Method for detecting the working status of CO isotope scrambler

Abstract

The embodiment of the present application provides a method for detecting the working state of a CO isotope scrambler. The detection method includes: using a mass spectrometer to detect CO gas to obtain a detection signal value, wherein the CO gas is obtained from the outlet of the CO isotope scrambler, and the CO gas includes multiple CO isotope gas components; according to preset conditions and the detection signal value, determining the abundance value of the carbon isotope and the abundance value of the oxygen isotope in the CO gas; according to the abundance value of the carbon isotope and the abundance value of the oxygen isotope, determining the theoretical abundance value of each CO isotope gas component in the CO gas; according to the detection signal value and the theoretical abundance value of each CO isotope gas component, determining the working state of the scrambler.

Description

Technical Field

[0001] The present application relates to the technical field of isotope preparation, and in particular to a method for detecting the working state of a CO isotope scrambler. Background Art

[0002] Carbon has two stable isotopes 12 C and 13 C. Oxygen has three stable isotopes 16 O. 17 O and 18 O, thus forming 12 C 16 O. 12 C 17 O. 12 C 18 O. 13 C 16 O. 13 C 17 O. 13 C 18 Six kinds of O molecules. Preparation of high abundance by cryogenic distillation of CO 13 The process of product C is to use the difference in boiling points of the six molecules to enrich the heavy components at the bottom of the distillation tower and the light components at the top of the tower, thereby obtaining an enriched 13 C of CO products. However, due to 12 CO / 13 The CO separation coefficient is very small, and the heavy components enriched at the bottom of the tower 12 C 18 O and 13 C 16 O is difficult to be further separated, which limits the bottom discharge of the tower. 13 C abundance. By adding an isotope scrambler after the distillation tower, the atoms are recombined and then passed into the next distillation tower, which can improve 13 C product abundance.

[0003] The working principle of the CO isotope scrambler is to separate the difficult-to-separate 12 C 18 O and 13 C 16 O is converted into easily separable 12 C 16 O and 13 C 18 O, through detection 12 C 18 O. 13 C 16 O and 12 C 16 O. 13 C 18The content of O can be used to calculate the conversion efficiency of the CO scrambler, and then the real-time working status of the scrambler can be determined. 12 C 16 O. 12 C 17 O. 12 C 18 O. 13 C 16 O. 13 C 17 O. 13 C 18 O six components, it is impossible to 12 C 18 O. 13 C 16 O is quantified, and thus the working status of the scrambler cannot be effectively detected. Summary of the invention

[0004] In view of the above problems, a method for detecting the working state of a CO isotope scrambler is provided, which overcomes the above problems or at least partially solves the above problems.

[0005] According to an embodiment of the present application, a method for detecting a working state of a CO isotope scrambler is provided, comprising: detecting CO gas using a mass spectrometer to obtain a detection signal value, wherein the CO gas is obtained from an outlet of the CO isotope scrambler, and the CO gas includes a plurality of CO isotope gas components; determining an abundance value of a carbon isotope and an abundance value of an oxygen isotope in the CO gas according to a preset condition and the detection signal value; determining a theoretical content of each CO isotope gas component in the CO gas according to the abundance value of the carbon isotope and the abundance value of the oxygen isotope; and determining a working state of the scrambler according to the detection signal value and the theoretical content of each CO isotope gas component.

[0006] The detection method of the working state of the CO isotope scrambler provided in the embodiment of the present application detects CO gas by a mass spectrometer, determines the abundance values ​​of carbon and oxygen isotopes in the CO gas according to the detection signal value, and then determines the theoretical abundance value of each CO isotope gas component in the CO gas. According to the theoretical abundance value and the detection signal value of the mass spectrometer, the working state of the scrambler can be determined. The embodiment of the present application can accurately determine the working state of the CO isotope scrambler, effectively preventing the catalyst filled with the CO isotope scrambler from working for a long time at high temperature and reducing the catalytic efficiency, which reduces the conversion efficiency of CO isotopes, causing the CO gas to enter the lower distillation tower without meeting the feeding requirements of the lower distillation tower, and causing the discharge of the material to be 13 C Product does not meet the requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0007] Other objects and advantages of the present invention will become apparent from the following description of the embodiments of the present invention with reference to the accompanying drawings, which will help to provide a comprehensive understanding of the present invention.

[0008] Figure 1 The figure is a flow chart of a method for detecting the working state of a CO isotope scrambler according to an embodiment of the present application.

[0009] Figure 2 The figure is a flow chart of a method for detecting the working state of a CO isotope scrambler according to another embodiment of the present application.

[0010] Figure 3 According to the embodiment of the present application, the distillation CO is produced 13 Schematic diagram of the process of C.

[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] In order to make the purpose, technical solution and advantages of the present application clearer, the technical solution of the present application will be clearly and completely described below in conjunction with the drawings of the embodiments of the present application. Obviously, the described embodiment is one embodiment of the present application, not all embodiments. Based on the described embodiments of the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0013] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in this application should be the usual meanings understood by people with general skills in the field to which this application belongs. If the full text involves descriptions such as "first" and "second", the "first" and "second" descriptions are only used to distinguish similar objects, and cannot be understood as indicating or implying their relative importance, sequence, or implicitly indicating the number of technical features indicated. It should be understood that the data described by "first" and "second" can be interchangeable under appropriate circumstances. If "and / or" appears in the full text, its meaning includes three parallel solutions. Taking "A and / or B" as an example, it includes Solution A, or Solution B, or a solution that satisfies both A and B.

[0014] The working principle of the CO isotope scrambler is to separate the difficult-to-separate 12 C 18 O and 13 C 16 O is converted into easily separable 12 C 16 O and 13 C 18 O. Among them, CO gas undergoes the following reaction in the scrambler:

[0015]

[0016] Measured by mass spectrometer 12 C 18 O. 13 C 16 O and 12 C 16 O. 13 C 18 The content of O can be used to calculate the conversion efficiency of the CO scrambler, and then the real-time working status of the scrambler can be determined. 12 C 16 O. 12 C 17 O. 12 C 18 O. 13 C 16 O. 13 C 17 O. 13 C 18 O six components, due to 12 C 17 O and 13 C 16 O has a mass number of 29. 12 C 18 O and 13 C 17 O has a mass number of 30, and the mass spectrometer cannot separate them 12 C 18 O. 13 C 16 O independent signal, resulting in difficulty in calculating the conversion efficiency of the CO scrambler, and also unable to detect the working status of the scrambler.

[0017] An embodiment of the present application provides a method for detecting the working state of a CO isotope scrambler.

[0018] Figure 1 FIG. 1 is a schematic diagram of a method for detecting the working state of a CO isotope scrambler according to an embodiment of the present application. Figure 1 As shown, the method 100 for detecting the working state of the CO isotope scrambler includes operations S101 to S104.

[0019] In operation S101, CO gas is detected by using a mass spectrometer to obtain a detection signal value, wherein the CO gas is obtained from an outlet of a CO scrambler and includes a plurality of CO isotope gas components.

[0020] In operation S102, the abundance value of the carbon isotope in the CO gas and the abundance value of the oxygen isotope in the CO gas are determined according to preset conditions and the detection signal value.

[0021] In operation S103, the theoretical content of each CO isotope gas component in the CO gas is determined according to the abundance value of the carbon isotope and the abundance value of the oxygen isotope.

[0022] In operation S104, the working state of the scrambler is determined according to the detection signal value and the theoretical content of each CO isotope gas component.

[0023] In this embodiment, the preset condition can be determined by assuming that the scrambler is in a normal working state, the CO isotope gas composition and the relationship between the isotopes contained therein.

[0024] In this embodiment, the multiple CO isotope gas components in the CO gas may include: 12 C 16 O. 12 C 17 O. 12 C 18 O. 13 C 16 O. 13 C 17 O. 13 C 18 O. In this embodiment, carbon isotopes may include 12 C and 13 C. Oxygen isotopes can include 16 O. 17 O and 18 O.

[0025] Specifically, by using a mass spectrometer to detect CO gas, detection signal values ​​with mass numbers of 12, 13, 28, 29, 30, and 31 can be obtained. By detecting the signal values, 12 C. 13 C. 12 C 16 O and 13 C 18 The preset condition can be that when the scrambler is working normally, there is a CO isotope gas component such as 12 C 16 The abundance of O is equal to the corresponding 12 The abundance of C and 16 The product of the abundance value of O. 12 C. 13 C. 12 C 16 O and 13 C 18 The abundance value of O can be obtained16 O. 17 O and 18 O abundance value. The corresponding CO isotope gas composition when the mass number is 29 is 12 C 17 O and 13 C 16 O. It can be based on the CO isotope gas composition 12 C 17 O and 13 C 16 The sum of the products of the carbon and oxygen abundance values ​​corresponding to O is determined 12 C 17 O and 13 C 16 The theoretical abundance value of O is compared with the detection signal value corresponding to the mass number 29 to determine the working state of the scrambler.

[0026] It can be understood that, assuming that the scrambler is in normal working condition, there is a CO isotope gas component equal to the product of the abundance value of the corresponding carbon isotope and the abundance value of the oxygen isotope, such as 12 C 16 The abundance of O is equal to 12 The abundance of C and 16 The working state of the scrambler can be determined according to the ratio of the detection signal value to the corresponding theoretical abundance value of the CO isotope gas component obtained by the above method.

[0027] For example, when the theoretical abundance value is consistent with the detection signal value obtained by the mass spectrometer, it can be determined that the working state of the scrambler is normal; otherwise, the working state of the scrambler is abnormal.

[0028] As described above, the detection method in this embodiment can accurately and effectively determine the working state of the CO isotope scrambler, effectively preventing the catalyst filled with the CO isotope scrambler from working at high temperature for a long time, resulting in a decrease in catalytic efficiency, and thus reducing the conversion efficiency of CO isotopes, and preventing CO gas from entering the lower distillation tower without meeting the feed requirements of the lower distillation tower, thereby ensuring the discharge of the material. 13 C. Product quality.

[0029] In some embodiments, the detection signal value includes a signal value corresponding to the mass number of the CO gas and a signal value corresponding to the mass number of the carbon isotope in the CO gas.

[0030] It can be understood that when CO gas is passed into the mass spectrometer, it will be at mass number 28 ( 12 C 16 O)、29( 12 C 17 O and 13 C 16O)、30( 12 C 18 O and 13 C 17 O)、31( 13 C 18 O) to obtain four detection signal values, and at the same time, CO gas will generate a certain proportion of 12 C + , 13 C + Fragment ions can be used to obtain detection signal values ​​at mass numbers 12 and 13 of the fragment ions. Therefore, the signal value corresponding to the mass number of CO gas may include signal values ​​corresponding to mass numbers 28, 29, 30 and 31. The signal value corresponding to the mass number of carbon isotopes in CO gas may include signal values ​​corresponding to mass numbers 12 and 13.

[0031] In addition, because the mass spectrometer always contains a water background, which will form signals with masses 16 (O), 17 (HO), and 18 (H2O), the signals with mass numbers 16, 17, and 18 cannot represent the oxygen isotope composition of CO.

[0032] In some embodiments, determining the abundance value of carbon isotopes and the abundance value of oxygen isotopes in CO gas according to preset conditions and detection signal values ​​may include: determining the abundance value of each carbon isotope according to the signal value corresponding to the mass number of the carbon isotope in the CO gas; determining the abundance value of each oxygen isotope according to the signal value corresponding to the mass number of the CO gas and the preset conditions.

[0033] In some embodiments, the preset condition may include presetting the abundance value of the CO isotope gas component to be equal to the product of the abundance value of the corresponding carbon isotope and the abundance value of the corresponding oxygen isotope. It can be understood that the CO isotope scrambler can balance all isotopes with each other. If the scrambler works properly, the abundance value of the preset CO isotope gas component is equal to the product of the abundance value of the corresponding carbon isotope and the abundance value of the corresponding oxygen isotope.

[0034] In some embodiments, determining the abundance value of the oxygen isotope according to the signal value corresponding to the mass number of the CO gas and preset conditions may include: determining the abundance value of a preset CO isotope gas component according to the signal value corresponding to the mass number of the CO gas; determining the corresponding abundance value of the oxygen isotope according to the abundance value of the preset CO isotope gas component and its corresponding abundance value of the carbon isotope.

[0035] As described above, the abundance value of the preset CO isotope gas component is equal to the product of the abundance value of the corresponding carbon isotope and the abundance value of the oxygen isotope. By assuming in advance that the scrambler works normally, it is beneficial to verify the true working state of the scrambler through preset verification conditions, so as to accurately judge the working state of the CO isotope scrambler, and to promptly deal with the scrambler with abnormal working state.

[0036] In this embodiment, the preset CO isotope gas component may be a CO isotope gas component that can be directly detected by a mass spectrometer to obtain a corresponding abundance value, such as: 12 C 16 O and 13 C 18 O. In the detection signal obtained by the mass spectrometer, the signal value at the mass number 28 is only related to one ion fragment (i.e. 12 C 16 O + ), therefore, according to the signal value at mass number 28 detected by the mass spectrometer, it can be determined that 12 C 16 O abundance. Similarly, the signal value at mass number 31 is only related to one ion fragment (i.e. 13 C 18 O + ), therefore, according to the signal value at mass number 31, it can be determined that 13 C 18 The abundance of O.

[0037] In this embodiment, according to the detection signal values ​​of CO gas at mass numbers of 28 and 31, we can obtain 12 C 16 The abundance of O and 13 C 18 Furthermore, combined with the above-mentioned preset conditions, the abundance value of O can be calculated based on 12 C 16 The abundance of O 12 The abundance value of C is obtained 16 O abundance value. 13 C 18 The abundance of O 13 The abundance value of C is obtained 18 O abundance value. Finally, according to 16 The abundance of O and 18 The abundance of O is 17 The abundance of O.

[0038] Specifically, according to the signal values ​​of the mass spectrum peaks of CO gas with mass numbers 12 and 13, it can be obtained that 12 C and 13The abundance value of C is obtained according to the signal values ​​of the mass spectrum peaks of CO gas at mass numbers 28 and 31. 12 C 16 The abundance of O and 13 C 18 O abundance value. Assuming that the scrambler works normally, when the scrambler works normally, there are CO isotope gas components such as 12 C 16 The abundance of O is equal to 12 The abundance of C and 16 The product of the abundance values ​​of O is 16 O abundance value. When the scrambler is working normally, there are CO isotope gas components such as 13 C 18 The abundance of O is equal to 13 The abundance of C and 18 The product of the abundance values ​​of O is 18 O abundance value. Finally, according to 16 The abundance of O and 18 The abundance of O is 17 The abundance of O.

[0039] For example, 12 The abundance value of C can be expressed as [ 12 C], as shown in the following formula (1):

[0040] [ 12 C]=

[12] =I 12 / (I 12 +I 13 ) (1)

[0041] 13 The abundance value of C can be expressed as [ 13 C], as shown in the following formula (2):

[0042] [ 13 C]=

[13] =I 13 / (I 12 +I 13 ) (2)

[0043] 12 C 16 The abundance of O can be expressed as [ 12 C 16 O], as shown in the following formula (3):

[0044]

[28] = 12 C 16 O]=I 28 / (I 28 +I 29 + I 30 +I31 ) (3)

[0045] 13 C 18 The abundance of O can be expressed as [ 13 C 18 O], as shown in the following formula (4):

[0046]

[31] = [ 13 C 18 O]=I 31 / (I 28 +I 29 + I 30 +I 31 ) (4)

[0047] 16 The abundance of O can be expressed as [ 16 O]; 17 The abundance of O can be expressed as [ 17 O]; 18 The abundance of O can be expressed as [ 18 O]; the preset conditions can be as shown in formula (5) and formula (6):

[0048] [ 12 C 16 O]= [ 12 C] 16 O] (5)

[0049] [ 13 C 18 O]= [ 13 C] 18 O] (6)

[0050] Among them, I 12 ,I 13 ,I 28 ,I 29 ,I 30 ,I 31 They respectively represent the signal values ​​of the mass spectrometer at mass numbers 12, 13, 28, 29, 30, and 31;

[12] ,

[13] ,

[28] ,

[29] ,

[30] , and

[31] respectively represent the ratios of the signal values ​​of the mass spectrometer at mass numbers 12, 13, 28, 29, 30, and 31.

[0051] According to formula (5) and formula (6), we can get 16 The abundance of O and 18 The abundance of O. 17 The abundance value of O can be expressed as shown in the following formula (7):

[0052] [ 17 O]=1 – [16 O] – [ 18 O] (7)

[0053] As described above, in this embodiment, the abundance value of the carbon isotope in the CO gas is determined by the signal value corresponding to the mass number of the carbon isotope in the CO gas. Furthermore, the abundance value of the oxygen isotope is determined according to the preset conditions, the abundance value of the carbon isotope, and the signal value corresponding to the mass number of the CO gas, which is conducive to determining the abundance of the oxygen isotope when there is a background of water in the mass spectrometer.

[0054] In some embodiments, determining the theoretical abundance value of each CO isotope gas component in the CO gas based on the abundance value of the carbon isotope and the abundance value of the oxygen isotope and the detection signal value may include: determining the theoretical abundance value of the CO isotope gas component with a preset mass number in the CO gas based on the abundance value of the carbon isotope and the abundance value of the oxygen isotope.

[0055] Specifically, the preset mass number may be 29 or 30. 12 C] and [ 13 C], filter the abundance values ​​of carbon isotopes related to mass number 29 or 30; from [ 16 O]、[ 17 O] and [ 18 O], screening the abundance values ​​of oxygen isotopes associated with mass numbers 29 or 30; pairing the screened carbon isotopes and oxygen isotopes with preset mass numbers, respectively, to obtain a plurality of CO isotope gas components corresponding to the preset mass numbers; and according to each CO isotope gas component corresponding to the preset mass number, determining the product value of the abundance value of the carbon isotope and the abundance value of the oxygen isotope corresponding to each CO isotope gas component, that is, the theoretical abundance value of the CO isotope gas molecule with the preset mass number.

[0056] Specifically, the CO isotope gas components corresponding to the preset mass number of 29 may include: 12 C 17 O and 13 C 16 O. The CO isotope gas components corresponding to the preset mass number of 30 may include: 12 C 18 O and 13 C 17 O. Then, 12 C 17 The theoretical abundance of O can be obtained by the above calculation 12 The abundance of C and 17 The theoretical abundance values ​​of CO isotope gas components with other preset mass numbers can also be expressed in the same form.

[0057] In some embodiments, determining the working state of the scrambler according to the detection signal value and the theoretical abundance value of each CO isotope gas component may include: determining the abundance measurement value of all CO isotope molecules corresponding to the preset mass number according to the detection signal value; calculating the ratio between the abundance measurement value and the theoretical abundance value of all CO isotope molecules corresponding to the preset mass number; and determining the working state of the scrambler according to the ratio.

[0058] Among them, the preset mass number is 29 or 30, and the preset mass number 29 corresponds to all CO isotope gas components including 12 C 17 O and 13 C 16 O, the preset mass number is 30 and the corresponding CO isotope gas components include 12 C 18 O and 13 C 17 The measured abundance value of all CO isotope molecules corresponding to the preset mass number of 29 is the ratio of the signal value at the mass number of 29 obtained by mass spectrometry, and the theoretical abundance value of all CO isotope molecules corresponding to the preset mass number of 29 is 12 C 17 O and 13 C 16 The total theoretical abundance of O.

[0059] Specifically, the ratio can be expressed as δ1, which can be used to determine the working state of the scrambler, as shown in the following formula (8):

[0060] δ1=

[29] / ([ 12 C] 17 O] + [ 13 C] 16 O]) (8)

[0061] Or the ratio can also be expressed as δ2, as shown in the following formula (9):

[0062] δ2=

[30] / ([ 12 C] 18 O] + [ 13 C] 17 O]) (9)

[0063] After the above ratio δ1 and / or δ2 is calculated, the ratio δ1 and / or δ2 can be compared with a preset threshold value. When it is determined that the ratio meets the threshold value, the scrambler is in a normal working state; when it is determined that the ratio does not meet the threshold value, the scrambler is in an abnormal working state. In this embodiment, if the scrambler is in a good working state, the value of δ1 or δ2 should be close to 1, that is, all components are in a balanced state.

[0064] As described above, in this embodiment, by determining the ratio for detecting the working state of the scrambler, it is helpful to determine the working state of the scrambler, and effectively prevent the catalyst filled with the CO isotope scrambler from working for a long time at high temperature, thereby reducing the catalytic efficiency and the conversion efficiency of CO isotopes.

[0065] Figure 2 FIG. 1 is a schematic diagram of a method for detecting the working state of a CO isotope scrambler according to another embodiment of the present application. Figure 2 As shown, the method 200 for detecting the working state of the CO isotope scrambler may include operations S201 to S207.

[0066] In operation S201, the CO gas is detected by a mass spectrometer to obtain a detection signal value, wherein the CO gas is produced by distilling CO. 13 The CO gas is obtained from the scrambler outlet in the C process, and the CO gas includes all CO isotope gas components.

[0067] In operation S202, the abundance value of the carbon isotope in the CO gas and the abundance value of the oxygen isotope in the CO gas are determined according to preset conditions and the detection signal value.

[0068] In operation S203, a ratio for judging a working state of a scrambler is determined according to the abundance value of the carbon isotope, the abundance value of the oxygen isotope, and the detection signal value.

[0069] In operation S204, when it is determined that the ratio meets the threshold, it is determined that the scrambler operating state is normal.

[0070] In operation S205, in a case where it is determined that the ratio does not satisfy the threshold, it is determined that the scrambler operating state is abnormal.

[0071] In operation S206, when it is determined that the scrambler is operating normally, the scrambler continues to be used.

[0072] In operation S207, in a case where it is determined that the operating state of the scrambler is abnormal, the catalyst filled in the scrambler is replaced.

[0073] In this embodiment, the preset condition can be determined by assuming that the scrambler is in normal working state and the relationship between the CO isotope gas components. All CO isotope gas components may include: 12 C 16 O. 12 C 17 O. 12 C 18 O. 13 C 16 O. 13 C 17 O. 13 C18 O. Carbon isotopes can include 12 C and 13 C. Oxygen isotopes can include 16 O. 17 O and 18 O. The ratio used to judge the working state of the scrambler (i.e., the ratio δ1 and / or δ2) can be determined according to the detection signal value corresponding to the mass number of CO and the theoretical abundance value of the CO isotope gas component corresponding to the mass number of CO. The threshold value can be determined according to the actual detection situation, for example, it can be 1.2.

[0074] It should be noted that if the scrambler is working properly, the signal value ratio of mass number 29 should be equal to 12 C 17 O and 13 C 16 The abundance values ​​of O are added together, and the signal value ratio of mass number 30 should be equal to 12 C 18 O and 13 C 17 The working state of the CO isotope scrambler can be determined based on the ratio of the signal values ​​of mass numbers 29 and 30 and the degree of agreement with the theoretical abundance value of the CO isotope gas component calculated from the abundance values ​​of carbon isotopes and oxygen isotopes.

[0075] In this embodiment, when the ratio (i.e., δ1 and / or δ2) is greater than a threshold value, it can be considered that the threshold value is not met. For example, when the ratio (i.e., δ1 and / or δ2) is greater than 1.2, it indicates that the working state of the scrambler is abnormal and the catalyst filled in the scrambler needs to be replaced.

[0076] In this embodiment, when the ratio (i.e., δ1 and / or δ2) is less than or equal to a threshold, it can be considered that the threshold is met. For example, when the ratio (i.e., δ1 and / or δ2) is less than or equal to 1.2, it indicates that the scrambler is working normally and the scrambler can continue to be used.

[0077] As described above, in this embodiment, the abundance values ​​of carbon and oxygen isotopes in the CO gas are determined by preset conditions and detection signal values, and then the working state of the CO isotope scrambler is accurately determined by comparing the ratio used to determine the working state of the scrambler with the threshold value, which is conducive to timely replacement of the catalyst filled in the scrambler with abnormal working state, so that the catalytic efficiency of the scrambler is improved, the conversion efficiency of the CO isotope is improved, and the CO gas entering the lower distillation tower can meet the feed requirements of the lower distillation tower, so that the discharge 13 CThe product meets the requirements.

[0078] Figure 3 According to the embodiment of the present application, the distillation CO production 13Schematic diagram of the method of C.

[0079] like Figure 3 As shown, distillation CO production 13 Method C may include the following steps: after the CO gas enters a primary distillation tower 1 , it passes through a scrambler 2 and finally enters a secondary distillation tower 3 .

[0080] It should be noted that Figure 3 The arrow in the middle indicates the direction of CO gas inflow and outflow. Both the primary distillation tower 1 and the secondary distillation tower 3 can be composed of a plurality of distillation towers connected in series.

[0081] Understandably, when the gas from the outlet of the CO isotope scrambler is passed into the mass spectrometer, the largest peak is the so-called mother peak, representing the singly ionized CO + These are peaks with mass numbers of 28 to 31. At the same time, CO molecules also produce C + and O + Ion fragments. C + The signals of the ions are at mass numbers 12 and 13, which can represent the overall carbon isotope composition. However, because the mass spectrometer always has a water background, and the water background will form signals of mass 16 (O), 17 (HO) and 18 (H2O), the signals of mass numbers 16, 17, and 18 cannot represent the oxygen isotope composition of CO.

[0082] The embodiment of the present invention also provides a method for quickly detecting the working state of a CO isotope scrambler, which may specifically include: using a mass spectrometer to detect CO gas, assuming that there is no 17 In the case of CO, each of the four CO mass numbers has a unique CO isotope gas component. At this time, the isotope equilibrium constant can be expressed as the following formula (10), and the isotope equilibrium constant K should be equal to 1.

[0083] K=[ 12 C 16 O][ 13 C 18 O]) / ([ 13 C 16 O][ 12 C 18 O])=

[28]

[31] / (

[29]

[30] ) (10)

[0084] Since the mass number 31 component is limited by the natural abundance of heavy combinations, for a poorly scrambled gas, K will be less than 1. For a good scrambled gas, K will be about 0.7-0.8. The reason why K is not equal to 1 is that there are some neglected 17 O. If the K value is low, the scrambling may be insufficient and you need to consider replacing the catalyst filled in the scrambler.

[0085] However, compared with the above assumptions 17 The detection method of the CO isotope scrambler working state provided by the embodiment of the present application has higher detection accuracy. For CO gas including all CO isotope gas components, accurate and effective detection can still be performed.

[0086] The present invention is described in detail above with reference to the accompanying drawings and embodiments, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of ordinary technicians in the field without departing from the purpose of the present invention. The contents not described in detail in the present invention can adopt the existing technology.

Claims

1. A method for detecting the working state of a CO isotope scrambler, wherein: include: S101: Detecting CO gas using a mass spectrometer to obtain a detection signal value, wherein the CO gas is obtained from an outlet of a CO isotope scrambler and includes a plurality of CO isotope gas components; the detection signal value includes: a signal value corresponding to the mass number of the CO gas and a signal value corresponding to the mass number of a carbon isotope in the CO gas; S102: determining the abundance value of each carbon isotope according to the signal value corresponding to the mass number of the carbon isotope in the CO gas, and determining the abundance value of each oxygen isotope according to a preset condition and the signal value corresponding to the mass number of the CO gas; The preset condition includes that the abundance value of the preset CO isotope gas component is equal to the product of the abundance value of the corresponding carbon isotope and the abundance value of the corresponding oxygen isotope, and the preset CO isotope gas component is 12 C 16 O or 13 C 18 O; Determine the abundance value of the preset CO isotope gas component according to the signal value corresponding to the mass number of the CO gas; determine the corresponding abundance value of the oxygen isotope according to the abundance value of the preset CO isotope gas component and the corresponding abundance value of the carbon isotope; S103: determining a theoretical abundance value of a CO isotope gas component of a preset mass number in the CO gas according to the abundance value of the carbon isotope and the abundance value of the oxygen isotope, wherein the preset mass number is 29 or 30; According to each of the CO isotope gas components corresponding to the preset mass number, the product value of the abundance value of the carbon isotope and the abundance value of the oxygen isotope corresponding to each of the CO isotope gas components is determined, that is, the theoretical abundance value of the CO isotope gas molecule of the preset mass number, thereby determining the theoretical abundance value of each CO isotope gas component in the CO gas; S104: determining the abundance measurement value of all CO isotope molecules corresponding to the preset mass number according to the detection signal value; calculating the ratio between the abundance measurement value of all CO isotope molecules corresponding to the preset mass number and the theoretical abundance value; The working state of the scrambler is determined according to the ratio; wherein, when it is determined that the ratio meets a threshold, the working state of the scrambler is normal, and when it is determined that the ratio does not meet the threshold, the working state of the scrambler is abnormal.

2. The method according to claim 1, wherein: Also includes: When determining that the scrambler is in a normal working state, continue to use the scrambler; When it is determined that the working state of the scrambler is abnormal, the catalyst filled in the scrambler is replaced.

3. The method according to claim 1, wherein: The CO gas includes: 12 C 16 O. 12 C 17 O. 12 C 18 O. 13 C 16 O. 13 C 17 O and 13 C 18 O.

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