CN119275081A - A sampling system and method for a stable isotope mass spectrometer - Google Patents
A sampling system and method for a stable isotope mass spectrometer Download PDFInfo
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- CN119275081A CN119275081A CN202411700369.3A CN202411700369A CN119275081A CN 119275081 A CN119275081 A CN 119275081A CN 202411700369 A CN202411700369 A CN 202411700369A CN 119275081 A CN119275081 A CN 119275081A
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Abstract
本发明公开了一种用于稳定性同位素质谱仪的进样系统及方法，涉及质谱仪技术领域。包括依次连接的采样装置、雾化装置、进样装置和质谱仪；采样装置，用于采取待测样品，将待测样品输送至雾化装置；雾化装置，用于产生质谱仪检测需要的雾化样品；进样装置，用于将雾化样品进样至质谱仪；质谱仪，用于对雾化样品进行质谱分析。本发明通过定量带入质谱仪的产气减小了测试结果的误差，提高了测试结果的准确度，实现了连续进样，保证了测试的连续性，提高了测试结果的准确度。
The present invention discloses a sampling system and method for a stable isotope mass spectrometer, and relates to the technical field of mass spectrometers. The system comprises a sampling device, an atomizing device, an injection device and a mass spectrometer connected in sequence; the sampling device is used to take a sample to be tested and convey the sample to be tested to the atomizing device; the atomizing device is used to produce an atomized sample required for detection by the mass spectrometer; the injection device is used to inject the atomized sample into the mass spectrometer; the mass spectrometer is used to perform mass spectrometry analysis on the atomized sample. The present invention reduces the error of the test result by quantitatively bringing the gas produced into the mass spectrometer, improves the accuracy of the test result, realizes continuous injection, ensures the continuity of the test, and improves the accuracy of the test result.
Description
Technical Field
The invention relates to the technical field of mass spectrometers, in particular to a sample injection system and method for a stable isotope mass spectrometer.
Background
In 1910, thomson, a laboratory of cambridge, camndi, england developed a first modern mass spectrometer, the birth of which marks the beginning of mass spectrometry, a new area of scientific research. The dual focus mass spectrometer that was born in 1934 is yet another milestone for the development of mass spectrometry. In 1943, the first commercial mass spectrometer emerged, and mass spectrometers have been introduced into the industrial and agricultural fields. The 50 th century of the 20 th century is an age of rapid development of mass spectrometry technology, and in terms of mass analyzers, the performance of high-resolution dual-focusing instruments is further improved, and quadrupole mass filters, pulse time-of-flight analyzers and the like are presented. At the end of the 60 s of the 20 world, tandem mass spectrometer development and gas chromatography and mass spectrometry were successful, so that mass spectrometry has a unique position in the analysis of complex organic mixtures. In the 90 s of the 20 th century, a new field for researching biological macromolecules by mass spectrometry technology is created by a matrix-assisted laser desorption ionization source, an electrospray ionization source, an atmospheric pressure chemical ionization source and an atmospheric pressure chemical ionization source. In 2002, the us scientist john feen shares the annual nobel chemical prize with the japanese scientist field intertillage, as "electrospray ionization and matrix-assisted laser desorption ionization mass spectrometry for biomacromolecules" was invented.
Mass spectrometry is the most versatile and accurate method in stable isotope analysis. The method comprises the steps of ionizing molecules or atoms in a sample to form similar ions of each isotope, and then separating ion flows with different mass to charge ratios under the action of an electric field and a magnetic field to detect.
Isotopes refer to elements having the same atomic number (number of protons) and different mass numbers (number of neutrons), and are called isotopes, and can be classified into stable isotopes and radioisotopes. Stable isotopes are a class of isotopes where no radioactivity is detectable by naturally occurring means of technology. The stable isotope is low in natural content, and it is difficult to express the difference of isotopes by absolute amounts, so that in practice, a relative measurement method is used, i.e., the isotope ratio (i.e., delta value) of a sample is obtained from the isotope ratio of the measured sample and the isotope ratio of the corresponding standard. Stable isotopes are widely used in the fields of soil, medicine, agriculture, biology, ecology, environment, etc.
The stable isotope mass spectrometer is a mass spectrometer (IRMS) specially used for measuring the ratio of C, H, O, N to S stable isotopes. Mass spectrometry is carried out in the form of a gas in the case of stable isotope analysis of light elements, so that the sample to be analyzed is first converted into a gas. In the ion source, gas molecules are ionized into positively charged ions, the ions are separated according to the mass-to-charge ratio by the action of an electric field and a magnetic field, and then the stable isotope ratio is measured according to the intensity of different ion beams, wherein the stable isotope mass spectrometry can be measured by adopting a single path or adopting a double path (a sample path and a standard path). The existing sample feeding mode needs to weigh the weight of the wrapped sample tinfoil, peel and weigh the weight of the sample, wrap the sample, and then feed the sample on a machine, so that the operation is complicated. Therefore, how to obtain an automatic sample injection system with simple operation and ensure the accuracy of the test result is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a sample injection system and a method for a stable isotope mass spectrometer, which reduce the error of a test result by quantifying the gas produced by the mass spectrometer, improve the accuracy of the test result, realize continuous sample injection, ensure the continuity of the test and improve the accuracy of the test result.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A sample injection system for a stable isotope mass spectrometer comprises a sampling device, an atomizing device, a sample injection device and a mass spectrometer which are connected in sequence;
the sampling device is used for taking a sample to be tested and conveying the sample to be tested to the atomizing device;
an atomizing device for generating an atomized sample required for mass spectrometer detection;
The sample injection device is used for injecting an atomized sample into the mass spectrometer;
a mass spectrometer for performing mass spectrometry on the atomized sample.
The system, optionally, further comprises a sample tray connected with the input end of the sampling device and used for carrying a tin boat filled with samples to be detected.
The system, optionally, the atomizing device comprises a liquid storage block, a hollow capillary tube and a cavity, one end of the hollow capillary tube is connected to the bottom of the liquid storage block as a sample injection end, the other end of the hollow capillary tube stretches into the cavity as a spray end, the sample injection device is communicated with the cavity, and the input auxiliary atomizing gas acts on the spray end of the hollow capillary tube.
The system, optionally, further comprises a vacuum device for providing a vacuum environment for the mass spectrometer, wherein the vacuum device is continuously operated by the diffusion pump after being pre-vacuumized by the mechanical pump so as to keep providing the vacuum environment for the mass spectrometer.
In the above system, optionally, the sample feeding device is provided with a plurality of filtering membrane nets, the filtering membrane nets are provided with holes, and outlets of the plurality of filtering membrane nets are converged at one outlet.
The system, optionally, further comprises a data monitoring and processing device, wherein the data monitoring and processing device is used for collecting data and calculation results, analyzing and judging results, storing and calling the data and monitoring various parameters of the system.
The system can be used for sampling the sample to be tested by using an airtight syringe.
A sample injection method for a stable isotope mass spectrometer, which is applied to a sample injection system for the stable isotope mass spectrometer, comprises the steps of continuously introducing gas into a sampling device, injecting a sample to be tested into an atomizing device by using an airtight injector, atomizing the sample to be tested and sending the atomized sample to a mass spectrometer, and analyzing the gas to be tested by the mass spectrometer.
Compared with the prior art, the sample injection system and method for the stable isotope mass spectrometer have the advantages that the error of a test result is reduced by quantifying the gas produced by the mass spectrometer, the accuracy of the test result is improved, continuous sample injection is realized, the continuity of the test is ensured, and the accuracy of the test result is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
Fig. 1 is a block diagram of a sample injection system for a stable isotope mass spectrometer.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the invention discloses a sample injection system for a stable isotope mass spectrometer, which comprises a sampling device, an atomizing device, a sample injection device and a mass spectrometer which are connected in sequence;
the sampling device is used for taking a sample to be tested and conveying the sample to be tested to the atomizing device;
an atomizing device for generating an atomized sample required for mass spectrometer detection;
The sample injection device is used for injecting an atomized sample into the mass spectrometer;
a mass spectrometer for performing mass spectrometry on the atomized sample.
Specifically, the mass spectrometer adopts a Flash EA 1112 type mass spectrometer and is provided with a continuous flow interface device ConfloIII.
Specifically, the sample to be measured is N 2、N2 O, NO or CO 2.
Further, the device also comprises a sample tray which is connected with the input end of the sampling device and is used for bearing a tin boat filled with samples to be detected.
Further, the atomizing device comprises a liquid storage block, a hollow capillary tube and a cavity, one end of the hollow capillary tube is connected to the bottom of the liquid storage block and used as a sample injection end, the other end of the hollow capillary tube extends into the cavity and used as a spray end, the sample injection device is communicated to the cavity, and auxiliary atomization gas is input to act on the spray end of the hollow capillary tube.
Further, the device also comprises a vacuum device for providing a vacuum environment for the mass spectrometer, wherein after the vacuum device adopts a mechanical pump to pre-vacuumize, the diffusion pump is used for continuously operating so as to keep providing the vacuum environment for the mass spectrometer.
In particular, the vacuum device is made of stainless steel and is detachably connected with other devices, so that all devices can be cleaned during pretreatment cleaning and maintenance.
Further, the sample injection device is provided with a plurality of filtering diaphragm nets, holes are formed in the filtering diaphragm nets, and outlets of the filtering diaphragm nets are converged at one outlet.
Specifically, the material of the filtering diaphragm net is copper, nickel and molybdenum.
Further, the system also comprises a data monitoring and processing device which is used for collecting data and calculation results, analyzing and judging results, storing and calling data and monitoring various parameters of the system.
Specifically, the data monitoring and processing device comprises a signal amplifier, a digital converter and a memory.
Further, the sample to be tested is injected by using an airtight syringe.
In one embodiment, the Flash EA 1112 type mass spectrometer system is started up and is heated after Carrier-He Carrier gas is introduced for 2.5 hours, the temperature of an oxidation column is set to 980 ℃, the temperature of a reduction column is set to 640 ℃, and the temperature of a water absorption column is set to 40 ℃.
The sample to be tested is sent into an EA oxidation column through a sample injection system of the invention under the tight package of a tin boat, the sample to be tested is instantaneously decomposed at high temperature in a peroxy environment, the formed mixed gas containing various components such as carbon, nitrogen, oxygen, sulfur and the like enters a continuous flow interface device ConfloIII under the carrying of high-purity helium (99.999%), in the process, the carbon in the sample is finally converted into CO 2 and is separated and purified with other gases through a chromatographic separation column, CO 2 is sent into an ion source of an IRMS under the carrying of high-purity helium (99.999%) after being rectified by the continuous flow interface device ConfloIII, the ion source ionizes atoms and molecules in the CO 2 sample into ions, a mass analyzer separates the ions according to the mass-to-charge ratio, the ion flow intensity is measured and recorded by an ion detector, the high-purity carbon dioxide (99.995%) is used as a reference standard to obtain a mass spectrogram, and finally the carbon isotope ratio of the sample is calculated through a data processing system.
In another embodiment, a 1mL gas tight injector is used to collect N 2 gas, the N 2 gas is injected into the sample injection system of the stable isotope mass spectrometer of the invention through a gas sample injection device, and the nitrogen isotope ratio of N 2 is determined.
Corresponding to the system shown in fig. 1, the embodiment of the invention also provides a sample injection method for the stable isotope mass spectrometer, which specifically comprises the steps of continuously introducing gas into a sampling device, injecting a sample to be tested into an atomizing device by using an airtight injector, atomizing the sample to be tested, and sending the atomized sample to the mass spectrometer, wherein the mass spectrometer analyzes the gas to be tested.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
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| Application Number | Priority Date | Filing Date | Title |
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| CN202411700369.3A CN119275081A (en) | 2024-11-26 | 2024-11-26 | A sampling system and method for a stable isotope mass spectrometer |
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| CN202411700369.3A CN119275081A (en) | 2024-11-26 | 2024-11-26 | A sampling system and method for a stable isotope mass spectrometer |
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