CN109470765A - The method of real-time of oxygen in fruit vegetables storing environment - Google Patents

The method of real-time of oxygen in fruit vegetables storing environment Download PDF

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Publication number
CN109470765A
CN109470765A CN201811227122.9A CN201811227122A CN109470765A CN 109470765 A CN109470765 A CN 109470765A CN 201811227122 A CN201811227122 A CN 201811227122A CN 109470765 A CN109470765 A CN 109470765A
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oxygen
gas
real
time
ion
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程沙沙
杨慧敏
谭明乾
李然然
王小荟
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Dalian Polytechnic University
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Dalian Polytechnic University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry

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  • Chemical & Material Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a kind of method of real-time of oxygen in fruit vegetables storing environment, environmental gas is passed through into the moisture in dehumidification device removal, the inert gas of environmental gas and certain flow after dehumidifying is by entering ion mobility spectrometry ionized region after the acquisition dilution of gas automatic sampling on-line dilution device, the electron reaction that oxygen molecule is formed under ionized region and inert gas conditions, form the oxygen product ion of feature, product ion enters migration area by the ion gate that pulse is opened, it is separated in migration area according to the difference of mobility, Faraday plate is reached to be detected, it is finally received by signal and receives and detect with detection system, form ion mobility spectrometry spectrogram, the signal response of oxygen molecule characteristic peak is monitored, realize the real-time monitoring of oxygen concentration in fruit and vegetable air-conditioning environment.The method of real-time of oxygen in fruit vegetables storing environment of the present invention, detection speed is fast, detection sensitivity is high.

Description

The method of real-time of oxygen in fruit vegetables storing environment
Technical field
The present invention relates to a kind of method of real-time of oxygen in fruit vegetables storing environment.
Background technique
Air conditioned storage refers to the cold preserving method in specific gaseous environment, and fresh fruit of vegetables is still carrying out after picking Vigorous respiration and evaporation, absorbs oxygen from air, and the nutriment of decomposition and consumption itself generates titanium dioxide Carbon, water and heat, since respiration will consume after fruit and vegetable picking the nutriment of itself, so extending the pass of fruit vegetables storing period Key is to reduce respiratory rate, and the variation of storage environment gas componant has significant impact to physiology after fruit and vegetable picking, and hypoxemia contains Amount can effectively inhibit respiration, reduce evaporation to a certain extent, suppress growth of microorganism, delay fruit to reach The physiological metabolism process of vegetable postpones ripening and senescence and prevents putrid and deteriorated purpose, therefore, to oxygen in fruit and vegetable air-conditioning storage environment Gas concentration is monitored, and putrid and deteriorated is had great importance for extending the shelf life of fruits and vegetables and slowing down.
Currently, the measuring method of oxygen content mainly has a chemical capacity method, and magnet and oxide analysing method, zirconium oxide concentration cell method, Electrochemical process, gas chromatography etc., these methods have their own characteristics each, and also have respective limitation, such as most widely used zirconium oxide Concentration cell method, although the response time is short, measurement range is wide, must use at high temperature, can't there is reducing impurity gas The presence of body, though gas chromatography high sensitivity, strong antijamming capability, detection speed is low, not readily portable and on-site test, Therefore, the novel oxygen method of real-time of one kind is developed to have great importance.
Summary of the invention
The object of the present invention is to provide a kind of real-time monitorings and standard for being advantageously implemented oxygen concentration in fruit and vegetable air-conditioning environment The method of real-time of oxygen in the fruit vegetables storing environment really judged.
Present invention technical solution used for the above purpose is: the real-time prison of oxygen in a kind of fruit vegetables storing environment Environmental gas is passed through the moisture in dehumidification device removal, the inertia of environmental gas and certain flow after dehumidifying by survey method Gas is by entering ion mobility spectrometry ionized region after the acquisition dilution of gas automatic sampling on-line dilution device, and oxygen molecule is in ionized region With the electron reaction formed under inert gas conditions, the oxygen product ion of feature is formed, product ion is opened by pulse Ion gate enters migration area, is separated in migration area according to the difference of mobility, reaches Faraday plate and is detected, finally It is received by signal and receives and detect with detection system, form ion mobility spectrometry spectrogram, the signal of oxygen molecule characteristic peak is responded It is monitored, realizes the real-time monitoring of oxygen concentration in fruit and vegetable air-conditioning environment.
The ion mobility spectrometry be equipped with radioactive ionization gauge source, vacuum ultraviolet light ionization source or corona discharge ionization source from Sub- migration spectrum, and detect in the negative ion mode.
The vacuum ultraviolet light ionization source ion mobility spectrometry is the acetone that easy photo-ionisation is introduced in carrier gas, toluene reagent point Son, the electronics generated using reagent molecule photo-ionisation, realizes effective ionization of oxygen.
The carrier gas of the ion mobility spectrometry and drift gas are one or both of inert gas.
The gas automatic sampling on-line dilution device passes through the tow channel gas of gas flow-control ion mobility spectrometry Body makes two-way gas mixing realize automatic sampling and the on-line dilution of oxygen sample.
The dehumidification device is glass tube or stainless steel tube equipped with dehumidizer, and the dehumidizer used is anhydrous hydroxide One or more of sodium, silica gel or molecular sieve.
The method of real-time of oxygen in a kind of fruit vegetables storing environment of the present invention, using the ion mobility spectrometry of negative ion mode It as the detecting element of oxygen, is reacted using the electronics and oxygen molecule formed in atmosphere of inert gases, realizes fruit and vegetable air-conditioning ring Effective detection of oxygen concentration in border;Based on Ion mobility spectrometry, in conjunction with gas automatic sampling on-line dilution device and dehumidifying Device realizes the real-time monitoring of the automatic continuous acquisition and oxygen concentration of fruit and vegetable air-conditioning environmental gas.
Detailed description of the invention
Fig. 1 is the method for real-time schematic illustration of oxygen in a kind of fruit vegetables storing environment of the present invention.
Fig. 2 is the radioactive ionization gauge source ion migration of the method for real-time of oxygen in a kind of fruit vegetables storing environment of the present invention 1.6% oxygen forms characteristic ion migration spectrum spectrogram in spectrum.
Fig. 3 is the radioactive ionization gauge source ion migration of the method for real-time of oxygen in a kind of fruit vegetables storing environment of the present invention The response curve of various concentration oxygen in spectrum.
Specific embodiment
The method of real-time of oxygen in fruit vegetables storing environment of the present invention is made using the ion mobility spectrometry 5 of negative ion mode For the detecting element of oxygen concentration, in conjunction with gas automatic sampling on-line dilution device 4 and dehumidification device 3, by oxygen and electricity The monitoring for the feature product ion intensity that son reaction generates, realizes the Real Time Monitoring of oxygen concentration in fruit and vegetable air-conditioning environment, As shown in Figure 1, specific monitoring method are as follows: fruit and vegetable air-conditioning environmental gas 1 first passes around dehumidification device 3 under the action of aspiration pump and goes Except moisture in the middle, flow is controlled by gas flowmeter;The inert gas 2 of environmental gas and certain flow after dehumidifying mixes Dilution;Gas after dilution enters ion mobility spectrometry ionized region, the electricity formed under oxygen molecule therein and inert gas conditions Son reaction, the product ion of the feature of formation;Product ion enters migration area by the ion gate that pulse is opened, in migration area It is separated according to the difference of mobility, reaches Faraday plate and detected;The signal detected is through data acquisition and processing (DAP) system System 6 receives, and is monitored to the signal response of oxygen molecule characteristic peak, realizes the real-time prison of oxygen concentration in fruit and vegetable air-conditioning environment It surveys.
Embodiment 1
The testing conditions of ion mobility spectrometry: operating voltage is 240 V/cm, and 100 DEG C of migration tube temperature, compressed air is as environment Gaseous sample, flow velocity 40ml/min, 460 ml/min of carrier gas flow velocity, 500 ml/min of make-up gas flow velocity, carrier gas and tail Air blowing is the high pure nitrogen handled by silica gel, active carbon and molecular sieve, and moisture content is lower than 10 ppm, as shown in Fig. 2, surveying The ion mobility spectrometry spectrogram oxygen obtained can form the feature of 9.43 ms of transit time under the conditions of high pure nitrogen with electron reaction Product ion.
Embodiment 2
The testing conditions of ion mobility spectrometry: operating voltage is 240 V/cm, and 100 DEG C of migration tube temperature, compressed air is as environment Comprehensive 500 ml/min of gaseous sample, environmental gas flow velocity and carrier gas flow velocity, by adjusting environmental gas and diluent gas flow Speed ratio example obtains the oxygen sample of various concentration, and 500 ml/min of make-up gas flow velocity, carrier gas and make-up gas are by silicon The high pure nitrogen of glue, active carbon and molecular sieve processing, moisture content are lower than 10 ppm;In to the ion mobility spectrometry measured Oxygen characteristics peak-to-peak signal intensity maps to oxygen concentration, obtains oxygen response curve as shown in Figure 3, as seen from the figure, with The increase of oxygen concentration in sample introduction gas, oxygen characteristics peak intensity gradually increase, when oxygen concentration is less than 0.015 in carrier gas, oxygen Gas feature peak intensity is with the increased fast speed of concentration;After more than 0.015, the increase of oxygen characteristics peak intensity slows down.

Claims (6)

1. the method for real-time of oxygen in a kind of fruit vegetables storing environment, it is characterised in that: environmental gas is passed through dehumidification device Moisture in removal, the inert gas of environmental gas and certain flow after dehumidifying is by gas automatic sampling on-line dilution device Enter ion mobility spectrometry ionized region, the electron back that oxygen molecule is formed under ionized region and inert gas conditions after acquisition dilution It answers, forms the oxygen product ion of feature, product ion enters migration area by the ion gate that pulse is opened, the root in migration area It is separated according to the difference of mobility, reaches Faraday plate and detected, finally received by signal and receive and examine with detection system It surveys, forms ion mobility spectrometry spectrogram, the signal response of oxygen molecule characteristic peak is monitored, realizes oxygen in fruit and vegetable air-conditioning environment The real-time monitoring of gas concentration.
2. the method for real-time of oxygen in a kind of fruit vegetables storing environment according to claim 1, it is characterised in that: described Ion mobility spectrometry is the ion mobility spectrometry for being equipped with radioactive ionization gauge source, vacuum ultraviolet light ionization source or corona discharge ionization source, and It detects in the negative ion mode.
3. the method for real-time of oxygen in a kind of fruit vegetables storing environment according to claim 2, it is characterised in that: described Vacuum ultraviolet light ionization source ion mobility spectrometry is acetone, the toluene reagent molecule that easy photo-ionisation is introduced in carrier gas, utilizes reagent The electronics that molecule photo-ionisation generates, realizes effective ionization of oxygen.
4. the method for real-time of oxygen in a kind of fruit vegetables storing environment according to claim 1, it is characterised in that: described The carrier gas of ion mobility spectrometry and drift gas are one or both of inert gas.
5. the method for real-time of oxygen in a kind of fruit vegetables storing environment according to claim 1, it is characterised in that: described Gas automatic sampling on-line dilution device passes through the two-way gas of gas flow-control ion mobility spectrometry, makes two-way gas Automatic sampling and the on-line dilution of oxygen sample are realized in mixing.
6. the method for real-time of oxygen in a kind of fruit vegetables storing environment according to claim 1, it is characterised in that: described Dehumidification device is glass tube or stainless steel tube equipped with dehumidizer, and the dehumidizer used is no water sodium hydroxide, silica gel or molecule One or more of sieve.
CN201811227122.9A 2018-10-22 2018-10-22 The method of real-time of oxygen in fruit vegetables storing environment Pending CN109470765A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1154268A2 (en) * 2000-05-09 2001-11-14 Air Products And Chemicals, Inc. Method for operating an ion mobility spectrometer used to detect trace atmospheric impurities in gases
CN1476534A (en) * 2000-12-22 2004-02-18 Method for measuring concentration of impurities in hitrgen, hydrogen and oxygen by means of ion mobility spetrometry
CN101382521A (en) * 2007-09-04 2009-03-11 中国科学院大连化学物理研究所 Method for enhancing sensitivity of ionic migration spectrum
CN106226384A (en) * 2016-09-22 2016-12-14 大连工业大学 A kind of trimethylamine detection method based on Ion mobility spectrometry

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1154268A2 (en) * 2000-05-09 2001-11-14 Air Products And Chemicals, Inc. Method for operating an ion mobility spectrometer used to detect trace atmospheric impurities in gases
CN1476534A (en) * 2000-12-22 2004-02-18 Method for measuring concentration of impurities in hitrgen, hydrogen and oxygen by means of ion mobility spetrometry
CN101382521A (en) * 2007-09-04 2009-03-11 中国科学院大连化学物理研究所 Method for enhancing sensitivity of ionic migration spectrum
CN106226384A (en) * 2016-09-22 2016-12-14 大连工业大学 A kind of trimethylamine detection method based on Ion mobility spectrometry

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MICHAL STANO ET AL.: "Ion mobility spectrometry study of negative corona discharge in oxygen/nitrogen mixtures", 《CHEM. LISTY》 *
王卫国 等: "新型光电离离子迁移谱及其应用", 《科技导报》 *
衡磊: "《现场物证的离子迁移谱方法研究》", 31 January 2009 *

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