Water Air Soil Pollut (2007) 186:365–371
DOI 10.1007/s11270-007-9471-4
Tantalum Dissolution Rate in Simulant Lung Fluid
C. Lima & M. J. Coelho & K. C. P. Dalia &
C. V. Barros Leite & G. Medeiros &
K. Dias da Cunha
Received: 10 November 2006 / Accepted: 8 July 2007 / Published online: 15 August 2007
# Springer Science + Business Media B.V. 2007
Abstract The aim of this study is to determine the
solubility rate of tantalum contained in pyrochlore,
columbite–tantalite and columbite in simulant lung
fluid. The International Commission on Radiological
Protection (ICRP), in its recommendation for limiting
intakes of radionuclide by workers, has consistently
recognized that the biological behavior of any specific
material after incorporation can significantly diverge
from model prevision. Model parameters should be
adjusted to adapt the model for each specific
substance material in order to estimate the dose due
to this element intake. The most recent ICRP
C. Lima : M. J. Coelho
Instituto Militar de Engenharia (IME),
Praça Gen. Tibúrcio, 80, Praia Vermelha,
Rio de Janeiro CEP 22290-271, Brazil
K. C. P. Dalia
Universidade Federal do Rio de Janeiro (UFRJ),
CCS-bloco G-Ilha do Fundão,
Rio de Janeiro, RJ CEP 21949-900, Brazil
C. V. B. Leite
Pontifícia Universidade Católica do Rio
de Janeiro (PUC-RIO),
Rua Marquês de São Vicente, 225, Gávea,
CEP 22451-041 Rio de Janeiro, Brazil
G. Medeiros : K. Dias da Cunha (*)
Instituto de Radioproteção e Dosimetria (IRD/CNEN),
Av. Salvador Allende s/n,
Rio de Janeiro CEP 22780-160, Brazil
e-mail: kenya@ird.gov.br
publication 66, respiratory tract dosimetry model,
point out that information as data like particle size,
aerosols solubility and the material chemical com-
pounds are important parameters in the dose coef-
ficients calculation. This paper studies the solubility
in Simulant Lung Fluid (SLF) of Ta present in mineral
dust particles. For this study 3 minerals were selected:
pyrochlore, columbite–tantalite and columbite. Tanta-
lum dissolution in vitro samples were obtained using
the Gamble solution and PIXE (Particle Induced
X-ray Emission) as analytical technique. In order to
characterize the worker exposure to Ta bearing
particles, one Brazilian niobium mine was selected.
The mineral dust particles were collected using a six-
stage cascade impactor and the elemental mass
concentrations and the MMAD (Mass Median Aero-
dynamic Diameter) were determined. Concentrations
of radionuclides from natural series of thorium and
uranium were also determined. The results show that
the workers are exposed to Ta bearing particles in the
respirable fraction of aerosols (aerodynamic diameter
(daer) <2.5 μm) during the mineral processing to
obtain Fe–Nb alloy. The solubility in Simulant Lung
Fluid (SLF) of Ta present in mineral dust particles
depends on the mineral characteristics. The solubility
half-time varies between 34 and 62 h depending on
the associated mineral.
Keywords Tantalum . Solubility . Dissolution rate .
Occupational exposure
366
1 Introduction
Tantalum abundance on the earth’s surface is typically
of the order of 1.7 ppm (Greenwood and Earshaw
1984) and the major Ta reserves are located in Brazil
and Australia representing 49.4 % and 32.0 % of the
world reserves, respectively. However, Brazilian
Ta2O5 production is about 256 t/year, whilst Australian
production is around 900 t/year.
The main Tantalum minerals are tantalite (Fe,Mn,
Th,U)(Ta,Nb)2O6, columbite–tantalite (Fe,Mn,Th,U)
(Nb,Ta)2O6, microlite (A)2(B)2(O,OH,F)7, where
A=Na, Ca, Fe+2, U+4, Sb+3, Pb, Th, Zr, Ce, Y and
B=Ta, Nb, Ti, Sn, Fe+3, W, euxenite (Y,Ca,Ce,U,Th)
(Nb,Ta,Ti)2O6 and pyrochlore (A)2(B)2(O,OH,F)7,
where A=Na, Ca mainly, but also Fe+2, U+4, Sb+3,
Pb, Th, Ce, Y and B=Ta, Nb, Ti mainly, but also Sn,
Fe+3, W (Frondel et al. 1967).
Tantalum (Ta) and its compounds are used in
different kinds of industry, for example, as eletronic
components, resitors and semicondutors divices used
in manufecturing process of mobile phones, pagers
and computers. Special tantalum alloys have also
been used in medicine for prosthesis manufacture.
Tantalum alloys have high tolerance to high temper-
atures; consequently, they have bean used in space
aircrafts and in the nuclear industry to produce special
components which need to resistant to high temper-
atures (Kock and Paschen 1989).
However, during the mining and milling processes
to obtain minerals concentrates and during the
metallurgical processes to produce metal alloys dust
particles can be generated and the workers can inhale
particles containing metals.
The basis for assessing the radiological conse-
quences due to human inhalation of actinide dust
particles is provided by the new ICRP human
respiratory tract model (HRTM) (ICRP 66, 1994). In
this model, clearance from lungs is represented as the
competition between particle transport and absorption
into the blood. The ICRP model assumes that particle
transport rates of one specific compound is the same
for all media; otherwise, the absorption of a specific-
compound depends on the media (Baily et al. 1989;
Kreyling et al. 1989; Stradling and Moody 1995). As
part of the recommended procedure for calculating
radiation doses from inhaled radioactive material, the
ICRP divides radionuclides into three transportability
classes on the basis of their dissolution half-times.
Water Air Soil Pollut (2007) 186:365–371
The dissolution half-times depending on the chemical
compound of each element: S (slow), M (moderated)
and F (fast) (ICRP 66, 1994). The same behavior can
be applied for not radioactive isotopes of each
element, considering no radioactive decay.
Assessments of the hazards for workers due to
mineral particle inhalation require an estimation of
the deposition rates and solubility in the lungs.
These parameters determine the amount of toxic
substances transferred to blood. But the solubility is
strongly dependent on the physical and chemical
characteristics of the inhaled particles. In general, it
is not possible to obtain these data from direct
observations in the human body and in vitro
solubility experiments have been used to estimate
the behavior of metal in the human lung (Kanapilly
et al. 1973; Eidson 1994).
Several studies have been published about human
exposure to metal-bearing particles (Ansoborlo et al.
1998; Cusbert et al. 1994; Eidson et al. 1989; Eidson
1994; Kanapilly and Goh 1973; Kanapilly et al. 1973;
Möller et al. 2001). However, few of these studies
report human exposure to Ta-bearing particles. One of
these studies is based on a human group accidentally
exposed to airborne particles containing radioactive
tantalum oxide. In these groups biological clearance
was not observed, suggesting that the retention half-
time was longer than 1,000 days (Sill et al. 1969).
Friedman and Tisi (1972), Gamsu et al. (1973) and
Nadel et al. (1968) used radiographic techniques to
determine the retention half-time in the lungs. They
showed that the retention half-time of Ta (as metal)
particles deposited in alveolar regions was higher than
1 year. Dogs were exposed to aerosol particles labeled
with 182Ta to study the biological half-time (Andrea
Blanco et al. 1974). The inhaled Ta-bearing particles
deposited in the alveolar region of the lung suggested
a prolonged retention in this region with a biological
removal half time larger than 2 years. In disagreement
with these studies, Llamas et al. (1969) and Edmunds
et al. (1970), also using a radiographic technique to
evaluate the Ta retention in the lungs, obtained a
retention half-time of some days.
Previous studies developed in Brazilian mines
show that the workers were exposure to mineral dust
particles containing metals in the respirable fraction
of aerosols and the inhalation was the main way of
incorporation (Dias da Cunha et al. 1998a, b, 2002;
Lipsztein et al. 2001).
Water Air Soil Pollut (2007) 186:365–371
In Brazil, there are about 4,000 workers involved
in the mining and milling processes of minerals
containing tantalum, niobium, thorium and uranium.
Some of them work in a plant where pyrochlore is
processed to obtain a Nb–Fe alloy. In order to
evaluate the exposure of these workers to mineral
dust particles it is necessary to determine the Mass
Median Aerodynamic Diameter (MMAD) of mineral
particles, elemental mass concentration in the respi-
rable fraction (particles that are able to penetrate deep
into the lung from nasal inhalation, daer <2.5 μm ) and
inhalable (particles that are able to enter the nose)
fractions of the aerosol and the solubility of the metal
compound in the lungs (Lippmann 1970; Task Group
on Lung Dynamics 1966; Lippmann and Albert 1969;
Chan and Lippmann 1980).
In the Southwesten part of the State of Goiás,
Brazil, a metallurgical plant has been installed for iron
and niobium production. Brazilian production of iron
and niobium represents 58% of the worldwide
demand. The existing mineralized body resulted from
the action of intensely severe climatic conditions over
the original carbonite body, resulting in a material
decayed, earthy, friable and unconsolidated. Thus, the
extraction of existing mineralized body is relatively
simple and is performed in an open-pit mine. Both
mineral and overburden are removed mechanically. In
this industrial complex, the pyrochlore ((A)2(B)2(O,
OH,F)7, where A=Na, Ca mainly, but also Fe+2, U+4,
Sb+3, Pb, Th, Ce, Y; B=Ta, Nb, Ti mainly, but also
Sn, Fe+3, W is upgraded to obtain a Fe–Nb alloy. The
workers involved in the process to obtain this alloy
can inhale and ingest mineral dust particles containing
metals. Pyrochlore is extracted from an open-pit mine
using mechanical processes. The workers involved in
these processes can inhale airborne particles contain-
ing Ta.
The aim of this study is to determine the solubility
rate of Tantalum contained in minerals in simulant
lung fluid.
2 Experimental Method
Three samples of minerals concentrated (columbite–
tantalite, pyrochlore, and columbite) were selected
for this study. The samples were collected and
stored using plastic tools. Each mineral sample
(10 kg) was homogenized using a mechanical
367
process in ceramic apparatus. Each sample was
then divided into four parts and one part was
selected. This part was homogenized and this
process was repeated twice more in order to obtain
an aliquot of 156 g. This sample was then sieved
using a 400-mesh sieve (diameter<37 μm). After
sieving process the sample volume was again
homogenized.
The static in vitro dissolution test was used for
determination of the solubility (Kanapilly et al. 1973;
Moss 1979; Eidson and Mewhinney 1983; Dennis et
al. 1982; Cusbert et al. 1994; Ansoborlo et al. 1998),
and the Simulant Lung Fluid (SLF) was the Gamble’s
solution (Gamble 1967; Ansoborlo et al. 1990).
100 ml of SLF containing 0.1 g of the mineral was
maintained in a closed recipient. The pH of the
solution was equal to 7.4 and the experimental
arrangement was kept at room temperature (22°C up
to 25°C). Variation in room temperature causes no
effect on the dissolution rate (Eidson and Mewhinney
1983). Samples of 10 ml of solution were collected at
different time intervals (24, 48, 72, 168 and 720 h)
using a Nuclepore filter (pore size 0.4 μm).
232
Th, 228Th, 238U and 234U concentrations were
determined in mineral samples (pyrochlore, colum-
bite–tantalite and columbite). A sequential analytical
method for the determination of these radionuclides
was used. Uranium and thorium isotopes were
initially separated using tri-n-octyl phosphine oxide
(TOPO) supported on a column of silica gel. The
uranium isotopes were extracted with TOPO using a
polymeric membrane. Thorium isotopes were co-
precipitated with lanthanum fluoride. 232Th, 228Th,
238
U and 234U concentrations were determined by
alpha spectrometry (Lauria and Godoy 1988). The
alpha spectra were obtained using an EG&G ORTEC
model 576 system.
The particle size distributions were determined
using a six-stage cascade impactor with an operational
flow rate of 12 l/min, and cut-off diameters of 0.64,
1.0, 2.4, 4.7, 9.9 and 19.4 μm (Dias da Cunha et al.
1998b). The cascade impactor was located near the
workers at the point of highest total dust concentra-
tion and at 1.5 m from the soil. The sampling time at
each point was chosen in order to avoid saturation in
stages of the cascade impactor.
The aerosol samples, SLF and mineral (pyrochlore,
columbite–tantalite and columbite) samples were
analyzed by PIXE using a 2 MeV proton beam
368
generated by a 4 MV Van de Graaff electrostatic
accelerator. The X-rays were detected by a Si-PIN
detector with a 0.2 mm-thick aluminum foil as an X-
ray absorber. The efficiency curve was determined
using reference standard material. The X-ray spectra
were analyzed using an updated version of custom-
designed software based on the stripping of a multi-
elemental spectrum.
3 Results and Discussion
3.1 Mineral Analyses
The elemental mass concentration present in colum-
bite–tantalite, columbite and pyrochlore samples are
shown in Fig. 1.
Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Zr, Nb, Ta, Pb, Th
and U were identified in minerals. Co was identified
only in pyrochlore and columbite samples. The ratios
Nb/Ta in pyrochlore, columbite and columbite–
tantalite were 6.9, 9.7 and 1.6, respectively. The
highest Zr concentration was observed in the colum-
bite sample. This sample was collected in a columbite
mine located in the Amazon forest that also processes
zirconite. Ca, Ti, Fe and Pb are also observed in the
crystal lattice of pyrochlore (Frondel et al. 1967). Th
and U identified in the X-rays spectra of three
Fig. 1 Elemental mass con-
centrations observed in co-
lumbite–tantalite, columbite
and pyrochlore samples
10
Concentration ppm
0,1
0,01
Ca Ti Cr Mn Fe Co Ni Cu Zn Zr Nb Ta Pb Th U
Water Air Soil Pollut (2007) 186:365–371
minerals were due to the fact that these radionuclides
are associated to the mineral crystal lattice.
232
Th, 228Th, 238U and 234U concentration in
minerals are shown in Fig. 2. The lowest thorium and
uranium concentrations were observed in columbite–
tantalite samples.
3.2 Aerosol Samples
The Brazilian plant located at the Southwesten part of
the State of Goiás processes pyrochlore to obtain Fe–
Nb alloy. The aerosols samples were collected using a
six-stage cascade impactor during the main steps of
industrial process (mineral concentration, metallurgi-
cal process and Fe–Nb alloy crushing). This sampling
showed that the workers were exposed to Ta particles
in respirable fraction of aerosols and the average mass
concentration of Ta during the leaching and flotation
processes was 0.0388 μg/m3, but during the alumi-
notermy and Fe–Nb alloy crushing Ta concentration
in repirable fraction was below the detection limit and
the MMAD (Mass Median Aerodynamic Diameter) of
Ta particles were 0.8 and 3.0 μm indicating that,
during this step of the process, there were dust
particles in the respirable fraction (daer <2.5 μm) and
in the inhalble fration (daer <10 μm). The local
conditions (humidity and high temperature) favor the
particles agglutination, increasing the particle sizes.
Elements
Columbite-tantalite Columbite Pyrochlore
Water Air Soil Pollut (2007) 186:365–371 369

inhalation. The solubility determines the fraction

which will be transported to body fluids and the
CONCENTRARION (Bq/g)

distribution rate in different tissues.

1
The simulant lung fluid (SLF) solution samples
were collected at different time intervals (24, 48, 72,
168 and 720 h) and analyzed by PIXE technique. The
fraction of total Ta present in the mineral and
0,1
dissolved in SLF were determined considering the
ratio between the Ta concentration in solution and in
mineral.
Ta is present in columbite–tantalite, columbite and
0,01
232Th 228Th 238U 234U pyrochlore as an oxide and its concentrations in these
RADIONUCLIDES minerals are 26.1%, 4.8% and 0.6%, respectively. The
Columbite-tantalite Columbite Pyrochlore solubility of Ta present in each mineral in SLF is
Fig. 2 232Th, 228Th, 238U and 234U concentrations in colum- shown in Fig. 3. Ta present in these minerals show
bite–tantalite, columbite and pyrochlore
fast solubility rate (<100 h). The dissolution life-time
(τ) in columbite is 34 h, in pyrochlore, 54 h and in
The aerosol monitoring also shows that during the columbite–tantalite, 64 h. The dissolution fraction of
pyrochlore processing to obtain Fe–Nb alloy, Ta observed in the columbite–tantalite samples could
the workers are exposed to Ta-bearing particles in the be explained by physical characteristics of each
respirable fraction; thus it is necessary to estimate the mineral such as crystal lattice and mineral density.
risk due to inhalation of particles containing Ta. The densities of columbite, pyrochlore and columbite–
tantalite are 5.1, 4.5 and 8.2 g/cm3, respectively. The
3.3 In vitro Solubility Test high density of columbite–tantalite can explain the low
solubility of Ta present in this mineral.
The solubility rate in lung fluid, besides the concen- These curves (Fig. 3) suggest that the solubility
tration and particle size, is one of the most important depends on the element and on the associated mineral,
factors in order to estimate the risk due to dust reinforcing the ICRP recommendation for determina-

Fig. 3 Dissolution fraction 25

curve for each mineral
y=21,9*(1-exp(-t/34))

20
DISSOLUTION FRACTION %

y=14,0*(1-exp(-t/54))
15

10

5
y=2,6*(1-exp(-t/62))

0
0 100 200 300 400 500 600 700 800
T IM E (h)
colum bite pyrochlore colum bite-tantalite
370
tion of the solubility fraction for each specific
material.
4 Conclusion
The results of aerosol characterization in the different
steps of process show that workers were exposed to
Ta-bearing particles in the respirable fraction. To
estimate the risk due to inhalation of dust particles
containing Ta besides the particle size, Ta air
concentration it is necessary to determine the Ta
compound solubility in stimulant lung fluid.
Three minerals containing Ta were selected for this
study columbite–tantalite, columbite and pyrochlore,
Ta was present in these three minerals as tantalum
oxide but in different concentrations 26.1%, 4.8% and
0.6%, respectively.
Ta compound in studied minerals it was deter-
mined different values for dissolution life-time. The
dissolution life-time of Ta in columbita was 34 h, in
pyrochlore was 54 h and in columbite–tantalite was
64 h. This could be explained by mineral density,
columbite pyrochlore and columbite–tantalite being,
5.1, 4.5 and 8.2 g/cm3, respectively. The high density
of columbite–tantalite can explain the low solubility
of Ta present in this mineral. The values of dissolu-
tion life-time determined for Ta suggest that solubility
rate of Tantalum oxide present in these minerals
should be classified as fast (<100 h).
These results suggest that the solubility of an
element present in a mineral depends on the mineral
crystal lattice, the mineral density and chemical
compound, reinforcing the ICRP 66 recommendation
for determination of the solubility fraction for each
specific material.
Acknowledgements The authors would like to thank CNPq
and PRONEX for the financial support.
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