CN109841484B - Photoionization mass spectrometry device and method for qualitatively and quantitatively analyzing isomer mixture - Google Patents
Photoionization mass spectrometry device and method for qualitatively and quantitatively analyzing isomer mixture Download PDFInfo
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Abstract
The invention provides a photoionization mass spectrometry device and a method for qualitatively and quantitatively analyzing an isomer mixture. The photoionization mass spectrometry device comprises an ionization source cavity with a closed upper end and an open lower end, an ion transmission area cavity with an open upper end and an open lower end, and a mass analyzer cavity with a closed upper end and an open lower end, which are sequentially arranged from top to bottom; and a flat-plate-shaped ionization source outlet electrode is arranged between the ionization source cavity and the ion transmission region cavity. The qualitative and quantitative analysis method of the isomer mixture is based on the characteristic that different components of the isomer have different fragmentation degrees under different dissociation electric fields, collision energy controllable collision induced dissociation is introduced into a photoionization mass spectrum, and characteristic spectrograms of the components and the mixture of the isomer under different dissociation electric field strengths are respectively obtained; and establishing an analysis algorithm according to the characteristic ion species and the relative strength of each component of the isomer, so that the quick and accurate qualitative and quantitative analysis of each component in the isomer mixture can be realized.
Description
Technical Field
The invention relates to a mass spectrometry instrument and a method, in particular to a photoionization mass spectrometry device and a method for qualitatively and quantitatively analyzing an isomer mixture.
Background
Volatile Organic Compounds (VOCs) and semi-volatile organic compounds (SVOCs) are widely distributed in the environment, although the content of the VOCs and the SVOCs is usually low, most of the VOCs and the SVOCs have biotoxicity, great harm to human bodies, high bioaccumulation, and even carcinogenesis, teratogenesis and mutagenicity, so that the analysis and research of the VOCs and the SVOCs in the environment, particularly the rapid online detection, are widely regarded. At present, the international and universal standard detection methods for VOCs and SVOCs in the environment, such as U.S. EPAMethod524.2 and 524.2 and national standard GB/T17130-. However, the off-line method is long in time consumption and high in cost, and the process of rapid dynamic change of the object to be measured is difficult to reflect.
The mass spectrometry has the characteristics of good universality, high resolution and sensitivity, high analysis speed and strong qualitative capability, is the most widely used analysis method in the field of analysis and test, particularly is the combination of the mass spectrometry and a soft ionization technology to form an online mass spectrometry technology, the obtained mass spectrogram mainly comprises a molecular ion peak or an excimer ion peak, and is simple, easy to analyze and suitable for the rapid analysis of complex components. The photoionization is an efficient soft ionization technology, and ionization is obtained by directly releasing electrons after a molecule of an object to be detected absorbs a photon (single photon ionization) with single photon energy larger than the ionization energy of the photon or photons with multiple photons with total energy larger than the ionization energy of the photon (multiphoton ionization). Because the photon energy absorbed by the molecules of the object to be detected is only slightly higher than the ionization energy of the molecules, the molecules of the object to be detected can generate a large amount of molecular ions after photoionization, almost no fragment ions exist, the obtained spectrogram is simple, rapid analysis can be carried out according to the molecular weight and mass spectrum peak intensity information of the substance, and the method is particularly suitable for rapid online detection of complex organic samples [ Chinese invention patent: 201010567335.3, 201610116956.7]. However, for organic isomers having the same molecular formula, i.e. the same molecular weight, but different molecular structures, only molecular ion peaks having the same mass-to-charge ratio can be given in the photoionization mass spectrogram, and due to the lack of fragment ion information, it is difficult to obtain the molecular structure of the analyte, and qualitative and quantitative analysis of the isomers is even impossible. Although a conventional Electron Ionization (EI) source in an organic matter mass spectrum can bombard molecules of an object to be detected by using 70eV electrons to obtain abundant fragment ions and molecular structure information, when a complex mixture is analyzed, a large number of fragment ions can cause serious overlapping of spectral peaks, so that spectrum recognition is difficult, and rapid online analysis is difficult to realize.
Therefore, the invention designs a photoionization mass spectrum device and a photoionization mass spectrum method for qualitatively and quantitatively analyzing an isomer mixture, which introduce collision energy controllable collision induced dissociation into the photoionization mass spectrum, can generate characteristic fragment ions of an object to be detected on the basis of photoionization mainly based on molecular ions, and acquire molecular structure information of the object to be detected. And establishing an analysis algorithm according to the difference of the characteristic fragment ion species or relative strength of each component of the isomer, thereby realizing the rapid and accurate qualitative and quantitative analysis of each component in the isomer mixture.
Disclosure of Invention
The invention aims to provide a photoionization mass spectrum device and a photoionization mass spectrum method for qualitative and quantitative analysis of an isomer mixture.
In order to achieve the purpose, the invention adopts the technical scheme that:
the photoionization mass spectrum device for qualitatively and quantitatively analyzing the isomeric mixture comprises an ionization source cavity with a closed upper end and an open lower end, an ion transmission area cavity with an open upper end and an open lower end and a mass analyzer cavity with an open upper end and an open lower end, which are sequentially arranged from top to bottom; a flat ionization source outlet electrode is arranged between the ionization source cavity and the ion transmission region cavity, and the lower opening end of the ionization source cavity and the upper opening end of the ion transmission region cavity are respectively connected with the ionization source outlet electrode in a sealing way; a flat-plate-shaped differential interface board is arranged between the ion transmission area cavity and the mass analyzer cavity, and the lower opening end of the ion transmission area cavity and the upper opening end of the mass analyzer cavity are respectively connected with the differential interface board in a sealing way; vacuum pump interfaces are respectively arranged on the side walls of the ionization source cavity, the ion transmission region cavity and the mass analyzer cavity;
the ionization source outlet electrode and the differential interface board are arranged in parallel, through holes are formed in the middle of the ionization source outlet electrode and the middle of the differential interface board, and the through holes are coaxial;
more than 1 flat ionization region electrode is arranged in the ionization source cavity, more than 1 ionization region electrode and ionization source outlet electrode are arranged in a spaced and parallel way, and the middle part of the ionization region electrode is provided with a through hole which is coaxial with the through hole of the ionization source outlet electrode; an ultraviolet light beam emitted by an ultraviolet light source is positioned in the ionization source cavity, passes through the central area of the electrode through hole in the ionization region and irradiates the surface of the electrode at the outlet of the ionization source, and the transmission direction of the ultraviolet light beam is coaxial with the electrode through hole in the ionization region; a sample gas inlet pipe penetrates through the outer wall of the ionization source cavity and extends into the ionization source cavity, the gas outlet end of the sample gas inlet pipe faces the through hole area of the ionization region electrode, and the gas inlet end of the sample gas inlet pipe is connected with an external sample gas source;
an ion transmission area inlet electrode and an electrostatic ion lens are sequentially arranged in the ion transmission area cavity along the axial direction from the ionization source outlet electrode to the differential interface plate through hole, and the ionization source outlet electrode, the ion transmission area inlet electrode, the electrostatic ion lens and the differential interface plate are arranged at intervals;
the ion transmission area inlet electrode is a flat plate type metal electrode with a through hole in the middle, or a conical metal electrode with an axial through hole, or a quadrupole rod, a hexapole rod or an octopole rod electrode consisting of 4, 6 or 8 metal round rods arranged in parallel; respectively loading different voltages on the ionization source outlet electrode and the ion transmission area inlet electrode from high to low, and forming a dissociation electric field E with the size of 1-500V/cm in the axial direction of the interval area between the ionization source outlet electrode and the ion transmission area inlet electrode;
a mass analyzer is disposed within the mass analyzer cavity.
The ultraviolet light source is a gas discharge lamp light source, a laser light source or a synchronous radiation light source;
the mass analyzer is a quadrupole mass analyzer, an ion trap mass analyzer, a magnetic mass analyzer or a time-of-flight mass analyzer.
A method for qualitatively and quantitatively analyzing an isomer mixture by adopting the device comprises the following steps:
selecting a group of dissociation electric fields E containing more than 2 different sizes;
sequentially testing a characteristic mass spectrogram of each component i in the isomer under each dissociation electric field E by using a photoionization mass spectrum;
calculating the mass-to-charge ratio of the ith component per unit concentration of the sample when the dissociation electric field is EjCharacteristic ion peak intensity σ ofi(Mj,E)；
Testing the characteristic mass spectrogram of the isomer mixture under each dissociation electric field E by using a photoionization mass spectrum;
calculating the sum mass-to-charge ratio of the spectrum of the isomer mixture as MjCharacteristic ion peak intensity ofMj；
The concentration C of each isomer component i in the mixture at a dissociation electric field of E was calculated according to the following formulai(E)：
IMj＝∑σi(Mj，E)*Ci(E)
The concentration C obtained under each dissociation electric field Ei(E)Adding and averaging to obtain the final concentration C of the component i in the isomeri：
The invention provides a photoionization mass spectrum device and a photoionization mass spectrum method for qualitative and quantitative analysis of an isomer mixture, which are characterized in that based on the characteristic that different components of the isomer have different fragmentation degrees under different dissociation electric fields, collision induced dissociation with controllable collision energy is introduced into the photoionization mass spectrum, and characteristic spectrograms of each component of the isomer and the mixture thereof under different dissociation electric fields are respectively obtained; and establishing an analysis algorithm to realize the rapid qualitative and quantitative analysis of each component in the isomer mixture according to the characteristic ion species and the relative strength of each component of the isomer.
Drawings
FIG. 1 is a schematic diagram of an apparatus for qualitative and quantitative analysis of photoionization mass spectrometry of isomeric mixtures according to the invention.
FIG. 2 is a schematic diagram of a method for qualitatively and quantitatively analyzing an isomer mixture by using the photoionization mass spectrometry device according to the present invention.
FIG. 3 shows the variation trend of the intensities of 4 characteristic ions with the dissociation electric field E when 6 monoterpene isomers are detected by the photoionization mass spectrometry device of the present invention.
FIG. 4 is a comparison of the ratios of the components of a mixture of 4 monoterpene isomers prepared by weighing, with qualitative and quantitative analysis results obtained based on the apparatus and method of the present invention.
FIG. 5 is a comparison of the ratios of the components of a mixture of 6 monoterpene isomers prepared by weighing, with qualitative and quantitative analysis results obtained based on the apparatus and method of the present invention.
Detailed Description
Referring to fig. 1, the photoionization mass spectrometry apparatus for qualitative and quantitative analysis of an isomer mixture according to the present invention includes an ionization source cavity 101 having a closed upper end and an open lower end, an ion transmission region cavity 102 having open upper and lower ends, and a mass analyzer cavity 103 having an open upper end and a closed lower end, which are sequentially disposed from top to bottom; a flat-plate-shaped ionization source outlet electrode 107 is arranged between the ionization source cavity 101 and the ion transmission region cavity 102, and the lower opening end of the ionization source cavity 101 and the upper opening end of the ion transmission region cavity 102 are respectively connected with the ionization source outlet electrode 107 in a sealing manner; a flat-plate differential interface board 110 is arranged between the ion transmission area cavity 102 and the mass analyzer cavity 103, and the lower opening end of the ion transmission area cavity 102 and the upper opening end of the mass analyzer cavity 103 are respectively connected with the differential interface board 110 in a sealing way; vacuum pump interfaces are respectively arranged on the side walls of the ionization source cavity 101, the ion transmission region cavity 102 and the mass analyzer cavity 103;
the ionization source outlet electrode 107 and the differential interface board 110 are arranged in parallel, through holes are formed in the middles of the ionization source outlet electrode 107 and the differential interface board 110, and the through holes are coaxial;
more than 1 flat-plate-shaped ionization region electrode 106 is arranged in the ionization source cavity 101, more than 1 ionization region electrode 106 and ionization source outlet electrode 107 are arranged in parallel at intervals, and the middle part of the ionization region electrode 106 is provided with a through hole which is coaxial with the through hole of the ionization source outlet electrode 107; an ultraviolet light beam 113 emitted by an ultraviolet light source 104 is positioned in the ionization source cavity 101, the ultraviolet light beam 113 passes through the central area of the through hole of the ionization region electrode 106 and irradiates the surface of the ionization source outlet electrode 107, and the transmission direction of the ultraviolet light beam 113 is coaxial with the through hole of the ionization region electrode 106; a sample gas inlet pipe 105 penetrates through the outer wall of the ionization source cavity 101 and extends into the ionization source cavity 101, the gas outlet end of the sample gas inlet pipe 105 faces the through hole area of the ionization region electrode 106, and the gas inlet end of the sample gas inlet pipe 105 is connected with an external sample gas source 112;
an ion transmission area inlet electrode 108 and an electrostatic ion lens 109 are sequentially arranged in the ion transmission area cavity 102 along the axial direction from the ionization source outlet electrode 107 to the through hole of the differential interface plate 110, and the ionization source outlet electrode 107, the ion transmission area inlet electrode 108, the electrostatic ion lens 109 and the differential interface plate 110 are arranged at intervals;
the ion transmission region inlet electrode 108 is a flat plate type metal electrode with a through hole in the middle, or a conical metal electrode with an axial through hole, or a quadrupole rod, a hexapole rod or an octopole rod electrode consisting of 4, 6 or 8 metal round rods arranged in parallel; respectively loading different voltages on the ionization source outlet electrode 107 and the ion transmission region inlet electrode 108 in the order of voltage from high to low, and forming a dissociation electric field E with the size of 1-500V/cm in the axial direction of a spacing region between the ionization source outlet electrode 107 and the ion transmission region inlet electrode 108;
a mass analyzer 111 is disposed within the mass analyzer chamber 103.
During application, sample gas in the sample gas source 112 enters the ionization source cavity 101 through the sample gas inlet tube 105, and under the irradiation of the ultraviolet light beam 113 emitted by the ultraviolet light source 104, sample molecular ions generated by photoionization enter the ion transport region cavity 102 through the through hole in the middle of the ionization source outlet electrode 107 under the action of the electric field of the ionization region electrode 106. Dissociation electric field E of sample molecular ions between ionization source outlet electrode 107 and ion transport region inlet electrode 108kThe sample molecules with different molecular structures collide with each other in the same dissociation electric field to induce dissociation so as to obtain the difference of the types or relative strengths of the fragment ions. Based on the difference of the characteristic fragment ions, an analysis algorithm can be established to realize qualitative and quantitative analysis of an isomer mixture, and the qualitative and quantitative analysis method comprises the following steps:
selecting a group of dissociation electric fields E containing more than 2 different sizes;
sequentially testing a characteristic mass spectrogram of each component i in the isomer under each dissociation electric field E by using a photoionization mass spectrum;
calculating the mass-to-charge ratio of the ith component per unit concentration of the sample when the dissociation electric field is EjIs defined as the effective photoionization-collision induced dissociation coefficient sigmai(Mj,E)；
Testing the characteristic mass spectrogram of the isomer mixture under each dissociation electric field E by using a photoionization mass spectrum;
calculating the sum mass-to-charge ratio of the spectrum of the isomer mixture as MjCharacteristic ion peak intensity ofMj(ii) a Then, in the isomeric mixture, at a specific dissociation electric field E, the mass-to-charge ratio is MjThe characteristic ion peak intensity of (A) is that M is generated by all components under the conditionjThe sum of the intensities of the characteristic ion peaks of (a):
IMj＝∑σi(Mj，E)*Ci(E)
j characteristic ions are selected to obtain an equation set consisting of j equations, wherein the number j of the selected characteristic ions is larger than or equal to the number i of each isomer component in the mixture, so that the concentration C of each isomer component i in the mixture when the dissociation electric field is E can be obtained by solving the equation seti(E)；
In order to reduce the systematic error and the calculation error of the instrument detection, the concentration C obtained under each dissociation electric field Ei(E)Adding and averaging to obtain the final concentration C of the component i in the isomeri：
Example 1
For the examination of the photoionization mass spectrometry device and the method for qualitatively and quantitatively analyzing an isomer mixture, according to the invention, an ion transmission region inlet electrode of the photoionization device adopts a quadrupole rod consisting of 4 metal round rods arranged in parallel, an ultraviolet light source adopts a gas discharge light source, namely a krypton discharge lamp (Kr lamp), and a mass analyzer adopts a flight time mass analyzer, 6 isomers of monoterpene substances, namely α -terpene, gamma-terpene, α -pinene, β -pinene, 3-carene and limonene, are selected as detection objects in the experiment, firstly, the 6 isomer components are respectively prepared into gas samples to be independently injected, the dissociation electric field E between an ionization source outlet electrode and the ion transmission region inlet electrode is adjusted, the species and the relative intensity variation trend of the characteristic ions of the 6 monoterpene isomers under different dissociation electric field intensities are obtained, as shown in fig. 3, the variation trend of the 4 characteristic ion intensities of the 6 monoterpene isomers along with the dissociation electric field intensity is analyzed, the variation trend of the 4 characteristic ion intensities along with the dissociation electric field E is found, the qualitative intensity of the monoterpene isomers is analyzed along with the same proportion of the electric field intensity, the comparison results of the monoterpene mixture, the comparison of the density of the mixture is taken, the comparison results of the mixture is taken under the comparative example, the comparison of the density of the monoterpene with the density of the mixture of 4-pinene, the mixture is taken, the mixture is taken, the comparison of the mixture is taken as 3975-10-80%, the density, the comparison results of the mixture, the density of the mixture is taken under the comparison results of the density of the mixture, the mixture is taken under the mixture, the mixture under the comparison of the density of the mixture, the density of the mixture under.
Example 2
Aiming at the examination of the photoionization mass spectrum device and the method for qualitatively and quantitatively analyzing the isomeric mixture, an ion transmission area inlet electrode of the photoionization device adopts a quadrupole rod consisting of 4 metal round rods arranged in parallel, an ultraviolet light source adopts a gas discharge light source, namely a krypton gas discharge lamp (Kr lamp), and a mass analyzer adopts a flight time mass analyzer, 6 isomeric bodies of monoterpene substances, namely α -terpene, gamma-terpene, α -pinene, β -pinene, 3-carene and limonene are selected in an experiment to prepare the isomeric mixture, the 6 monoterpene isomeric bodies respectively account for 15% of α -terpene, 25% of gamma-terpene, 20% of α -pinene, 5% of β -pinene, 15% of 3-carene and 20% of limonene, the qualitative and quantitative analysis results of the isomeric mixture are respectively tested under the conditions that the electric field intensity of a dissociation electric field E is 50, 75 and 100V/cm, the quantitative analysis results of the isomeric mixture are only obtained according to a comparison result of a 0.33% of a collision induced analytical algorithm, and the quantitative analysis results are only obtained by using a weight analysis algorithm.
The foregoing is merely a preferred embodiment of this invention and all changes and modifications that come within the spirit, construction and principles of the invention are desired to be protected.
Claims (2)
1. A method for qualitatively and quantitatively analyzing an isomer mixture based on a photoionization mass spectrometry device is characterized by comprising the following steps: the photoionization mass spectrum device for qualitatively and quantitatively analyzing the isomeric mixture comprises an ionization source cavity (101) with a closed upper end and an open lower end, an ion transmission area cavity (102) with an open upper end and an open lower end and a mass analyzer cavity (103) with an open upper end and an open lower end, which are sequentially arranged from top to bottom; a flat-plate-shaped ionization source outlet electrode (107) is arranged between the ionization source cavity (101) and the ion transmission region cavity (102), and the lower opening end of the ionization source cavity (101) and the upper opening end of the ion transmission region cavity (102) are respectively connected with the ionization source outlet electrode (107) in a sealing way; a flat-plate-shaped differential interface board (110) is arranged between the ion transmission area cavity (102) and the mass analyzer cavity (103), and the lower opening end of the ion transmission area cavity (102) and the upper opening end of the mass analyzer cavity (103) are respectively connected with the differential interface board (110) in a sealing way; vacuum pump interfaces are respectively arranged on the side walls of the ionization source cavity (101), the ion transmission region cavity (102) and the mass analyzer cavity (103);
the ionization source outlet electrode (107) and the differential interface board (110) are arranged in parallel, through holes are formed in the middles of the ionization source outlet electrode (107) and the differential interface board (110), and the through holes are coaxial;
more than 1 flat-plate-shaped ionization region electrode (106) is arranged in the ionization source cavity (101), more than 1 ionization region electrode (106) and ionization source outlet electrode (107) are arranged in parallel at intervals, and the middle part of the ionization region electrode (106) is provided with a through hole which is coaxial with the through hole of the ionization source outlet electrode (107); an ultraviolet light beam (113) emitted by an ultraviolet light source (104) is positioned in the ionization source cavity (101), the ultraviolet light beam (113) passes through the central area of the through hole of the ionization region electrode (106) and irradiates the surface of the ionization source outlet electrode (107), and the transmission direction of the ultraviolet light beam (113) is coaxial with the through hole of the ionization region electrode (106); a sample gas inlet pipe (105) penetrates through the outer wall of the ionization source cavity (101) and extends into the ionization source cavity (101), the gas outlet end of the sample gas inlet pipe (105) faces the through hole area of the ionization region electrode (106), and the gas inlet end of the sample gas inlet pipe (105) is connected with an external sample gas source (112);
an ion transmission area inlet electrode (108) and a static ion lens (109) are sequentially arranged in the ion transmission area cavity (102) along the axial direction from an ionization source outlet electrode (107) to a through hole of a differential interface plate (110), and the ionization source outlet electrode (107), the ion transmission area inlet electrode (108), the static ion lens (109) and the differential interface plate (110) are arranged at intervals;
the ion transmission area inlet electrode (108) is a flat plate type metal electrode with a through hole in the middle, or a conical metal electrode with an axial through hole, or a quadrupole rod, a hexapole rod or an octopole rod electrode consisting of 4, 6 or 8 metal round rods arranged in parallel; respectively loading different voltages on the ionization source outlet electrode (107) and the ion transmission region inlet electrode (108) from high to low, and forming a dissociation electric field E with the size of 1-500V/cm in the axial direction of a spacing region between the ionization source outlet electrode (107) and the ion transmission region inlet electrode (108);
a mass analyzer (111) is arranged in the mass analyzer cavity (103);
the method for qualitatively and quantitatively analyzing the isomer mixture by adopting the device comprises the following steps:
selecting a group of dissociation electric fields E containing more than 2 different sizes;
sequentially testing a characteristic mass spectrogram of each component i in the isomer under each dissociation electric field E by using a photoionization mass spectrum;
calculating the mass-to-charge ratio of the ith component per unit concentration of the sample when the dissociation electric field is EjCharacteristic ion peak intensity σ ofi(Mj,E)；
Testing the characteristic mass spectrogram of the isomer mixture under each dissociation electric field E by using a photoionization mass spectrum;
calculating the sum mass-to-charge ratio of the spectrum of the isomer mixture as MjCharacteristic ion peak intensity ofMj；
The concentration C of each isomer component i in the mixture at a dissociation electric field of E was calculated according to the following formulai(E)：
The concentration C obtained under each dissociation electric field Ei(E)Adding and averaging to obtain the final concentration C of the component i in the isomeri：
2. The method of claim 1, wherein:
the ultraviolet light source (104) is a gas discharge lamp light source, a laser light source or a synchrotron radiation light source;
the mass analyzer (111) is a quadrupole mass analyzer, an ion trap mass analyzer, a magnetic mass analyzer or a time-of-flight mass analyzer.
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| CN103500696A (en) * | 2013-09-26 | 2014-01-08 | 中国科学技术大学 | Mass spectrum analyzer with multiple-reflection vacuum ultraviolet ionization source |
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