CN116818954A - Method for detecting boron-10 isotope abundance by adopting GC-MS - Google Patents
Method for detecting boron-10 isotope abundance by adopting GC-MS Download PDFInfo
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- CN116818954A CN116818954A CN202310943668.9A CN202310943668A CN116818954A CN 116818954 A CN116818954 A CN 116818954A CN 202310943668 A CN202310943668 A CN 202310943668A CN 116818954 A CN116818954 A CN 116818954A
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- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract 17
- 238000001514 detection method Methods 0.000 claims abstract description 17
- 150000001793 charged compounds Chemical class 0.000 claims abstract description 16
- 238000005070 sampling Methods 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 8
- 238000010586 diagram Methods 0.000 claims description 6
- 238000002309 gasification Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000005452 bending Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 description 23
- 239000007789 gas Substances 0.000 description 11
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 8
- 229910052796 boron Inorganic materials 0.000 description 8
- 230000001133 acceleration Effects 0.000 description 3
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical group B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 241000233805 Phoenix Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZOXJGFHDIHLPTG-IGMARMGPSA-N boron-11 atom Chemical compound [11B] ZOXJGFHDIHLPTG-IGMARMGPSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000176 thermal ionisation mass spectrometry Methods 0.000 description 1
- 238000001269 time-of-flight mass spectrometry Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A method for detecting the abundance of boron-10 isotopes using GC-MS, comprising the steps of: s1, preparing a sample for detection; s2, gasifying the sample; s3, ionizing sample gas molecules and separating according to mass-to-charge ratio (m/z); s4, collecting molecular ion peaks to obtain a total ion flow graph; s5, data processing is carried out according to the following formula:s6, correcting deviation of data. Compared with the prior art, the technical scheme provided by the invention has the following advantages: the investment of equipment cost is low, and the detection result is quick, accurate, efficient and high in practicability.
Description
Technical Field
The invention relates to boron-10 isotope abundance detection, in particular to a method for detecting boron-10 isotope abundance by adopting GC-MS.
Background
Boron is known in nature to have two stable isotopes, boron-10 and boron-11, with relative abundances of about 20% and 80%, respectively. However, the composition of boron isotopes varies greatly in different regions, environments and substances. With the continuous progress of human science and technology, the demand for boron is increasing, for example, aluminum borohydride can be utilized to realize light weight of structural materials in the field of internet equipment, photoelectric conversion efficiency can be improved by boron doping in the field of solar cells, a brake material which can be used for nuclear fission reaction by utilizing the characteristic of high neutron absorption efficiency of boron in the field of nuclear, a plugboard which can be used for manufacturing body armor or bulletproof nonmetallic armor on armored vehicles and armed helicopters by utilizing the specific light and high-hardness boron carbide structure in the field of security, and the like.
Thus, there is a need for a method that can rapidly and cost-effectively determine the abundance of boron isotopes in a substance.
For example, chinese patent application publication No. CN108267497a entitled analysis device and method for measuring boron isotopes by thermal ionization time-of-flight mass spectrometry discloses: the ion detector comprises a thermal ionization ion source, a classical lens, a gate valve, a detector, a field-free drift region, a detection high-voltage circuit, a grid voltage and a reflection voltage, wherein the gate valve is arranged between the thermal ionization ion source and the classical lens, ions generated by the thermal ionization ion source are focused through the electrostatic lens after passing through the gate valve, the focused ions deflect under the action of pulse voltage applied to a repulsive plate and enter an acceleration region, then the ions finally reach the detector through the field-free drift region and the like according to a specific path, when no voltage exists on the repulsive plate, the ions are directly received by the Faraday cup, the field-free drift region is arranged below the acceleration voltage, the detector and the acceleration voltage are arranged above the field-free drift region in parallel, the detection high-voltage circuit is arranged on the detector, the grid voltage is arranged below the field-free drift region, and the reflection voltage is arranged below the grid voltage. Although the invention can rapidly and accurately measure the abundance of boron isotopes, the adopted thermal surface ionization mass spectrometer Phoenix has high cost and is not suitable for realizing low-cost detection.
For another example, chinese application publication No. CN113049667a entitled thermal ionization mass spectrometry method for detecting the abundance of boron-10 in boron carbide discloses: comprises the following steps: sample treatment; step 2: measuring a sample; step 3: and calculating the abundance of the sample according to a specific formula. However, the detection method is certainly based on using a thermal ionization isotope mass spectrometer Isoprobe T, and the problems that the instrument is expensive in cost and not suitable for realizing low-cost detection can not be overcome.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a boron-10 isotope detection method which adopts a low-cost detection instrument to realize rapidness, accuracy, high efficiency and strong practicability.
The invention mainly adopts the following technical scheme:
a method for detecting the abundance of boron-10 isotopes using GC-MS, comprising the steps of:
s1, preparing a sample for detection;
s2, carrying out gasification treatment on the sample:
sucking a sample by using a sample injection needle and injecting the sample into a sample injection port of the GC-MS, wherein the sample forms sample gas molecules in a gasification chamber of the GC-MS;
s3, ionizing sample gas molecules and separating according to mass-to-charge ratio (m/z):
separating the sample gas molecules by a chromatographic column of the GC-MS, then sending the sample gas molecules into an ion source of the GC-MS for ionization treatment, pumping the formed molecular ions into a mass analyzer of the GC-MS for separation according to mass-to-charge ratio (m/z), collecting the molecular ion flow by a detector of the GC-MS, and measuring the intensity of the molecular ion flow;
s4, collecting molecular ion peaks to obtain a total ion flow diagram:
pressing the Start key of GC-MS to collect molecular ion peak, sampling once every 1min for 5 times, clicking Stop key on computer screen to complete the first collection,
determining to complete at least one collection operation according to the column effect of the chromatographic column;
s5, data processing:
the peak height (H) of the 262 ion peak is read in the integral and percent report from the total ion flow graph 262 ) And peak height of 263 ion peak (H 263 ) The boron-10 is calculated according to the following formula 10 B) Abundance of isotopes:
discarding discrete data in the data obtained by at least one acquisition operation, and calculating to obtain an average value;
s6, correcting deviation of data:
and (3) processing standard substances with similar abundance by adopting the steps S2-S5, and rectifying the average value according to data obtained by the standard substances to control the deviation within 0.1%.
Wherein, the step S1 adopts an extraction separation method to prepare a sample for detection.
Wherein, in the step S5, the discrete data is determined by Grubbs checking table, when T is more than or equal to Ta, the Ta is a critical value checked according to Grubbs checking table, whereinWherein X is i And (3) sampling the obtained data for each sampling of the acquisition work, wherein n is the sampling times, and X is the average value of the obtained data for n sampling of the acquisition work.
Wherein the length of the chromatographic column of the GC-MS is 25m to 30m, the inner diameter is 0.1mm to 0.53mm, and the film thickness is 0.1um.
The mass analyzer of the GC-MS comprises a flight tube and a magnet, wherein the flight tube is arranged in a bending mode, and the magnet is arranged above the flight tube.
Wherein the flight time of the flight tube is 30us to 200us.
According to the technical scheme of the invention, the method has the following beneficial effects: the invention can adopt a gas chromatograph-mass spectrometer (GC-MS) with low cost to detect the abundance of the boron-10 isotope, reduces the expense of enterprises or scientific research institutions, and can realize the purposes of high detection speed, high accuracy and strong practicability.
Drawings
Fig. 1 is a total ion flow diagram of the 262 ion peaks.
Fig. 2 is a total ion flow diagram of the 263 ion peak.
Detailed Description
The invention is further elucidated below in connection with the accompanying drawings:
a method for detecting the abundance of boron-10 isotopes using GC-MS, comprising the steps of:
s1, preparing a sample for detection;
s2, carrying out gasification treatment on the sample:
sucking a sample by using a sample injection needle and injecting the sample into a sample injection port of the GC-MS, wherein the sample forms sample gas molecules in a gasification chamber of the GC-MS;
s3, ionizing sample gas molecules and separating according to mass-to-charge ratio (m/z):
separating the sample gas molecules by a chromatographic column of the GC-MS, then sending the sample gas molecules into an ion source of the GC-MS for ionization treatment, pumping the formed molecular ions into a mass analyzer of the GC-MS for separation according to mass-to-charge ratio (m/z), collecting the molecular ion flow by a detector of the GC-MS, and measuring the intensity of the molecular ion flow;
s4, collecting molecular ion peaks to obtain a total ion flow diagram:
pressing the Start key of GC-MS to collect molecular ion peak, sampling once every 1min for 5 times, clicking Stop key on computer screen to complete the first collection,
determining to complete at least one collection operation according to the column effect of the chromatographic column;
s5, data processing:
the peak height (H) of the 262 ion peak is read in the integral and percent report according to the total ion flow diagram, as shown in fig. 1 and 2 262 ) And peak height of 263 ion peak (H 263 ) The boron-10 is calculated according to the following formula 10 B) Abundance of isotopes:
discarding discrete data in the data obtained by at least one acquisition operation, and calculating to obtain an average value;
s6, correcting deviation of data:
and (3) processing standard substances with similar abundance by adopting the steps S2-S5, and rectifying the average value according to data obtained by the standard substances to control the deviation within 0.1%. Preferably, in step S3, the sample gas molecules are separated by feeding them with a carrier gas to a GC-MS column. Preferably, the ion source of the GC-MS employs an electron bombardment ionization (EI) method of 70eV to strip electrons from the sample gas molecules.
Further, the step S1 is to prepare a sample for detection by an extraction separation method.
Further, in the step S5, the discrete data is determined by Grubbs 'test table, and when T is not less than Ta, the discrete data is determined, wherein Ta is a critical value according to Grubbs' test table, whereinWherein X is i And (3) sampling the obtained data for each sampling of the acquisition work, wherein n is the sampling times, and X is the average value of the obtained data for n sampling of the acquisition work. Preferably, n.gtoreq.5.
Further, the GC-MS chromatographic column has a length of 25m to 30m, an inner diameter of 0.1mm to 0.53mm, and a film thickness of 0.1um. Preferably, the GC-MS chromatographic column has a length of 30m, an inner diameter of 0.32mm to 0.53mm, and a film thickness of 0.1um.
Further, the mass analyzer of the GC-MS includes a flight tube and a magnet, the flight tube being disposed in a curved manner, the magnet being disposed above the flight tube.
Further, the flight time of the flight tube is 30us to 500us.
While the foregoing has been with reference to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes may be made in this embodiment without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.
Claims (6)
1. A method for detecting the abundance of boron-10 isotopes by GC-MS, characterized in that: the method comprises the following steps:
s1, preparing a sample for detection;
s2, carrying out gasification treatment on the sample:
sucking a sample by using a sample injection needle and injecting the sample into a sample injection port of the GC-MS, wherein the sample forms sample gas molecules in a gasification chamber of the GC-MS;
s3, ionizing sample gas molecules and separating according to mass-to-charge ratio (m/z):
separating the sample gas molecules by a chromatographic column of the GC-MS, then sending the sample gas molecules into an ion source of the GC-MS for ionization treatment, pumping the formed molecular ions into a mass analyzer of the GC-MS for separation according to mass-to-charge ratio (m/z), collecting the molecular ion flow by a detector of the GC-MS, and measuring the intensity of the molecular ion flow;
s4, collecting molecular ion peaks to obtain a total ion flow diagram:
pressing the Start key of GC-MS to collect molecular ion peak, sampling once every 1min for 5 times, clicking Stop key on computer screen to complete the first collection,
determining to complete at least one collection operation according to the column effect of the chromatographic column;
s5, data processing:
the peak height (H) of the 262 ion peak is read in the integral and percent report from the total ion flow graph 262 ) And peak height of 263 ion peak (H 263 ) The boron-10 is calculated according to the following formula 10 B) Abundance of isotopes:
discarding discrete data in the data obtained by at least one acquisition operation, and calculating to obtain an average value;
s6, correcting deviation of data:
and (3) processing standard substances with similar abundance by adopting the steps S2-S5, and rectifying the average value according to data obtained by the standard substances to control the deviation within 0.1%.
2. The method for detecting the abundance of boron-10 isotopes by GC-MS of claim 1, wherein: the step S1 is to prepare a sample for detection by adopting an extraction separation method.
3. The method for detecting the abundance of boron-10 isotopes by GC-MS of claim 1, wherein: the step S5In the step, the discrete data is determined by Grubbs 'test table lookup, and is determined to be the discrete data when T is more than or equal to Ta, wherein Ta is a critical value searched according to the Grubbs' test table lookup, wherein Wherein X is i And (3) sampling the obtained data for each sampling of the acquisition work, wherein n is the sampling times, and X is the average value of the obtained data for n sampling of the acquisition work.
4. A method for detecting the abundance of boron-10 isotopes by GC-MS according to any of claims 1-3, characterized in that: the GC-MS chromatographic column has a length of 25m to 30m, an inner diameter of 0.1mm to 0.53mm, and a film thickness of 0.1um.
5. A method for detecting the abundance of boron-10 isotopes by GC-MS according to any of claims 1-3, characterized in that: the mass analyzer of the GC-MS comprises a flight tube and a magnet, wherein the flight tube is arranged in a bending mode, and the magnet is arranged above the flight tube.
6. The method for detecting the abundance of boron-10 isotopes by GC-MS of claim 5, wherein: the flight time of the flight tube is 30 to 200us.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310943668.9A CN116818954A (en) | 2023-07-31 | 2023-07-31 | Method for detecting boron-10 isotope abundance by adopting GC-MS |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104330515A (en) * | 2014-11-19 | 2015-02-04 | 上海化工研究院 | Method for testing isotope abundance and chemical purity of <13>C marked straight-chain fatty acid |
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| CN113049667A (en) * | 2019-12-26 | 2021-06-29 | 中核北方核燃料元件有限公司 | Thermal ionization mass spectrum detection method for boron-10 abundance in boron carbide |
| CN116413328A (en) * | 2021-12-31 | 2023-07-11 | 中核北方核燃料元件有限公司 | Method for measuring abundance of boron-10 in zirconium diboride |
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2023
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