27.2 Experimental
27.2.1 Reagents
Ultrapure grade NaOH solution (3 M) was purchased from Kanto Kagaku.
Ultrapure grade of tetramethyl ammonium hydroxide (TMAH) solution was purchased from Tama Chemicals. The other reagents were all analytical grade or
higher and purchased from Wako Chemical. Empore solid extraction disks,
Anion-SR, were purchased from 3 M. Standard solution of
129 I (35.8 kBq/g
129 I;
chemical composition, 50 μg/g NaI and 50 μg/g Na 2 S 2 O 3 in H 2 O) was purchased
from AREVA and diluted with H 2 O before use. Potassium iodide (analytical grade,
99.9 %) and KIO 3 (analytical standard material grade, 99.98 %) were purchased
from Wako Pure Chemical Industries, and
127 I
À and
127 IO 3
À were prepared from
these reagents, respectively, because the stable iodine isotope is only
127 I.
27.2.2 Separation Using Anion-SR
Figure 27.1 shows the experimental procedure for the solution samples. Sodium
iodide-129 (
129 I: 0.1 Bq ¼ 15 ng) and K
127 IO 3
À (
127
I: 1 μg) were added to 50 ml
3 M NaOH solution or 50 ml diluted HCl solution (pH ¼ 2) with and without
reductant (0.1 ml 0.1 M NaHSO 3 ) to study iodine species behavior in the analysis
using Anion-SR. After addition of the iodine species, the solutions were allowed to
stand for 1 day before separation with Anion-SR. The reductant was added approximately 20 min before the separation. The operation of Anion-SR was based on
Shimada et al. [3]. Briefly, the Anion SR disk was centered on the base of the
filtration funnel and the reservoir was clamped on the top of the disk. The appropriate solution was poured into the reservoir followed by suction filtration The
Anion-SR disk was conditioned with acetone, methanol, ultrapure water, 4 w/v%
NaOH, and ultrapure water. After conditioning, the sample solution was introduced
into the Anion-SR disk and washed with ultrapure water. The extracted I was
recovered with 9.5 ml 1 M HNO 3 . To oxidize I
À to IO 3
À , 0.1 ml NaClO solution
(effective Cl concentration, >5 %) was added to the recovered solution. Additionally, 0.1 ml 2 ppm Rh standard solution was added to the recovered solution as an
internal standard. Finally, 1 M HNO 3 was added to the recovered solution to a final
volume of 10 ml. The concentration of I was measured by inductively coupled
plasma mass spectrometry with dynamic reaction cell (DRC-ICP-MS). In the
reaction cell, oxygen gas was collided with ions. Because the order of ionization
potential is I > O > Xe, O reacts with Xe to neutralize but I does not react with
O. As a result, the count of
129 Xe, impurity of Ar gas, was decreased. The
experimental conditions of DRC-ICP-MS were consistent with the conditions
reported by Kameo et al. [7]. Percent recovery was calculated as in Eq. (27.1).
27 Development of a Rapid Analytical Method. . .
313
27.2.1 Reagents
Ultrapure grade NaOH solution (3 M) was purchased from Kanto Kagaku.
Ultrapure grade of tetramethyl ammonium hydroxide (TMAH) solution was purchased from Tama Chemicals. The other reagents were all analytical grade or
higher and purchased from Wako Chemical. Empore solid extraction disks,
Anion-SR, were purchased from 3 M. Standard solution of
129 I (35.8 kBq/g
129 I;
chemical composition, 50 μg/g NaI and 50 μg/g Na 2 S 2 O 3 in H 2 O) was purchased
from AREVA and diluted with H 2 O before use. Potassium iodide (analytical grade,
99.9 %) and KIO 3 (analytical standard material grade, 99.98 %) were purchased
from Wako Pure Chemical Industries, and
127 I
À and
127 IO 3
À were prepared from
these reagents, respectively, because the stable iodine isotope is only
127 I.
27.2.2 Separation Using Anion-SR
Figure 27.1 shows the experimental procedure for the solution samples. Sodium
iodide-129 (
129 I: 0.1 Bq ¼ 15 ng) and K
127 IO 3
À (
127
I: 1 μg) were added to 50 ml
3 M NaOH solution or 50 ml diluted HCl solution (pH ¼ 2) with and without
reductant (0.1 ml 0.1 M NaHSO 3 ) to study iodine species behavior in the analysis
using Anion-SR. After addition of the iodine species, the solutions were allowed to
stand for 1 day before separation with Anion-SR. The reductant was added approximately 20 min before the separation. The operation of Anion-SR was based on
Shimada et al. [3]. Briefly, the Anion SR disk was centered on the base of the
filtration funnel and the reservoir was clamped on the top of the disk. The appropriate solution was poured into the reservoir followed by suction filtration The
Anion-SR disk was conditioned with acetone, methanol, ultrapure water, 4 w/v%
NaOH, and ultrapure water. After conditioning, the sample solution was introduced
into the Anion-SR disk and washed with ultrapure water. The extracted I was
recovered with 9.5 ml 1 M HNO 3 . To oxidize I
À to IO 3
À , 0.1 ml NaClO solution
(effective Cl concentration, >5 %) was added to the recovered solution. Additionally, 0.1 ml 2 ppm Rh standard solution was added to the recovered solution as an
internal standard. Finally, 1 M HNO 3 was added to the recovered solution to a final
volume of 10 ml. The concentration of I was measured by inductively coupled
plasma mass spectrometry with dynamic reaction cell (DRC-ICP-MS). In the
reaction cell, oxygen gas was collided with ions. Because the order of ionization
potential is I > O > Xe, O reacts with Xe to neutralize but I does not react with
O. As a result, the count of
129 Xe, impurity of Ar gas, was decreased. The
experimental conditions of DRC-ICP-MS were consistent with the conditions
reported by Kameo et al. [7]. Percent recovery was calculated as in Eq. (27.1).
27 Development of a Rapid Analytical Method. . .
313