Method for determining components of solution for removing boron and method for reducing memory effect of boron isotope test by adopting solution

Abstract

The embodiment of the invention relates to the technical field of solution treatment by adopting an ion exchange method, in particular to a method for determining components of a solution for removing boron and a method for reducing a memory effect of a boron isotope test by adopting the solution. In one aspect, the embodiment of the invention provides a method for determining components of a solution for removing boron, and the solution is suitable for removing boron residues in a pipeline of a mass spectrometer; in the second aspect, the embodiment of the invention further provides a method for reducing the memory effect of the boron isotope test, and the solution with the components determined according to the method in the first aspect of the application is adopted. By means of the method, the boron removal solution which can stably and effectively remove boron residues, cannot generate new residue problems and is short in consumed time can be obtained, in the boron isotope test, the solution is used for cleaning a pipeline, the boron residues of the last test can be rapidly eliminated, the situation that the boron residues interfere with the test result of the next test is avoided, and the test efficiency is improved. Therefore, the test memory effect is reduced, and the test precision is improved.

Description

Technical Field

[0001] Embodiments of the present application relate to the technical field of treating solutions by ion exchange, and in particular to a method for determining the composition of a solution for removing boron and a method for reducing the memory effect of a boron isotope test by using the solution. Background Art

[0002] The statements herein merely provide background information related to the present application and do not necessarily constitute prior art.

[0003] Boron has two stable isotopes 10 B and 11 B, the relative mass of the two is relatively large, so it is often used as a stable isotope tracer in the fields of chemistry, environment, and earth. In order to determine the abundance of boron isotopes, boron isotope testing methods such as thermal ionization mass spectrometry, inductively coupled plasma mass spectrometry, multi-collector inductively coupled plasma mass spectrometry and secondary ion mass spectrometry are usually used. Among them, multi-collector inductively coupled plasma mass spectrometry is widely used because of its liquid injection and applicable sample types.

[0004] However, there are still many problems in the process of using multi-collector inductively coupled plasma mass spectrometry to test boron isotopes, which affect the accuracy and stability of boron isotope test results. Summary of the invention

[0005] A brief overview of the present application is provided below in order to provide a basic understanding of certain aspects of the present application. It should be understood that this overview is not an exhaustive overview of the present application. It is not intended to identify the key or important parts of the present application, nor is it intended to limit the scope of the present application. Its purpose is merely to present certain concepts in a simplified form as a prelude to a more detailed description discussed later.

[0006] In a first aspect, an embodiment of the present application provides a method for determining the composition of a solution for removing boron, wherein the solution is suitable for removing boron residues in a pipeline of a mass spectrometer, and the method comprises the following steps: S10: preparing a boron solution for testing, and inputting the boron solution into the pipeline until the mass spectrometer obtains a stable boron isotope signal and stops; S20: adding a predetermined amount of methanol to deionized water, and mixing them evenly to obtain a first mixed solution; S30: inputting the first mixed solution into the pipeline, and recording the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t 1 ; S40: adding a predetermined amount of propylene glycol to the first mixed solution, mixing evenly to obtain a second mixed solution; S50: repeating step S10, inputting the second mixed solution into the pipeline, and recording the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t 2; S60: adding a predetermined amount of ammonium fluoride to the second mixed solution, mixing evenly to obtain a third mixed solution; S70: repeating step S10, inputting the third mixed solution into the pipeline, and recording the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t 3 ; S80: Compare t 1 ,t 2 and t 3 , based on the comparison results, determine the composition of the solution for removing boron.

[0007] In a second aspect, an embodiment of the present application further provides a method for reducing the memory effect of boron isotope testing, which uses a solution whose composition is determined by the method according to any embodiment of the first aspect of the present application.

[0008] Through the method in the embodiments of the present application, a solution can be obtained that can stably and effectively remove boron residues without causing new residue problems and that consumes a short time to remove boron. During the boron isotope test, the pipeline is cleaned with the solution in the interval between each two times the sample to be tested is input into the pipeline, which can quickly eliminate the boron residues from the previous test and avoid interfering with the test results of the next test, thereby reducing the memory effect of the test and improving the test accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Other objects and advantages of the present application will become apparent from the following description of the embodiments of the present application with reference to the accompanying drawings, and will help to provide a comprehensive understanding of the present application.

[0010] Figure 1 The present invention is a flowchart of a method for determining the composition of a solution for removing boron according to an embodiment of the present application.

[0011] It should be noted that the drawings are not necessarily drawn to scale, but are merely shown in a schematic manner that does not affect the reader's understanding. DETAILED DESCRIPTION

[0012] Exemplary embodiments of the present application will be described below in conjunction with the accompanying drawings. For the sake of clarity and conciseness, not all features of the actual implementation are described in the specification. However, it should be understood that many implementation-specific decisions must be made in the process of developing any such actual implementation in order to achieve the developer's specific goals, such as meeting those constraints related to the system and business, and these constraints may vary from implementation to implementation. In addition, it should be understood that although the development work may be very complex and time-consuming, it is only a routine task for those skilled in the art who benefit from the content of this application.

[0013] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, only the device structure and / or processing steps closely related to the scheme according to the present application are shown in the accompanying drawings, while other details that are not very relevant to the present application are omitted.

[0014] The inventors of the present application have discovered that, during the boron isotope testing process, the sample to be tested is prone to remain in the pipeline of the mass spectrometer, affecting the test results of subsequent samples. For this reason, a measure usually taken is to clean the pipeline with a boron removal solution after the sample test is completed. However, the boron removal solutions commonly used at present, such as nitric acid, dilute ammonia water, dilute ammonium nitrate or mannitol solutions, have problems such as unpredictable removal effects, low efficiency and easy to cause new residues.

[0015] Based on this, an embodiment of the present application provides a method for determining the composition of a solution for removing boron, wherein the solution is suitable for removing boron residues in a pipeline of a mass spectrometer, such as Figure 1 As shown, Figure 1 A flow chart showing a method for determining the composition of a solution for removing boron according to an embodiment of the present application is shown. The method includes the following steps S10 to S80:

[0016] S10: Prepare a boron solution for testing, and inject the boron solution into the pipeline until the mass spectrometer obtains a stable boron isotope signal.

[0017] S20: adding a predetermined amount of methanol into deionized water, and mixing them evenly to obtain a first mixed solution.

[0018] S30: The first mixed solution is introduced into the pipeline, and the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value is recorded as t 1 .

[0019] S40: adding a predetermined amount of propylene glycol to the first mixed solution, and mixing them evenly to obtain a second mixed solution.

[0020] S50: Repeat step S10, input the second mixed solution into the pipeline, and record the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t 2 .

[0021] S60: adding a predetermined amount of ammonium fluoride to the second mixed solution, and mixing them evenly to obtain a third mixed solution.

[0022] S70: Repeat step S10, input the third mixed solution into the pipeline, and record the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t 3 .

[0023] S80: Comparison 1 ,t 2and t 3 , based on the comparison results, determine the composition of the solution for removing boron.

[0024] The method provided in the embodiment of the present application utilizes the characteristics that ammonium fluoride has a good boron elimination effect without residue, alcohol reagents have a good lipidization effect on boron and have no residue themselves, and alcohol reagents and fluorides have a synergistic effect on boron elimination. Predetermined amounts of methanol, glycerol and ammonium fluoride are added to deionized water in sequence, and are respectively input into the pipeline with residual test boron solution, and the time consumed by the mixed solutions of three different components to remove boron in the pipeline is obtained. By comparing the time, it is determined which solution has the best boron removal effect, thereby obtaining a boron removal solution that can stably and effectively remove boron residues without causing new residue problems and consumes a short time.

[0025] In some embodiments, in step S10, the boron solution used for testing is a boron solution with a concentration of 1.0 μg / ml to simulate the sample to be tested in the actual boron isotope test. On this basis, an experiment is conducted to determine the composition of the solution for removing boron, thereby ensuring the effectiveness and accuracy of the experiment, so that the solution with the composition determined by the experiment can be used for actual testing to effectively remove boron residues in the pipeline.

[0026] In step S10, when the boron solution is input into the pipeline, a peristaltic pump may be used to pump the boron solution into the pipeline so that the boron solution can be stably input into the pipeline at a predetermined flow rate and speed, so that the mass spectrometer can obtain a stable isotope signal.

[0027] In some embodiments, in step S20, the ratio of the content of methanol to deionized water in the first mixed solution is 1:10, for example, when the content of methanol in the first mixed solution is 50 ml, the content of deionized water is 500 ml. The first mixed solution prepared according to the ratio in this embodiment can achieve a better removal effect of boron residue than the currently commonly used solution.

[0028] In some embodiments, in step S40, the ratio of the content of methanol to glycerol in the second mixed solution is 5:1. For example, when the deionized water in the second mixed solution is 500 ml, the content of methanol is 50 ml and the content of glycerol is 10 g. In this embodiment, the alcohol reagent has a good esterification effect on boron and has no residue. Another alcohol reagent is added to the first mixed solution, so that the second mixed solution can achieve a better removal effect on boron residue than the first mixed solution.

[0029] In step S40, the following steps may also be included:

[0030] S41: adjusting a predetermined amount of glycerol to obtain a second mixed solution having different contents of multiple components.

[0031] S42: Introduce a plurality of second mixed solutions into the pipelines respectively, and record a plurality of times consumed for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value.

[0032] S43: Compare multiple times and determine the predetermined amount of glycerol according to the comparison result.

[0033] In this embodiment, under the condition that the composition of the first mixed solution remains unchanged, the predetermined amount of glycerol is changed to determine the content of glycerol in the second mixed solution that is most effective in removing boron residues.

[0034] In some embodiments, in step S40, it further includes:

[0035] S41: adding a predetermined amount of methanol as in step S20 into deionized water to re-prepare the first mixed solution.

[0036] S42: adding a predetermined amount of propylene glycol to the re-prepared first mixed solution, and mixing them evenly to obtain a second mixed solution.

[0037] In this embodiment, the first mixed solution with the same composition as step S20 is re-prepared, and the second mixed solution is prepared based on the first mixed solution that has not been tested, so as to avoid using the tested solution to affect the boron removal effect of the second mixed solution and ensure the test accuracy.

[0038] In some embodiments, in step S60, it further includes:

[0039] S61: adding the same predetermined amount of methanol as in step S20 into deionized water to re-prepare the first mixed solution.

[0040] S62: adding the same predetermined amount of propylene glycol as in step S40 to the reconstituted first mixed solution, and mixing them evenly to obtain a reconstituted second mixed solution.

[0041] S63: adding a predetermined amount of ammonium fluoride to the re-prepared second mixed solution, and mixing them evenly to obtain a third mixed solution.

[0042] In this embodiment, by re-preparing the first mixed solution with the same ingredients as in step S20, re-preparing the second mixed solution with the same ingredients as in step S40 on the basis of the first mixed solution, and preparing the third mixed solution on the basis of the second mixed solution, the use of solutions that have been tested is avoided, interference factors are further eliminated, and the test accuracy is ensured.

[0043] In some embodiments, in step S60, the content ratio of methanol, glycerol and ammonium fluoride in the third mixed solution is 10:2:1. For example, when the deionized water in the third mixed solution is 500 ml, the methanol is 50 ml, the glycerol is 10 g, and the ammonium fluoride is 5 g. In this embodiment, the ammonium fluoride is added to the second mixed solution by utilizing the good elimination effect of ammonium fluoride on boron without residue and the synergistic effect of fluoride and alcohol reagents on the elimination of boron, so that the third mixed solution can achieve a better removal effect on boron residue than the second mixed solution.

[0044] In some embodiments, in steps S30, S50 and S70, the predetermined value is 1% of the boron isotope signal intensity obtained by the mass spectrometer in step S10. For example, when the boron isotope signal intensity obtained in step S10 is 5800 mV, the predetermined value is 58 mV. By setting a higher standard, it is ensured that the solution whose composition is determined by the experiment can effectively remove boron residues in actual applications.

[0045] An embodiment of the present application also provides a method for reducing the memory effect of boron isotope testing, which uses a solution whose composition is determined by the method according to any embodiment of the first aspect of the present application.

[0046] In some embodiments, the method for reducing the memory effect of boron isotope testing may include the following steps S1 to S6:

[0047] S1: Input the sample to be tested into the pipeline to perform boron isotope testing on the sample.

[0048] S2: Prepare a boron removal solution according to the determined components and component content ratios.

[0049] S3: After the test is completed, the boron-removed solution is input into the pipeline, and the boron isotope signal is continuously obtained by the mass spectrometer.

[0050] S4: When the boron isotope signal obtained by the mass spectrometer drops to the background value of the mass spectrometer, stop inputting the boron removal solution into the pipeline.

[0051] S5: Deionized water is introduced into the pipeline for a predetermined time.

[0052] S6: Input another sample to be tested into the pipeline and repeat steps S2 to S5.

[0053] The method in this embodiment is to clean the pipeline with a solution of composition determined by the method of any embodiment of the first aspect of the present application in the interval between each two times the sample to be tested is input into the pipeline, so as to quickly eliminate the boron residue from the previous test and avoid interference with the test results of the next test, thereby reducing the memory effect of the test and improving the test accuracy.

[0054] In step S5, deionized water is introduced into the pipeline for a predetermined time to further clean the residual solution in the pipeline, so as to keep the pipeline as clean as possible and further improve the test accuracy. The deionized water may be secondary deionized water.

[0055] The following is a specific example to further illustrate the process of the method for determining the solution components for removing boron in the present application.

[0056] A boron solution with a concentration of 1.0 μg / ml was prepared for testing. The boron solution was pumped into the pipeline using a peristaltic pump until the mass spectrometer obtained a stable boron isotope signal and then stopped. At this time, the signal intensity was 5800 mV. A 0.1 mol / L dilute nitric acid solution was input into the pipeline. The time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV was recorded as 18 min. 50 ml of methanol was added to 500 ml of deionized water, and the mixture was mixed to obtain a first mixed solution. The first mixed solution was input into the pipeline. The time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV was recorded as t 1 , t 1 The value is 12.5min; 50ml of methanol and 5g of glycerol are added to 500ml of deionized water, and the second mixed solution is obtained after mixing evenly. The second mixed solution is input into the pipeline, and the time consumed by the boron isotope signal obtained by the mass spectrometer to drop to 58mV is recorded as t 2 ',t 2 Keeping the concentration of methanol unchanged, increase the glycerol to 10g to prepare the second mixed solution, input the second mixed solution into the pipeline, and record the time consumed by the boron isotope signal obtained by the mass spectrometer to drop to 58mV as t 2 , t 2 The value is 5.5min; 50ml of methanol, 10g of glycerol and 5g of ammonium fluoride are added to 500ml of deionized water, mixed evenly to obtain a third mixed solution, the third mixed solution is input into the pipeline, and the time consumed by the boron isotope signal obtained by the mass spectrometer to drop to 58mV is recorded as t 3 , t 3 The value of is 3.2min; compared with t 1 ,t 2 and t 3 , due to t 3 <t 2 <t 1 , and t 3 The expected time has been reached, so the composition of the boron removal solution is determined to be methanol, glycerol and ammonium fluoride, with the proportion of the components being 10:2:1.

[0057] Regarding the embodiments of the present application, it should also be noted that, in the absence of conflict, the embodiments of the present application and the features therein can be combined with each other to obtain new embodiments.

[0058] The above are only specific implementation methods of the present application, but the protection scope of the present application is not limited thereto. The protection scope of the present application shall be based on the protection scope of the claims.

Claims

1. A method for determining the composition of a solution for removing boron, the solution being suitable for removing boron residues in a mass spectrometer pipeline, characterized in that: It includes the following steps: S10: preparing a boron solution for testing, and injecting the boron solution into the pipeline until the mass spectrometer obtains a stable boron isotope signal; S20: adding a predetermined amount of methanol into deionized water and mixing them evenly to obtain a first mixed solution; S30: inputting the first mixed solution into the pipeline, and recording the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t1; S40: adding a predetermined amount of glycerol to the first mixed solution, and mixing them evenly to obtain a second mixed solution; S50: repeating step S10, inputting the second mixed solution into the pipeline, and recording the time taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t2; S60: adding a predetermined amount of ammonium fluoride to the second mixed solution, and mixing them evenly to obtain a third mixed solution; S70: repeating step S10, inputting the third mixed solution into the pipeline, and recording the time consumed by the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value as t3; S80: Compare t1, t2 and t3, and determine the composition of the boron removal solution according to the comparison result.

2. The method according to claim 1, characterized in that In step S40, the method further includes: S41: adding a predetermined amount of methanol as in step S20 into deionized water to re-formulate the first mixed solution; S42: adding a predetermined amount of propylene glycol to the re-prepared first mixed solution, and mixing them evenly to obtain the second mixed solution.

3. The method according to claim 1, characterized in that In step S60, the following steps are also included: S61: adding the same predetermined amount of methanol as in step S20 into deionized water to re-formulate the first mixed solution; S62: adding the same predetermined amount of glycerol as in step S40 to the re-formulated first mixed solution, and mixing them evenly to obtain the re-formulated second mixed solution; S63: adding a predetermined amount of ammonium fluoride to the re-prepared second mixed solution, and mixing them evenly to obtain the third mixed solution.

4. The method according to claim 1, characterized in that: In step S10, the boron solution for testing is a boron solution with a concentration of 1.0 μg / ml.

5. The method according to claim 4, characterized in that In step S20, the content ratio of methanol to deionized water in the first mixed solution is 1:

10.

6. The method according to claim 5, characterized in that In step S40, the content ratio of methanol to glycerol in the second mixed solution is 5:

1.

7. The method according to claim 5, characterized in that In step S60, the content ratio of methanol, glycerol and ammonium fluoride in the third mixed solution is 10:2:

1.

8. The method according to claim 1, characterized in that In steps S30, S50 and S70, the predetermined value is 1% of the boron isotope signal intensity obtained by the mass spectrometer in step S10.

9. A method for reducing the memory effect of boron isotope testing, characterized in that: The solution is prepared by using the method according to any one of claims 1 to 8 to determine the composition.

10. The method according to claim 9, characterized in that It includes the steps of: S1: inputting a sample to be tested into the pipeline to perform a boron isotope test on the sample; S2: preparing a boron removal solution according to the determined components and component content ratios; S3: After the test is completed, the boron-removed solution is introduced into the pipeline, during which the boron isotope signal is continuously obtained by the mass spectrometer; S4: when the boron isotope signal obtained by the mass spectrometer drops to the background value of the mass spectrometer, stopping the input of the boron removal solution into the pipeline; S5: injecting deionized water into the pipeline for a predetermined time; S6: Input another sample to be tested into the pipeline, and repeat steps S2 to S5.

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