 14.80 0.50 6.43 0.36
PGP-1 Oil scale 166.000 3.60 25.60 0.60 6.48 0.29
PGP-1 Oil Scale 169.000 3.67 24.40 0.64 6.93 0.33
For this study was verified transient equilibrium between 214Bi and
226
Ra for the 238U decay series and between 228Ac and 228Ra for the
232
Th decay series. Transient equilibrium is obtained when the ratio of Table 6
two short-lived radionuclides of the same decay series is 1 (partial se- Specific activity (Bq/g) of 19 samples from Namorado-2 Platform (PNA-2) and
214
cular equilibrium). In case of transient equilibrium, the radionuclides Bi/228Ac ratio. Adapted from (Petrobras, 2006a,b,c, 2007a,b, 2008).
cannot be used for obtaining the sought after geochemical signature. Platform Material 214
Bi S. D. 228
Ac S. D. 214
Bi/228Ac Error
The comparison of 214Pb and 214Bi in NORM waste coming from three
different oil NORM samples, one from Brazil and two from Egypt PNA-2 Sand 0.76 0.01 0.66 0.01 1.15 0.03
(Table 2), indicates that all three sample groups are in secular equili- PNA-2 Oil scale 23.70 0.22 15.40 0.13 1.54 0.03
PNA-2 Sand 27.00 0.22 17.00 0.13 1.59 0.02
brium, although each group has different specific activities. It can be
PNA-2 Oil sludge 23.60 0.23 14.50 0.13 1.63 0.03
deduced from Table 2 that the ratios 214Pb/214Bi are nearly 1. PNA-2 Oil sludge 1.58 0.04 0.95 0.03 1.66 0.09
This study is based on analyses from oil NORM samples from four PNA-2 Sand 23.60 0.19 13.90 0.10 1.70 0.03
Brazilian platforms in the Campos basin: Cherne, Garoupa-1, PNA-2 Sand 1.70 0.07 1.00 0.06 1.70 0.16
PNA-2 Sand 24.90 0.23 14.00 0.13 1.78 0.03
Namorado-1 and Namorado-2 platforms, Campos basin, Brazil. Samples
PNA-2 Sand 2.47 0.06 1.38 0.04 1.79 0.09
of oil sludge, scale, sand, rock, and cleaning water were analyzed by PNA-2 Sand 23.60 0.20 13.10 0.01 1.80 0.02
gamma spectrometry using a High-Purity Germanium Detector (CAN- PNA-2 Sand 23.60 0.19 12.70 0.09 1.86 0.03
BERRA) in the Instituto de Radiometria e Dosimetria (IRD/CNEN) and PNA-2 Oil scale 2.54 0.06 1.36 0.04 1.87 0.10
the results presented in reports by Petrobras (Petrobras, 2006a,b,c, PNA-2 Oil sludge 1.44 0.04 0.76 0.03 1.90 0.11
PNA-2 Sand 2.00 0.05 1.02 0.03 1.96 0.10
2007a,b, 2008).
PNA-2 Oil sludge 2.39 0.08 1.21 0.06 1.98 0.17
The here described approach to obtain geochemical signatures of PNA-2 Oil scale 24.70 0.09 11.60 0.04 2.13 0.02
NORM waste is to model isotopic ratios from different decay series of PNA-2 Oil sludge 2.91 0.07 1.31 0.03 2.22 0.10
radionuclides normally present in oil NORM. The specific activities of PNA-2 Oil sludge 12.50 0.31 5.33 0.15 2.35 0.12
214 PNA-2 Oil sludge 0.69 0.26 0.26 0.02 2.67 1.23
Bi and 228Ac from NORM samples of different localities are plotted in

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G.T. De-Paula-Costa et al.
228
Fig. 1. Specific activities (Bq/g) of
a scatter diagram (228Ac, 214Bi). If they plot in distinct field and show
different trends, this method can be used for creating the desired geo-
chemical signature.
Considering the errors reported for each sample analyzed, the error
of 214Bi/228Ac is calculated by derivative method. Being F(x) = f(x)/g
(x), the error F’(x) is defined as follows:
f ′ (x ) f (x ) ⎫
F ′ (x ) = + g ′ (x ) ⎧ 2
g (x ) ⎨
⎩ [g (x )] ⎬
⎭ sition using methods like ICP-MS, ICP-OES, X-Ray fluorescence and
A total of 83 samples was used for this study: 46 samples from
Garoupa-1 platform; 7 samples of Cherne-2 platform; 11 samples from
Namorado-1 platform; and 19 samples from Namorado-2 platform. The
values for the specific activities of 214Bi, 228Ac, 214Bi/228Ac of samples
from each platform and their respective standard deviation and error
are presented in Tables 3–6.
5. Results and discussions
Modeling of specific activities in a scatter diagram where x = spe-
cific activity of 228Ac and y = specific activity of 214Bi shows linear
relations for the samples of four Brazilian oil platforms (Fig. 1). These
relations and resulting equations for each oil NORM waste may serve as
geochemical signature of the reservoirs and so indicate the location of
the NORM.
Fig. 1 shows clearly that most of the oil NORM waste samples from
the four oil fields plot in different areas when modeling radioisotopes of
the 238U decay series versus those of the 232Th decay series, specifically
228
Ac versus 214 Bi. This is expected mainly because each oil well has
distinct geological characteristics. Also using different oil/gas extrac-
tion processes may affect the waste characteristics. The platforms Na-
morado-1 and Namorado-2 (PNA-1 and PNA-2) are in the same oil field
(Namorado field). This may explain why values of their samples are on
the same linear trend line.
6. Conclusions
The conclusions can be summarized as below:
- Ratios between radionuclides of the same decay series do not pro-
vide geochemical signatures for NORM waste coming from the oil
Journal of Environmental Radioactivity 189 (2018) 202–206
214
Ac versus Bi of NORM waste samples from four oil platforms.
industry.
- Relations between radioisotopes of the 238U and 232Th decay series
may provide signatures for oil NORM wastes.
- The results of this case study indicate that the here presented
method is viable and worth further investigation.
- In continuation of this project it is planned to collect samples of oil
sludge, tube scales and crude oil from different Brazilian oil fields
and analyze them for their geochemical and mineralogical compo-
(1)
gamma spectrometry, and finally model more radionuclides rela-
tions to obtain precise signatures for the origin of the oil NORM.
Acknowledgments
Special thanks to the Department of Radioactive Waste of the CNEN
for supporting the project with information and analytical data and to
the anonymous scientific reviewer for constructive comments. This
research did not receive any specific grant from funding agencies in the
public, commercial, or not-for-profit sectors.
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