CN109900773A - A method of composition of air in accurate quickly analysis submarine - Google Patents
A method of composition of air in accurate quickly analysis submarine Download PDFInfo
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- CN109900773A CN109900773A CN201711305779.8A CN201711305779A CN109900773A CN 109900773 A CN109900773 A CN 109900773A CN 201711305779 A CN201711305779 A CN 201711305779A CN 109900773 A CN109900773 A CN 109900773A
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Abstract
The present invention provides a kind of methods of composition of air in accurate quickly analysis submarine, belong to the application field of hyperbar photo-ionisation time of-flight mass spectrometer, this method is established for composition of air complicated difficult in submarine with accurate qualitative problem, main process is that sample gas in airbag is directly then pumped into mass spectrograph using the vacuum pump to connect with mass spectrograph and carries out ionization analysis by being connected directly equipped with the airbag of different location and the composition of air of time in submarine with above-mentioned mass spectrometric sample introduction capillary.Since hyperbar photo-ionisation mode can realize molecular ion or the ionization of quasi-molecular ion formula of material molecule, the accurate qualitative of multicomponent gaseous mixture may be implemented.Based on above method, to composition of air in submarine, sample introduction is analyzed, easy to operate, method is simple, fast and reliable without the pre-treatment steps such as sample preconcentration.
Description
Technical field
The present invention relates to a kind of methods of composition of air in accurate quickly analysis submarine, belong to the application technology neck of instrument
Domain.Specifically be exactly under the premise of without any sample pre-treatments, by sample gas in airbag directly with instrument sample introduction hair
Tubule is connected and then quick sampling analysis.Entire method and Sampling analysis process do not need pretreating device and step, operation letter
Single, sampling is quickly, qualitative accurate.
Background technique
Due to submarine cabin there are narrow space, equipment is various the features such as, when submarine submariner, equipment operation,
Material, which discharges, and the activity of people is with metabolism can be such that the various pernicious gas types in the room air of cabin increase, concentration
Increase, to endanger ship person's health.Currently, the method for gas mainly uses oxygen measurement set, suitable in detection submarine bay
Magnetic, infrared spectrometer and chromatography-mass spectrograph (GC-MS).But these usual detection times of traditional analysis method are long, and
The type of compound to be checked is again more, is not easy accurately qualitative, and result can just be obtained by generally requiring a variety of detection means and combining.By
This, accurate quick analytic instrument device and method become research hotspot in recent years.Especially flight time mass spectrum (TOF-MS) combines
Soft ionization techniques and direct injected method based on photo-ionisation, quickly grow.TOF-MS has the quick detection speed of Microsecond grade
The advantages of degree and single pass are up to full spectrum；Soft ionization techniques based on photo-ionisation can obtain the molecular ion of material composition
Or quasi-molecular ion spectral peak, it is suitble to the accurate qualitative of multicomponent environmental sample；And direct injected method has abandoned complicated sample
Pre-treatment step greatly shortens sample analysis time, therefore can be made extensively at the accurate quick aspect of environmental sample
With.
This paper's is designed to provide a kind of accurate new method for quickly analyzing composition of air in submarine.This method is based on true
Hyperbar photo-ionisation (VUV-HPPI)-TOFMS of empty ultraviolet lamp, the spy of composition of air in submarine is obtained by direct injected mode
Levy full spectrogram.Using the soft ionization advantage and feature of VUV-HPPI, contained component in air can be directly obtained in submarine, significantly
Accurate qualitative ability is improved, and nearly all organic matter can be analyzed, and the auxiliary of other instruments is not needed.In addition, directly
Input mode avoids many and diverse sample pre-treatments step, easy to operate, time-consuming short, efficiently solves above-mentioned traditional analysis
Deficiency, provide a kind of simple and quick, accurately and reliably analysis means for the analysis of composition of air in submarine.
Summary of the invention
The object of the present invention is to provide a kind of methods of composition of air in accurate quickly analysis submarine.
To achieve the above object, technical scheme is as follows:
A method of composition of air in accurate quickly analysis submarine, which is characterized in that flown using hyperbar photo-ionisation
Time mass spectrum instrument is analyzed, and is operated according to the following steps:
A. it firstly, adjusting the ionized region air pressure of hyperbar photo-ionisation time of-flight mass spectrometer, is allowed to maintain required air pressure
Value；
B. secondly, when by passing through a two-way valve and hyperbar photo-ionisation flight equipped with the escape pipe of the airbag of air in submarine
Between the connection of mass spectrometric sample introduction capillary seal；
C. two-way valve is opened, sample gas starts the ionized region for being drawn into hyperbar photo-ionisation time of-flight mass spectrometer in airbag
It is ionized, starts simultaneously at acquisition, obtain the feature spectrogram of sample gas component in airbag.
Airbag needs the purging using baking oven baking and vapor before sampling, guarantees clean free from admixture interference in airbag.
Hyperbar photo-ionisation time of-flight mass spectrometer uses hyperbar photo-ionisation mode, soft ionization can be realized to substance, i.e.,
Main ionization obtain substance molecular ion peak or or quasi-molecular ion peak, fragment ion is seldom, can be to multicomponent sample reality
It is now accurate qualitative；It is 400~1000Pa that the ionized region of hyperbar photo-ionisation time of-flight mass spectrometer, which is applicable in air pressure range, general meeting
One optimal atmospheric pressure value is obtained by optimization in conjunction with detection sensitivity and the spectral peak feature of substance, to obtain inspection as high as possible
Survey sensitivity and characteristic ion peak as simple as possible.
The mass analyzer of hyperbar photo-ionisation time of-flight mass spectrometer be time-of-flight mass analyzer, can obtain to
The full spectrogram of component is surveyed, the separation analysis of multi-component complex sample is suitble to.
Operation of the present invention and device are very simple, do not need sample preconcentration, time-consuming short, analysis speed is fast, hyperbar light
Ionization mode can realize the soft ionization of substance, mainly obtain the molecular ion or a small amount of characteristic ion of substance, fragment ion is few, can
It is accurate qualitative to realize.
Detailed description of the invention
Fig. 1 is the schematic illustration of composition of air in accurate quickly analysis submarine；1- airbag；2- escape pipe；3- two-way valve；
4- sample introduction capillary；5- hyperbar photo-ionisation time of-flight mass spectrometer.
Fig. 2 is the full spectrogram of composition of air feature at two kinds of submarine positions.
Table 1 is the corresponding material composition in leading ion peak in Fig. 2.
Specific embodiment
Firstly, Fig. 1 is a kind of accurate method for quickly analyzing composition of air in submarine, which is characterized in that use hyperbar
Photo-ionisation time of-flight mass spectrometer 5 is analyzed, and is operated according to the following steps:
A. it firstly, adjusting the ionized region air pressure of hyperbar photo-ionisation time of-flight mass spectrometer 5, is allowed to maintain required air pressure
Value；
B. secondly, the escape pipe 2 equipped with the airbag 1 of air in submarine is flown by a two-way valve 3 with hyperbar photo-ionisation
The sample introduction capillary 4 of row time mass spectrum instrument 5 is tightly connected；
C. two-way valve 3 is opened, sample gas starts the electricity for being drawn into hyperbar photo-ionisation time of-flight mass spectrometer 5 in airbag 1
It is ionized from area, starts simultaneously at acquisition, obtain the feature spectrogram of sample gas component in airbag 1.
Airbag 1 needs the purging using baking oven baking and vapor before sampling, guarantees clean free from admixture interference in airbag.
Hyperbar photo-ionisation time of-flight mass spectrometer 5 uses hyperbar photo-ionisation mode, soft ionization can be realized to substance, i.e.,
Main ionization obtain substance molecular ion peak or or quasi-molecular ion peak, fragment ion is seldom, can be to multicomponent sample reality
It is now accurate qualitative；It is 400~1000Pa that the ionized region of hyperbar photo-ionisation time of-flight mass spectrometer 5, which is applicable in air pressure range, generally
One optimal atmospheric pressure value can be obtained by optimization in conjunction with detection sensitivity and the spectral peak feature of substance, it is as high as possible to obtain
Detection sensitivity and characteristic ion peak as simple as possible.
The mass analyzer of hyperbar photo-ionisation time of-flight mass spectrometer 5 is time-of-flight mass analyzer, can be obtained
The full spectrogram of component to be measured is suitble to the separation analysis of multi-component complex sample.
Wherein, it for the vacuum UV lamp of 10.6eV is ion that hyperbar photo-ionisation time of-flight mass spectrometer, which uses photon energy,
Source can realize effectively ionization to most organic matters；Mass spectrograph designs for orthogonal acceleration, is detected with MCP detector, in airbag
A part of sample gas is directly pumped into mass spectrometric ionized region by the vacuum to connect with ionized region and carries out anticyclonic photo-ionisation
Analysis.Wherein the air pressure of ionized region can pass through internal diameter, length and the vacuum to connect with ionized region of change sample introduction capillary
The valve of pump is adjusted.The sample introduction capillary used in experiment is stainless steel metal capillary, and internal diameter is 250 μm, and length is about
For 10cm, gas flow about 50ml/min.Ionized region total gas pressure maintains 700Pa or so.
Embodiment 1
For a kind of accurate examination for quickly analyzing the method performance of composition of air in submarine of the present invention, test with same
The air of two different locations is sample gas in one submarine, is tested using hyperbar photo-ionisation time of-flight mass spectrometer.In experiment
The ionization mode of ionization source ionizes mode using vacuum ultraviolet hyperbar photo-ionisation (VUV-HPPI), and ionized region air pressure maintains
700Pa or so.It was sampled under cleaned air atmosphere before this, each point sampling time is 50s, to ensure in sample introduction capillary
Wall and instrument internal cleaning free from admixture.Later, the airbag equipped with air sample in submarine is connected with sample introduction capillary, ionized region
Air pressure is basically unchanged, and each sample parallel testing 3 times samples 50s every time.Before carrying out next sample test, it need to guarantee sample introduction
Capillary and instrument internal no sample Molecular Adsorption, in order to avoid influence the test result of next sample.Fig. 2 is the submarine analyzed
Composition of air spectrogram at interior two different locations.Although being obtained it can be found that position is different in same submarine
Characteristic ion type and intensity have notable difference.Table 1 is the characteristics of combining hyperbar photo-ionisation, to the leading ion in Fig. 2
The material composition that peak is belonged to.It can be found that composition of air is complicated in submarine after after a period of time closed, contain
There are many kinds of substance such as benzene homologues, amine, aldehydes, acids even essence class.Wherein, benzene homologues and aldehydes are likely to mainly by submarine
Interior material release generates, and amine and acids may be that internal staff's metabolism generates, and essence class is likely to internal staff institute
It is discharged and is generated with daily chemical products.
Table 1 is the corresponding material composition in leading ion peak in Fig. 2.
Claims (4)
1. a kind of method of composition of air in accurate quickly analysis submarine, which is characterized in that when using hyperbar photo-ionisation flight
Between mass spectrograph (5) analyzed, according to the following steps operate:
A. it firstly, adjusting the ionized region air pressure of hyperbar photo-ionisation time of-flight mass spectrometer (5), is allowed to maintain required air pressure
Value；
B. secondly, the escape pipe (2) equipped with the airbag (1) of air in submarine is passed through a two-way valve (3) and hyperbar photo-ionisation
The sample introduction capillary (4) of time of-flight mass spectrometer (5) is tightly connected；
C. two-way valve (3) are opened, airbag (1) interior sample gas starts to be drawn into hyperbar photo-ionisation time of-flight mass spectrometer (5)
Ionized region is ionized, and acquisition is started simultaneously at, and obtains the feature spectrogram of airbag (1) interior sample gas component.
2. according to the method described in claim 1, it is characterized by:
Airbag (1) needs the purging using baking oven baking and vapor before sampling, guarantees clean free from admixture interference in airbag.
3. according to the method described in claim 1, it is characterized by:
Hyperbar photo-ionisation time of-flight mass spectrometer (5) uses hyperbar photo-ionisation mode, and soft ionization can be realized to substance, i.e., main
Ionize to obtain substance molecular ion peak or or quasi-molecular ion peak, fragment ion is seldom, can realize to multicomponent sample
It is accurate qualitative；It is 400~1000Pa that the ionized region of hyperbar photo-ionisation time of-flight mass spectrometer (5), which is applicable in air pressure range, generally
One optimal atmospheric pressure value can be obtained by optimization in conjunction with detection sensitivity and the spectral peak feature of substance, it is as high as possible to obtain
Detection sensitivity and characteristic ion peak as simple as possible.
4. according to the method described in claim 1, it is characterized by:
The mass analyzer of hyperbar photo-ionisation time of-flight mass spectrometer (5) be time-of-flight mass analyzer, can obtain to
The full spectrogram of component is surveyed, the separation analysis of multi-component complex sample is suitble to.
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Cited By (5)
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| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN112946059A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Analysis method for enhancing detection of oxygen-containing volatile organic small molecules |
| CN112986370A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Mass spectrum detection method for trace volatile components |
| CN113219042A (en) * | 2020-12-03 | 2021-08-06 | 深圳市步锐生物科技有限公司 | Device and method for analyzing and detecting components in human body exhaled air |
| CN116776104A (en) * | 2023-08-21 | 2023-09-19 | 华南理工大学 | Method and system for analyzing change rule of atmospheric components based on machine learning |
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| CN106932464A (en) * | 2017-05-23 | 2017-07-07 | 安徽中烟工业有限责任公司 | A kind of real-time analytical equipment of gaseous phase of main stream smoke of cigarette composition |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN112946059A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Analysis method for enhancing detection of oxygen-containing volatile organic small molecules |
| CN112986370A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Mass spectrum detection method for trace volatile components |
| CN113219042A (en) * | 2020-12-03 | 2021-08-06 | 深圳市步锐生物科技有限公司 | Device and method for analyzing and detecting components in human body exhaled air |
| CN116776104A (en) * | 2023-08-21 | 2023-09-19 | 华南理工大学 | Method and system for analyzing change rule of atmospheric components based on machine learning |
| CN116776104B (en) * | 2023-08-21 | 2023-11-10 | 华南理工大学 | Method and system for analyzing change rule of atmospheric components based on machine learning |
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Application publication date: 20190618 |