CN111856546B - Sample preparation method for radiochemical analysis of Cs-137 in marine organism ash - Google Patents
Sample preparation method for radiochemical analysis of Cs-137 in marine organism ash Download PDFInfo
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Abstract
The invention provides a sample preparation method for Cs-137 radiochemical analysis in marine organism ash, which comprises the following steps: weighing a gray sample, and adding a cesium carrier for ashing; leaching the ash sample twice by using 6-9Mol/L concentrated nitric acid, filtering or centrifuging after leaching and cooling, and combining the filtrates; adding a proper amount of ammonium phosphomolybdate into the filtrate, and keeping the precipitate; dissolving ammonium phosphomolybdate with high-concentration sodium hydroxide solution, and collecting filtrate; adjusting the volume and the Ph value of the filtrate by using distilled water and nitric acid, and adding masking agent citric acid; evaporating the solution on a low-temperature electric heating plate until the solution is nearly dry, and observing the solution after cooling; if the solution is not turbid and is not solidified, putting the solution in an ice water bath, adding glacial acetic acid and a sodium iodobismuthate solution, and observing; and if no reddish brown gel exists, preparing a source, measuring, and calculating to obtain the activity concentration of the Cs-137 in the sample. The method provided by the invention can avoid turbidity and solidification in the process of adding citric acid, ensures that cesium iodobismuthate is precipitated and successfully prepared, has the source preparation success rate of 100 percent, is favorable for radioactivity measurement, and ensures that the analysis result is more accurate and reliable.
Description
Technical Field
The invention belongs to the technical field of radiation environment monitoring, and particularly relates to a sample preparation method for Cs-137 radiochemical analysis in marine organism ash.
Background
The artificial radionuclide Cs-137 is mainly derived from nuclear tests, nuclear fuel post-treatment, nuclear reactors and nuclear accident disasters, has a half-life of about 30 years, and is a toxic nuclide which is one of important radionuclides in environmental monitoring. With the construction and application of coastal nuclear power stations in China, the continuous emission of artificial radioactive nuclides can increase the radioactivity level of offshore marine organisms and ecological systems thereof, thereby causing harm to human health. Through the monitoring of marine radionuclide, the condition that the sea is polluted by radioactivity can be known, and marine organisms can concentrate a plurality of radioactive elements and carry out radioactivity measurement on the radioactive elements, so that the condition that the living sea area of the marine organisms is polluted can be better reflected. Secondly, the marine products are one of the human food sources, and in order to prevent the radioactive substances from causing harm to people through the seafood, regular radioactive monitoring of the seafood is necessary. In addition, through investigation, the transfer of the radioactive substance by marine organisms can be known, so that the movement law of the radioactive substance after entering the sea can be revealed.
In the method, ammonium phosphomolybdate is adopted to concentrate cesium, and cesium iodobismuthate is generated under the action of masking agent citric acid and under the conditions of high purity glacial acetic acid and sodium iodobismuthate for beta measurement. The standard method for radiochemical analysis of cesium-137 in biological sample ash, GB 11221-89, was drafted by sandanmao et al, the institute for radiation protection, china (laboratory), which used large amounts of land-based plant ash and small amounts of animal ash for method validation.
The method itself has certain limitations in the application of marine biological samples. Crustaceans, molluscs, fishes, seaweeds and the like, such as crabs, shrimps, squid, shells, sea fish, lithospermum, kelp and other marine organism samples, are subject to sample preparation failure according to Cs-137 analyzed in the industrial standard HJ 816-2016, with a probability of more than 60%. A great deal of practical experience shows that the content of halogen elements and other elements of marine organisms is greatly different from that of terrestrial organisms, citric acid is a bismuth masking agent and is also a gelling agent, and turbidity and solidification phenomena can occur in the process of carefully evaporating citric acid added in the actual operation process, and if the phenomenon even occurs in the process of precipitating cesium iodobismuthate.
The success rate of sample preparation strictly in accordance with the radiochemical analysis method for cesium-137 in water and biological sample ash (HJ816-2016) is very low, and the cesium iodobismuthate precipitate source contains a large amount of impurities. The impurities of the measuring source are not beneficial to the accurate measurement of the radioactivity. Therefore, it is necessary to provide a sample preparation method for the radiochemical analysis of Cs-137 in marine organism ash to solve the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the sample preparation method for the radiochemical analysis of the Cs-137 in the marine organism ash, which can avoid the phenomena of turbidity and solidification in the process of adding citric acid, ensure the success of preparing the source by precipitating cesium iodobismuthate, ensure the success rate of preparing the source to be 100 percent, be beneficial to the radioactive measurement and ensure that the analysis result is more accurate and reliable.
In order to achieve the above purposes, the invention adopts a technical scheme that: a method of sample preparation for radiochemical analysis of Cs-137 in marine bioash, said method comprising:
(1) weighing an ash sample, and adding a cesium carrier for ashing;
(2) leaching the ash sample twice by using 6-9Mol/L concentrated nitric acid, filtering or centrifuging after leaching and cooling, and combining the filtrates;
(3) adding a proper amount of ammonium phosphomolybdate into the filtrate, stirring, removing the filtrate, and keeping the precipitate;
(4) Dissolving ammonium phosphomolybdate with high-concentration sodium hydroxide solution, and collecting filtrate;
(5) adjusting the volume and the pH value of filtrate by using distilled water and nitric acid, and adding masking agent citric acid;
(6) repeating the steps (3) to (5), evaporating the solution on a low-temperature electric heating plate until the solution is nearly dry, and observing whether the phenomena of turbidity, solidification and salt crystallization appear after cooling;
(7) if the turbid and solidification phenomena do not occur, placing the solution in an ice water bath, adding glacial acetic acid and a sodium iodobismuthate solution, continuously stirring the glass rod with a wall brush until cesium iodobismuthate precipitates, placing the glass rod in the ice water bath, and observing whether reddish brown gel appears or not;
(8) if no reddish brown gel exists, the source preparation and the measurement are carried out according to the requirements of HJ 816-2016, and the activity concentration of the Cs-137 in the sample is calculated.
Further, the step (7) further comprises: and (5) if the phenomena of turbidity, solidification and salt crystallization occur, transferring the solution in the beaker to a large-capacity beaker, diluting the solution to 250mL by using distilled water, adding concentrated nitric acid, repeating the steps (3) to (5), and adsorbing cesium by using ammonium phosphomolybdate again.
Further, the step (8) further comprises: if a reddish brown gel appears, 50mL of nitric acid (1+9) is added, after heating to evaporate iodine, the mixture is cooled and transferred to an appropriate large beaker, and then 100mL of nitric acid (1+9) is added, and steps (6) to (7) are repeated.
Further, 10-20 mg of ash sample is taken in the step (1), and 30-60 mg of cesium carrier is taken.
Further, the volume of the leachate in the step (2) is controlled to be 300mL, and the leachate is diluted to 1500mL by using distilled water so as to ensure that the ammonium phosphomolybdate adsorption system is about nitric acid (1+ 9).
Further, 2 plus or minus 0.2g of ammonium phosphomolybdate is added in the step (3).
Further, in the step (4), the concentration range of the high-concentration sodium hydroxide solution is as follows: 8-12Mol/L, stopping adding ammonium phosphomolybdate when ammonium phosphomolybdate is dissolved, and controlling the sodium hydroxide solution to be less than 5 mL.
Further, solid citric acid which is equal to the ammonium phosphomolybdate in the step (3) is added in the step (5).
Further, the pH value of the filtrate adjusted in the step (5) is less than 2, and the volume is 250 ml.
Further, the pH value of the filtrate adjusted in the step (5) is less than 2, and the volume is 250 ml.
Further, the precipitation process should be washed with glacial acetic acid several times in a small amount in the step (7).
The method has the advantages that the method can avoid turbidity and solidification in the process of adding citric acid, ensure the success of cesium iodobismuthate precipitation source preparation, ensure the success rate of source preparation to be 100 percent, be beneficial to radioactive measurement and ensure more accurate and reliable analysis results.
Drawings
FIG. 1 is a schematic flow chart of an embodiment of a sample preparation method for Cs-137 radiochemical analysis in marine organism ash according to the present invention.
Detailed Description
In order to make the technical problems solved, the technical solutions adopted, and the technical effects achieved by the present invention clearer, the technical solutions of the embodiments of the present invention will be further described in detail with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Referring to fig. 1, fig. 1 is a schematic technical route of an embodiment of a sample preparation method for radiochemical analysis of Cs-137 in marine organism ash according to the present invention. The invention provides a sample preparation method for Cs-137 radiochemical analysis in marine organism ash, which comprises the following steps:
(1) weighing the ash sample, and adding cesium carrier for ashing.
Wherein 10-20 mg of the ash sample is taken, and 30-60 mg of the cesium carrier is taken. Ashing is performed as required for HJ 816-2016, e.g., ashing of cesium at 450 ℃ or below is pretreated.
(2) Leaching the ash sample twice by using 6-9Mol/L concentrated nitric acid, filtering or centrifuging after leaching and cooling, and combining the filtrates.
The method specifically comprises the following steps: the volume of the leachate was controlled at 300mL and diluted to 1500mL with distilled water to ensure that the ammonium phosphomolybdate adsorption system was about nitric acid (1+ 9).
It should be noted that in the prior art, the (1+9) nitric acid is used for leaching once, and the hot solution is filtered. In order to fully leach the Cs-137 in the ash sample, on one hand, high-concentration acid is adopted for twice leaching, and the filtering is carried out only under the condition of cooling, silicate is precipitated after cooling, a large amount of silicate is brought into a leaching solution after hot filtering, and the success rate of subsequent sample preparation is seriously influenced. On the other hand, the adoption of large-volume ammonium phosphomolybdate adsorption can avoid the phenomena of turbidity, solidification and salt crystallization during the process of adding citric acid when small-volume ammonium phosphomolybdate is adsorbed.
(3) Adding a proper amount of ammonium phosphomolybdate into the filtrate, stirring, removing the filtrate, and keeping the precipitate.
In a particular embodiment, the ammonium phosphomolybdate is added in an amount of 2. + -. 0.2 g.
(4) Dissolving ammonium phosphomolybdate with high concentration sodium hydroxide solution, and collecting filtrate.
The concentration range of the high-concentration sodium hydroxide solution is as follows: 8-12Mol/L, stopping adding ammonium phosphomolybdate when ammonium phosphomolybdate is dissolved, and controlling the sodium hydroxide solution to be less than 5 mL. It is noted that the HJ 816-2016 standard utilizes a low concentration sodium hydroxide solution.
(5) The filtrate volume and the pH value are adjusted by distilled water and nitric acid, and then masking agent citric acid is added.
Adding solid citric acid with the same amount of ammonium phosphomolybdate in the step (3).
The adjusted filtrate had a pH of less than 2 and a volume of 250 ml.
(6) And (5) repeating the steps (3) to (5), evaporating the solution on a low-temperature electric heating plate until the solution is nearly dry, and observing whether the phenomena of turbidity, solidification and salt crystallization appear after cooling.
In one embodiment, the solution is evaporated to 5-8ml on a low temperature hot plate to ensure that the concentration of glacial acetic acid added meets the sample preparation requirements.
(7) If the turbid and solidification phenomena do not occur, placing the solution in an ice water bath, adding glacial acetic acid and a sodium iodobismuthate solution, continuously stirring the glass rod with a wall brush until cesium iodobismuthate precipitates, placing the glass rod in the ice water bath, and observing whether reddish brown gel appears or not;
at this time, the precipitation process should be washed several times with glacial acetic acid in a small amount.
The method further comprises the following steps: and (3) if the phenomena of turbidity, solidification and salt crystallization occur, transferring the solution in the beaker to a large-capacity beaker, diluting the solution to 250mL by using distilled water, adding 2mL of concentrated nitric acid, repeating the steps (3) to (5), and adsorbing cesium by using ammonium phosphomolybdate again.
Note that the second adsorption is shifted to a small volume adsorption. In addition, in this time, the amount of ammonium phosphomolybdate added to adsorb cesium was 0.8g, which was consistent with the HJ 816-2016 standard.
8) If no reddish brown gel exists, the source preparation and measurement are carried out according to the requirements of HJ816-2016, and the activity concentration of the Cs-137 in the sample is calculated.
This step further includes: if a reddish brown gel appears, 50mL of nitric acid (1+9) is added, after heating to evaporate iodine, the mixture is cooled and transferred to an appropriate large beaker, and then 100mL of nitric acid (1+9) is added, and steps (6) to (7) are repeated.
The invention adopts the high-success-rate sample preparation technology when carrying out radiochemical analysis on the marine organism ash Cs-137. The success rate of sample preparation strictly in accordance with the radiochemical analysis method for cesium-137 in water and biological sample ash (HJ816-2016) is only 20%, and even if the sample preparation is successful, the recovery rate is more than 120% because the cesium iodobismuthate precipitation source contains a large amount of impurities. The impurities of the measuring source are not beneficial to the accurate measurement of radioactivity.
The technology avoids the phenomena of turbidity, solidification and salt crystallization during the process of adding citric acid during the adsorption of small-volume ammonium phosphomolybdate, effectively ensures the success rate of cesium iodobismuthate precipitation source preparation, has the source preparation success rate of nearly 100 percent, is favorable for radioactivity measurement, ensures more accurate and reliable analysis results, and can be applied to the conventional analysis and detection work of marine organism ash Cs-137. The details are as follows.
TABLE 110 samples HJ 816 and the success rate of source preparation and the whole-course recovery rate of the technology
Table 1 lists 10 samples of HJ 816 and the success rate of source production and overall recovery rate of the technique.
(I) two times adsorption of large volume ammonium phosphomolybdate
The method is used for the sea fish such as the turbot and the sea bass, more than half of marine organisms are adsorbed by the large-volume ammonium phosphomolybdate twice, and the sample preparation can be successfully carried out, and the recovery rate is more than 85 percent.
(II) three times adsorption of large volume ammonium phosphomolybdate
The soft bodies such as oysters and seaweed such as purple vegetables adopt the technology, the samples can be successfully prepared only by adopting large-volume ammonium phosphomolybdate for three times of adsorption, and the phenomena of turbidity, solidification and salt crystallization appear in the evaporation process of the citric acid after cooling. The recovery rate of the third adsorption is more than 70%.
(III) four-time adsorption of large-volume ammonium phosphomolybdate
The phenomenon of turbidity, solidification and salt crystallization of a few marine products such as certain shrimps in the citric acid evaporation process after cooling is still red brown gel in the source preparation stage after three times of adsorption. The source can be successfully prepared only by four times of adsorption, and the recovery rate is about 50 percent.
Different from the prior art, the sample preparation method for the radiochemical analysis of the Cs-137 in the marine organism ash provided by the invention adopts large-volume ammonium phosphomolybdate for multiple adsorption, avoids the phenomena of turbidity, solidification and salt crystallization in the process of adding citric acid during the adsorption of small-volume ammonium phosphomolybdate, effectively ensures the success rate of preparing the source by precipitating cesium iodobismuthate, is close to 100 percent, is favorable for radioactive measurement, ensures that the analysis result is more accurate and reliable, and can be applied to the conventional analysis and detection work of the marine organism ash Cs-137.
It will be appreciated by persons skilled in the art that the method of the present invention is not limited to the examples described in the specific embodiments, and that the above detailed description is for the purpose of illustrating the invention only and is not intended to limit the invention. Other embodiments will be apparent to those skilled in the art from the following detailed description, which is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing a sample for radiochemical analysis of Cs-137 in marine organism ash, said method comprising:
(1) weighing an ash sample, and adding a cesium carrier for ashing;
(2) leaching the ash sample twice by using 6-9Mol/L concentrated nitric acid, filtering or centrifuging after leaching and cooling, and combining the filtrates;
(3) adding a proper amount of ammonium phosphomolybdate into the filtrate, stirring, removing the filtrate, and keeping the precipitate;
(4) dissolving ammonium phosphomolybdate with high-concentration sodium hydroxide solution, and collecting filtrate;
(5) adjusting the volume and the Ph value of the filtrate by using distilled water and nitric acid, and adding masking agent citric acid;
(6) repeating the steps (3) to (5), evaporating the solution on a low-temperature electric heating plate, and observing whether the phenomena of turbidity, solidification and salt crystallization appear after cooling;
(7) if the turbid and solidification phenomena do not occur, placing the solution in an ice water bath, adding glacial acetic acid and a sodium iodobismuthate solution, continuously stirring the glass rod with a wall brush until cesium iodobismuthate precipitates, placing the glass rod in the ice water bath, and observing whether reddish brown gel appears or not;
(8) If no reddish brown gel exists, the source preparation and measurement are carried out according to the requirements of HJ 816-2016, and the activity concentration of the Cs-137 in the sample is calculated.
2. The method of claim 1, wherein step (7) further comprises: and (5) if the phenomena of turbidity, solidification and salt crystallization occur, transferring the solution in the beaker to a large-capacity beaker, diluting the solution to 250mL by using distilled water, adding concentrated nitric acid, repeating the steps (3) to (5), and adsorbing cesium by using ammonium phosphomolybdate again.
3. The method of claim 1, wherein step (8) further comprises: if a reddish brown gel appears, 50mL of nitric acid (1+9) is added, after heating to evaporate iodine, the mixture is cooled and transferred to an appropriate large beaker, and then 100mL of nitric acid (1+9) is added, and steps (6) to (7) are repeated.
4. The method according to claim 1, wherein 10-20 mg of the ash sample and 30-60 mg of the cesium carrier are used in the step (1).
5. The method according to claim 1, wherein the volume of the leachate in the step (2) is controlled to be 300mL, and the leachate is diluted with distilled water to 1500 mL.
6. The method of claim 1, wherein 2 ± 0.2g of ammonium phosphomolybdate is added in step (3).
7. The method according to claim 1, wherein the concentration range of the high-concentration sodium hydroxide solution in the step (4) is as follows: 8-12Mol/L, stopping adding ammonium phosphomolybdate when ammonium phosphomolybdate is dissolved, and controlling the sodium hydroxide solution to be less than 5 mL.
8. The method of claim 1, wherein an amount of solid citric acid equivalent to the amount of ammonium phosphomolybdate in step (3) is added in step (5).
9. The method of claim 1, wherein the adjusted pH of the filtrate of step (5) is less than 2 and has a volume of 250 ml.
10. The method according to claim 1, wherein the precipitation process is washed with glacial acetic acid in step (7) several times in small amounts.
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