Methods of determining the composition of a boron-removing solution and methods of reducing memory effects in boron isotope testing using the solution

Abstract

Embodiments of the present application relate to the technical field of treating solutions using ion exchange methods, and in particular to a method for determining the composition of a boron-removing solution and a method for reducing memory effects in boron isotope testing using the solution. In a first aspect, embodiments of the present application provide a method for determining the composition of a boron-removing solution suitable for removing boron residues from the tubing of a mass spectrometer. In a second aspect, embodiments of the present application also provide a method for reducing memory effects in boron isotope testing using a solution having a composition determined according to the method of the first aspect. Through the method of the present application, a boron-removing solution that is stable and effective in removing boron residues without causing new residue problems, and that consumes less time, can be obtained. In boron isotope testing, using the solution to clean the tubing can quickly eliminate boron residues from the previous test, avoid interference with the test results of the next test, thereby reducing the memory effects of the test and improving the test accuracy.

Description

TECHNICAL FIELD

[0001] Embodiments of the present application relate to the technical field of treating solutions using ion exchange methods, and in particular to a method of determining the composition of a boron-removing solution and a method of reducing memory effects in boron isotope testing using the solution. BACKGROUND

[0002] The statements herein are merely provided to give a background of the present application and are not necessarily the prior art.

[0003] The element boron includes two stable isotopes 10 B and 11 B, both of which have a relatively large mass, and thus are often used as a stable isotope tracer in the fields of chemistry, the environment, the earth, etc. 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 commonly used. Among these, multi-collector inductively coupled plasma mass spectrometry is widely used because it is a liquid sampling method and is suitable for a wider variety of 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 the results of boron isotope testing. SUMMARY

[0005] A brief summary of the present application is presented in the following to provide a basic understanding of some aspects of the present application. It should be understood that this summary is not an extensive overview of the present application. It is not intended to identify key or critical elements of the present application or to delineate the scope of the present application. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is presented later.

[0006] In a first aspect, embodiments of the present application provide a method for determining a composition of a boron-removing solution, which is suitable for removing boron residues in a pipeline of a mass spectrometer, comprising 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; S20: adding a predetermined amount of methanol into deionized water, and obtaining a first mixed solution after mixing; S30: inputting the first mixed solution into the pipeline, and recording a time t1 consumed for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value; S40: adding a predetermined amount of glycerol into the first mixed solution, and obtaining a second mixed solution after mixing; S50: repeating step S10, inputting the second mixed solution into the pipeline, and recording a time t2 consumed for the boron isotope signal obtained by the mass spectrometer to drop to the predetermined value; S60: adding a predetermined amount of ammonium fluoride into the second mixed solution, and obtaining a third mixed solution after mixing; S70: repeating step S10, inputting the third mixed solution into the pipeline, and recording a time t3 consumed for the boron isotope signal obtained by the mass spectrometer to drop to the predetermined value; and S80: comparing t1, t2 and t3, and determining the composition of the boron-removing solution according to a comparison result.

[0007] In a second aspect, embodiments of the present application also provide a method for reducing a memory effect of boron isotope testing, which uses a solution with a composition determined according to any of the embodiments of the first aspect of the present application.

[0008] By the method in the embodiments of the present application, a boron-removing solution can be obtained, which can stably and effectively remove boron residues without causing new residue problems, and the time consumed is short. During the boron isotope testing, the solution is used to clean the pipeline in the interval between inputting two samples to be tested into the pipeline, which can quickly eliminate the boron residues of the previous test, avoid interference with the test results of the next test, thereby reducing the memory effect of the test, and improving the test accuracy. BRIEF DESCRIPTION OF DRAWINGS

[0009] Other objects and advantages of the present application will be more fully apparent from the following description of embodiments of the present application, taken in conjunction with the accompanying drawings.

[0010] Figure 1 is a flowchart of a method for determining a composition of a boron-removing solution 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 intended to illustrate the illustrative aspects of the present application. DETAILED DESCRIPTION

[0012] Exemplary embodiments of the present application will be described herein below with reference to the accompanying drawings. For the purpose of clarity and a concise description, all the features of the practical embodiments are not described in the specification. It should be appreciated, however, that numerous implementation-specific decisions must be made in order to develop any such practical embodiment and that these specific decisions will have profound impact on the implementation of the application, for example, compliance with system- and business-related constraints, which will vary from one implementation to another. Moreover, it should be appreciated that although the development work can be very complex and time-consuming, it would be a routine undertaking for those of ordinary skill in the art having the benefit of this disclosure.

[0013] It should also be noted herein that, in order not to obscure the application with unnecessary detail, only the structures of the equipment and / or the processing steps that are closely related to the solution according to the present application are shown in the drawings, while other details that are not closely related to the present application are omitted.

[0014] The inventors of the present application have found that, in the process of boron isotope testing, the sample to be tested is prone to be left in the pipeline of the mass spectrometer, affecting the test results of subsequent samples. Therefore, the common measure taken is to clean the pipeline with a boron-removing solution after the sample testing is completed. However, the currently commonly used boron-removing solutions, such as nitric acid, dilute ammonia water, dilute ammonium nitrate or mannitol solution, have problems such as difficult-to-predict removal effect, low efficiency and easy to cause new residues.

[0015] Based on this, the embodiments of the present application provide a method for determining the composition of a boron-removing solution, which is suitable for removing boron residues in the pipeline of a mass spectrometer, as shown in Figure 1 Figure 1 A flow chart of the method for determining the composition of a boron-removing solution according to an embodiment of the present application is shown, which includes the following steps S10 to S80:

[0016] S10: Prepare a boron solution for testing, and input the boron solution into the pipeline until the stable boron isotope signal of the mass spectrometer is obtained, and then stop.

[0017] S20: Add a predetermined amount of methanol to the deionized water, and mix uniformly to obtain a first mixed solution.

[0018] S30: Input the first mixed solution into the pipeline, and record the time t1 consumed for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value.

[0019] S40: Add a predetermined amount of glycerol to the first mixed solution, and mix uniformly to obtain a second mixed solution.

[0020] ​S50: repeat step S10, input the second mixed solution into the pipeline, and record the time t2 consumed for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value.

[0021] S60: add a predetermined amount of ammonium fluoride to the second mixed solution, and obtain a third mixed solution after uniform mixing.

[0022] S70: repeat step S10, input the third mixed solution into the pipeline, and record the time t3 consumed for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value.

[0023] S80: compare t1, t2, and t3, and determine the composition of the solution for removing boron according to the comparison result.

[0024] The method provided by the embodiment of the application has the characteristics that the elimination effect of ammonium fluoride on boron is good and no residue is left, the alkylation effect of the alcohol reagent on boron is good and no residue is left, and the alcohol reagent and the fluoride have a synergistic effect on the elimination of boron. By adding a predetermined amount of methanol, glycerol, and ammonium fluoride into deionized water in sequence and inputting them into the pipeline in which the test boron solution is left, the time consumed for removing boron in the pipeline by the mixed solution with three different compositions is obtained, and by comparing the time, it is determined which solution has the best effect on removing boron, so that a solution for removing boron that can stably and effectively remove boron residue and does not cause new residue problems and has a short time consumption is obtained.

[0025] In some embodiments, in step S10, the test boron solution is a boron solution with a concentration of 1.0 μg / ml, which simulates the sample to be detected when the boron isotope test is actually performed, and on this basis, the test for determining the composition of the solution for removing boron is performed, so as to ensure the effectiveness and accuracy of the test, and make the solution with the determined composition be able to be used for actual testing and effectively remove boron residue in the pipeline.

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

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

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

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

[0030] S41: adjusting the predetermined amount of glycerol to obtain a plurality of second mixed solutions with different component contents.

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

[0032] S43: comparing the plurality of times, and determining the predetermined amount of glycerol according to the comparison result.

[0033] In this embodiment, the predetermined amount of glycerol is changed under the condition that the components of the first mixed solution remain unchanged, so as to determine the content of glycerol in the second mixed solution which has the best effect on removing boron residue.

[0034] In some embodiments, in the step S40, the following steps are also included:

[0035] S41: adding the same predetermined amount of methanol as in the step S20 to the deionized water to reconfigure the first mixed solution.

[0036] S42: adding the predetermined amount of glycerol to the reconfigured first mixed solution, and obtaining the second mixed solution after mixing uniformly.

[0037] In this embodiment, the first mixed solution with the same components as in the step S20 is reconfigured, and the second mixed solution is prepared based on the first mixed solution which has not been tested, so as to avoid affecting the removal effect of the second mixed solution on boron by using the solution which has been tested, and to ensure the test accuracy.

[0038] In some embodiments, in the step S60, the following steps are also included:

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

[0040] S62: adding the same predetermined amount of glycerol as in the step S40 to the reconfigured first mixed solution, and obtaining the reconfigured second mixed solution after mixing uniformly.

[0041] S63: A predetermined amount of ammonium fluoride is added to the reconfigured second mixed solution, and after mixing uniformly, a third mixed solution is obtained.

[0042] In this embodiment, the first mixed solution with the same components as those in S20 is reconfigured, and the second mixed solution with the same components as those in S40 is reconfigured on the basis of the first mixed solution, and the third mixed solution is prepared on the basis of the second mixed solution, thereby avoiding the use of the solution that has been tested, further eliminating interference factors, and ensuring the test accuracy.

[0043] In some embodiments, in the step S60, the content ratio of the components of the 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 elimination effect of ammonium fluoride on boron is good and there is no residue, and the characteristics of fluoride and alcohol reagents on the elimination of boron play a synergistic role. The ammonium fluoride is added to the second mixed solution, so that the third mixed solution has a better removal effect on the boron residue than the second mixed solution.

[0044] In some embodiments, in the steps S30, S50 and S70, the predetermined value is 1% of the signal intensity of the boron isotope obtained by the mass spectrometer in the step S10, for example, when the signal intensity of the boron isotope obtained in the step S10 is 5800 mV, the predetermined value is 58 mV, so as to set a higher standard to ensure that the solution with the determined components can effectively remove the boron residue in actual application through the test.

[0045] The embodiments of the present application also provide a method for reducing the memory effect of boron isotope test, which uses the solution with the determined components according to any one of the embodiments of the first aspect of the present application.

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

[0047] S1: inputting the sample to be tested into the pipeline to test the sample for boron isotope.

[0048] S2: preparing a boron-removing solution according to the determined components and the content ratio of the components.

[0049] S3: after the test is completed, inputting the boron-removing solution into the pipeline, and continuously obtaining the boron isotope signal by the mass spectrometer during the inputting.

[0050] S4: stopping inputting the boron-removing solution into the pipeline after the boron isotope signal obtained by the mass spectrometer decreases to the background value of the mass spectrometer.

[0051] S5: inputting deionized water into the pipeline for a predetermined time.

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

[0053] The method in the embodiment can clean the pipeline with the solution of the components determined by the method of any one of the first aspect of the application between every two times of inputting the sample to be tested into the pipeline, so as to quickly eliminate the boron residue of the last test and avoid the interference of the boron residue on the test result of the next test, thereby reducing the memory effect of the test and improving the test precision.

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

[0055] The process of determining the components of the solution for removing boron in the application will be further described in specific embodiments.

[0056] A boron solution with a concentration of 1.0 μg / ml is prepared for testing, the boron solution is pumped into the pipeline by using a peristaltic pump, and the pumping is stopped after the mass spectrometer obtains a stable boron isotope signal, at this time the signal intensity is 5800 mV, 0.1 mol / L dilute nitric acid solution is input into the pipeline, and the time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV is recorded as 18 min; 50 ml of methanol is added to 500 ml of deionized water, and a first mixed solution is obtained after mixing uniformly, the first mixed solution is input into the pipeline, and the time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV is recorded as t1, the value of t1 is 12.5 min; 50 ml of methanol and 5 g of glycerol are added to 500 ml of deionized water, and a second mixed solution is obtained after mixing uniformly, the second mixed solution is input into the pipeline, and the time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV is recorded as t2', the value of t2' is 7 min; the concentration of methanol is kept unchanged, the glycerol is increased to 10 g to re-prepare the second mixed solution, the second mixed solution is input into the pipeline, and the time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV is recorded as t2, the value of t2 is 5.5 min; 50 ml of methanol, 10 g of glycerol, and 5 g of ammonium fluoride are added to 500 ml of deionized water, and a third mixed solution is obtained after mixing uniformly, the third mixed solution is input into the pipeline, and the time consumed for the boron isotope signal obtained by the mass spectrometer to drop to 58 mV is recorded as t3, the value of t3 is 3.2 min; t1, t2, and t3 are compared, since t3 < t2 < t1 and t3 has reached the expected time, it is determined that the components of the solution for removing boron are methanol, glycerol, and ammonium fluoride, and the content ratio of the components is 10:2:1.

[0057] For the embodiments of the present application, it also needs to be explained that the embodiments and the features in the embodiments of the present application can be combined with each other to obtain new embodiments without conflict.

[0058] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto, and the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A method for determining the composition of a solution for removing boron, said solution being suitable for removing boron residue from the tubing of a mass spectrometer, characterized in that, It includes the following steps: S10: Prepare the boron solution for testing, and input the boron solution into the pipeline until the mass spectrometer obtains a stable boron isotope signal and then stops. S20: Add a predetermined amount of methanol to deionized water, mix well to obtain the first mixed solution; S30: Input the first mixed solution into the pipeline and record the time t1 taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value; S40: Add a predetermined amount of glycerol to the first mixed solution, mix thoroughly to obtain a second mixed solution; S50: Repeat step S10, input the second mixed solution into the pipeline, and record the time t2 taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value. S60: Add a predetermined amount of ammonium fluoride to the second mixed solution, mix thoroughly to obtain a third mixed solution; S70: Repeat step S10, input the third mixed solution into the pipeline, and record the time t3 taken for the boron isotope signal obtained by the mass spectrometer to drop to a predetermined value. S80: Compare t1, t2, and t3, and determine the composition of the boron-removing solution based on the comparison results. Step S40 also includes: S41: Add the same predetermined amount of methanol as in step S20 to the deionized water to reformulate the first mixed solution; S42: Add a predetermined amount of the glycerol to the newly prepared first mixed solution, and mix thoroughly to obtain the second mixed solution; Step S60 also includes: S61: Add the predetermined amount of methanol, the same as in step S20, to the deionized water to reconstitute the first mixed solution; S62: Add the same predetermined amount of glycerol as in step S40 to the newly prepared first mixed solution, mix thoroughly to obtain the newly prepared second mixed solution; S63: Add the predetermined amount of the ammonium fluoride to the newly prepared second mixed solution, and mix thoroughly to obtain the third mixed solution.

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

3. The method according to claim 2, characterized in that, In step S20, the ratio of methanol to deionized water in the first mixed solution is 1:

10.

4. The method according to claim 3, characterized in that, In step S40, the ratio of methanol to glycerol in the second mixed solution is 5:

1.

5. The method according to claim 3, characterized in that, In step S60, the ratio of methanol, glycerol, and ammonium fluoride in the third mixed solution is 10:2:

1.

6. 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.

7. A method for reducing the memory effect in boron isotope testing, characterized in that, The solution is prepared by means of any one of claims 1-6.

8. The method according to claim 7, characterized in that, It includes the following steps: S1: Input the sample to be tested into the pipeline to perform boron isotope testing on the sample; S2: Prepare a boron removal solution according to the determined components and component content ratios; S3: After the test is completed, the boron-removing solution is introduced into the pipeline, and boron isotope signals are continuously acquired by the mass spectrometer during the process. S4: When the boron isotope signal obtained by the mass spectrometer drops to the background value of the mass spectrometer, stop feeding the boron removal solution into the pipeline; S5: Introduce 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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