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17/12/2018 Rapid determination of technetium-99 by electrothermal vaporization-inductively coupled plasma-mass spectrometry with sodium c…

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Analytica Chimica Acta


Volume 413, Issues 1–2, 18 May 2000, Pages 207-215

Rapid determination of technetium-99 by electrothermal


vaporization-inductively coupled plasma-mass spectrometry
with sodium chlorate and nitric acid as modifiers
Ming Song, Thomas U. Probst
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https://doi.org/10.1016/S0003-2670(00)00832-1 Get rights and content

Abstract
An electrothermal vaporization-inductively coupled plasma-mass spectrometric (ETV-ICP-
MS) method based on the suppression of ruthenium by using nitric acid and sodium chlorate
as modifiers has been developed for determination of in the presence of ruthenium. A
1000 fold excess of Ru in the presence of 100 pg/ml resulted in an 4% signal increase
in the signal of mass 99 amu. Both nitric acid and sodium chlorate act in this case as
chemical modifiers, rather than simply as mere physical carriers. The recommended
concentrations of nitric acid and sodium chlorate are 1 and 0.7%, respectively. The limit of
detection of is 1.4 pg/ml (0.9 mBq/ml) and 28 fg (18 μBq) absolute. The concentration
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in three spiked samples with various matrices was determined. ×

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Keywords
ETV-ICP-MS; Technetium-99; Ruthenium-99; Separation of isobars; Modifier

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1. Introduction
Technetium-99, a soft beta-emitting radionuclide with a maximum beta energy of 292 keV, a
half-life of 2.1×105 years, is produced by nuclear fission as one of the main fission products
with a fission yield of 6.161% on masses 99 amu. Its long half-life and relatively high
mobility in the environment might cause concerns about its distribution and behaviour in the
environment. Therefore, a rapid and accurate method for determinations of low-level in
environmental samples is necessary. However, either the conventional β−–counting method
which needs electro-deposition, elimination of other β−–emitters and rather long counting
time of about 1400 min [1], [2], or the nebulization inductively coupled plasma-mass
spectrometry (ICP-MS) [3] which, used for environmental samples in recent years, is quick
in measurements but still needs a time-consuming and tedious preseparation of ruthenium
and molybdenum [4], [5], [6], [7], [8], [9], are not convenient for environmental samples. Up
to now, the major difficulty of measuring by ICP-MS is still the isobaric interference
caused by , a natural stable isotope of ruthenium with much higher concentrations than
in the environment. In addition, ICP-MS determination of can be impaired by
peak tailing of and . Since concentrations of in usual environmental and
biological samples are below the detection limit of ICP-MS, preconcentration is needed.
Hollenbach et al. [10] developed a fast method for the determination of based on flow
injection preconcentration with TEVA·Spec extraction resin followed by ICP-MS
measurements. Hence, the achieved detection limit for in soil was 0.02 ng/g
(13 mBq/g) [10].

Meanwhile, electrothermal vaporization (ETV) was used increasingly in recent years as a


sample introduction technique for ICP-MS with several advantages, e.g. better sensitivity,
minor polyatomic interferences, over nebulization of solutions [11], [12], [13], [14], [15], [16],
[17], [18], [19], [20], [21], [22]. Another important ability of ETV is that the sample matrix, e.g.
salts and organic components, which might clog the nebulizer, the sampler and skimmer
orifices can be separated selectively from the analytes. In addition, matrix effects, which
quench the plasma and enhance polyatomic interferences, are attenuated by sample drying
and sample ashing in the graphite furnace [23], [24]. In ETV-ICP-MS sample volumes of 10–
100 μl only are employed which is particularly important for analyzing biological samples
and for radiation safety when handling samples of highest activities. Hepiegne et al. [25]
reported the first employment of ETV-ICP-MS for the determination of , with which a

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detection limit of 0.3 pg/ml (0.2 mBq/ml) and of 15 fg absolute (10 μBg) for
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solution was obtained, but no effort was made to separate the isobaric
standard
in the graphite
×
tubes.

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experiments, we noted the following facts: the boiling points of
technetium(VII) oxide and ruthenium(VIII) oxide are 310.5 and 40°C, respectively [26]; in
1 M sulfuric acid solution 99% of Ru is volatilized in 30 min at 100°C in the presence of
NaClO, while Tc is left in the solution, no volatilization of Tc was found by heating at 100°C
for 4 h [27]; Tc can be distilled out from sulfuric acid, nitric acid, or perchloric acid [28]; and
ruthenium(VIII) oxide is produced when acidified solutions of Ru are heated with strong

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17/12/2018 Rapid determination of technetium-99 by electrothermal vaporization-inductively coupled plasma-mass spectrometry with sodium c…

oxidizing agents such as potassium permanganate, periodic acid, Ce(IV) or chlorine [29],
[30]. With all these aforementioned in mind, it seems possible to separate from in
a graphite furnace in the presence of acids and strong oxidizing agents, i.e. Ru may be
removed as RuO4 first at low temperature then Tc can be volatilized as Tc2O7 at a higher
temperature. Thus, the tedious preseparation procedures applied to determination of Tc can
be omitted. Such methods have not been reported in the literature to date. Expecting to
develop such an method, we started this work with using HNO3, the favourite acid of ICP-
MS, and several oxidizing agents as modifiers. In contrast to our expectations, no significant
ETV-signals which could be referred to as RuO4 and Tc2O7 were obtained from the HNO3-
oxidizing solutions, both Tc and Ru volatilized only at temperatures above 1700°C.
Nevertheless, a signal suppression of Ru was observed first when a strong oxidizing agent,
i.e. KMnO4 was added, based on which a method for the determination of Tc in the
presence of Ru by ETV-ICP-MS was established.

2. Experimental

2.1. Apparatus
The quadrupole ICP-MS ELAN 5000 of Perkin Elmer & SCIEX, which is equipped with a Pt-
sampler, a Pt-skimmer cone, a quartz injector tube in the Fassel torch, and an active film
multiplier type AF 570 (ETP Pty Ltd, Ermington, Australia) is used for the presented
experiments. The ETV device HGA-600 MS (Perkin Elmer) is coupled to the ICP-MS by a
straight PTFE tube of 95 cm length and 6 mm internal diameter. Argon with a purity of
99.999% (Messer Griesheim) and pyrolytically coated graphite tubes (Perkin Elmer) are
used throughout. Disposable precleaned polystyrene cups are used in the autosampler (AS-
60, Perkin Elmer). The operating conditions are summarized in Table 1, Table 2. Count rates
are obtained by manual peak area calculations of either 3 or 6 replicates. The interferences
of ruthenium is defined as the ratio of count rates of to . The count rates are
calculated from the mean values of the count rates obtained from Ru masses 101, 102 and
104 amu according to their relative abundances. The dead time correction is 35 ms.

Table 1. ETV-ICP-MS operating conditions

ETV

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Sample volume 20 μl
×
Modifier.volume
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Read delay 5s

Closure delay Register for free −6 s

Injection speed 100%

ICP

rf power 1050 W

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Ar flow rate

Nebulizer 825 ml/min

Auxiliary 0.8 l/min

Coolant 11 l/min

MS

AFM voltage 3.472 kV

Basic vacuum 4×10−7 torr

Running vacuum 9×10−6 torr

Ion lens settings B, P, E1, S2 44, 46, 28, 41

Peak scan parameters

Number of replicates 3 or 6

Points per peak 1

Sweeps per reading 1

Readings per replicate 100

Resolution Normal

Scanning mode Peak hop transient

Dwell time 12 ms

Table 2. ETV program for determination of technetium

Heating step Temperature (°C) Ramp time (s) Hold time (s) Internal Ar (ml/min) Comment

1 100 1 60 300 Drying

2 2450 0.5 10 0 Volatilization

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5 5 300 Cooling
×

Pipet sequence Solution Activate cell


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1 Sodium chlorate

2 Sample

3 Nitric acid

4 From 1 to 3

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2.2. Sample and standard preparation


Storage and sampling of all radioactive samples are carried out according to safety
restrictions and administrative limits. Technetium-99 standard solutions are prepared from a
standard stock solution of 991 mg/l (630 MBq/l) Tc-99 in 2.5 M nitric acid, prepared in the
Institut für Radiochemie, Technische Universität München, by diluting with water. Ruthenium
standard solutions are prepared by diluting of a ruthenium atomic absorption standard
solution of 1005 μg/ml Ru in 5% HCl (Aldrich) with water. The hydrochloric acid from the Ru
standard solution is neutralized with sodium carbonate (Fluka, p.a.) to decrease the
interference of Ru. Nitric acid (65%, GR, Merck) is purified by repeated subboiling distillation
in a Berghof BSP 929 subboiling apparatus before use. Sodium chlorate (puriss grade) are
obtained from Fluka. All other reagents used are of GR or higher grade. All solutions are
prepared with high purity water (18 MΩ cm), first purified using a Millipore Milli-Q cartridge
kit and subsequently by a Millipore Milli-Q Plus system.

3. Results and discussion

3.1. Selection of the modifiers


For the selection of the first modifier, several common oxidizing agents, which are listed in
Table 3, were found to suppress selectively the volatilization of Ru from the graphite furnace
in the presence of nitric acid. The oxidizing agents were added in the same molar
concentration. The Ru signal suppression at a concentration of 100 ng/ml in the presence of
0.1 ng/ml Tc was investigated to select the best oxidizing agent. The signal suppression is
defined as the ratio of Ru count rates obtained with addition of an oxidizing agent to those
without it. Sodium chlorate with a suppression power of 0.004 was found to be most
effective. Sodium bromate was not used since the data of and could not be
obtained due to great peak tails of mass 102 and 104 which probably arise from
and . Considering that NaClO is not stable, it was not employed,
although it was recommended by Chen et al. [27]. Potassium perchlorate does not exhibit
obvious suppression power over Ru, neither in the presence of nitric acid nor in the
presence of hydrochloric acid. Suppressing the volatility of Ru by employing NaF, NaCl or
NaNO3 in the presence of HNO3 was not successful. In pure Tc solutions, enhancements of
Tc signals were observed when NaCl, NaClO3 or NaNO3 were added together with 1%

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HNO3. The enhancing powers of 0.5% NaCl, 0.7% NaClO3 and 1% NaNO3 on 100 pg/ml

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are 1.8, 2.9 and 2.1, respectively. In this context we should realize that the
suppression powers of 0.5% NaCl and 1% NaNO3 on 100 ng/ml Ru are only 0.79 and 0.75,
respectively. The effects of NaCl and NaNO3 were investigated because they are probably
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formed in the graphite furnace deviceforbyfree
heating NaClO3 together with HNO3. Therefore,
signal suppression of Ru will primarily result from the oxidition potential of NaClO3 in acidic
solution. Even in neutral solution, a solution of 0.5% NaClO3 suppresses the signal
intensities of 100 ng/ml Ru to a level of about 0.1. Nevertheless, the enhancing power of
NaClO3 for Tc will result also from its property to act as physical carrier [20], because only a
minor part of the employed amount is required for oxidation of Tc.

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Table 3. Interference of Ru in a concentration of 100 ng/ml in the presence of 1% HNO3 and of in a


concentration of 100 pg/ml caused by oxidizing agents. All standard deviations are calculated from six
replicates

Oxidizing agent Concentration (%) Ru interference (%)

Sodium chlorate 0.80 3.69±0.55

Sodium bromate 1.14 3.67±0.67a

Potassium chlorate 0.92 15.5±2.26

Potassium bromate 1.26 8.16±1.22

Potassium permanganate 1.19 27.0±2.19

a
Calculation according to the count rates of mass 101 only.

As a second modifier various acids, i.e. HNO3, HCl, H2SO4, H3PO4, H3PO3, and H3BO3,
were investigated with and without addition of NaClO3. Since, NaClO3 is applied as the first
modifier, the best results were obtained for signal suppression of Ru when a solution of 1%
HNO3 is used as the second modifier. Apparent volatilizations of RuO4, the generally
expected product, seem never to occur, neither in the combination of HNO3 with NaClO3,
KClO3, NaBrO3, KBrO3, KMnO4, or KClO4, nor in the combination of NaClO3 with HCl,
H2SO4, H3PO4, or H3BO3. A reasonable explanation might be decomposition of RuO4[31] to
RuO2 or direct formation of RuO2. We conclude from the fact of large variations in the signal
intensities of Ru, due to the employed acidic modifiers, that various Ru compounds are
formed. The Ru compound formed in the presence of HNO3 and NaClO3 results in signals
of smallest intensity. We conclude from the course of the volatilization temperatures, that no
apparent volatilizations of Tc2O7 takes place when NaClO3 as the first modifier and 1% HCl,
1% HNO3, 1% H3PO4, or 1% H3BO3 as the second modifier are employed. This is beyond
our expectation. Only when NaClO3 and H2SO4 modifiers were employed, a signal probably
attributable to an easily volatile Tc compound was observed, which is in further
investigations [35].

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The recommended concentrations of sodium chlorate and nitric acid are 0.7 and 1%,

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respectively (Fig. 1, Fig. 2). The increasing interference of Ru obtained with increasing
×
NaClO3 or HNO3 concentrations can be attributed to their physically carrying effect [20]. The
minimal Ru signal was obtained from the pipet sequence of NaClO3, sample, and nitric acid
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followed by a drying step, see Table for free
2. Greater interferences on the Tc signal were observed
if nitric acid was addded into the Tc standard solutions in advance instead of being used as
a modifier. In a first simple model, the observed effect of the selected pipet sequence might
be due to formation of a volatile Ru compound, e.g. RuO4 (bp, 40°C). Hence, a sandwich
pipetting procedure is perfomed, which minimizes the reaction time of Ru and nitric acid,
during sampling in the graphite furnace. The interference of various Ru concentrations on a

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17/12/2018 Rapid determination of technetium-99 by electrothermal vaporization-inductively coupled plasma-mass spectrometry with sodium c…

100 pg/ml solution is shown in Table 4. It should be noted that a 1000-fold excess of
Ru resulted only in a signal increase of mass 99 amu of 4%. Summerizing all mentioned
facts, it can be concluded that both HNO3 and NaClO3 act as real chemical modifiers in
suppressing the volatilization of Ru, rather than simply as physical carriers as usually
regarded [12], [20].

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Fig. 1. Optimization of the sodium chlorate concentration used as the first modifier. Tc-99: 100 pg/ml,
nitric acid: 1%.

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Fig. 2. Optimization of the nitric acid concentration used as the second modifier. Tc-99: 100 pg/ml,
×

sodium chlorate: 0.7%.

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Table 4. Interference of various Ru concentrations on a 100 pg/ml solution. All standard deviations
are calculated from six replicates

Concentration of Ru (ng/ml) 0.00 0.10 1.00 10.0 100

Interference of Ru (%) 0.54±0.33 0.29±0.13 0.42±0.27 1.43±0.32 3.69±0.55


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3.2. Optimization of pretreatment and volatilization temperatures


A pretreatment step at a temperature higher than 100°C for 10 s enhances the interferences
of on , see Fig. 3, Fig. 4. This decrease in the volatility of Tc after pretreatment is
possibly due to the reduction of pertechnetate by the carbon of the hot graphite tube forming
less volatile carbides or carbon intercalates on the graphite surface. For Ru, not such
carbides but other more volatile compounds, probably nitrosyl complexes, seem to form. In
the following investigations, the standard pretreatment temperature 100°C is employed.

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Fig. 3. Optimization of the pretreatment temperature for Tc and Ru in a standard solution. Tc-99:
100 pg/ml, Ru: 100 ng/ml, sodium chlorate: 0.7%, nitric acid: 1%.

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Fig. 4. Interference of Ru-99 on Tc-99 due to pretreatment temperature given as the signal ratio Ru-
99/Tc-99. Experimental conditions as given in Fig. 3.

Probst et al. [12] published in 1996 three basic types of curves of volatilization temperature
due to choice and concentration of the modifier. These curves are confirmed by previous
investigations of volatilization of , [11] as well as of and in this paper. As
shown in Fig. 5, Fig. 6, there is a very selective volatilization of in the presence of 1000
fold excess Ru. The volatility of Tc increases in a linear way from 1700 to 2200°C. From
2200°C onwards, volatilization approaches a maximum of about 2700°C, close to the
maximum of volatilization temperature of 2850°C employed for ETV devices. From the
course of temperature dependent volatilization, it can be deduced that Tc does not volatilize
as Na3TcO5, which decomposes above 650°C [32], as KTcO4, which decomposes above
1000°C [33], nor as TcO2, which decomposes above 1100°C [33], but as TcC (mp:
1835±50°C [32]). Thus, the further increase of Tc volatility above 2600°C should result from
the enhanced decomposition of surface-bonded carbides due to the break-up of
TcC(surface)–C(graphite) bond, just as the carbon on graphite surface vaporizes.
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Considering the visible carbon deposition in the transfer line and in the sampling valve of the
furnace from heating to above 2600°C, which causes serious memory effects, the
×

recommended volatilization temperature is 2450°C, according to a minimal


interference, shown in Fig.Register
6. for free

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Fig. 5. Optimization of the volatilization temperature for Tc and Ru in a standard solution. Experimental
conditions as given in Fig. 3.

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Fig. 6. Interference of Ru-99 on Tc-99 due to volatilization temperature given as the signal ratio Ru-99/Tc-
99. Experimental conditions as given in Fig. 3.

3.3. Detection limit

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The detection limit of is determined according to the method described by Currie [34]
with the error type I and II set to 5%: DL=3.52σ/b. The standard deviation of the blank σ,
calculated from 20 replicates, is 110 cps. The slope b of the calibration curve is determined
in the range from 10 to 100 pg/ml. Thus, the calculated detection limit is 1.4 pg/ml
(0.9 mBq/ml) and 28 fg (18 mBq) absolute.

3.4. Determination of Tc in Samples


Three samples spiked by in a concentration of 100 pg/ml and with 100-fold and 1000-
fold excess of Ru, respectively, were investigated by the elaborated ETV-ICP-MS method
(see Table 5), since no certified reference material for is available. First, brook water
was collected as a natural environmental sample. Second, an aqua regia sample was
created to simulate digest solutions of solid nuclear waste and environmental samples.
Third, a 1% NaNO3 sample was made to simulate liquid nuclear wastes with high amounts
of salts. The brook water sample was collected near the institute and passed through a
0.45 μm filter before use. The observed Ru interference of 25% on with 100-fold
excess of Ru in the brook water might result from several effects of its organic matrix. First,
decomposition of the matrix into gaseous products e.g. CO2, H2O, NH3, during volatilization
at a temperature of 2450°C might form volatile Ru compounds e.g. RuO4. Second, organic
particles can act for Ru as physical carriers from furnace to the ICP flame. In the presence
of aqua regia, which causes an interference of Ru of 19.4%, the vaporization of Ru is due to
enhanced concentrations of nitric acid which promotes either the formation of volatile Ru
compounds or physically carrying effect of the modifier, see Fig. 3, Fig. 4, [20]. The result of
the 1% NaNO3 sample seems to contradict the enhancing power of NaNO3 on Tc and its
suppression power on Ru, which causes an interference of Ru of 14.5%, but it should be
noted that these above-mentioned effects were observed only since no second modifier, i.e.
NaClO3 was employed. It should be noted that the results obtained by ETV-ICP-MS for both
the samples in aqua regia and in 1% NaNO3 are very close together, which indicate either
the formation of a volatile Ru compound or the physically carrying effect of a nitrate modifier.
However, the applicability of the elaborated separation procedure is achieved for samples
with 100-fold excess of Ru (Table 5). This limit is deduced from Ru interferences in the
range from 58 to 111%, if 1000-fold excess of Ru is employed.

Table 5. ETV-ICP-MS determinations of samples spiked with 100 pg/ml

Sample (%)
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1% Aqua regia 1% NaNO3 Brook water ×
Interference of Rua 19.4±2.1 14.5±2.7 24.6±2.8

a
Recovery of 73.3±5.7 72.0±4.8 107.4±8.4
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Interference of Rub 90.4±14.5 58.0±5.6 110.5±13.5

b
Recovery of 86.1±12.8 66.1±5.0 106.6±13.2

a
10ng/ml Ru, three replicates.

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b
100ng/ml Ru, six replicates.

These results show that it is possible to eliminate the isobaric interference of on


up to an 100-fold excess of Ru in samples with matrix contents by an optimized ETV
procedure employing two modifiers. In contrast to radiometric methods, no separation
procedures are required and in highly active samples no sample pretreatment other than
dilution or digestion is necessary. This ETV-ICP-MS method is especially suitable for the
sensitive determination of in reprocessing samples. The total measurement time in
ETV-ICP-MS is roughly 6 min per sample. Better limits of detection are to be expected by
improved ETV devices [36] and by newer ICP-MS.

Acknowledgements
The authors thank the Alexander von Humboldt Foundation for a one-year research
fellowship. T.U. Probst is grateful to the Deutsche Forschungsgemeinschaft (DFG) for being
granted by a Habilitationsstipendium. The authors would also like to thank M. Hug for all of
his assistance.

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