Method for determining helium content in hydrogen isotopes based on a mass spectrometer

Abstract

The application provides a method for determining the content of helium in hydrogen isotopes based on a mass spectrometer. The provided method comprises the following steps: (1) performing first detection on standard hydrogen of a national standard substance by using the mass spectrometer, so as to calibrate the sensitivity of hydrogen, which is S1; (2) performing second detection on standard helium of the national standard substance by using the mass spectrometer, so as to calibrate the sensitivity of helium, which is S2; (3) determining the correction coefficient of helium according to S1 and S2, that is, Δ = S2 / S1; (4) based on the correction coefficient of helium, performing detection on the content of helium in mixed gas with different concentration ratios by using the mass spectrometer, fitting the obtained detection result of the content of helium with the theoretical value of helium in the mixed gas, and obtaining a standard curve; and (5) performing detection on the to-be-detected gas by using the mass spectrometer, and determining the content of helium in the to-be-detected gas based on the standard curve. The provided method can realize the determination of the content of helium, has high accuracy, strong applicability and wide application range.

Description

Technical Field

[0001] This invention relates to the field of hydrogen isotope determination technology, specifically to a method for determining the helium content in hydrogen isotopes based on a mass spectrometer. Background Technology

[0002] Currently, the main methods for measuring hydrogen and helium isotopes are chromatography and mass spectrometry. Chromatography uses a thermal conductivity chromatograph, while mass spectrometry uses a low-resolution or high-resolution mass spectrometer. Mass spectrometry has many advantages, such as high sensitivity, accuracy, and a wide measurement concentration range. However, in the current process of sample analysis, when using mass spectrometry to detect hydrogen-helium mixtures, the significant difference in sensitivity between helium and hydrogen makes it impossible to establish a direct detection method to determine their content, which brings difficulties to process analysis.

[0003] Further improvements are needed in the determination and analysis of helium content in hydrogen isotopes. Summary of the Invention

[0004] This invention aims to at least partially solve one of the technical problems existing in the prior art. This invention provides a method for determining the helium content in hydrogen isotopes based on mass spectrometry. The method provided by this invention can indirectly determine the helium content in a hydrogen-helium mixture, with high accuracy, strong applicability, and a wide range of applications.

[0005] Specifically, the present invention provides the following technical solution:

[0006] This invention provides a method for determining the helium content in hydrogen isotopes using a mass spectrometer, comprising: (1) using a mass spectrometer to perform a first detection on standard hydrogen (a national standard reference material) to calibrate hydrogen sensitivity, wherein the hydrogen sensitivity meter is S1; (2) using a mass spectrometer to perform a second detection on standard helium (a national standard reference material) to calibrate helium sensitivity, wherein the helium sensitivity meter is S2; (3) determining a helium correction coefficient based on the hydrogen sensitivity S1 and the helium sensitivity S2, wherein the helium correction coefficient is Δ = S2 / S1; (4) using a mass spectrometer to detect the helium content in a mixture of gases with different concentration ratios, and fitting the obtained detection results of helium content with the theoretical helium content in the mixture to obtain a standard curve; (5) using a mass spectrometer to detect the gas to be tested, and determining the helium content in the gas to be tested based on the standard curve.

[0007] This invention provides a method for indirectly determining the helium content in a hydrogen-helium mixture, which can accurately determine the hydrogen and helium content in the mixture, and has strong applicability and wide range of applications.

[0008] According to embodiments of the present invention, the method provided above may further include the following technical features:

[0009] According to an embodiment of the present invention, the range of hydrogen sensitivity S1 in step (1) is [0-20]. The hydrogen sensitivity mentioned is obtained by calibrating hydrogen with an instrument, and the calibrated hydrogen sensitivity is between 0 and 20, for example, 20, 19, 18, 17, 16, 15, 14, 13, 12, 11, 10, 9, 8, 7, 6, 5, 4, 3, etc.

[0010] According to an embodiment of the present invention, the range of helium sensitivity S2 in step (2) is [0 to 20]. The helium sensitivity mentioned is obtained by calibrating helium with an instrument, and the calibrated helium sensitivity is 20, 19, 18, 17, 16, 15, 14, 13, 12, 11, 10, 9, 8, 7, 6, 5, 4, 3, etc.

[0011] According to an embodiment of the present invention, the mixed gas in step (4) contains standard hydrogen and standard helium, and the content of standard helium in the mixed gas ranges from 0% to 100%. For example, the content of standard helium in the mixed gas ranges from 8% to 55%.

[0012] According to an embodiment of the present invention, the mixed gas in step (4) contains standard hydrogen and standard helium, and the content of standard helium in the mixed gas ranges from 0% to 100%. For example, the content of standard helium in the mixed gas ranges from 18% to 50%.

[0013] According to embodiments of the present invention, the helium content in the gas to be tested ranges from 0% to 100%. For example, the helium content in the gas to be tested ranges from 8% to 55%.

[0014] According to an embodiment of the present invention, the content of helium in the gas to be tested ranges from 0% to 100%. For example, the content of helium in the gas to be tested ranges from 18% to 50%.

[0015] According to an embodiment of the present invention, the range of the correction coefficient in step (3) is 1% to 20%. Studies have shown that when the value of the correction coefficient is too large or too small, it indicates that there is a problem with the calibration of at least one of the sensitivities S1 or S2, resulting in an error in the percentage measurement of the correction coefficient, thereby affecting the subsequent results.

[0016] According to an embodiment of the present invention, the gas to be tested is selected from at least one of hydrogen, helium, oxygen, and nitrogen.

[0017] The beneficial effects achieved by this invention are as follows:

[0018] 1) This invention uses a mass spectrometer to indirectly determine the helium content in hydrogen isotopes, which can determine the hydrogen and helium content in a hydrogen-helium mixture.

[0019] 2) It has the characteristic of high accuracy. Using this method, the hydrogen and helium content in a hydrogen-helium mixture can be accurately obtained.

[0020] 3) It has the characteristic of being highly instructive. This method can be used to determine the content of other mixed gases with large differences in sensitivity that cannot be directly detected by mass spectrometer.

[0021] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Detailed Implementation

[0022] This invention establishes a method for determining the helium content in hydrogen isotopes based on mass spectrometry. The method provided by this invention can accurately determine the percentage content of hydrogen and helium in the isotopes.

[0023] This invention provides a method for determining the helium content in hydrogen isotopes using a mass spectrometer, comprising: (1) using a mass spectrometer to perform a first detection on standard hydrogen (a national standard reference material) to calibrate hydrogen sensitivity, wherein the hydrogen sensitivity meter is S1; (2) using a mass spectrometer to perform a second detection on standard helium (a national standard reference material) to calibrate helium sensitivity, wherein the helium sensitivity meter is S2; (3) determining a helium correction coefficient based on the hydrogen sensitivity S1 and the helium sensitivity S2, wherein the helium correction coefficient is Δ = S2 / S1; (4) using a mass spectrometer to detect the helium content in a mixture of gases with different concentration ratios, and fitting the obtained detection results of helium content with the theoretical helium content in the mixture to obtain a standard curve; (5) using a mass spectrometer to detect the gas to be tested, and determining the helium content in the gas to be tested based on the standard curve.

[0024] This invention provides a method for indirectly determining the helium content in a hydrogen-helium mixture, which can accurately determine the hydrogen and helium content in the mixture, and has strong applicability and wide range of applications.

[0025] According to a specific embodiment of the present invention, the hydrogen sensitivity in step (1) is 0 to 20.

[0026] According to a specific embodiment of the present invention, the helium sensitivity in step (2) is 0 to 20.

[0027] According to a specific embodiment of the present invention, the mixed gas in step (4) contains standard hydrogen and standard helium, and the content of standard helium in the mixed gas ranges from 0% to 100%, for example, from 8% to 55%. When the content of standard helium in the mixed gas is within this range, the accuracy of the obtained measurement results is high, and the error range does not exceed 0.5%.

[0028] According to a specific embodiment of the present invention, the mixed gas in step (4) contains standard hydrogen and standard helium, and the content of standard helium in the mixed gas ranges from 0% to 100%, for example, it can be 18% to 50% (0%-100%). When the content of standard helium in the mixed gas is within this range, the accuracy of the obtained measurement results is high, and the error range does not exceed 0.5%.

[0029] According to a specific embodiment of the present invention, the helium content in the gas to be tested ranges from 0% to 100%, for example, it can be from 8% to 55%.

[0030] According to a specific embodiment of the present invention, the content of helium in the gas to be tested ranges from 0% to 100%, for example, it can be from 18% to 50%.

[0031] The present invention will be explained below with reference to embodiments. Those skilled in the art will understand that the following embodiments are for illustrative purposes only and should not be considered as limiting the scope of the invention. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in the field or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all commercially available conventional products. The mass spectrometer used is a single-analyzer mass spectrometer.

[0032] Example 1

[0033] Example 1 describes the use of mass spectrometry to determine the helium content in a hydrogen-helium mixture, and the accuracy of this determination was experimentally verified. The provided method includes the following steps:

[0034] 1) Hydrogen sensitivity calibration:

[0035] The sensitivity of hydrogen was determined to be S1 by using the national standard reference material standard hydrogen in a mass spectrometer.

[0036] 2) Helium sensitivity calibration:

[0037] Sensitivity calibration experiments were conducted using national standard helium in a mass spectrometer, and the sensitivity of helium was determined to be S2.

[0038] 3) Determine the correction coefficients

[0039] By comparing the sensitivity of hydrogen and helium, the correction factor for helium was calculated to be Δ = S2 / S1.

[0040] 4) Fitting the standard curve

[0041] Experiments were conducted by preparing mixed gases with different concentration ratios and substituting helium correction coefficients, and a standard curve was fitted. The experimental data are shown in Table 1.

[0042] Table 1. Experimental data for standard curve fitting

[0043] Theoretical helium content (%) in the gas mixture Mass spectrometer detection of helium content (%) 1 41.63 39.43 2 45.78 43.55 3 50.26 47.69 4 55.04 52.52 5 30 28.50 6 23.02 21.78 7 18 17.09 8 8.62 8.09

[0044] 5) Accuracy verification

[0045] The helium content in the gas to be tested was calculated based on the fitted standard curve, and the calculation results are shown in Table 2.

[0046] Table 2 Calculation results of the fitted curve

[0047] Serial Number Theoretical helium content (%) in the gas mixture Mass spectrometer detection of helium content (%) Relative error (%) 1 41.63 41.49 -0.33 2 45.78 45.80 0.05 3 50.26 50.15 -0.22 4 55.04 55.20 0.29 5 30 30.04 0.14 6 23.02 23.01 -0.05 7 18 17.99 -0.04 8 8.62 8.66 0.44

[0048] As shown in Table 2, when the helium concentration increases from 8% to 55%, the relative error between the helium ratio obtained in each group of experiments and the helium ratio prepared in the experiment does not exceed 0.5%.

[0049] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "specific implementation," or "implementation," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0050] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.

Claims

1. A method for determining the helium content in hydrogen isotopes using a mass spectrometer, characterized in that, include: (1) The national standard reference material standard hydrogen is first detected by mass spectrometer in order to calibrate the hydrogen sensitivity. The hydrogen sensitivity meter is S1. (2) A mass spectrometer is used to perform a second detection using national standard helium to calibrate the helium sensitivity. The helium sensitivity meter is S2. (3) Determine the helium correction coefficient based on the hydrogen sensitivity S1 and the helium sensitivity S2, wherein the helium correction coefficient is Δ=S2 / S1; (4) Based on the helium correction coefficient, the helium content in the mixed gas with different concentration ratios is detected by mass spectrometer, and the detected helium content is fitted with the theoretical helium content in the mixed gas to obtain a standard curve. (5) Use a mass spectrometer to detect the gas to be tested, and determine the helium content in the gas to be tested based on the standard curve; Wherein, the range of hydrogen sensitivity S1 in step (1) is [0~20]; The range of helium sensitivity S2 mentioned in step (2) is [0~20]; The mixed gas in step (4) contains standard hydrogen and standard helium, and the content of standard helium in the mixed gas ranges from 18% to 50%. The content of helium in the gas to be tested ranges from 18% to 50%. The range of the correction coefficient mentioned in step (3) is 1% to 20%.

2. The method according to claim 1, characterized in that, The mixed gas in step (4) contains standard hydrogen and standard helium, and the content of standard helium in the mixed gas ranges from 8% to 55%.

3. The method according to claim 1, characterized in that, The gas to be tested contains helium in the range of 8% to 55%.

4. The method according to claim 1, characterized in that, The gas to be tested is selected from at least one of hydrogen, helium, oxygen, and nitrogen.