JP6464475B2 - Method for analyzing radioactive strontium - Google Patents

Description

  The present invention relates to a rapid analysis method for radioactive strontium.

  For example, when decommissioning a nuclear power plant, it may be necessary to treat contaminated water, concrete, soil, wood, etc. containing radioactive material strontium 90. In order to perform an appropriate treatment, it is important to measure the amount of strontium 90 contained in the object to be treated.

  The Ministry of Education, Culture, Sports, Science and Technology's Science and Technology Policy Bureau, Nuclear Safety Division, Disaster Prevention and Environmental Measures Office, “Analysis and measurement of radioactivity and radiation in environmental radiation monitoring around fallout and nuclear facilities has been unified from the viewpoint of data evaluation. From the standpoint of “It is desirable to be implemented by a method”, a “radioactive strontium analysis method” generally called an official method is provided as a manual (Non-patent Document 1).

  However, the manual provided in 2003 lacks the viewpoint of quickly measuring and promptly implementing the necessary treatments, and is an analytical method with many complicated chemical treatments for accuracy. It has become. For this reason, it takes about one month to obtain the measurement result (see FIG. 2), but such a measurement method cannot meet the current needs for rapid measurement.

"Radiotron Strontium Analysis" November 10, 2003 1st edition, publisher: Japan Analysis Center

  This invention is made | formed in view of the said situation, and provides the analysis method of radioactive strontium which can refine | purify and analyze strontium rapidly by a simple method.

In order to achieve the above object, the present invention provides the following means.
[1] A liquid sample containing strontium and one or more contaminants is brought into contact with the first adsorbent, and strontium in the liquid sample is adsorbed on the first adsorbent, and then the liquid sample, the first adsorbent, A first purification step of separating at least one of the contaminants together with the liquid sample, and an eluent containing strontium eluted from the first adsorbent by bringing the eluent into contact with the first adsorbent The elution solution is brought into contact with a second adsorbent that has the property of being able to adsorb the contaminants that may remain in the eluate and difficult to adsorb strontium. Thereafter, the eluate containing strontium and the second adsorbent are separated, and the contaminants are removed together with the second adsorbent to obtain a separation liquid containing strontium, and included in the separation liquid Be An analysis step of qualitatively or quantitatively analyze radioactive strontium, a method of analyzing the radioactive strontium that have a,
The first preparation step of measuring at least one content X1 of the stable isotopes of strontium contained in the liquid sample with a mass spectrometer, and the stable isotope species of strontium measured in the first preparation step, A second preparatory step of measuring the content X2 contained in the separated liquid with a mass spectrometer, according to the following formula (1):
Content X1 ÷ Content X2 x 100% (1)
By calculating the recovery rate of strontium, the content of radioactive strontium in the separation liquid is quantified by mass spectrometry or radiation measurement, and based on the recovery rate, the content of radioactive strontium contained in the liquid sample A method for analyzing radioactive strontium, characterized in that
[2] A liquid sample containing strontium and calcium is brought into contact with the first adsorbent, and after the strontium in the liquid sample is adsorbed on the first adsorbent, the liquid sample and the first adsorbent are separated, A first purification step for removing calcium together with the liquid sample, an elution step for bringing an elution chemical solution into contact with the first adsorbent to obtain an eluate containing strontium eluted from the first adsorbent, and mixing in the eluate. The adsorbent containing the strontium and the second adsorbent after contacting the eluate with the second adsorbent capable of adsorbing the contaminants that may be adsorbed and not easily adsorbing strontium And removing the contaminants together with the second adsorbent to obtain a separation liquid containing strontium, and qualitative or quantitative determination of strontium 90 contained in the separation liquid. The analysis method of radioactive strontium according to [1], which has a, an analysis step of analyzing.

  According to the method for analyzing radioactive strontium of the present invention, it is possible to rapidly purify and analyze target strontium from a liquid sample.

It is a flowchart which shows an example of the analysis method of radioactive strontium concerning this invention. It is a flowchart which shows the procedure of the analysis method of the radioactive strontium by the conventional official method.

  The method for analyzing radioactive strontium according to the first embodiment of the present invention includes a first purification step, an elution step, a second purification step, and an analysis step. Details of each step will be described below, but steps or processes other than these steps may be included.

<First purification step>
In the first purification step of this embodiment, a liquid sample containing strontium and one or more contaminants is brought into contact with the first adsorbent, and strontium in the liquid sample is adsorbed on the first adsorbent, and then the liquid sample and This is a step of separating the first adsorbent and removing at least one of the contaminants together with the liquid sample.

Strontium in the first purification step includes strontium 90 ( ⁹⁰ Sr) and strontium 89 ( ⁸⁹ Sr) as radioactive strontium, as well as naturally occurring stable isotopes of strontium ( ⁸⁴ Sr, ⁸⁶ Sr, ⁸⁷ Sr, ⁸⁸ Sr ) May be included. The majority of radioactive strontium in specimens derived from nuclear power generation is strontium 90 (half life 28.8 years), and strontium 89 (half life 50.5 days) is often small or substantially free.
In this specification, unless stated otherwise, the term “strontium” refers to both radioactive strontium and its stable isotopes.

  The first adsorbent is preferably capable of adsorbing strontium and hardly adsorbing contaminants. The strontium adsorbed on the first adsorbent may be a simple substance, may form an arbitrary compound or complex, or may be an ion. Since it is easy to control, a divalent cation (Sr (II)) is preferable.

  For example, by introducing the liquid sample into the first column filled with the first adsorbent, the first adsorbent and the liquid sample can be brought into contact with each other, and strontium in the liquid sample can be adsorbed on the first adsorbent. . Thereafter, by discharging the liquid sample from the first column, strontium remains in the first adsorbent, and other contaminants can be removed together with the liquid sample out of the first column. Furthermore, by passing a cleaning solution that hardly elutes strontium and easily elutes contaminants through the first column, excess contaminants adhering to the first adsorbent can be washed away.

  Examples of contaminants removed in the first purification step include substances containing elements other than strontium. The contaminant may be a radioactive substance or a non-radioactive substance. Specific examples include transition metals, alkaline earth metals, alkali metals, and ions thereof. As an alkaline earth metal, for example, calcium (Ca (II)) is mentioned as a main contaminant. This is because calcium (Ca carrier) may be added in advance as a strontium precipitation accelerator in the pretreatment stage of preparing the liquid sample to be used in the first purification step.

Examples of the liquid sample include those obtained by extracting radioactive strontium by a known method from incombustible waste, combustible waste, contaminated water or the like collected from a decontamination area.
Examples of non-combustible waste include soil, concrete, roof tiles, and building materials. Examples of combustible waste include hay that has been discarded from fields and farms, and wood that has been discarded from forests. As the contaminated water, for example, water discharged in the decommissioning process of a nuclear reactor can be cited.

  In order to improve the analysis accuracy of radioactive strontium, it is preferable to concentrate strontium in the liquid sample and increase the concentration of radioactive strontium in the liquid sample in the pretreatment stage. The concentration method is not particularly limited, and a known method can be applied. For example, as described in the official method, it is preferable to add at least one of Sr carrier and Ca carrier. After adding these carriers, a low concentration radioactive strontium contained in the liquid sample can be easily precipitated together with the carrier by adding a reagent for precipitating the carriers. A precipitate containing radioactive strontium is collected by a known method such as centrifugation, filtration, decantation, etc., dried, and then redissolved in a predetermined solution (for example, 8M nitric acid), thereby the first purification step. The liquid sample can be used for

Calcium derived from the Ca carrier contained in the liquid sample used in the above concentration treatment is a contaminant in the analysis method of the present embodiment. In addition, components other than strontium, such as organic substances and transition metals, may be mixed as contaminants in the liquid sample from the original waste from which strontium has been extracted.
Among these contaminants, it is preferable to separate and remove at least calcium from the target strontium 90 by the first purification step described above.

  Examples of the first adsorbent that adsorbs strontium include known column packing materials in which a substance having a high distribution coefficient or adsorption degree for strontium and a substance having a low distribution coefficient or adsorption degree for contaminant substances is bonded to the support. Specifically, a commercially available Sr resin in which 4,4 ′ (5 ′)-di-t-butylcyclohexano 18-crown-6 (crown ether) is bound to a chemically inert chromatographic support is suitable. It is.

  Sr resin exhibits a high partition coefficient for strontium (Sr (II)) in nitric acid at a high concentration of about 8M and strongly adsorbs strontium, and also contains calcium (Ca (II)) and radium (Ra (Ra ( II)) and barium (Ba (II)) have relatively low partition coefficients. For this reason, by using Sr resin as the first adsorbent, strontium can be highly purified from contaminants in the liquid sample in the first purification step.

In addition to the above Sr resin, a substance having a property of preferentially binding an alkaline earth metal (Group 2 element) to which strontium belongs can be applied as the first adsorbent on the periodic table.
The first adsorbent is at least one element selected from the group consisting of alkali metals, transition metals, group 12 elements including zinc, group 13 elements including boron, and group 14 elements including lead, other than alkaline earth metals. Or it is preferable to have the property that it is difficult to bind the ions.

<Elution process>
The elution step of the present embodiment is a step of obtaining an eluate containing strontium eluted from the first adsorbent by bringing the elution chemical into contact with the first adsorbent.
The type of the eluting chemical is appropriately selected according to the type of the first adsorbent used. As an example, when the aforementioned Sr resin is used as the first adsorbent, nitric acid having a low concentration of about 0.01M is brought into contact with the Sr resin instead of the 8M nitric acid used as the solvent of the liquid sample in the first purification step. Thus, the adsorbed strontium can be eluted. By thoroughly washing the Sr resin with 8M nitric acid before elution, the degree of purification of the eluted strontium can be further increased.

<Second purification step>
The second purification step of the present embodiment has the property that it can adsorb contaminants that may remain or be mixed in the eluate containing strontium obtained in the elution step, and it is difficult to adsorb strontium. The eluate is brought into contact with the second adsorbent. Thereafter, the eluate containing strontium that does not bind to the second adsorption and the second adsorbent are separated, and the contaminants are removed together with the second adsorbent to obtain a separation liquid containing strontium.

  Here, “the property of hardly adsorbing strontium” means the property that strontium has a lower partition coefficient or degree of adsorption than a contaminant in a predetermined solvent.

  For example, by introducing the eluate into the second column filled with the second adsorbent, the second adsorbent and the eluate can be brought into contact with each other, and contaminants in the eluate can be adsorbed on the second adsorbent. it can. At that time, strontium hardly adsorbs on the second adsorbent and is contained in the separation liquid discharged from the second column. As a result, since the contaminant substance contained in the eluate remains in the second adsorbent, a separation liquid containing strontium separated from the contaminant substance is obtained. Even if no contaminants remain or are mixed in the eluate, a separation liquid containing no contaminants can be obtained by the same operation as described above.

  Examples of hybrid substances to be removed in the second purification step, that is, contaminant substances that may be contained in the eluate, include substances that can be contained in a liquid sample together with strontium, substances that can be adsorbed to the first adsorbent together with strontium, Examples include substances whose chemical properties are close to strontium. Specifically, for example, alkaline earth metals (Group 2 elements) other than strontium, yttrium, titanium, zirconium, other transition metals, and the like are included as contaminants that are highly likely to be contained in the eluate.

Examples of the second adsorbent that hardly adsorbs strontium include known column fillers in which a substance having a low distribution coefficient for strontium and a high distribution coefficient for contaminants is bound to the support. Specifically, octylphenyl-N, N-di-isobutylcarbamoylmethylphosphine
Commercially available TRU resins with oxide (CMPO) bound to a chemically inert chromatographic support are preferred.

  TRU resin shows a low partition coefficient for strontium in about 2M nitric acid and hardly adsorbs, while the above impurities, plutonium (Pu (IV)), neptunium (Np (IV)), uranium (U (VI )) And americium (Am (III)) are adsorbed with a high partition coefficient. For this reason, by using TRU resin as the second adsorbent, strontium can be separated from contaminants in the eluate in the second purification step.

  According to the method of the present embodiment, strontium in the liquid sample is adsorbed by the first adsorbent, impurities that are difficult to adsorb on the first adsorbent are removed, and then the strontium eluted from the first adsorbent remains. Of the contaminants, only the contaminants are adsorbed on the second adsorbent and obtained as a separation liquid without adsorbing strontium, so that highly purified strontium can be obtained easily and quickly. Can get to.

  Further, the volume of the liquid sample can be reduced to about 10 to 60 times as compared with the so-called official method described in the conventional “radioactive strontium analysis method”. This is because the strontium purification efficiency and recovery efficiency in this embodiment are high. In the conventional official method, since only one type of column purification is performed, the purification efficiency is low, and since the precipitation purification is performed a plurality of times in addition to the column purification, the recovery efficiency is also low.

  Compared to a conventional official method, the ability to reduce the volume of a liquid sample in this embodiment is synonymous with the ability to reduce the time and amount of reagent required for column purification. Specifically, in the conventional official method, 700 mL of the sample solution and 2000 mL of 3M hydrochloric acid are introduced into a cation exchange column (Dowex50Wx8: column volume 500 mL). On the other hand, in this embodiment, if a 10 ml to 50 ml liquid sample and a 20 ml washing solution are used, a purification level equal to or higher than that of the conventional one can be achieved.

  In the conventional official method, after preparing a sample solution concentrated from about 10 liters of sample solution containing strontium extracted from waste or the like to about 700 mL, β-ray measurement derived from strontium 90 is finally performed to obtain strontium 90 It takes about 1 month and various reagents to obtain a purified sample that can be quantitatively analyzed (see FIG. 2). The required amount of liquid sample and reagent per specimen is generally as follows.

・ Liquid sample = 700 mL (the volume to be introduced into the column after concentration of the sample solution)
・ Concentrated hydrochloric acid (12M hydrochloric acid) = 600 mL (500 mL of which is diluted and used as 2000 mL of 3M hydrochloric acid)
・ Ca, Sr, Y, La, Ba, Fe = 5 to 250 mg each (the amount to be added as a carrier)
-Potassium chromate = 0.3 g
・ Sodium carbonate = 20 g
・ Ammonium carbonate = 40 g
・ Ammonia water = 30 mL
・ Ammonium acetate = 1 g
・ Acetic acid = 1 mL

  In this embodiment, even if 10 liters of a sample solution containing strontium extracted from waste or the like is prepared as in the conventional official method, strontium with high purity and high recovery rate is obtained by two-stage column purification thereafter. Therefore, the volume of the liquid sample introduced into the column purification by concentrating 10 liter of the sample solution can be remarkably reduced. For this reason, it takes two days and a small amount of reagent to finally obtain a purified sample capable of quantitative analysis of strontium 90 by performing β-ray measurement or ICP-MS measurement derived from strontium 90 (see FIG. 1). The required amount of liquid sample and reagent per specimen is generally as follows.

・ Liquid sample = 50 mL (the volume to be introduced into the first column after concentration of the sample solution)
・ Concentrated nitric acid = 50 mL
・ Ammonium oxalate = 10 g
・ Ca, Sr = 1 to 500 mg each (the amount added as a carrier)
・ Ammonia water = 10 mL

<Analysis process>
The analysis step of the present embodiment is a step of qualitatively or quantitatively analyzing radioactive strontium contained in the separation liquid.
Depending on the amount and type of contaminants contained in the liquid sample before purification, the above separation liquid obtained in the second purification step is highly purified if it is a liquid sample to which a conventional official method can be applied. Yes. For example, yttrium 90 ( ⁹⁰ Y) and zirconium 90 ( ⁹⁰ Zr) produced by β-disintegration of strontium 90 can be removed as contaminants in the second purification step. For this reason, the radioactive substance which can inhibit the quantitative analysis of strontium 90 is hardly contained.

  Therefore, the radioactive strontium in the separation liquid of this embodiment can be quantitatively analyzed by β-ray measurement, ICP-MS measurement, or the like, as in the purified sample obtained by the conventional official method. Moreover, a qualitative analysis can also be performed by a well-known method as needed.

  In the method of the present embodiment, the following first preparation step and second preparation step are performed, and the amount of strontium in the liquid sample before performing the purification by the above-described two-stage column is 100%, after the purification. It is preferable to determine the recovery rate of strontium in the separation liquid. Thereby, the exact content of strontium 90 in the liquid sample can be calculated.

<First preparation process>
The first preparation step of the present embodiment includes a stable isotope of strontium (mass number 84 ( ⁸⁴ Sr), 86 ( ⁸⁶ Sr), 87 ( ⁸⁷ Sr), 88 ( ⁸⁸ Sr)) included in the liquid sample, This is a step of measuring at least one content X1 by mass spectrometry.
From the viewpoint of accurately obtaining the recovery rate of strontium, it is preferable to measure any two or more, and more preferably to measure any three or four.

  For example, strontium of each mass number in a liquid sample can be obtained by a known method using ICP-MS (inductively coupled plasma mass spectrometer).

Here, if strontium 90 ( ⁹⁰ Sr) in the liquid sample before purification can be quantified by ICP-MS, it is not necessary to purify as described above, and complicated purification steps in the conventional official method. Is also unnecessary. However, in practice, strontium 90 in the liquid sample before purification cannot be accurately quantified. This is because strontium 90 undergoes β decay, so that yttrium 90 and zirconium 90 may be contained in the liquid sample. In addition, the possibility that a radioisotope or a stable isotope of another element having a mass number of 90 is included cannot be denied. Therefore, it is necessary to obtain a separation liquid obtained by chemically purifying strontium as described above.

<Second preparation process>
The second preparation step of the present embodiment is a step of measuring the content X2 contained in the separated liquid with a mass spectrometer for the stable isotope species of strontium measured in the first preparation step.
It is preferable to measure by ICP-MS as in the first preparation step.

For a given strontium stable isotope species obtained in the above process,
“Content in liquid sample X1 ÷ Content in separation liquid X2 × 100 (%)” (1)
From the above formula, the recovery rate of strontium after purification can be calculated.

<Quantitative determination of strontium 90>
The element with a mass number of 90 contained in the separated liquid is mostly strontium 90, and other elements are removed by the purification process. Therefore, the content X3 of strontium 90 in the separation liquid is determined by ICP-MS measurement. Further, the content X3 of strontium 90 in the separation liquid is determined by β-ray measurement.

Subsequently, the content X4 of strontium 90 in the liquid sample before purification is calculated based on the recovery rate. For example, Formula (2);
“Content X4 = (Strontium 90 content X3 in the separation liquid) × (Content X1 ÷ Content X2)”
Can be calculated.

<Flowchart>
The procedure of the flowchart shown in FIG. 1 according to the present embodiment will be briefly described below. This procedure is an example of the radioactive strontium analysis method of this embodiment.

  First, 10 L of a sample solution containing strontium is obtained, filtered and weighed in the same manner as the official method. A portion of the filtrate (for example, 10 ml) is collected, and the stable isotope of strontium is quantified by ICP-MS. To the filtrate, 0.5 g of known Ca carrier and 1 mg of Sr carrier are added, and 200 ml of saturated ammonium oxalate solution is further added. Subsequently, strontium and calcium in the filtrate are precipitated by adjusting to pH 6 with aqueous ammonia. The precipitate is collected by a decantation method, a filtration method, or a centrifugal separation method, and heated at 500 ° C. for 6 hours to decompose or denature organic substances in the precipitate. After adding 50 ml of 8M nitric acid to the precipitate and sufficiently stirring, insoluble matters are removed by centrifugation to obtain about 50 ml of a liquid sample containing strontium and calcium (Ca carrier).

  Next, about 50 ml of the liquid sample is introduced into the Sr resin (column volume: about 5 ml) to adsorb strontium, and almost all of the ions of calcium, barium, radium, and iron that are difficult to adsorb to the Sr resin together with the effluent. Remove. After washing the Sr resin with 20 ml of 8 M nitric acid, 20 ml of 0.01 M nitric acid is introduced to obtain an eluate containing strontium eluted from the Sr resin. About 20 ml of sample solution adjusted to 2 M nitric acid by adding concentrated nitric acid to the eluate is introduced into TRU resin (column volume: about 2 ml), and transition metals, zirconium, yttrium, uranium, etc. that can be contained as contaminants are added to TRU resin. And strontium hardly adsorbed on the TRU resin is discharged from the column to obtain a separation liquid containing strontium.

  The separated solution is weighed, a part of the separated solution (for example, 10 ml) is collected, and the stable isotope of strontium is quantified by ICP-MS. Based on the strontium content before purification and the strontium content after purification, the recovery rate of strontium is determined.

  The radioactive strontium in the separation liquid can be quantified by measuring the β-ray of the separation liquid. At this time, it may be concluded that most of the β-rays are derived from strontium 90 based on the half-life, the source of the sample, and the like. Further, strontium 90 in the separation liquid can be quantified by ICP-MS measurement. Since the zirconium 90 and the yttrium 90 are removed by the TRU resin, it can be determined that the substance having a mass number of 90 is strontium 90.

  Based on the strontium 90 content in the quantified separation liquid and the strontium recovery rate, the strontium 90 content in the original liquid sample (about 50 ml) is calculated. Furthermore, based on the known concentration rate, the content of strontium 90 in 10 liters of the original sample solution is calculated.

  As mentioned above, although embodiment of the analysis method of radioactive strontium by this invention was described, this invention is not limited to said embodiment, In the range which does not deviate from the meaning, it can change suitably. It is possible to appropriately replace the constituent elements in the embodiments described above with known constituent elements.

[Example 1]
A nonflammable decontamination waste (soil) containing 15.04 g of strontium 90 was dried at 110 ° C. for 24 hours, and then dried at 500 ° C. for 22 hours to obtain an ashed sample.
Place the sample in a pressure bottle, add 500 mg of Ca carrier (compound name: calcium chloride), 1 mg of Sr carrier (compound name: strontium chloride), 40 ml of 8M nitric acid, boil for 4 hours to evaporate the water to about 10 ml. A concentrated liquid sample was obtained.

The stable isotope of strontium (isotopic species: ⁸⁸ Sr) contained in the liquid sample was quantified by ICP-MS (manufactured by Agilent).

The above liquid sample is passed through a column packed with Sr resin (manufactured by Eichrom Technologies) to adsorb the strontium in the liquid sample to the Sr resin, and the calsim and other contaminants in the liquid sample flow out of the column. I let you.
The Sr resin was washed with 20 ml of 8M nitric acid, and then 20 ml of 0.01M nitric acid was passed through the column to obtain an eluate containing strontium.

  The above eluate is passed through a column packed with TRU resin (manufactured by Eichrom Technologies), and zirconium 90 and yttrium 90, zirconium and yttrium produced by β-disintegration of strontium 90 that may be contained in the eluate. Were adsorbed to TRU resin, and strontium in the eluate was allowed to pass out of the column, and the effluent fraction was obtained as a separation liquid.

The stable isotope of strontium (isotopic species: ⁸⁸ Sr) contained in the separated liquid was quantified by the above ICP-MS.
The recovery rate of strontium obtained through a series of purification treatments was strontium content in the separation liquid ÷ strontium content in the liquid sample × 100% = 73%.

The β-ray measurement of a measurement sample obtained by evaporating the separated liquid to dryness and redissolving with a small amount of hydrochloric acid was performed by a conventional method using a liquid scintillation detector (manufactured by Hitachi Aloka).
Since the radioactive substance contained in the separation liquid after the above purification treatment is considered to be only strontium 90, it was considered that the observed β-rays were derived only from strontium 90.

  From the strontium recovery rate calculated above, the content of strontium 90 contained in the incombustible decontamination waste is (100% ÷ recovery rate 73%) times that of strontium 90 contained in the separation liquid. I was able to conclude. The results of Example 1 are shown in Table 1.

[Example 2]
Quantitative analysis of strontium 90 was performed in the same manner as in Example 1 using 16.64 g of flammable decontamination waste (field hay) containing strontium 90. The results are shown in Table 1.
[Example 3]
Quantitative analysis of strontium 90 was performed in the same manner as in Example 1 using 17.38 g of combustible decontamination waste (forest forest hay) containing strontium 90. The results are shown in Table 1.

[Example 4]
To 3 liters of leachate containing strontium 90 obtained from the decontamination area, 500 mg of Ca carrier (compound name: calcium chloride) and 1 mg of Sr carrier (compound name: strontium chloride) are added, and 200 mL of saturated aqueous oxalic acid solution is added. Strontium and calcium containing strontium 90 were precipitated. The precipitate collected using the filter paper was baked in an electric furnace at 500 ° C. to decompose organic substances contained in the precipitate. The obtained fired product was dissolved in 20 ml of 8M nitric acid, and the insoluble matter was removed by centrifugation to obtain a liquid sample.

The stable isotope of strontium (isotopic species: ⁸⁸ Sr) contained in the liquid sample was quantified by ICP-MS (manufactured by Agilent).

  In the same manner as in Example 1, the liquid sample was purified using a column packed with Sr resin and a column packed with TRU resin in order to obtain a separated liquid.

The stable isotope of strontium (isotopic species: ⁸⁸ Sr) contained in the separated liquid was quantified by the above ICP-MS.
The recovery rate of strontium obtained through a series of purification treatments was strontium content in the separation liquid ÷ strontium content in the liquid sample × 100% = 68%.

The β-ray measurement of a measurement sample obtained by evaporating the separated liquid to dryness and redissolving with a small amount of hydrochloric acid was performed by a conventional method using a liquid scintillation detector (manufactured by Hitachi Aloka).
Since the radioactive substance contained in the separation liquid after the above purification treatment is considered to be only strontium 90, it was considered that the observed β-rays were derived only from strontium 90.

  From the strontium recovery rate calculated above, the content of strontium 90 contained in the incombustible decontamination waste is (100% ÷ recovery rate 68%) times that of strontium 90 contained in the separation liquid. I was able to conclude. The results of Example 4 are shown in Table 2.

[Example 5]
Quantitative analysis of strontium 90 was performed in the same manner as in Example 4 using 3 liters of leachate containing strontium 90 obtained from a decontamination area different from that in Example 4. The results are shown in Table 2.

  From the above results, it was confirmed that by using Sr resin and TRU resin in combination, strontium contained in the analysis sample was purified to high purity, and strontium 90 could be analyzed qualitatively and quantitatively.

  The configurations and combinations thereof in the embodiments described above are examples, and the addition, omission, replacement, and other modifications of the configurations can be made without departing from the spirit of the present invention.

  The present invention can be widely applied to the field of handling radioactive materials.

Claims (2)

A liquid sample containing strontium and one or more contaminants is brought into contact with the first adsorbent, strontium in the liquid sample is adsorbed on the first adsorbent, and then the liquid sample and the first adsorbent are separated. A first purification step of removing at least one of the contaminants together with the liquid sample;
An elution step of bringing an elution chemical solution into contact with the first adsorbent to obtain an eluate containing strontium eluted from the first adsorbent;
The strontium containing strontium after contacting the eluate with a second adsorbent capable of adsorbing the contaminants that may remain in the eluate and having a property of hardly adsorbing strontium Separating the eluate from the second adsorbent, removing the contaminant together with the second adsorbent, and obtaining a separation liquid containing strontium;
A analysis process and analysis method of radioactive strontium that have a that the separation liquid qualitatively or quantitatively analyze radioactive strontium contained in,
A first preparation step of measuring the content X1 of at least one of the stable isotopes of strontium contained in the liquid sample with a mass spectrometer;
For the stable isotope species of strontium measured in the first preparation step, the second preparation step of measuring the content X2 contained in the separated liquid with a mass spectrometer,
By the following formula (1)
Content X1 ÷ Content X2 x 100% (1)
Calculate the strontium recovery rate,
The radioactive strontium content in the separated liquid is quantified by mass spectrometry or radiation measurement, and the radioactive strontium content contained in the liquid sample is obtained based on the recovery rate. Analysis method. A liquid sample containing strontium and calcium is brought into contact with the first adsorbent, and after the strontium in the liquid sample is adsorbed on the first adsorbent, the liquid sample and the first adsorbent are separated, and calcium is A first purification step to be removed together with the liquid sample;
An elution step of bringing an elution chemical solution into contact with the first adsorbent to obtain an eluate containing strontium eluted from the first adsorbent;
The elution containing strontium after contacting the eluate with a second adsorbent capable of adsorbing contaminants that may be mixed in the eluate and having a property of hardly adsorbing strontium Separating the liquid and the second adsorbent, removing the contaminant together with the second adsorbent, and obtaining a separation liquid containing strontium;
The method for analyzing radioactive strontium according to claim 1, further comprising an analysis step for qualitatively or quantitatively analyzing strontium 90 contained in the separated liquid.

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